Technologically, the vulcanization process is the transformation of "raw" rubber into rubber. As a chemical reaction, it involves the integration of linear rubber macromolecules, which easily lose stability when exposed to external influences, into a single vulcanization network. It is created in three-dimensional space due to cross chemical bonds.

Such a kind of "cross-linked" structure gives rubber additional strength characteristics. Its hardness and elasticity, frost and heat resistance improve with a decrease in solubility in organic substances and swelling.

The resulting mesh has a complex structure. It includes not only nodes that connect pairs of macromolecules, but also those that unite several molecules at the same time, as well as cross chemical bonds, which are like “bridges” between linear fragments.

Their formation occurs under the action of special agents, the molecules of which partially act as a building material, chemically reacting with each other and rubber macromolecules at high temperature.

Material properties

The performance properties of the resulting vulcanized rubber and products made from it largely depend on the type of reagent used. These characteristics include resistance to exposure to aggressive environments, the rate of deformation during compression or temperature rise, and resistance to thermal-oxidative reactions.

The resulting bonds irreversibly limit the mobility of molecules under mechanical action, while maintaining high elasticity of the material with the ability to plastic deformation. The structure and number of these bonds is determined by the method of rubber vulcanization and the chemical agents used for it.

The process is not monotonous, and individual indicators of the vulcanized mixture in their change reach their minimum and maximum at different times. The most suitable ratio of physical and mechanical characteristics of the resulting elastomer is called the optimum.

The vulcanizable composition, in addition to rubber and chemical agents, includes a number of additional substances that contribute to the production of rubber with desired performance properties. According to their purpose, they are divided into accelerators (activators), fillers, softeners (plasticizers) and antioxidants (antioxidants). Accelerators (most often it is zinc oxide) facilitate the chemical interaction of all ingredients of the rubber mixture, help reduce the consumption of raw materials, the time for its processing, and improve the properties of vulcanizers.

Fillers such as chalk, kaolin, carbon black increase the mechanical strength, wear resistance, abrasion resistance and other physical characteristics of the elastomer. Replenishing the volume of feedstock, they thereby reduce the consumption of rubber and lower the cost of the resulting product. Softeners are added to improve the processability of processing rubber compounds, reduce their viscosity and increase the volume of fillers.

Also, plasticizers are able to increase the dynamic endurance of elastomers, resistance to abrasion. Antioxidants stabilizing the process are introduced into the composition of the mixture to prevent the “aging” of rubber. Various combinations of these substances are used in the development of special raw rubber formulations to predict and correct the vulcanization process.

Types of vulcanization

Most commonly used rubbers (butadiene-styrene, butadiene and natural) are vulcanized in combination with sulfur by heating the mixture to 140-160°C. This process is called sulfur vulcanization. Sulfur atoms are involved in the formation of intermolecular cross-links. When adding up to 5% sulfur to the mixture with rubber, a soft vulcanizate is produced, which is used for the manufacture of automotive tubes, tires, rubber tubes, balls, etc.

When more than 30% sulfur is added, a rather hard, low-elastic ebonite is obtained. As accelerators in this process, thiuram, captax, etc. are used, the completeness of which is ensured by the addition of activators consisting of metal oxides, usually zinc.

Radiation vulcanization is also possible. It is carried out by means of ionizing radiation, using electron flows emitted by radioactive cobalt. This sulfur-free process results in elastomers with particular chemical and thermal resistance. For the production of special rubbers, organic peroxides, synthetic resins and other compounds are added under the same process parameters as in the case of sulfur addition.

On an industrial scale, the vulcanizable composition, placed in a mold, is heated at elevated pressure. To do this, the molds are placed between the heated plates of the hydraulic press. In the manufacture of non-molded products, the mixture is poured into autoclaves, boilers or individual vulcanizers. Heating rubber for vulcanization in this equipment is carried out using air, steam, heated water or high-frequency electric current.

The largest consumers of rubber products for many years remain automotive and agricultural engineering enterprises. The degree of saturation of their products with rubber products is an indicator of high reliability and comfort. In addition, parts made of elastomers are often used in the production of plumbing installation, footwear, stationery and children's products.

1. CURRENT STATUS OF THE PROBLEM AND STATEMENT OF THE RESEARCH PROBLEM.

1.1. Vulcanization with elemental sulfur.

1.1.1. Interaction of sulfur with accelerators and activators.

1.1.2. Vulcanization of rubber with sulfur without an accelerator.

1.1.3. Vulcanization of rubber with sulfur in the presence of an accelerator.

1.1.4. The mechanism of individual stages of sulfur vulcanization in the presence of accelerators and activators.

1.1.5. Secondary reactions of polysulfide cross-links. Phenomena of postvulcanization (overvulcanization) and reversion.

1.1.6. Kinetic description of the sulfur vulcanization process.

1.2. Modification of elastomers by chemical reagents.

1.2.1. Modification with phenols and donors of methylene groups.

1.2.2. Modification with polyhaloid compounds.

1.3. Structuring by cyclic derivatives of thiourea.

1.4 Features of the structure and vulcanization of mixtures of elastomers.

1.5. Evaluation of the kinetics of non-isothermal vulcanization in products.

2. OBJECTS AND METHODS OF INVESTIGATION.

2.1. Objects of study

2.2. Research methods.

2.2.1. Study of the properties of rubber compounds and vulcanizates.

2.2.2. Determination of the concentration of cross-links.

2.3. Synthesis of heterocyclic derivatives of thiourea.

3. EXPERIMENTAL AND DISCUSSION

RESULTS

3.1. Study of the kinetic features of the formation of a vulcanization network under the action of sulfur vulcanizing systems.

