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A technology of bisimide and vulcanizing agent is applied in the field of analysis and testing, which can solve the problems of complex vulcanization reaction, and achieve the effects of simple sample preparation, fast testing speed and small sample consumption.
Active Publication Date: 2016-08-17
BEIJING RED AVENUE INNOVA
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Problems solved by technology
In the NR compound of the sulfur vulcanization system containing PDM, the vulcanization reaction is extremely complicated
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Embodiment 1
[0036] A 20.0 mg sample of 1,3-(citraconimidomethyl)benzene (Perkalink 900) was weighed and added to an agate mortar. Then add 2.0 mg of zinc oxide, 1.0 mg of stearic acid, 1.0 mg of sulfur, and 4.0 mg of vulcanization accelerator NS, and grind the above solids thoroughly to make them evenly mixed.
[0037] Weigh two crucibles of similar weight, one 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 100°C to 200°C.
[0038] The measured DSC spectrum is shown in the accompanying drawing, figure 1 .
Embodiment 2、3
[0040] Sample preparation method and DSC test conditions are the same as in Example 1, and the specific sample preparation formula is shown in Table 1
[0041] Table 1 Example 2~3 sample preparation formula (consumption of each component: mg)
[0042] Example 2 Example 3 1,6-Bismaleimidohexane (BMH) 20.0 N, N'-m-phenylene bismaleimide (PDM) 20.0 Zinc oxide 2.0 2.0 stearic acid 1.0 1.0 sulfur 1.0 1.0 Vulcanization accelerator NS 4.0 4.0
[0043] Table 2 Maximum exothermic peak temperature
[0044] exothermic peak, ℃ Exothermic peak area, J / g Example 1 151.0 22.14 Example 2 148.6 192.05 Example 3 170.2 176.13
[0045] figure 1 And in table 2, it can be seen that embodiment 1, 2, 3 all have reaction exothermic peaks, illustrate that they all can react with sulfur. Embodiment 1, 2 reaction exothermic temperature is lower, and their activity with sulfur reaction is higher, reacts...
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Abstract
The invention discloses a method for testing a bisimide vulcanizing agent. A structure of the bisimide vulcanizing agent is as shown in a formula (I). According to the testing method, the reaction exothermal condition of a bisimide compound and sulphur under the action of a vulcanization activator zinc oxide, stearic acid and a vulcanization accelerator is tested by differential scanning calorimetry. By comparing the highest exothermal temperatures of reaction exothermal peaks and peak areas of the exothermal peaks, reactivity and reaction degrees of the bisimide vulcanizing agents with different structures can be distinguished, and anti-reversion behaviors of the substances after rubber reversion can be further speculated. With reference to the chemical formula in the description, R1 is selected from straight-chain alkylidene of which the carbon atom number is 1 to 10, alkylidene with a branched chain, of which the carbon atom number is 2 to 10, and alkaryl or aralkyl of which the carbon atom number is 7 to 20; R2, R3, R4 and R5 are the same or different, and are respectively and independently selected from one of hydrogen, carboxyl, aldehyde, alkyl with a straight chain or a branched chain, of which the carbon atom number is 1 to 5, and aryl of which the carbon atom number is 6 to 20.
Description
technical field [0001] The invention belongs to the field of analysis and testing, and in particular relates to a method for analyzing the chemical activity of bisimide vulcanizing agents by testing the heat absorption and exothermic reaction between bisimide vulcanizing agents and sulfur by means of differential scanning calorimetry. Background technique [0002] The vulcanization process of natural rubber is a very complex multi-chemical reaction, including the interaction between vulcanization activator, vulcanization accelerator, sulfur, the interaction between rubber macromolecules and sulfur, the interaction between rubber macromolecules and cross-linking bonds. Shortening, rearrangement, cleavage, main chain modification and other reactions occurred. Under the action of sulfur vulcanization system, the crosslinking network of vulcanizate is dominated by polysulfide crosslinking bonds. [0003] One of the main reasons for vulcanization reversion of natural rubber is t...
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