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A kind of method for preparing rubber accelerator ns and rubber accelerator ns

A technology of rubber accelerator and accelerator, which is applied in the field of rubber accelerator preparation, can solve the problems of unsuitable conversion of intermediate products, consumption of large oxidant, and influence on product quality, so as to improve reaction efficiency and product yield, and increase reaction yield , the effect of low comprehensive production cost

Active Publication Date: 2022-06-24
BEIJING RED AVENUE INNOVA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, according to several patents, at the beginning of the experiment, the mass ratio of accelerator M to water was mostly around 1:10. On the one hand, the materials involved in the reaction were insufficient, and the amount of NS that could be generated in each reaction was not much, and most of them were water; On the other hand, in this reaction, tert-butylamine and M will react preferentially to obtain the intermediate product ammonium salt, which is easily soluble in water, but the product NS is insoluble in water. Due to the existence of a large amount of water, the intermediate product is not suitable for conversion, so it must consume a large amount of Oxidants, causing peroxidation, and the production of by-products of associated resins, even need to add a decoking agent to solve the problem, which will affect the quality of the product, and at the same time, the conversion rate of NS will also decrease

Method used

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  • A kind of method for preparing rubber accelerator ns and rubber accelerator ns
  • A kind of method for preparing rubber accelerator ns and rubber accelerator ns
  • A kind of method for preparing rubber accelerator ns and rubber accelerator ns

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Add accelerator M 34.4g (0.2mol), neodecanoic acid glyceride 0.35g, tert-butylamine 167g (2.3mol), lanthanum oxide 0.2g into the 500ml reaction flask equipped with stirring device, thermometer and reflux condenser, stir well; The peristaltic pump uniformly added 32.9 g (0.29 mol) of hydrogen peroxide with a concentration of 30% to the reaction vessel, and the reaction temperature was controlled to 35 ° C; the hydrogen peroxide was added dropwise for 90 min, and the reaction was continued for 30 min after the dropwise addition. To obtain the tert-butylamine recovery solution, add 170 g of distilled water to the remaining material, cool down to 25 °C, settle, filter, and recycle the filtrate as a sedimentation solution in the experiment again. The yield is 92.9%, the initial melting point measured by the melting point tester is 107.9°C, and the product is detected by liquid chromatography HPLC, and the purity is 99.2%.

Embodiment 2-6

[0044] Under the premise of not changing the consumption of accelerator M, the addition amount and type of raw materials (tert-butylamine, catalyst, hydrogen peroxide), and reaction conditions such as time and temperature were changed, and the preparation process of accelerator in Example 1 was repeated. The specific data are shown in Table 2 below.

[0045] Table 2

[0046] Example Example 2 Example 3 Example 4 Example 5 Example 6 tert-Butylamine(mol) 1.05 2.6 1.5 1.8 2.0 Hydrogen peroxide (mol) 0.4 0.22 0.25 0.30 0.33 Type of catalyst Yttrium oxide + praseodymium chloride Dysprosium chloride scandium sulfate praseodymium chloride Samarium nitrate Amount of catalyst (g) 0.05+0.10 0.05 0.8 0.3 0.5 Reaction temperature (℃) 40 50 38 30 43 Dropping time (min) 135 120 60 90 100 NS yield (g) 46.0 44.7 46.8 45.1 43.6 NS yield (%) 94.4 91.7 96.0 92.5 89.5 Initial melting point ...

Embodiment 7

[0047] Example 7 Pilot scale-up experiment

[0048] Accelerator M 3440g (20mol), sodium dodecylbenzene sulfonate 30g, tert-butylamine 10200g (140mol), samarium nitrate 60g are added in the pilot-scale reaction kettle of 50L equipped with stirring device, thermometer and reflux condenser, stir well The peristaltic pump uniformly adds 50% concentration of hydrogen peroxide 1632g (24mol) in the reaction vessel, and controls the reaction temperature to 33 ℃; Hydrogen peroxide is added dropwise for 120min, and the dropwise addition is continued for 30min after the completion of the reaction. In the tert-butylamine recovery solution, 15000g of distilled water was added to the remaining material, cooled to 20°C, sedimentation, filtration, and the product was dried at 45°C for 12 hours to obtain 4650g of white granular product NS product, the yield was 95.4%, and the initial melting point measured by the melting point tester was 108.2 ℃, the product was detected by liquid chromatograp...

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Abstract

The invention relates to a method for preparing rubber accelerator NS and the rubber accelerator NS in the field of rubber accelerator preparation. The method comprises the following steps: a. Oxidation process: Add hydrogen peroxide dropwise to the reaction raw material to oxidize until the end of the reaction to obtain a material; the reaction raw material includes a promoter M, tert-butylamine, and a rare earth compound catalyst; b. Post-treatment of the reactant: Recycle the material to obtain tert-butylamine; process the remaining material to obtain the finished accelerator NS. The molar ratio of the accelerator M, tert-butylamine, and hydrogen peroxide is 1: (5-15): (1-2); except for the hydrogen peroxide participating in the reaction, the method does not add water and organic solvents, which can effectively improve the reaction efficiency; The rare earth compound with high activity and high selectivity is used as the catalyst, the product has high purity, good color, almost no by-products and waste water are generated, the process is simple, clean and environmentally friendly.

Description

technical field [0001] The invention relates to the field of preparation of rubber accelerators, in particular to a method for preparing rubber accelerators NS and the rubber accelerators NS. Background technique [0002] As we all know, in rubber processing, vulcanization accelerator is used to reduce the vulcanization temperature, shorten the vulcanization time, reduce the amount of vulcanizing agent, and improve the physical and mechanical properties of the vulcanizate. At present, with the improvement of people's awareness of environmental safety and labor safety, while paying attention to the application effect, they also pay more attention to the problem of raw material toxicity. [0003] Rubber vulcanization accelerator NS (also known as TBBS), the chemical name is N-tert-butyl-2-benzothiazole sulfenamide, is one of the important varieties of sulfenamide vulcanization accelerators, and has both scorch resistance, With the characteristics of fast vulcanization and env...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D277/80
CPCC07D277/80
Inventor 张洁阮振刚胡小娜张成董栋张宁
Owner BEIJING RED AVENUE INNOVA
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