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Method for increasing yield of rubber accelerator TBBS

A technology of rubber accelerator and accelerator, which is applied in the field of improving the yield of rubber accelerator TBBS, can solve problems such as unfound methods, and achieve the effects of improving product purity, increasing reaction contact rate, and reducing usage

Active Publication Date: 2019-12-17
SHANDONG SUNSINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the highest yield of TBBS synthesized by sodium hypochlorite oxidation method can only reach 93%. For many years, researchers have devoted themselves to improving the yield of TBBS, but still have not found a suitable method.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1 A kind of method that adds salt and tensio-active agent improves rubber accelerator TBBS yield:

[0026] Add 42g accelerator MBT, 0.1g sodium dodecylbenzenesulfonate, 10g industrial sodium chloride, and 100ml water to a three-necked flask equipped with a stirrer, a thermometer, and a water bath, and start stirring at a speed of 90 rpm. After 30 minutes, slowly add 60ml of tert-butylamine and stir for 10 minutes. At the temperature t=25-35°C, add sodium hypochlorite with an available chlorine content of 15-20g / ml dropwise, and use starch-potassium iodide-ammonium sulfate indicator near the end Carry out end-point detection, the blue-black color is the end point, stop the reaction, filter, wash with water, and dry to obtain 58.47g rubber accelerator TBBS product, the yield reaches 97.7%, and the melting point reaches 106.5°C.

Embodiment 2

[0027] Embodiment 2 A kind of method that adds salt and tensio-active agent improves rubber accelerator TBBS yield:

[0028] Add 42g accelerator MBT, 0.1g sodium dodecylbenzenesulfonate, 10g industrial sodium chloride, and 100ml water to a three-necked flask equipped with a stirrer, a thermometer, and a water bath, and start stirring at a speed of 90 rpm. For 30 minutes, slowly add 58ml of tert-butylamine mother liquor and 42ml of neo-tert-butylamine obtained in Example 1, stir for 10 minutes, and when the temperature t=25-35°C, dropwise add sodium hypochlorite with an available chlorine content of 15-20g / ml to it, approaching the end When using starch-potassium iodide-ammonium sulfate indicator to detect the end point, the end point is blue and black, stop the reaction, filter, wash, and dry to obtain 58.12g rubber accelerator TBBS product, the yield reaches 97.1%, and the melting point reaches 106.9°C.

Embodiment 3

[0029] Embodiment 3 A kind of method that adds salt and tensio-active agent improves rubber accelerator TBBS yield:

[0030] Add 42g accelerator MBT, 0.1g sodium dodecylbenzenesulfonate, 10g industrial sodium chloride, and 100ml water to a three-necked flask equipped with a stirrer, a thermometer, and a water bath, and start stirring at a speed of 90 rpm. For 30 minutes, slowly add 72ml of the tert-butylamine mother liquor obtained in Example 2 and 28ml of neo-tert-butylamine, stir for 10 minutes, and when the temperature t=25-35°C, dropwise add sodium hypochlorite with an available chlorine content of 15-20g / ml to it, approaching the end When using starch-potassium iodide-ammonium sulfate indicator to detect the end point, the end point is blue and black, stop the reaction, filter, wash, and dry to obtain 57.59g of rubber accelerator TBBS product, the yield reaches 96.20%, and the melting point reaches 106.7°C.

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Abstract

The invention discloses a method for increasing the yield of the rubber accelerator TBBS, belonging to the field of fine chemical engineering. According to the invention, the accelerator MBT, tert-butylamine and sodium hypochlorite are used as raw materials, water is used as a medium, and sodium chloride and sodium dodecyl benzene sulfonate are added into a reaction system to synthesize the rubberaccelerator TBBS. The dispersion degree of MBT particles in water is increased by utilizing the dispersion effect of the surfactant, and after tert-butylamine is added, the contact surface of the MBTparticles and the tert-butylamine is increased, so the synthesis rate of an M-amine salt is increased; and since NaCl is added to increase the polarity of a reaction environment, the M-amine salt isbetter dissolved in the polar environment, is in full contact with sodium hypochlorite molecules and fully participates in the reaction, so a conversion rate is increased, and the consumption of tert-butylamine is reduced. NaCl and the surfactant sodium dodecyl benzene sulfonate are added, so product yield is greatly improved and is 96% or above; and meanwhile, the synthesized material is white inappearance, high in melting point and high in purity.

Description

technical field [0001] The invention relates to the field of fine chemical industry, in particular to a method for increasing the yield of rubber accelerator TBBS. Background technique [0002] Vulcanization accelerator TBBS, chemical name N-tert-butyl-2-benzothiazole sulfenamide, is used as an aftereffect vulcanization accelerator for natural rubber and triene synthetic rubber. [0003] Vulcanization accelerator TBBS is a post-effect vulcanization accelerator with safe operation at high temperature, good scorch performance and high elongation strength. It conforms to the concept of green development in the vulcanization process of accelerator rubber, and is called "standard accelerator". Accelerator TBBS is used more and more, and has a very broad development prospect. [0004] At present, the method for synthesizing TBBS is mainly the sodium hypochlorite oxidation method, and the process is relatively perfect. The highest yield of TBBS synthesized by this method can only...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/80
CPCC07D277/80
Inventor 刘园园张颂吕桂中
Owner SHANDONG SUNSINE CHEM
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