CN112505313A - Method for evaluating processability of rubber compound - Google Patents
Method for evaluating processability of rubber compound Download PDFInfo
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- CN112505313A CN112505313A CN202011201077.7A CN202011201077A CN112505313A CN 112505313 A CN112505313 A CN 112505313A CN 202011201077 A CN202011201077 A CN 202011201077A CN 112505313 A CN112505313 A CN 112505313A
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 117
- 239000005060 rubber Substances 0.000 title claims abstract description 117
- 150000001875 compounds Chemical class 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000012360 testing method Methods 0.000 claims abstract description 33
- 239000000203 mixture Substances 0.000 claims abstract description 25
- 238000003490 calendering Methods 0.000 claims abstract description 20
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 18
- 238000010057 rubber processing Methods 0.000 claims abstract description 18
- 239000010959 steel Substances 0.000 claims abstract description 18
- 244000043261 Hevea brasiliensis Species 0.000 claims abstract description 10
- 229920003052 natural elastomer Polymers 0.000 claims abstract description 9
- 229920001194 natural rubber Polymers 0.000 claims abstract description 9
- 238000012545 processing Methods 0.000 claims abstract description 6
- 238000005070 sampling Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 4
- 238000001514 detection method Methods 0.000 abstract description 3
- 238000011156 evaluation Methods 0.000 abstract description 3
- 230000006872 improvement Effects 0.000 description 8
- 238000000265 homogenisation Methods 0.000 description 4
- 230000008676 import Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 230000035945 sensitivity Effects 0.000 description 4
- 238000005227 gel permeation chromatography Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 101100434170 Oryza sativa subsp. japonica ACR2.1 gene Proteins 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 150000003904 phospholipids Chemical class 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/44—Resins; Plastics; Rubber; Leather
- G01N33/445—Rubber
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
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- General Health & Medical Sciences (AREA)
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- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
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Abstract
The application belongs to the technical field of rubber detection, and particularly relates to an evaluation method for processability of rubber compound. The method comprises a rubber processing analyzer testing method, wherein the rubber processing analyzer testing method comprises the steps of carrying out frequency scanning on natural rubber and a mixture thereof under fixed strain to determine the minimum frequency under the lowest modulus, carrying out time scanning according to the minimum frequency, selecting an integral area under certain time scanning to evaluate, wherein the evaluation standard is the natural rubber and the mixture thereof with the minimum integral area, and the better the processability of the rubber compound in steel wire calendering is, the less the rubber compound is prone to stick to a roller. The method evaluates the processing performance of the natural rubber and the mixture thereof during steel wire calendering by the rubber processing analyzer, is simple, convenient, objective and comprehensive, and can be used for selecting the formula and the process of the tire belt compound.
Description
Technical Field
The application belongs to the technical field of rubber detection, and particularly relates to an evaluation method for processability of rubber compound.
Background
Natural Rubber (NR) has been receiving attention from users as an important strategic material and industrial raw material, and its quality and properties have been in the spotlight. Due to different regions, climates, rubber tree types and production methods, the performances of rubber compounds have obvious differences, and the rubber compounds are generally divided into five grades of 5L, 5, 10, 20, 50 and the like according to seven items of impurity content, initial plastic value, plastic retention rate, nitrogen content, volatile matter content, ash content, color index and the like in raw rubber, wherein the impurity content is taken as a main index, and the impurity content is divided into five grades according to the number of impurities.
For rubber product enterprises such as tires, the processability of rubber compounds has a great influence on the homogenization and mixing of rubber compounds. The processability of rubber mixes depends on the viscoelasticity of the rubber mix, the main parameters influencing the viscoelasticity of the rubber mix being the relative molecular weight and its molecular weight distribution.
At present, various large rubber product enterprises always use the Mooney viscosity as one of the quality indexes of rubber compound, and the Mooney viscosity value is considered to be large, which indicates that the flow resistance of raw rubber is large, the relative molecular weight is large, and the processability is poor. However, it has been demonstrated through extensive field tests that the processability of rubbers having the same Mooney viscosity values still differ greatly. This is because the molecular weight of the rubber itself is too large, the movement of the rubber molecular chain is small, and when the rubber is forced to flow by the rapid rotation in the Mooney viscosity test, slipping or the rotor stopping rotation is easily caused. The Mooney viscosity results are therefore independent of the relative molecular weight of the rubber at this time.
