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Method for preparing rubber accelerator NS and rubber accelerator NS

A rubber accelerator and accelerator technology are applied in the field of rubber accelerator preparation, which can solve the problems of unsuitable conversion of intermediate products, consumption of large oxidants, affecting product quality, etc., so as to improve reaction efficiency, product yield, and reaction yield. , The effect of low comprehensive production cost

Active Publication Date: 2021-05-04
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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  • Method for preparing rubber accelerator NS and rubber accelerator NS
  • Method for preparing rubber accelerator NS and rubber accelerator NS
  • Method for preparing rubber accelerator NS and rubber accelerator NS

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Add 34.4g (0.2mol) of accelerator M, 0.35g of neodecanoin glyceride, 167g (2.3mol) of tert-butylamine, and 0.2g of lanthanum oxide into a 500ml reaction flask equipped with a stirring device, a thermometer and a reflux condenser, and stir evenly; Add 32.9g (0.29mol) of 30% concentration of hydrogen peroxide to the reaction vessel at a constant speed by the peristaltic pump, and control the reaction temperature at 35°C; add the hydrogen peroxide dropwise for 90 minutes, continue the reaction for 30 minutes after the addition, and cool down to 30°C for distillation under reduced pressure after the reaction. To obtain the recovered solution of tert-butylamine, add 170g of distilled water to the remaining material, cool down to 25°C, settle and filter, and recycle the filtrate as the sedimentation liquid in the experiment again. The product is dried in an oven at 45°C for 12 hours to obtain 45.3g of white granular NS product. The yield was 92.9%, the initial melting point wa...

Embodiment 2-6

[0044] Under the premise of not changing the amount of accelerator M, change the addition amount and type of raw materials (tert-butylamine, catalyst, hydrogen peroxide), and reaction conditions such as time and temperature, and repeat the preparation process of the accelerator in Example 1. See Table 2 below for specific data.

[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 Catalyst type Yttrium oxide + Praseodymium chloride Dysprosium chloride scandium sulfate Praseodymium chloride Samarium nitrate Catalyst dosage (g) 0.05+0.10 0.05 0.8 0.3 0.5 Reaction temperature (°C) 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 (°C) 108.8 108.6 107.9 ...

Embodiment 7

[0047] Example 7 Pilot Scale-up Experiment

[0048] Add 3440g (20mol) of accelerator M, 30g of sodium dodecylbenzenesulfonate, 10200g (140mol) of tert-butylamine, and 60g of samarium nitrate into a 50L pilot test reactor equipped with a stirring device, a thermometer and a reflux condenser, and stir evenly Add 1632g (24mol) of 50% concentration of hydrogen peroxide into the reaction vessel at a constant speed by the peristaltic pump, and control the reaction temperature at 33°C; add the hydrogen peroxide dropwise for 120min, continue the reaction for 30min after the dropwise addition, and cool down to 30°C for distillation under reduced pressure after the end of the reaction to obtain For the tert-butylamine recovery solution, add 15000g of distilled water to the remaining material, cool down to 20°C, settle, filter, and dry the product at 45°C for 12h to obtain 4650g of white granular NS product with a yield of 95.4%. The initial melting point of the melting point tester is 10...

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Abstract

The invention relates to a method for preparing a rubber accelerator NS and the rubber accelerator NS in the field of preparation of rubber accelerators. The method comprises the following steps: a, oxidation process: dropwise adding hydrogen peroxide into a reaction raw material for oxidation until the reaction is finished to obtain a material, wherein the reaction raw materials comprise an accelerant M, tert-butylamine and a rare earth compound catalyst; b, post-treatment of reactants: treating and recycling the materials to obtain tert-butylamine; and treating residual materials to obtain the finished product of the accelerator NS. The molar ratio of the accelerant M to the tert-butylamine to the hydrogen peroxide is 1:(5-15):(1-2); according to the method, except for hydrogen peroxide participating in the reaction, no water or organic solvent is added, so that the reaction efficiency can be effectively improved; and the rare earth compound with high activity and high selectivity is selected as the catalyst, the product is high in purity and good in color, almost no by-product or wastewater is generated, and 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 accelerator NS and the rubber accelerator NS. Background technique [0002] As we all know, in rubber processing, vulcanization accelerators are substances used to reduce the vulcanization temperature, shorten the vulcanization time, reduce the amount of vulcanizing agent, and improve the physical and mechanical properties of vulcanized rubber. 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 toxicity of raw materials. [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 anti-scorch properties, With the characteristics of fast vulcanization s...

Claims

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Application Information

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Patent Type & Authority Applications(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