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Method for directly synthesizing rubber vulcanization accelerator TBBS from resin in waste water

A vulcanization accelerator, synthetic rubber technology, applied in the direction of organic chemistry, etc., can solve the problems of affecting the heat exchange efficiency of the cooling process, blockage of pipes, high COD treatment of wastewater, etc., to save the process of high temperature solvent dissolution and sedimentation, and reduce the difficulty of wastewater treatment. , The effect of reducing COD in wastewater

Inactive Publication Date: 2019-01-11
KEMAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is very troublesome. Firstly, the resin recovered from TBBS wastewater is heating up. The solubility in these solvents is very small, and the dissolution process takes a long time, and after high temperature dissolution, it becomes a sticky liquid-solid mixture. It is more complicated to filter. Filtration and centrifugal drying are easy to block the pores of the filter cloth and filter screen. Generally, it needs to be placed in a settling tank, and the upper layer solution is extracted after cooling down and settling. However, even in this way, a part of the floating viscous resin will enter the pipeline, and it will precipitate and block the pipeline for a long time.
Moreover, the material obtained in this way is relatively sticky, hanging on the surface of equipment and pipes, affecting the heat transfer efficiency of the cooling process, requiring more heat and regular cleaning, usually at least once a week
The material of the MBT purity 85% that obtains then is by beating, then adds a large amount of tertiary butylamines, by dripping hyposodium or hydrogen peroxide oxidation synthetic accelerator TBBS, the yield of this method is very low only about 90% (according to MBT conversion), the waste water COD high processing complex

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1: a kind of method that resin directly synthesizes rubber vulcanization accelerator TBBS in waste water, comprises the following steps:

[0022] 1) At room temperature, mix the resin with 32% NaOH aqueous solution at a mass ratio of 1:1 to prepare the M-Na salt solution evenly. The mixing temperature is 50°C, the configuration time is 2h, and the upper layer M-Na salt is extracted by sedimentation The solution is ready for use;

[0023] 2) 1.5 parts by weight of tert-butylamine and 2 parts by weight of water are put into the reactor, and stirred evenly to obtain an aqueous solution of tert-butylamine;

[0024] 3) 2 parts by weight of M-Na salt, 1.5 parts by weight of hydrochloric acid and 2.5 parts by weight of oxidant sodium hypochlorite obtained in step 1) were mixed and dropped into the reactor containing the aqueous tert-butylamine solution in step 2). First add 1 / 10 mass part of the acid dropwise, and then add the M-Na salt, the remaining acid and the ...

Embodiment 2

[0026] Embodiment 2: a kind of method that resin directly synthesizes rubber vulcanization accelerator TBBS in waste water, comprises the following steps:

[0027] 1) At room temperature, mix the resin with 35% NaOH aqueous solution at a mass ratio of 1:0.5 to prepare M-Na salt solution evenly. The mixing temperature is 0°C, the configuration time is 3h, and the upper layer of M-Na is extracted after settling for 1h. saline solution for use;

[0028] 2) drop 3 parts by weight of tert-butylamine and 3 parts by weight of water into the reactor, and stir to obtain an aqueous solution of tert-butylamine;

[0029] 3) 3 parts by weight of M-Na salt obtained in step 1), 1 part by weight of sulfuric acid and 2 parts by weight of hydrogen peroxide are mixed and dropped into the reactor containing the aqueous tert-butylamine solution in step 2). First add 1 / 10 parts by mass of the acid dropwise, and then add the M-Na salt, the remaining acid and the oxidizing agent dropwise within 2.5 ...

Embodiment 3

[0032] A kind of method that resin directly synthesizes rubber vulcanization accelerator TBBS in waste water, comprises the steps:

[0033] 1) At room temperature, mix the resin with 25% NaOH aqueous solution according to the mass ratio of 1:1.5 to prepare the M-Na salt solution evenly under stirring. The solution is ready for use;

[0034] 2) Put 2 parts by weight of tert-butylamine and 2.5 parts by weight of water into the reactor, and stir to obtain an aqueous solution of tert-butylamine;

[0035] 3) 3.5 parts by weight of M-Na salt obtained in step 1), 2 parts by weight of nitric acid and 3 parts by weight of sodium hypochlorite were mixed and dropped into the reactor containing the aqueous tert-butylamine solution in step 2). First add 1 / 10 mass part of the acid dropwise, and then add the M-Na salt, the remaining acid and the oxidizing agent dropwise within 1.5 h.

[0036] 4) After the reacted material was first settled and stratified for 0.75h, the lower layer material...

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PUM

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Abstract

The invention belongs to the field of wastewater treatment and particularly relates to a method for directly synthesizing a rubber vulcanization accelerator TBBS from resin in waste water. The methodcomprises: 1) mixing resin and an aqueous solution of NaOH under stirring at a normal temperature to obtain an M-Na salt solution, 2) adding 1.5 to 3 parts by weight of t-butylamine and 2 to 3 parts by weight of water into a reactor and carrying out uniform stirring to obtain a t-butylamine aqueous solution, 3) mixing the M-Na salt and acid obtained in the step 1), and an oxidant, and adding the mixture into the reactor in the step 2), and 4) carrying out setting layering on the reaction product for 0.5-1h and carrying out centrifugation spin-drying on the lower layer material to obtain a product. The method is free of a high temperature solvent dissolution and sedimentation process and is simple and easy to operate. The method is free of heating, can selectively use a solvent, reduces energy source consumption, reduces the environmental pollution caused by the volatilization of the solvent and has a target product TBBS yield of more than 99.0% (on the basis of MBT content).

Description

technical field [0001] The invention belongs to the field of wastewater treatment, and in particular relates to a method for directly synthesizing a rubber vulcanization accelerator TBBS from resin in wastewater. Background technique [0002] Rubber vulcanization accelerator TBBS (chemical name N-tert-butyl-2-benzothiazole sulfenamide, also known as NS) is one of the important varieties of sulfenamide accelerators. It is safe and low-toxic, and does not produce carcinogenic nitrous amine. Rubber vulcanization accelerator TBBS has the functions of anti-scorch, non-toxic and fast vulcanization. It is called "standard accelerator" and is mainly used in natural rubber, butadiene rubber, styrene-butadiene rubber and isoprene rubber. [0003] At present, in order to improve the quality of TBBS in the industry, a large proportion of tert-butylamine is used to produce TBBS, tert-butylamine: MBT=2-4 (molar ratio), and excess tert-butylamine is recycled by distillation. Though impro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/80
CPCC07D277/80
Inventor 孙风娟
Owner KEMAI CHEM
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