Based on the difference in Mooney viscosity versus relative molecular weight characterization of the rubber compound, researchers have generally used Gel Permeation Chromatography (GPC) to test the relative molecular weight of the rubber compound and its molecular weight distribution, but proteins, phospholipids, phosphate groups, and the like in the rubber compound can generate similar physical cross-linking points, affecting GPC testing relative molecular weight.
In addition, many rubber companies and researchers have employed Rubber Processing Analyzers (RPAs) to measure the rheological properties of rubber. The properties of rubber are generally judged by the modulus and tan σ as measured by strain or frequency sweep.
Disclosure of Invention
The application aims to provide the method for evaluating the processability of the rubber compound, which has the advantages of simple operation, high sensitivity, reliable result and no pollution to the environment.
In order to achieve the above object, the present application adopts the following technical solutions:
a method for evaluating the processability of rubber compound comprises the following steps:
1) taking the calendering processing temperature of the rubber compound as a testing temperature, fixing the testing temperature and strain in a frequency region, and performing frequency scanning on a raw rubber sample of the rubber compound by using a rubber processing analyzer;
2) plotting the modulus G' measured at each frequency scanned in the frequency region with the frequency as the abscissa of the curve to obtain a frequency-modulus curve;
3) determining the minimum frequency corresponding to the value of the lowest modulus G';
4) applying strain under the minimum frequency, fixing and testing temperature, frequency and strain, and scanning the rubber raw rubber sample in time by using a rubber processing analyzer;
5) plotting the modulus G 'measured at each time of said time sweep against time to obtain a time-modulus curve, time being the abscissa of the curve and modulus G' being the ordinate of the curve;
6) the integral area in the time-modulus curve is used as a basis for judging the processability of the rubber compound, and the smaller the integral area is, the better the processability of the rubber compound during steel wire calendering is, and the roller adhesion is difficult to occur.
As a further improvement, the method also comprises the steps of sampling raw rubber samples of the rubber compound from the same position on a raw rubber block in sequence and standing for 1-2 hours before the step 1).
As a further improvement, the test temperature in step 1) is 100 ℃, 110 ℃ or 120 ℃.
As a further improvement, the strain tested in step 1) is 0.28% to 42%, preferably 0.28%.
As a further improvement, the frequency region of the frequency scanning in the step 1) is 0-60 HZ.
As a further improvement, the rubber process analyzer is an RPA2000 rubber process analyzer manufactured by alpha corporation, USA.
As a further improvement, the time scanning is carried out on the natural rubber and the mixture thereof within the area of 0-26 min to obtain a time-modulus curve, the integral area is obtained by integrating the curve, and the curve integral area method comprises the following steps:
and f (x) is the curve of different rubber mixtures scanned over time.
The application carries out dynamic rheological detection to the rubber gross rubber in viscoelastic region, and the rubber gross rubber shows different modulus responses under frequency variation this moment, can not exert an influence to the structure of rubber gross rubber itself in the testing process moreover. The elastic modulus and the viscous modulus obtained by frequency scanning of a rubber processing analyzer are plotted against the frequency change, the curve not only can show the magnitude of the modulus, but also can visually distinguish the elastic modulus and the viscous modulus of the rubber compound, and the performance of the rubber compound produced by using the rubber compound during calendering is deduced according to the minimum modulus and the corresponding frequency. The method provided by the application is simple to operate, high in sensitivity, accurate and reliable in test result and free of pollution to the environment.
Drawings
FIG. 1 is a graphical representation of the modulus G' as measured in a frequency sweep of the rubber mixtures according to the invention against frequency.
FIG. 2 is a graphical representation of the modulus G' measured in a time sweep of the rubber mixtures according to the application against time.
