Low-temperature continuous synthesis method of rubber vulcanization accelerator NS

A rubber vulcanization and synthesis method technology, applied in the direction of organic chemistry, can solve the problems of high process risk, low yield of main product NS, and high difficulty in equipment manufacturing, so as to reduce the consumption of tert-butylamine, facilitate industrialization, and solve difficult wastewater treatment Effect

Pending Publication Date: 2020-02-11
SHANDONG YANGGU HUATAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the synthesis method in the prior art, there are still many technical problems: for example, the product quality obtained by using the sodium hypochlorite method to synthesize NS is good, but the saline waste water produced is difficult to handle; The yield of the main product NS is low and the product purity is poor. According to literature reports, the highest yield is only 90%; the product quality of the accelerator NS synthesized by the oxygen method is good, and the waste water does not contain salt, but the unreacted oxygen in the system is mixed with the steam of tert-butylamine Explosion is easy to occur in the end, the process is more dangerous, the process adopts high-pressure reaction, and the equipment manufacturing is difficult and expensive

Method used

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  • Low-temperature continuous synthesis method of rubber vulcanization accelerator NS
  • Low-temperature continuous synthesis method of rubber vulcanization accelerator NS
  • Low-temperature continuous synthesis method of rubber vulcanization accelerator NS

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Step 1: Add 50g of rubber vulcanization accelerator M and 198g of rubber vulcanization accelerator DM into the reaction kettle, add 1000g of water into the kettle, start stirring at a speed of 300r / min, and weigh the 500g of good tert-butylamine is slowly added dropwise into the reaction kettle, and the dropping time is 30min;

[0029] Step 2: After the dropwise addition, control the switch valve of the condensing circulating water to control the temperature in the reactor at 5°C, and start slowly feeding in 123.1g of air at a rate of 3.18L / min to carry out the oxidation reaction, the reaction time For 30 minutes, take a sample to detect whether the product has reached the reaction end point, and test the purity by high performance liquid chromatography. The purity > 96% means that the reaction end point is reached; the purity detected by high performance liquid chromatography is 95.5%. Chromatography test purity is 97.5%;

[0030] Step 3: Filter, wash and dry the reac...

Embodiment 2

[0034] Step 1: Add 100g of rubber vulcanization accelerator and 99.4g of rubber vulcanization accelerator DM into the reaction kettle, add 1000g of water into the kettle, start stirring at a speed of 350r / min, after the materials in the kettle are mixed evenly, weigh A good 500g of tert-butylamine is slowly added dropwise into the reaction kettle, and the dropping time is 30min:;

[0035] Step 2: After the dropwise addition, control the switch valve of the condensing circulating water to control the temperature in the reactor at 10°C, and start to slowly introduce 98.84g of air at a rate of 2.19L / min to carry out the oxidation reaction. The reaction time It was 35min, and the purity of the sample was 98.5% by high performance liquid chromatography;

[0036] Step 3: Filter, wash and dry the reactant obtained in step 2 to obtain the NS product and mother liquor of the accelerator of the present invention. The obtained NS product has an average purity of 99.2%, and an average yi...

Embodiment 3

[0040] Step 1: Put 100g of rubber vulcanization accelerator M and 66.27g of rubber vulcanization accelerator DM into the reaction kettle, add Example 2 to the kettle to obtain 1000g of mother liquor, start stirring at a speed of 200r / min, and wait until the materials in the kettle are mixed evenly , slowly drop 500g of tert-butylamine weighed into the reaction kettle, and the dropping time is 27min;

[0041] Step 2: After the dropwise addition, control the switch valve of the condensing circulating water to control the temperature in the reactor at 8°C, and start slowly introducing 68.68g of air at a rate of 1.83L / min to carry out the oxidation reaction. For 40min, sampling with high performance liquid chromatography test purity is 98.3%;

[0042] Step 3: Filter, wash and dry the reactant obtained in step 2 to obtain the NS product and mother liquor of the accelerator of the present invention. The average purity of the obtained NS product was 99.1%, and the average yield was ...

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Abstract

The invention provides a low-temperature continuous synthesis method of a rubber vulcanization accelerator NS. The low-temperature continuous synthesis method comprises the following steps: 1, addinga rubber vulcanization accelerator M and a rubber vulcanization accelerator DM into a reaction kettle, adding water, carrying out stirring, and slowly dropwise adding tert-butylamine within 30 min; 2,reducing the temperature of a reaction system in the step 1 to -10 to 40 DEG C, introducing air or compressed air within 10 to 50 min for a reaction, and carrying out sampling to detect the reactionendpoint of the product; and 3, filtering, washing and drying the product obtained in the step 2 to obtain the finished product N-tert-butyl-2-benzothiazole sulfenamide, and recycling mother liquor. According to the method, the lowest reaction temperature can reach -10 DEG C, and reaction time reaches 40-80 min; air / compressed air is used as an oxidizing agent, so production process is safe, and salt-containing wastewater cannot be generated; and the amount of byproducts contained in the mother liquor is low, and the mother liquor can be recycled without treatment of other process steps such as evaporation.

Description

technical field [0001] The invention relates to the technical field of rubber vulcanization accelerators, in particular to a low-temperature continuous synthesis method of rubber vulcanization accelerator NS. Background technique [0002] Rubber vulcanization accelerator NS (or 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 and It has two advantages of fast vulcanization speed. It is used in the production of rubber products such as natural rubber, styrene-butadiene rubber, butadiene rubber, and isoprene rubber. Its activity is greater than that of the currently used accelerators CBS and NOBS. [0003] The main method of synthesizing the rubber vulcanization accelerator NS is to use the accelerator M as the raw material and oxidize it with an oxidizing agent. The commonly used oxidizing agents include sodium hypochlorite, hydrogen peroxide, oxyge...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/80
CPCC07D277/80
Inventor 宋彦哲杜丽丽韩涛宋来崇王克军
Owner SHANDONG YANGGU HUATAI CHEM
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