Method determing valcunisation parameters on initial stage of process

FIELD: rubber technology.

SUBSTANCE: method is characterised by that, a sample is prepared for analysis during the vulcanisation process, for which 25 cm3 of toluene is added to a precise batch of the sample, with subsequent keeping the rubber mixture-toluene for 4 hours, after which gel-sol analysis is carried out. To carry out gel-sol analysis, the obtained system is filtered. The residue is dried until a constant mass is obtained. The content of gel in the system and concentration of polymer in the filtrate is calculated and its characteristic viscosity is determined. A graph is drawn with coordinates of characteristic viscosity - vulcanisation time and gel content - vulcanisation time, and from the character of the obtained graphic dependence the parameters of the vulcanisation process are determined. Two regions on the graph of the relationship between the characteristic viscosity of solutions and vulcanisation time are marked. On the first region, characteristic viscosity increases during the vulcanisation time of the sample in an almost linear relationship. In this case, the system contains gel, which shows that, in this period there not enough intermolecular transverse bonds in the sample to form a spatial structure, while the increase in characteristic viscosity is only a result of change in the length of caoutchouc macromolecules. The beginning of the vulcanisation process is shown by the increase in the characteristic viscosity of the investigated solution by 5% relative its minimum value. Content of gel increases from 0 to 100% in the second region. At the point with 90% gel content the sample is completely insoluble in toluene.

EFFECT: increased accuracy and efficiency of determining vulcanisation parameters on the initial stage of the process.

3 dwg

 

The invention relates to technology of rubber, namely, to measure and control process parameters of vulcanization of the rubber mixtures, and can be used in laboratory practice and research in the relevant technological industry.

The closest in technical essence and the achieved effect is a method of determining a characteristic viscosity of toluene solutions of rubber, which allows us to estimate the magnitude of the molecular weight rubbers [a Practical guide to synthesis and investigation of properties of polymers. The Federal Republic of Germany. 1971. TRANS. with it. Under. editor Prof. chem. Sciences. VP Zubov. M.: Chemistry, 1976. - 286 S.].

The disadvantage of this method is that it has a relatively low accuracy and efficiency determination of parameters of partially crosslinked and/or destructuring polymers.

The technical problem of the invention is to improve the accuracy and efficiency define the parameters of vulcanization at the initial stage of the process.

The technical problem is achieved by a method for determining parameters of vulcanization at the initial stage of the process, characterized in that it envisages a process of vulcanization of the rubber mixture, sampling during the implementation process, the preparation of samples for analysis, for which the exact sample sample add toluene displacement 25,0 cm 3with subsequent keeping system rubber mixture of toluene for 4.0 hours, followed by a gel-Sol analysis, to this end, the system was filtered, the precipitate is dried to obtain a constant amount of mass, calculate the content of gel in the system and the concentration of polymer in the filtrate and determine its characteristic viscosity, and then build the graphs in the coordinate characteristic viscosity - vulcanization time and content of the gel - time of vulcanization and the nature of the resulting graphical dependencies define the parameters of the vulcanization process, the graphical dependence of the characteristic viscosity of the solutions from the time of vulcanization of the sample emit two sections, the first part of the characteristic viscosity increases during the time of vulcanization of the sample in accordance with the dependence is close to linear, but the system does not contain gel, which suggests that in this period produced is not sufficient for the formation of spatial patterns in the sample the number of intermolecular cross-linking, and the growth of the characteristic viscosity is determined only by the length of the macromolecules rubber, and about the beginning of the vulcanization process is shown in the increase of the characteristic viscosity of the investigated solution by 5.0% relative to its minimum value, the and the second site, the content of the gel is increased from 0.0 to 100.0%, this is an intensive crosslinking and the dependence of the characteristic viscosity of the solution from the time of vulcanization of the sample is not straightforward, the point at which the gel content is 90,0±3.0%, the sample is completely insoluble in toluene, and the formation of spatial patterns in the sample is completed.

The technical result is to increase the accuracy and efficiency define the parameters of vulcanization at the initial stage of the process.

The rubber mixture under study, are loaded into pre-heated to the working temperature of the mold, which is then placed in a press and close the plate. Periodically plate unlock and take samples of the rubber. Interval sampling 1,0±0.3 minutes, the mass of the sample is 1.5±of 0.5 was Selected for the study samples of the rubber mixtures are prepared for analysis by the following procedure: in a clean, dry volumetric flask with polished tube placed weighed on an analytical balance with an accuracy of ±0.0002 g a portion of the rubber, the weight of 0.03±0.005 g, then pipette prilisaetsa 25,0 cm3of toluene. After that, the solutions leave 4.0 h, for the best samples dissolution and homogenization of the system it is advisable to place the bulb on vibrostimulation.