3.2. Influence of modifiers on the structuring effect of sulfur curing systems.

3.3 Kinetics of vulcanization of rubber mixtures based on heteropolar rubbers.

3.4. Design of vulcanization processes for elastomeric products.

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Introduction to the thesis (part of the abstract) on the topic "Investigation of the kinetics of vulcanization of diene rubbers by complex structuring systems"

The quality of rubber products is inextricably linked with the conditions for the formation in the process of vulcanization of the optimal structure of the spatial network, which makes it possible to maximize the potential properties of elastomer systems. In the works of B. A. Dogadkin, V. A. Shershnev, E. E. Potapov, I. A. Tutorsky, JI. A. Shumanova, Tarasova Z.N., Dontsova A.A., W. Scheele, A.Y. Coran et al. scientists established the main regularities of the course of the vulcanization process, based on the existence of complex, parallel-sequential reactions of crosslinking elastomers with the participation of low molecular weight substances and active centers - actual vulcanization agents.

Works that continue this direction are topical, in particular, in the field of describing the vulcanization characteristics of elastomeric systems containing combinations of accelerators, vulcanization agents, secondary structuring agents and modifiers, covulcanization of rubber mixtures. Sufficient attention has been paid to various approaches in the quantitative description of rubber crosslinking, however, finding a scheme that maximally takes into account the theoretical description of the kinetics of the action of structuring systems and experimental data from industrial laboratories obtained under various temperature and time conditions is an urgent task.

This is due to the great practical significance of methods for calculating the rate and parameters of the process of non-isothermal vulcanization of elastomer products, including the computer design method based on the data of a limited laboratory experiment. The solution of problems that allow achieving optimal performance properties during the production processes of vulcanization of tires and rubber products largely depends on the improvement of methods for mathematical modeling of non-isothermal vulcanization used in automated control systems.

Consideration of the problems of sulfur vulcanization, which determine the physicochemical and mechanical properties of vulcanizates, concerning the kinetics and reaction mechanism of the formation and decomposition of the cross-link structure of the vulcanization network, is of obvious practical importance for all specialists associated with the processing of general-purpose rubbers.

An increased level of elastic-strength, adhesive properties of rubbers, dictated by modern trends in design, cannot be achieved without the widespread use of polyfunctional modifiers in the formulation, which are, as a rule, vulcanizing co-agents that affect the kinetics of sulfur vulcanization, the nature of the resulting spatial network .

The study and calculation of vulcanization processes is currently based largely on experimental material, empirical and graph-analytical calculation methods, which have not yet found a sufficient generalized analysis. In many cases, the vulcanization network is formed by chemical bonds of several types, non-uniformly distributed between the phases. At the same time, the complex mechanisms of intermolecular interaction of components with the formation of physical, coordination and chemical bonds, the formation of unstable complexes and compounds, extremely complicate the description of the vulcanization process, leading many researchers to construct approximations for narrow ranges of factor variation.

The aim of the work is to study, clarify the mechanism and kinetics of non-stationary processes occurring during the vulcanization of elastomers and their mixtures, develop adequate methods for the mathematical description of the vulcanization process by multicomponent modifying structuring systems, including tires and multilayer rubber products, establish factors affecting individual stages of the process in the presence of secondary structuring systems. Development on this basis of methods for variant-optimization calculations of the vulcanization characteristics of compositions based on rubbers and their combinations, as well as their vulcanization parameters.

Practical significance. The multicriteria optimization problem is reduced for the first time to solving the inverse kinetic problem using 6 methods for planning kinetic experiments. Models have been developed that make it possible to purposefully optimize the composition of structural-modifying systems of specific tire rubbers and achieve the maximum level of elastic-rigidity properties in finished products.

Scientific novelty. The multicriteria problem of optimizing the vulcanization process and predicting the quality of the finished product is proposed to solve the inverse chemical problem using the methods of planning kinetic experiments. Determining the parameters of the vulcanization process allows you to effectively control and regulate in a non-stationary area

Approbation of the work was carried out at Russian scientific conferences in Moscow (1999), Yekaterinburg (1993), Voronezh (1996) and scientific and technical conferences of the VGTA in 1993-2000.

