Preparation method of novel antioxidant for high-temperature rubber

An antioxidant and high-temperature technology, which is applied in the field of preparation of new high-temperature rubber antioxidants, can solve the problems of weakening the effect of alkylated diphenylamine, compatibility and adverse effects of volatility, and achieve tensile strength and fracture High elongation retention rate, shorten synthesis time, improve formation speed and effect

Inactive Publication Date: 2019-03-19
中广核高新核材科技(苏州)有限公司
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Problems solved by technology

The mass fraction of nitrogen in alkylated diphenylamine is generally 2% to 6%. If the nitrogen content is too low, the effect of alkylated diphenylamine will be weakened. If the nitrogen content is too high, the compatibility of alkylated diphenylamine in lubricating oil will be affected. Sexuality and volatility adversely affect

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  • Preparation method of novel antioxidant for high-temperature rubber

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Effect test

Embodiment 1

[0042] Embodiment 1: a kind of preparation method of novel high temperature rubber antioxidant, comprises the following steps:

[0043] Step 1. Add 5mmol ZrCL4, 5mmol terephthalic acid, 0.8ml concentrated HCL (37%) to 30mLN ， In N-dimethylformamide;

[0044] Step 2. After dissolving, add 5mL of deionized water dissolved with a certain amount of CA (citric acid) and CTAB (cetyltrimethylammonium bromide) into the above solution, mix well and transfer to a tank equipped with PTFE. Crystallize at 120°C for 24 hours in an ethylene-lined autoclave;

[0045] Step 3, after the reaction kettle is cooled to room temperature, the white colloidal product obtained is sprayed with N ， N-dimethylformamide solution and methanol solution were washed three times respectively, and then refluxed with methanol at 70° C. for 4 h;

[0046] Step 4. Transfer the sample to a constant temperature oven and dry it overnight.

Embodiment 2

[0047] Embodiment 2: a kind of preparation method of novel high-temperature rubber antioxidant, comprises the following steps:

[0048] Step 1. Add 10mmol ZrCL4, 10mmol terephthalic acid, 1.6ml concentrated HCL (37%) to 30mLN ， In N-dimethylformamide;

[0049] Step 2. After dissolving, add 5mL of deionized water dissolved with a certain amount of CA (citric acid) and CTAB (cetyltrimethylammonium bromide) into the above solution, mix well and transfer to a tank equipped with PTFE. Crystallize at 120°C for 24 hours in an ethylene-lined autoclave;

[0050] Step 3, after the reaction kettle is cooled to room temperature, the white colloidal product obtained is sprayed with N ， N-dimethylformamide solution and methanol solution were washed three times respectively, and then refluxed with methanol at 70° C. for 4 h;

[0051] Step 4. Transfer the sample to a constant temperature oven and dry it overnight.

Embodiment 3

[0052] Embodiment 3: a kind of preparation method of novel high temperature rubber antioxidant, comprises the following steps:

[0053] Step 1. Add 5mmol ZrCL4, 5mmol terephthalic acid, 0.8ml concentrated HCL (37%) to 30mLN ， In N-dimethylformamide;

[0054] Step 2. After dissolving, add 10mL of deionized water dissolved with a certain amount of CA (citric acid) and CTAB (cetyltrimethylammonium bromide) into the above solution, mix evenly and transfer to a tank equipped with PTFE. Crystallize at 120°C for 24 hours in an ethylene-lined autoclave;

[0055] Step 3, after the reaction kettle is cooled to room temperature, the white colloidal product obtained is sprayed with N ， N-dimethylformamide solution and methanol solution were washed three times respectively, and then refluxed with methanol at 70° C. for 4 h;

[0056] Step 4. Transfer the sample to a constant temperature oven and dry it overnight.

[0057] The TGA spectra of the novel antioxidants for high-temperature ru...

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Abstract

The invention discloses a preparation method of a novel antioxidant for high-temperature rubber. The preparation method comprises the following steps: dissolving zirconium tetrachloride and terephthalic acid, adding an acid solution, and pouring the solution into N,N-dimethylformamide; after dissolving, adding deionized water dissolved with a certain amount of citric acid and a certain amount of cetyl trimethyl ammonium bromide into the solution, uniformly mixing, transferring the solution into a high-pressure reaction kettle provided with a polytetrafluoroethylene liner, and crystallizing at120 DEG C; and after the reaction kettle is cooled to the room temperature, respectively repeatedly washing an obtained white colloidal product with an N,N-dimethylformamide solution and a methanol solution for several times, and carrying out reflux at 70 DEG C by virtue of methanol; and transferring the sample into a 100-DEG C constant temperature oven, and drying for one night, so as to obtain the antioxidant. The prepared novel antioxidant has the beneficial effects that the tensile strength and elongation at break after high-temperature thermo-oxidative aging are high, the heat resistanceis obviously increased, and the aging of silicone rubber is effectively inhibited.

Description

technical field [0001] The invention relates to the technical field of high-temperature resistant antioxidants, in particular to a preparation method of a novel high-temperature rubber antioxidant. Background technique [0002] Asia is the fastest growing region in the world for plastic production and consumption, with an average annual growth rate of double digits, and the production and demand for natural antioxidants are also increasing rapidly. Manufacturers are mainly concentrated in China, South Korea, Taiwan and Japan. Miaochun Company in Taiwan, China has a 7000t / a device, plus other small factories, the production capacity is about 10,000 t / a; the production capacity of mainland China is about 37,000 t / a; the production capacity of South Korea is about 10,000 t / a a; Japan's production capacity is about 7000t / a; Asia's production capacity is about 67,000t / a, and the output in 2002 is about 43,000t. [0003] The thermal oxidation process of organic compounds is a se...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L83/04C08L87/00C08G83/00
CPCC08G83/008C08L83/04C08L2201/08C08L87/00
Inventor 徐思奕
Owner 中广核高新核材科技(苏州)有限公司
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