After settling system rubber compound is toluene hold gel-Sol analysis, this is the first composition is filtered and nerastvorim part of the rubber mixture is dried in a desiccator at room temperature until constant weight. Fraction of total mass of gel ω determined by the formula:

where mc- weight of completely dry gel, g,

m0- the original mounting rubber mixture,

The concentration of polymer solution (g/DL) determined by the formula:

The characteristic viscosity of the filtrate samples of the rubber is determined by the following method: in a capillary viscometer of the type VPG is filled with pure toluene and measured the time it expires through capillary t0, with. Then in the viscometer is filled with the test solution and measured the time of its expiration, t, sec. Measurement timeout carried out at a temperature of 30.0°C.

Characteristic viscosity of each solution is calculated according to the formula Schulz-Blaschke:

where ηbeatsis the specific viscosity,orwhere t is the expiry time of the polymer solution, C; t0- the expiration time of the solvent, C;η=0,28 constant.

The experiment results build graphs in the coordinate content of the gel - time of vulcanization and the characteristic viscosity of the time of vulcanization.

In figure 1, 2 presents, for example, the graphical dependence of the characteristic viscosity of the time of vulcanization and figure 3 with the holding gel - the vulcanization time for the rubber mixtures based on General purpose rubbers.

Based on the analysis of graphic dependences of the characteristic viscosity of the solutions from the time of vulcanization obtained for rubber General purpose curve (Fig.1-3), there are two plot I plot from the origin to the point of gelation (tG), The second plot from the point of gelation (tG) to the point tX. At site I, the rubber mixture contains no gel, and about the beginning of the vulcanization process is shown in the increase of the characteristic viscosity of the investigated solution is 5.0% (t0) relative to its minimum value (point t) with subsequent increased to 70.0±2,0% (tG), and in this period is not formed, the number of intermolecular cross-linking sufficient for the formation of spatial patterns in the sample, and the change in viscosity is caused only by changing the length of the macromolecules. At site II (figure 3) in the rubber compound is present in the gel and its content varies from 0.0% to 100.0%, i.e. at site II is an intensive formation of intermolecular bonds during vulcanization. At the point in which the content of the gel is 90,0±3.0%, the sample is completely insoluble in toluene, and the formation of spatial patterns in the sample is completed.

From the analysis of the graphical dependence (Fig.1-3) to define the individual indicators:

t - vulcanization time corresponding to the minimum value of the characteristic viscosity (the period of time that corresponds to the induction period of vulcanization), min;

t0the time of vulcanization, the corresponding viscosity increase by 5.0%, - start of the vulcanization reaction, min;

tGthe time of vulcanization, the corresponding increase in viscosity on 70,0±2,0%, the point of gelation, min;

tXthe time of vulcanization, the complete loss of solubility of the samples (gel content 90,0±3,0%), - formation of the spatial grid, minutes

Determination of the parameters of the vulcanization process is carried out through periodic sampling vulkanizetas rubber compound and subsequent determination of the characteristic viscosity combined with gel-Sol analysis of their solutions. The method can be applied for the evaluation of vulcanization properties of mixtures based on General purpose rubbers.

The proposed method of determination of parameters of vulcanization at the initial stage of the process allows to improve the accuracy and efficiency determine the vulcanization properties of the rubber compound.

The method of determining parameters of vulcanization at the initial stage of the process, characterized in that it envisages a process of vulcanization of the rubber mixture, the sampling for the implementation of the ia process, the preparation of samples for analysis, for which the exact sample sample add toluene displacement of 25 cm3with subsequent keeping system rubber mixture of toluene for 4 h, followed by gel-Sol analysis, to this end, the system was filtered, the precipitate is dried to obtain a constant amount of mass, calculate the content of gel in the system and the concentration of polymer in the filtrate and determine its characteristic viscosity, and then build the graphs in the coordinate characteristic viscosity - vulcanization time and content of the gel - time of vulcanization, and the nature of the resulting graphical dependencies define the parameters of the vulcanization process, the graphical dependence of the characteristic viscosity of the solutions from the time of vulcanization of the sample emit two sections, the first part of the characteristic viscosity increases during the time of vulcanization of the sample in accordance with the dependence is close to linear, but the system does not contain gel, which suggests that in this period produced is not sufficient for the formation of spatial patterns in the sample the number of intermolecular cross-linking, and the growth of the characteristic viscosity is determined only by the length of the macromolecules rubber, and about the beginning of the vulcanization process is illustrated by the increasing feature : the static viscosity of the investigated solution of 5% relative to its minimum value, the second part of the gel content increases from 0%to 100%, with an intensive crosslinking and the dependence of the characteristic viscosity of the solution from the time of vulcanization of the sample is not straightforward, the point at which the gel content is 90±3%, the sample is completely insoluble in toluene and the formation of spatial patterns in the sample is completed.



 

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