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• Shungite - a new ingredient for rubber compounds based on chlorine-containing elastomers 2011, Candidate of Chemical Sciences Artamonova, Olga Andreevna

• Environmental assessment and ways to reduce the emission of accelerators of sulfur vulcanization of rubbers in the production of rubber products 2011, candidate of chemical sciences Zakiyeva, Elmira Ziryakovna

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Dissertation conclusion on the topic "Technology and processing of polymers and composites", Molchanov, Vladimir Ivanovich

1. A scheme describing the patterns of sulfur vulcanization of diene rubbers is theoretically and practically substantiated on the basis of supplementing the known equations of the theory of the induction period with the reactions of formation, destruction of polysulfide bonds and modification of elastomer macromolecules. The proposed kinetic model allows describing the periods: induction, crosslinking and reversion of vulcanization of rubbers based on isoprene and butadiene rubbers and their combinations in the presence of sulfur and sulfenamides, the effect of temperature on the modules of vulcanizates.

2. The constants and activation energies of all stages of the sulfur vulcanization process in the proposed model were calculated by solving inverse kinetic problems by the polyisothermal method, and their good agreement with the literature data obtained by other methods was noted. An appropriate choice of model parameters makes it possible to describe with its help the main types of kinetic curves.

3. Based on the analysis of the regularities of formation and destruction of the cross-link network, a description is given of the dependence of the rate of the vulcanization process of elastomer compositions on the composition of structuring systems.

4. The parameters of the equations of the proposed reaction scheme were determined to describe sulfur vulcanization in the presence of RU modifier and hexol. It has been established that with an increase in the relative concentration of modifiers, the content and rate of formation of stable cross-links increase. The use of modifiers does not have a significant effect on the formation of polysulfide bonds. The rate of disintegration of the polysulfide units of the vulcanization mesh does not depend on the concentration of the components of the structuring system.

5. It has been established that the dependences of the torque measured on the rheometer and the conditional stress at low elongations on the ratio of polychloroprene and styrene-butadiene rubbers in elastomer compositions vulcanized, along with metal oxide, sulfur vulcanizing systems, cannot always be described by a smooth curve. The best estimate of the dependence of the conditional stress on the phase ratio of the rubbers in the composition obtained using Altax as an accelerator is described by a piecewise continuous approximation. At average values ​​of the volume ratios of the phases (a = 0.2 - 0.8), the Davis equation for interpenetrating polymer networks was used. At concentrations below the percolation threshold (a = 0.11 - 0.19), the effective moduli of the composition were calculated using the Takayanagi equation based on the concept of a parallel arrangement of the anisotropic elements of the dispersed phase in the matrix.

6. It has been shown that cyclic derivatives of thiourea increase the number of bonds at the interface between elastomeric phases, the conditional stress during elongation of the composition and change the nature of the dependence of the modulus on the phase ratio in comparison with Altax. The best estimate of the concentration dependence of the conditional stress was obtained using the logistic curve at low cross-link density and the logarithmic curve at high ones.

8. Modular programs have been developed for calculating kinetic constants according to the proposed models, calculating temperature fields and the degree of vulcanization in thick-walled products. The developed software package allows you to perform calculations of technological modes of vulcanization at the stage of product design and recipe creation.

9. Methods have been developed for calculating the processes of heating and vulcanization of multilayer rubber products according to the calculated kinetic constants of the proposed kinetic models of vulcanization.

The accuracy of the coincidence of the calculated and experimental data meets the requirements.

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Kuznetsov A.S. 1 , Kornyushko V.F. 2

1 Postgraduate student, 2 Doctor of Technical Sciences, Professor, Head of the Department of Information Systems in Chemical Technology, Moscow Technological University

PROCESSES OF MIXING AND STRUCTURING OF ELASTOMER SYSTEMS AS CONTROL OBJECTS IN A CHEMICAL-TECHNOLOGICAL SYSTEM

annotation

In the article, from the standpoint of system analysis, the possibility of combining the processes of mixing and structuring into a single chemical-technological system for obtaining products from elastomers is considered.

Keywords: mixing, structuring, system, system analysis, management, control, chemical-technological system.

Kuznetsov A. S. 1 , Kornushko V. F. 2

1 Postgraduate stadent, 2 PhD in Engineering, Professor, Head of the department of Informational systems in chemical technology, Moscow State University

MIXING AND STRUCTURING PROCESSES AS CONTROL OBJECTS IN CHEMICAL-ENGINEERING SYSTEM

Abstract

The article describes the possibility of combining on the basis of system analysis the mixing and vulcanization processes in the unified chemical-engineering system of elastomer’s products obtaining.

keywords: mixing, structuring, system, system analysis, direction, control, chemical-engineering system.

Introduction

The development of the chemical industry is impossible without the creation of new technologies, an increase in output, the introduction of new technology, the economical use of raw materials and all types of energy, and the creation of low-waste industries.

Industrial processes take place in complex chemical-technological systems (CTS), which are a set of devices and machines combined into a single production complex for the production of products.

Modern production of products from elastomers (obtaining an elastomer composite material (ECM), or rubber) is characterized by the presence of a large number of stages and technological operations, namely: preparation of rubber and ingredients, weighing solid and bulk materials, mixing rubber with ingredients, molding a raw rubber mixture - semi-finished product, and, in fact, the process of spatial structuring (vulcanization) of the rubber mixture - blanks for obtaining a finished product with a set of specified properties.