Detailed Description
The application provides a method for evaluating the processability of a rubber compound during steel wire calendering after the rubber compound is used for producing the rubber compound, which comprises the following steps:
(1) and taking the processing temperature of the raw rubber sample of the rubber compound as a testing temperature, selectively applying a corresponding strain value in the frequency range area, fixing the testing temperature and the strain value, and performing frequency scanning on the sample of the rubber compound by using a rubber processing analyzer.
(2) And plotting the relation between the modulus G 'measured at each frequency of the frequency scanning and the frequency to obtain a frequency-modulus curve, wherein the frequency is changed into an abscissa, and the modulus G' is an ordinate.
(3) And taking the minimum frequency corresponding to the minimum modulus G' value determined in the frequency-modulus curve as a fixed frequency, applying a corresponding strain value in the time range region, fixing the test temperature and the strain value, and performing time scanning on a sample of the rubber compound by using a rubber processing analyzer.
(4) Plotting the measured modulus G 'at each time of the time sweep versus time as abscissa and the modulus G' as ordinate yields a time-modulus curve.
(5) And the integral area in the time-modulus curve is used as a basis for judging the processability of the rubber compound during steel wire calendering after the rubber compound is produced, and the smaller the integral area is, the better the processability of the rubber compound after the rubber compound is produced during steel wire calendering is, and the roller is not easy to stick.
The present application generally determines the minimum frequency at the lowest modulus G' of a rubber mix sample, then fixes the frequency, time scans the rubber mix sample, and determines the integrated area. It is also preferred herein that the rubber mix sample is subjected to thin-pass homogenization and standing in sequence before determining the minimum frequency at the lowest modulus G' of the rubber mix sample. In the present application, the thin-pass homogenization is carried out on an open mill according to the method in GB/T15340-; the standing time is 8-24 h.
In the present application, the method of determining the integral area by fixing the frequency and time-scanning the rubber mix sample is preferably: fixing the test temperature, the test frequency and the test strain, performing time scanning on the raw rubber sample of the rubber compound by using a rubber processing analyzer, and determining the curve integral area of the raw rubber sample of the rubber compound according to the measured modulus G' at each time of the time scanning and the curve of the time. In the application, the test temperature is preferably the calendering temperature of the rubber compound, and the calendering temperature is generally 100-120 ℃, so that the test temperature can be selected within the temperature range, and specifically can be 100 ℃, 110 ℃ and 120 ℃; the test frequency is the minimum frequency determined according to a frequency-modulus curve; the test strain is 0.28% to 42%, preferably 0.28%. The rubber processing analyzer has no special requirement, and can be a rubber processing analyzer well known in the field, and in the specific embodiment of the application, the model of the rubber processing analyzer is RPA2000 (manufactured by alpha company, USA). The specific operation method of the frequency scanning is not particularly required in the present application, and a method well known to those skilled in the art can be adopted.
After the time scan is completed, the present application plots the measured modulus at each time in the time scan against time to obtain a time-modulus curve, with the time as the abscissa and the modulus G "as the ordinate. Scanning the natural rubber and the mixture thereof for time within the area of 0-26 min to obtain a time-modulus curve, and integrating the curve to obtain an integral area, wherein the method for the integral area of the curve comprises the following steps:
the method is characterized in that the method is a curve obtained by scanning different rubber compounds with time, and the integral area of the curve is used as a basis for judging the processability of the rubber compounds after the rubber compounds are used for producing the rubber compounds during steel wire calendering, and the smaller the integral area is, the better the processability of the rubber compounds after the rubber compounds are used for producing the rubber compounds during steel wire calendering is, and the roller adhesion is less.
The smaller the integral area is, the smaller the modulus of the rubber compound under time scanning is, the smallest modulus and frequency under frequency scanning are, the least molecular chain is tangled in the rubber compound, the molecular chain stretching can enable the polymer macromolecular chain to be oriented, the shear deformation on the surfaces of the roller and the steel wire can enable the dispersed phase of the macromolecular chain in the rubber compound to be distributed in a sheet shape, the viscosity of the dispersed phase is smaller than that of other rubbers, and therefore, after the rubber compound is produced by using the dispersed phase, the steel wire is pressed for delay, the processing performance is optimal, and the roller is not easy to stick.
