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Testing method for detecting activity of vulcanizing activator

A technology of vulcanization activator and testing method, which is applied in the field of analysis and testing, can solve the problems of exothermic reaction that no one has done before, and achieve the effects of fast testing speed, simple testing method and small sample consumption

Inactive Publication Date: 2016-08-10
BEIJING RED AVENUE INNOVA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using squalene as a natural rubber model to study the reaction exotherm in the rubber vulcanization process by DSC has not yet been carried out

Method used

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  • Testing method for detecting activity of vulcanizing activator
  • Testing method for detecting activity of vulcanizing activator
  • Testing method for detecting activity of vulcanizing activator

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Weigh 40.0 mg of HTS sample and add to an agate mortar. Then add 18.9mg of zinc stearate, fully grind HTS and zinc stearate (grind for about 5 minutes), and mix them evenly. Finally, 400 mg of squalene was added, and then fully ground (for about 5 minutes) to mix the samples evenly.

[0038]Weigh two crucibles of similar weight, one empty crucible as a reference crucible and one as a sample crucible. Weigh 5.0 mg of the sample prepared above and add it into the sample crucible. Put the reference crucible and sample crucible into the DSC instrument. Nitrogen gas at a flow rate of 50 ml / min was introduced into the DSC. The DSC test conditions are set at a heating rate of 5°C / min, and the temperature range is 80°C to 160°C.

[0039] The measured DSC spectrum is shown in the accompanying drawing, figure 1 .

Embodiment 2～5

[0041] The sample preparation method and DSC test conditions are the same as in Example 1, except for the type and amount of the vulcanization activator. The specific formula is shown in Table 1.

[0042] Table 1 Example 2-5 sample preparation formula

[0043]

[0044]

[0045] Table 2 embodiment 1-5 exothermic temperature

[0046]

120℃~130℃ Maximum exothermic temperature, ℃

Example 1

128.2

Example 2

126.2

Example 3

121.5

Example 4

120.2

Example 5

121.5

[0047] figure 1 For adopting the test result of DSC test embodiment 1~5 sample, wherein upward peak is exothermic peak, and downward peak is endothermic peak, these five samples of embodiment 1~5 all have very high temperature at 120 ℃~130 ℃. Sharp exothermic peak, which is the exothermic peak when Duralink HTS cross-links with squalene, and its maximum exothermic peak temperature is shown in Table 2.

[0048] The metal content of the activators u...

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Abstract

The invention provides a testing method for detecting activity of a vulcanizing activator. The testing method comprises the following steps: step 1, preparation of a sample: weighing an organic thiosulfate sample, adding the organic thiosulfate sample into a mortar, adding the vulcanizing activator, then adding squalene and carrying out adequate grinding so as to realize uniform mixing of the sample; step 2, differential scanning calorimetric (DSC) testing; and step 3, analysis of a DSC pattern: finding out exothermic peaks in the DSC pattern and marking temperature or time corresponding to a maximum exothermic peak. Compared with conventional methods which carry out physical property testing after mixing of natural rubber, the testing method employing DSC to testing exothermic conditions of reactions with squalene as a natural rubber analogue in the invention has the following obvious advantages: consumption of the sample is small; sample preparation is simple; and the testing method is simple and is rapid in testing speed. Meanwhile, test results of the testing method and the results of physical property testing after natural rubber mixing can confirm each other; and the testing method can prejudge the results of physical property testing after natural rubber mixing and enables physical property testing to be more targeted.

Description

technical field [0001] The invention belongs to the field of analysis and testing, in particular to a rubber testing method by means of differential scanning calorimetry analysis. Background technique [0002] Natural rubber is a natural polymer compound with polyisoprene as the main component, and its molecular formula is (C 5 h 8 )n, is unsaturated rubber, which is easy to vulcanize with vulcanizing agent, oxidize and crack with peroxide, oxygen and ozone, and have halogenation with halogen. However, since the structure of natural rubber is a macromolecular chain structure, the order of magnitude of the average molecular weight is 10 6 , therefore, the above reactions are difficult to track and detect. Chain triterpenoid squalene C 30 h 50 (Also known as squalene, squalene, tricosahexaene, squalene or cod liver oil terpene, etc.) is a colorless oily liquid with a pleasant smell, and becomes viscous like linseed oil after oxygen absorption. The melting point is -75°C,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N25/20
CPCG01N25/20
Inventor 刘哲甄博鸣姚居峰赵丽丽董栋
Owner BEIJING RED AVENUE INNOVA
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