All processes for the production of products from elastomers are closely interconnected, therefore, exact observance of all established technological parameters is necessary to obtain products of proper quality. Obtaining conditioned products is facilitated by the use of various methods for monitoring the main technological quantities in production in the central factory laboratories (CPL).

The complexity and multi-stage nature of the process of obtaining products from elastomers and the need to control the main technological indicators imply considering the process of obtaining products from elastomers as a complex chemical-technological system that includes all technological stages and operations, elements of analysis of the main stages of the process, their management and control.

1. General characteristics of mixing and structuring processes

The receipt of finished products (products with a set of specified properties) is preceded by two main technological processes of the system for the production of products from elastomers, namely: the mixing process and, in fact, the vulcanization of the raw rubber mixture. Monitoring compliance with the technological parameters of these processes is a mandatory procedure that ensures the receipt of products of proper quality, intensification of production, and prevention of marriage.

At the initial stage, there is rubber - a polymer base, and various ingredients. After weighing the rubber and ingredients, the mixing process begins. The mixing process is the grinding of the ingredients, and is reduced to a more uniform distribution of them in the rubber and better dispersion.

The mixing process is carried out on rollers or in a rubber mixer. As a result, we get a semi-finished product - a raw rubber compound - an intermediate product, which is subsequently subjected to vulcanization (structuring). At the stage of the raw rubber mixture, the uniformity of mixing is controlled, the composition of the mixture is checked, and its vulcanization ability is evaluated.

The uniformity of mixing is checked by the indicator of plasticity of the rubber compound. Samples are taken from different parts of the rubber mixture, and the plasticity index of the mixture is determined; for different samples, it should be approximately the same. The plasticity of the mixture P must, within the limits of error, coincide with the recipe specified in the passport for a particular rubber compound.

The vulcanization ability of the mixture is checked on vibrorheometers of various configurations. The rheometer in this case is an object of physical modeling of the process of structuring elastomeric systems.

As a result of vulcanization, a finished product is obtained (rubber, an elastomeric composite material. Thus, rubber is a complex multicomponent system (Fig. 1.)

Rice. 1 - Composition of the elastomeric material

The structuring process is a chemical process of converting a raw plastic rubber mixture into elastic rubber due to the formation of a spatial network of chemical bonds, as well as a technological process for obtaining an article, rubber, elastomeric composite material by fixing the required shape to ensure the required function of the product.

1. Building a model of a chemical-technological system
   production of products from elastomers

Any chemical production is a sequence of three main operations: the preparation of raw materials, the actual chemical transformation, the isolation of target products. This sequence of operations is embodied in a single complex chemical-technological system (CTS). A modern chemical enterprise consists of a large number of interconnected subsystems, between which there are subordination relations in the form of a hierarchical structure with three main steps (Fig. 2). The production of elastomers is no exception, and the output is a finished product with desired properties.

Rice. 2 - Subsystems of the chemical-technological system for the production of products from elastomers

The basis for building such a system, as well as any chemical-technological system of production processes, is a systematic approach. A systematic point of view on a separate typical process of chemical technology allows developing a scientifically based strategy for a comprehensive analysis of the process and, on this basis, building a detailed program for the synthesis of its mathematical description for the further implementation of control programs.

This scheme is an example of a chemical-technological system with a serial connection of elements. According to the accepted classification, the smallest level is a typical process.

In the case of the production of elastomers, separate stages of production are considered as such processes: the process of weighing ingredients, cutting rubber, mixing on rollers or in a rubber mixer, spatial structuring in a vulcanization apparatus.

The next level is represented by the workshop. For the production of elastomers, it can be represented as consisting of subsystems for supplying and preparing raw materials, a block for mixing and obtaining a semi-finished product, as well as a final block for structuring and detecting defects.

The main production tasks to ensure the required level of quality of the final product, the intensification of technological processes, the analysis and control of mixing and structuring processes, the prevention of marriage, are carried out precisely at this level.

1. Selection of the main parameters for the control and management of technological processes of mixing and structuring

The structuring process is a chemical process of converting a raw plastic rubber mixture into elastic rubber due to the formation of a spatial network of chemical bonds, as well as a technological process for obtaining an article, rubber, elastomeric composite material by fixing the required shape to ensure the required function of the product.

In the processes of production of products from elastomers, the controlled parameters are: temperature Tc during mixing and vulcanization Tb, pressure P during pressing, time τ of processing the mixture on the rollers, as well as vulcanization time (optimum) τopt..

The temperature of the semi-finished product on the rollers is measured by a needle thermocouple or a thermocouple with self-recording instruments. There are also temperature sensors. It is usually controlled by changing the flow of cooling water for the rollers by adjusting the valve. In production, cooling water flow regulators are used.

The pressure is controlled by using an oil pump with a pressure sensor and appropriate regulator installed.

Establishment of the parameters for the manufacture of the mixture is carried out by the roller according to the control charts, which contain the necessary values ​​of the process parameters.

The quality control of the semi-finished product (raw mixture) is carried out by the specialists of the central factory laboratory (CPL) of the manufacturer according to the passport of the mixture. At the same time, the main element for monitoring the quality of mixing and evaluating the vulcanization ability of the rubber mixture are vibrorheometry data, as well as the analysis of the rheometric curve, which is a graphical representation of the process, and is considered as an element of control and adjustment of the process of structuring elastomeric systems.