The method for judging the processability of the rubber compound during steel wire calendering is simple to operate, high in sensitivity, accurate and reliable in test result and free of environmental pollution.
The method for determining the processability of the rubber composition during steel wire rolling after the composition is produced is described in detail below with reference to examples.
Example (b):
raw materials: import SVR3L (vietnam), import SVR10# (vietnam) mix a + ( harbor plant), import STR20# (tai) mix, import SVR10# (vietnam) mix a + (synthesis plant). Sequentially recording the four rubber compound rubbers as samples 1-4;
the dosage of raw materials is as follows: 20-30 g;
testing equipment: rubber processing analyzer (RPA2000, manufactured by American alpha company)
Judging the processability of the four rubber compounds during steel wire calendering, wherein the specific test method comprises the following steps:
(1) the four rubber compound samples were subjected to thin-pass homogenization on an open mill according to the method in GB/T15340-2008,
standing for 8h, and weighing a proper amount of sample for testing;
(2) setting the test temperature to be 120 ℃ and the strain to be 0.28%, respectively carrying out frequency scanning on the four samples, wherein the frequency range is 0-60 Hz, and the modulus G' under each frequency is measured and shown in figure 1. The minimum frequency corresponding to the minimum modulus G' is obtained from the frequency-modulus curve in fig. 1, and is listed in table 1.
TABLE 1 determination of minimum frequency after frequency scanning of four rubber compound samples
| Sample (I) | Minimum modulus G'/kPa | Minimum frequency/ |
| Sample | ||
| 1 | 44.82 | 0.02 |
| Sample 2 | 35.34 | 0.01 |
| Sample 3 | 44.04 | 0.02 |
| Sample No. 4 | 35.96 | 0.01 |
(3) Setting the test temperature to be 120 ℃, the strain to be 0.28 percent and the frequency to be 0.01Hz and 0.02Hz, respectively scanning the four samples for 0-26 min, and measuring the modulus G' at each time as shown in figure 2. The integrated area was obtained from the time-modulus curve in fig. 2, and is listed in table 2.
TABLE 2 integral area after time scanning of four rubber compound samples
| Sample (I) | |
| Sample | |
| 1 | 6621.822 |
| Sample 2 | 5282.762 |
| Sample 3 | 6590.361 |
| Sample No. 4 | 5767.499 |
As can be seen from FIG. 1, the trends of the curves of sample 1 and sample 3 are close to those of sample 2 and sample 4, and it is difficult to judge the processability of the rubber composition in steel wire calendering after the composition has been produced from the rubber composition based on the frequency-modulus relationship shown in FIG. 1.
The time sweep was therefore performed for the minimum frequency corresponding to the minimum modulus G' in fig. 1, resulting in a time-modulus curve, and it is noted in particular that the minimum frequency for each sample corresponds to the minimum frequency obtained according to fig. 1 when the time sweep for the minimum frequency was performed.
From fig. 2 and table 2, in terms of integral area, the ^ sample 2 < ^ sample 4 < ^ sample 3 < ^ sample 1 can be obtained. It can be seen that sample 2 produced the compound rubber with the best processability during steel wire calendering, the lowest internal modulus in a certain time, the lowest energy consumption for processing, and the difficulty in adhering to the roller during steel wire calendering.
A rubber compound is produced according to the mixture of the four natural rubbers, and steel wire calendering is carried out, so that the obtained result accords with the RPA test result.
The embodiment shows that the method provided by the application is simple to operate, high in sensitivity, accurate and reliable in test result and free of pollution to the environment.
The foregoing is only a preferred embodiment of the present application and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present application, and the improvements and modifications should also be within the scope of the present application.