The procedure for evaluating the vulcanization characteristics is carried out by the technologist according to the passport of the mixture and the databases of rheometric tests of rubbers and rubbers.

Control of obtaining a conditioned product - the final stage - is carried out by specialists of the department for technical quality control of finished products according to the test data of the technical properties of the product.

When controlling the quality of a rubber compound of one specific composition, there is a certain range of values ​​of property indicators, subject to which products with the required properties are obtained.

Findings:

1. The use of a systematic approach in the analysis of the processes of production of products from elastomers makes it possible to most fully track the parameters responsible for the quality of the structuring process.
2. The main tasks to ensure the required indicators of technological processes are set and solved at the workshop level.

Literature

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4. Novakov I.A., Wolfson S.I., Novopoltseva O.M., Krakshin M.A. Rheological and vulcanization properties of elastomer compositions. - M.: ICC "Akademkniga", 2008. - 332 p.
5. Kuznetsov A.S., Kornyushko V.F., Agayants I.M. \Rheogram as a process control tool for structuring elastomeric systems \ M:. NXT-2015 p.143.
6. Kashkinova Yu.V. Quantitative interpretation of the kinetic curves of the vulcanization process in the system of organizing the workplace of a technologist - a rubber worker: Abstract of the thesis. dis. … cand. tech. Sciences. - Moscow, 2005. - 24 p.
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References

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The determination of vulcanization kinetics is of great importance in the manufacture of rubber products. The vulcanizability of rubber compounds is not identical to their ability to scorch, and to evaluate it, methods are needed that allow one to determine not only the beginning (by decreasing fluidity), but also the optimum vulcanization upon reaching the maximum value of some indicator, for example, the dynamic modulus.39

The usual method for determining vulcanizability is to make several samples from the same rubber compound, differing in the duration of the heat treatment, and test them, for example, in a tensile tester. At the end of the test, a vulcanization kinetics curve is plotted. This method is very laborious and time consuming.39

Rheometer tests do not answer all questions, and for greater accuracy, the results of determining the density, tensile strength and hardness must be processed statistically and cross-checked with curves vulcanization kinetics. At the end of the 60s. In connection with the development of control of the preparation of mixtures using rheometers, the use of larger closed rubber mixers began to be used and mixing cycles were significantly reduced in some industries, it became possible to produce thousands of tons of refills of rubber compounds per day.

Significant improvements have also been noted in the speed at which material moves through the plant. These advances have led to a backlog of test technology. A plant that prepares 2,000 batches of mixes daily requires that a test be carried out for about 00 control parameters (Table 17.1), assuming at 480

Definition of kinetics rubber vulcanization mixtures

When designing thermal modes of vulcanization, simultaneous and interconnected thermal (dynamic change in the temperature field along the product profile) and kinetic (formation of the degree of rubber vulcanization) processes are simulated. As a parameter for determining the degree of vulcanization, any physical and mechanical indicator for which there is a mathematical description of the kinetics of non-isothermal vulcanization can be chosen. However, due to differences in the vulcanization kinetics for each417

The first part of Chapter 4 describes the existing methods for assessing the effect of the curing action of time-varying temperatures. Approximation of the simplifying assumptions underlying the assessment accepted in the industry becomes apparent in the light of consideration of the general patterns of changes in the properties of rubber during vulcanization (vulcanization kinetics for various indicators of properties determined by laboratory methods).

The formation of rubber properties during vulcanization of multilayer products proceeds differently than thin plates used for laboratory mechanical tests from a homogeneous material. In the presence of materials of different deformability, the complex stressed state of these materials has a great influence. The second part of Chapter 4 is devoted to the mechanical behavior of materials of a multilayer product in vulcanization molds, as well as methods for evaluating the achieved degrees of vulcanization of rubber in products.7
It should also be noted that when determining vulcanization kinetics according to this property, the test mode is not indifferent. For example, standard rubber made of natural rubber at 100°C has a different optimum, plateau and distribution of tear resistance indicators than at 20°C, depending on degree of vulcanization.

As follows from the consideration of the dependence of the basic properties of rubber on the degree of its cross-linking, carried out in the previous section, the assessment of the kinetics and degree of vulcanization can be done in various ways. The methods used are divided into three groups: 1) chemical methods (determination of the amount of reacted and unreacted vulcanization agent by chemical analysis of rubber) 2) physicochemical methods (determination of thermal effects of the reaction, infrared spectra, chromatography, luminescent analysis, etc.) 3) mechanical methods (determination of mechanical properties, including methods specially developed for determining the kinetics of vulcanization).

Radioactive isotopes (labeled atoms) are easy to detect by measuring the radioactivity of the product that contains them. To study the vulcanization kinetics, after a certain reaction time of rubber with radioactive sulfur (vulcanization agent), the reaction products are subjected to cold continuous extraction with benzene for 25 days. The unreacted curing agent is removed with the extract, and the concentration of the remaining bound agent is determined from the radioactivity of the final reaction product.

The second group of methods serves to determine the actual kinetics of vulcanization.

GOST 35-67. Rubber. Method for determining kinetics vulcanization of rubber compounds.

The development in recent years of new polymerization methods has contributed to the creation of rubber types with more advanced properties. Changes in properties are mainly due to differences in the structure of rubber molecules, and this naturally increases the role of structural analysis. The spectroscopic determination of 1,2-, cis-, A-, and 1,4-grain structures in synthetic rubbers is of the same practical and theoretical importance as the analysis of the physicochemical and performance characteristics of a polymer. The results of quantitative analysis make it possible to study 1) the effect of the catalyst and polymerization conditions on the structure of rubber 2) the structure of unknown rubbers (identification) 3) the change in the microstructure during vulcanization (isomerization) and the kinetics of vulcanization 4) the processes occurring during oxidative and thermal degradation of rubber (structural changes when drying rubber, aging) 5) the effect of stabilizers on the stability of the rubber molecular framework and the processes occurring during grafting and plasticization of rubber 6) the ratio of monomers in rubber copolymers and, in this regard, to give a qualitative conclusion about the distribution of blocks along the lengths in butadiene-styrene copolymers ( separation of block and random copolymers).357

When selecting organic rubber vulcanization accelerators for industrial use, the following should be taken into account. The accelerator is chosen for a certain type of rubber, because depending on the type and structure of rubber, a different effect of the accelerator on the vulcanization kinetics is observed.16

To characterize the kinetics of vulcanization at all stages of the process, it is advisable to observe the change in the elastic properties of the mixture. As one of the indicators of elastic properties during tests carried out in a stationary loading mode, the dynamic modulus can be used.

Details about this indicator and methods for its determination will be discussed in Section 1 of Chapter IV, devoted to the dynamic properties of rubber. As applied to the problem of controlling rubber compounds by the kinetics of their vulcanization, the determination of the dynamic modulus is reduced to the observation of the mechanical behavior of a rubber compound subjected to multiple shear deformation at an elevated temperature.

Vulcanization is accompanied by an increase in the dynamic modulus. The completion of the process is determined by the cessation of this growth. Thus, continuous monitoring of the change in the dynamic modulus of the rubber compound at the vulcanization temperature can serve as the basis for determining the so-called optimum vulcanization (modulo), which is one of the most important technological characteristics of each rubber compound.37

In table. 4 shows the values ​​of the temperature coefficient of the rate of vulcanization of natural rubber, determined from the rate of binding of sulfur. The temperature coefficient of the vulcanization rate can also be calculated from the kinetic curves of changes in the physical and mechanical properties of rubber during vulcanization at different temperatures, for example, by the modulus value. The values ​​of the coefficients calculated from the kinetics of modulus change are given in the same table.76

The method for determining the degree of vulcanization (T) on the product section limiting the vulcanization process. In this case, methods and devices for optimal control of the vulcanization modes of products are distinguished, in which the kinetics of non-isothermal vulcanization is determined 419

Place of definition (T). Methods and devices are known that allow determining the kinetics of non-isothermal vulcanization 419

The kinetic curves obtained using the described methods are used to calculate such parameters as rate constants, temperature coefficients and activation energy of the process in accordance with the equations of formal kinetics of chemical reactions. For a long time, it was believed that most kinetic curves are described by a first-order equation. It was found that the temperature coefficient of the process is equal to an average of 2, and the activation energy varies from 80 to kJ/mol, depending on the vulcanization agent and the molecular structure of rubber. However, a more accurate determination of the kinetic curves and their formal kinetic analysis carried out by W. Scheele 52 showed that in almost all cases the reaction order is less than 1 and equals 0.6-0.8, and the vulcanization reactions are complex and multistage.

Curometer model VII by Wallace (Great Britain) determines the kinetics of vulcanization of rubber compounds under isothermal conditions. The sample is placed between plates, one of which is displaced at a certain angle. The advantage of this design is that there is no porosity in the sample because it is under pressure, and the possibility of using smaller samples, which reduces the warm-up time.499

The study of the kinetics of vulcanization of rubber compounds is not only of theoretical interest, but also of practical importance for assessing the behavior of rubber compounds during processing and vulcanization. To determine the modes of technological processes in production, the indicators of the vulcanizability of rubber compounds should be known, i.e. their tendency to premature vulcanization - the beginning of vulcanization and its speed (for processing), and for the actual vulcanization process - in addition to the above indicators - the optimum and plateau vulcanization, reversion area.

The book was compiled on the basis of lectures given to US rubber engineers at the University of Akron by leading American researchers. The purpose of these lectures was a systematic presentation of the available information about the theoretical foundations and technology of vulcanization in an accessible and fairly complete form.

In accordance with this, at the beginning of the book, the history of the issue and the characteristics of changes in the basic properties of rubber that occur during vulcanization are presented. Further, when presenting the kinetics of vulcanization, chemical and physical methods for determining the speed, degree and temperature coefficient of vulcanization are critically considered. The influence of the dimensions of the workpiece and the thermal conductivity of rubber compounds on the rate of vulcanization has been discussed.8

Instruments for determining the kinetics of vulcanization usually operate either in the mode of a given amplitude value of displacement (volcameters, viscurometers or rheometers), or in the mode of a given amplitude value of the load (curometers, SERAN). Accordingly, the amplitude values ​​of the load or displacement are measured.