Claims (7)
1. A method for evaluating the processability of rubber compound comprises the following steps:
1) taking the calendering processing temperature of the rubber compound as a testing temperature, fixing the testing temperature and strain in a frequency region, and performing frequency scanning on a raw rubber sample of the rubber compound by using a rubber processing analyzer;
2) plotting the modulus G' measured at each frequency scanned in the frequency region with the frequency as the abscissa of the curve to obtain a frequency-modulus curve;
3) determining the minimum frequency corresponding to the value of the lowest modulus G';
4) applying strain under the minimum frequency, fixing and testing temperature, frequency and strain, and scanning the rubber raw rubber sample in time by using a rubber processing analyzer;
5) plotting the measured modulus G '' at each time of the time scan against time to obtain a time-modulus curve, time being the abscissa of the curve and modulus G '' being the ordinate of the curve;
6) the integral area in the time-modulus curve is used as a basis for judging the processability of the rubber compound, and the smaller the integral area is, the better the processability of the rubber compound during steel wire calendering is, and the roller adhesion is difficult to occur.
2. The method of claim 1, further comprising sampling the raw rubber sample from the same location on the raw rubber block and standing for 1-2 hours prior to step 1).
3. A method of evaluating the processability of a rubber compound according to claim 1, wherein the test temperature in step 1) is 100 ℃, 110 ℃ or 120 ℃.
4. The method for evaluating the processability of a rubber compound according to claim 1, wherein the strain in step 1) is 0.28% to 42%, preferably 0.28%.
5. The method for evaluating the processability of a rubber compound according to claim 1, wherein the frequency region of the frequency sweep in step 1) is 0 to 60 HZ.
6. The method of claim 1, wherein the rubber processing analyzer is an RPA2000 rubber processing analyzer manufactured by alpha corporation, usa.
7. The method for evaluating the processability of a rubber compound as claimed in claim 1, wherein the time scanning is performed on the natural rubber and the mixture thereof for 0-26 min to obtain a time-modulus curve, and the integral area is obtained by integrating the curve, and the method of the integral area of the curve is as follows:
，
the curves are scanned over time for different rubber mixes.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114235607A (en) * | 2021-11-12 | 2022-03-25 | 中策橡胶集团股份有限公司 | Method and equipment for evaluating pre-crosslinking of carcass cord fabric rubber compound and computer readable carrier medium |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1041384A1 (en) * | 1999-03-29 | 2000-10-04 | PIRELLI PNEUMATICI Società per Azioni | Method for determining the behaviour of a viscoelastic material |
| US20140163906A1 (en) * | 2012-12-06 | 2014-06-12 | Sumitomo Rubber Industries, Ltd. | Method for estimating vulcanization degree of rubber compound |
| CN110596359A (en) * | 2019-10-15 | 2019-12-20 | 中国热带农业科学院农产品加工研究所 | Method for judging raw rubber processing performance of natural rubber |
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- 2020-11-02 CN CN202011201077.7A patent/CN112505313A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1041384A1 (en) * | 1999-03-29 | 2000-10-04 | PIRELLI PNEUMATICI Società per Azioni | Method for determining the behaviour of a viscoelastic material |
| US20140163906A1 (en) * | 2012-12-06 | 2014-06-12 | Sumitomo Rubber Industries, Ltd. | Method for estimating vulcanization degree of rubber compound |
| CN110596359A (en) * | 2019-10-15 | 2019-12-20 | 中国热带农业科学院农产品加工研究所 | Method for judging raw rubber processing performance of natural rubber |
Non-Patent Citations (4)
| Title |
|---|
| 《兵器工业科学技术辞典》编辑委员会: "《兵器工业科学技术辞典 火药与炸药》", 31 December 1991 * |
| ＪＯＨＮＳＤ等: "RPA2000橡胶加工性能分析仪的应用", 《橡胶工业》 * |
| 刘凤岐等: "《高分子物理》", 31 October 1995 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114235607A (en) * | 2021-11-12 | 2022-03-25 | 中策橡胶集团股份有限公司 | Method and equipment for evaluating pre-crosslinking of carcass cord fabric rubber compound and computer readable carrier medium |
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Address after: 310008 No. 1, No. 1 Street, Qiantang District, Hangzhou, Zhejiang Applicant after: Zhongce Rubber Group Co.,Ltd. Address before: No.2, 10th Street, Qiantang New District, Hangzhou, Zhejiang Province, 310008 Applicant before: ZHONGCE RUBBER GROUP Co.,Ltd. |
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