Since samples 25 are usually used for laboratory tests, prepared from plates with a thickness of 0.5-2.0 mm, which are vulcanized almost under isothermal conditions (Г == = onst), the vulcanization kinetics for them is measured at a constant vulcanization temperature. On the kinetic curve, the duration of the induction period, the time of the onset of the vulcanization plateau, or optimum, the magnitude of the plateau, and other characteristic times are determined.

Each of them corresponds to certain vulcanization effects, according to (4.32). Equivalent vulcanization times will be those times which at a temperature of 4kv = onst will lead to the same effects as at variable temperatures. Thus

If the vulcanization kinetics at T = onst is given by equation (4.20a), in which t is the time of the actual reaction, the following method can be proposed definitions of kinetics non-isothermal vulcanization reaction.

Operational control of the vulcanization process allows the implementation of special devices for determining the kinetics of vulcanization - vulcanometers (curometers, rheometers), continuously fixing the amplitude of the shear load (in the mode of a given amplitude of harmonic shift) or shear deformation (in the mode of a given amplitude of shear load). The most widely used devices are vibration type, in particular Monsanto 100 and 100S rheometers, which provide automatic testing with obtaining a continuous diagram of changes in the properties of the mixture during vulcanization according to ASTM 4-79, MS ISO 3417-77, GOST 35-84.492

The choice of curing or vulcanization mode is usually carried out by studying the kinetics of changes in any property of the cured system of electrical resistance and dielectric loss tangent, strength, creep, modulus of elasticity under various types of stress state, viscosity, hardness, heat resistance, thermal conductivity, swelling, dynamic mechanical characteristics , refractive index and a number of other parameters, -. The methods of DTA and TGA, chemical and thermomechanical analysis, dielectric and mechanical relaxation, thermometric analysis and differential scanning calorimetry are also widely used.

All these methods can be conditionally divided into two groups: methods that allow you to control the speed and depth of the curing process by changing the concentration of reactive functional groups, and methods that allow you to control a change in any property of the system and set its limiting value. The methods of the second group have the common drawback that one or another property of the curing system is clearly manifested only at certain stages of the process, so the viscosity of the curing system can be measured only up to the gelation point, while most of the physical and mechanical properties begin to clearly manifest themselves only after the gelation point. On the other hand, these properties strongly depend on the measurement temperature, and if a property is continuously monitored during the process, when it is necessary to change the reaction temperature in the course of the reaction or the reaction develops essentially non-isothermally to achieve the completeness of the reaction, then the interpretation of the measurement results of the kinetics of property change in such a process becomes already quite complex.37

A study of the kinetics of copolymerization of ethylene with propylene on the VO I3-A12(C2H5)3C1e system showed that its modification with tetrahydrofuran makes it possible, under certain conditions, to increase the integral yield of the copolymer. This effect is due to the fact that the modifier, by changing the ratio between the rates of chain growth and termination, promotes the formation of copolymers with a higher molecular weight. The same compounds are used in a number of cases in the copolymerization of ethylene and propylene with dicyclopentadiene, norbornene, and other cyclodienes. The presence of electron-donating compounds in the reaction sphere during the preparation of unsaturated terpolymers prevents the subsequent slower reactions of cross-linking of macromolecules and makes it possible to obtain copolymers with good vulcanization properties.45

Kinetics of sulfur addition. The kinetic Weber curves, as can be seen from Fig. , have the form of broken lines.

Weber explained this type of curves by the fact that at certain moments of vulcanization, various stoichiometric compounds of rubber with sulfur are formed - sulfides of the composition KaZ, KaZr. Ka33, etc. Each of these sulfides is formed at its own rate, and the formation of a sulfide with a certain sulfur content does not begin until the previous stage of formation of a sulfide with a smaller number of sulfur atoms has ended.

However, later and more thorough research by Spence and Young led to the simpler kinetic curves depicted in Fig. and. As can be seen from these302

The results of determining the structural parameters of the vulcanization mesh using the sol-gel analysis, in particular, the data on the kinetics of changes in the total number of mesh chains (Fig. 6A), show that the most important feature of dithiodimorpholine vulcanizates is a significantly lower reversion and, as a consequence, a smaller decrease in the strength properties of vulcanizates with an increase in curing temperature. On fig. 6B shows the kinetics of the change in the tensile strength of mixtures at 309

Science Noobs - Kinetic Sand

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findings

Based on a system analysis of the process of gumming a galvanized strip, models and methods are determined, the application of which is necessary for the implementation of the control method: a simulation model of the polymer coating drying process, a method for optimizing the technological parameters of the polymerization process based on a genetic algorithm, and a neuro-fuzzy process control model.

It has been determined that the development and implementation of a method for controlling the process of vulcanization of a galvanized strip on a polymer coating unit based on neuro-fuzzy networks is an urgent and promising scientific and technical task in terms of economic benefits, cost reduction and production optimization.

It has been established that the process of vulcanization of a galvanized strip in the furnaces of a metal coating unit is a multiply connected object with a distribution of parameters along the coordinate, operating under nonstationary conditions and requires a systematic approach to study.

The requirements for the mathematical support of the control system for multi-connected thermal objects of the metal coating unit are determined: ensuring the functioning in the mode of direct connection with the object and in real time, the variety of functions performed with their relative invariance during operation, the exchange of information with a large number of its sources and consumers in the process of solving the main problems, operability in conditions that limit the time for calculating control actions.

MATHEMATICAL SOFTWARE OF THE NEURO-FUZZY CONTROL SYSTEM FOR MULTIPLE-CONNECTED THERMAL OBJECTS OF A GUDDED METAL COATING UNIT

System Analysis of the Control of Multiconnected Thermal Objects of the Rubberized Coating Unit

Conceptual design is the initial design stage, at which decisions are made that determine the subsequent appearance of the system, and research and coordination of the parameters of the created solutions with their possible organization are carried out. At present, it is gradually becoming realized that in order to build systems at a qualitatively different level of novelty, and not just their modernization, it is necessary to be armed with theoretical ideas about the direction in which systems develop. This is necessary to organize the management of this process, which will increase both the quality indicators of these systems and the efficiency of their design, operation and operation processes.

At this stage, it is necessary to formulate a control problem, from which we will obtain research problems. After analyzing the process of polymerization of a galvanized strip as a control object, it is necessary to determine the boundaries of the subject area that are of interest when building a process control model, i.e. determine the required level of abstraction of the models to be built.

The most important method of system research is the representation of any complex systems in the form of models, i.e. application of the method of cognition, in which the description and study of the characteristics and properties of the original is replaced by the description and study of the characteristics and properties of some other object, which in the general case has a completely different material or ideal representation. It is important that the model does not display the object of study itself in the form closest to the original, but only those of its properties and structures that are of greater interest to achieve the goal of the study.

The task of control is to set such values ​​of the parameters of the vulcanization process of a galvanized strip, which will allow achieving the maximum adhesion coefficient with a minimum consumption of energy resources.

A number of requirements are imposed on the quality of pre-painted rolled products, which are described in GOST, listed in section 1.3. The drying process in the ovens of the gum coating unit only affects the quality of adhesion to the substrate. Therefore, defects such as coating unevenness, gloss deviation, and potholes are not considered in this paper.

To carry out the drying process of the polymer coating, it is necessary to know the following set of technological parameters: temperatures of 7 furnace zones (Tz1 ... Tz7), line speed (V), density and heat capacity of the metal substrate (, s), thickness and initial temperature of the strip (h, Tin.) , the temperature range of polymerization of the applied paint ().

These parameters in production are usually called a recipe.

Such parameters as the power of the fans installed in the furnace zones, the volume of clean air supplied, the parameters of the explosion hazard of varnishes are excluded from consideration, since they affect the heating rate of the zones before drying and the concentration of explosive gases, which are not disclosed in this work. Their regulation is carried out separately from the management of the vulcanization process itself.

Let's define the research tasks that need to be performed to achieve the goal of management. Note that the current state of system analysis imposes special requirements on decisions made on the basis of the study of the obtained models. It is not enough just to obtain possible solutions (in this case, the temperatures of the furnace zones) - it is necessary that they be optimal. System analysis, in particular, allows us to propose decision-making methods for the purposeful search for acceptable solutions by discarding those that are obviously inferior to others according to a given quality criterion. The purpose of its application to the analysis of a specific problem is to apply a systematic approach and, if possible, rigorous mathematical methods, to increase the validity of the decision made in the context of analyzing a large amount of information about the system and many potential solutions.

Due to the fact that at this stage we know only the input and output parameters of the models, we will describe them using the “black box” approach.

The first task to be solved is to build a simulation model of the coating drying process, i.e. obtain a mathematical description of the object, which is used to conduct experiments on a computer in order to design, analyze and evaluate the functioning of the object. This is necessary to determine to what extent the temperature of the metal surface (Tp. out.) will increase when leaving the furnace for given values ​​of the strip speed, thickness, density, heat capacity and initial temperature of the metal, as well as temperatures of the furnace zones. In the future, a comparison of the value obtained at the output of this model with the polymerization temperature of the paint will make it possible to draw a conclusion about the quality of adhesion of the coating (Figure 10).

Figure 10 - Conceptual simulation model of the coating drying process

The second task is to develop a method for optimizing the technological parameters of the galvanized strip vulcanization process. To solve it, it is necessary to formalize the control quality criterion and build a model for optimizing technological parameters. Due to the fact that the temperature regime is controlled by changing the temperatures of the furnace zones (Tz1 ... Tz7), this model should optimize their values ​​(Tz1opt ... Tz7opt) according to the control quality criterion (Figure 11). This model also receives vulcanization temperatures as input, since without them it is impossible to determine the quality of paint adhesion to the metal substrate.

Figure 11 - Conceptual model for optimizing process parameters