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Novel environment-friendly production method of accelerant CBS without production of waste salt and wastewater

A production method and accelerator technology, applied in the direction of organic chemistry, can solve the problems of low or high salt wastewater yield, and achieve the effect of simple process, low cost and significant economic benefits

Inactive Publication Date: 2019-12-31
SHANDONG SUNSINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to make up for the deficiencies of the existing technology and solve the problem of producing a large amount of high-salt wastewater and the yield is not high in the production of the rubber vulcanization accelerator CBS in the prior art, the present invention provides a new type of environmentally friendly accelerator CBS that does not generate waste salt wastewater. production method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A new environmentally friendly production method of CBS, a promoter that does not produce waste salt wastewater, includes the steps:

[0029] 1) Using 2.55 L of isopropanol solvent, completely dissolve 270g of dry product M at 63°C;

[0030] 2) Add cyclohexylamine dropwise while stirring, the molar ratio of cyclohexylamine to dry product M is 1:1;

[0031] 3) After 158.7g of cyclohexylamine has been added dropwise, isopropanol is used to prepare 8% hydrogen peroxide by mass to volume; 8% hydrogen peroxide is added dropwise to the reaction system to the end of the reaction;

[0032] 4) Add one drop of ammonium sulfate, one drop of starch solution, one drop of potassium iodide reagent on the drip plate, and add 1-2 of the reaction solution dropwise to the above mixture. If it turns blue, it means the end point. After the end point, stir for 30 minutes and cool to At 30°C, the product is separated out, filtered, washed with isopropanol, and dried to obtain the finished product CBS...

Embodiment 2

[0034] A new environmentally friendly production method of CBS, a promoter that does not produce waste salt wastewater, includes the steps:

[0035] 1) Using 3.05 L of isopropanol solvent, completely dissolve 270g of dry product M at 57°C;

[0036] 2) Add cyclohexylamine dropwise while stirring, the molar ratio of cyclohexylamine to dry product M is 1:1.05;

[0037] 3) After 151.1g of cyclohexylamine has been added dropwise, isopropanol is used to prepare 10% hydrogen peroxide by mass to volume; 10% by mass hydrogen peroxide is added dropwise to the reaction system to the end of the reaction;

[0038] 4) Add one drop of ammonium sulfate, one drop of starch solution, one drop of potassium iodide reagent on the drip plate, and add 1-2 of the reaction solution dropwise to the above mixture. If it turns blue, it means the end point. After the end point, stir for 30 minutes and cool to At 25°C, the product is separated out, filtered, washed with isopropanol, and dried to obtain the finishe...

Embodiment 3

[0041] In step 1), the solvent is isopropanol obtained by distillation in Example 2.

[0042] A new environmentally friendly production method of CBS, a promoter that does not produce waste salt wastewater, includes the steps:

[0043] 1) Using 3.05 L of the isopropanol solvent obtained by distillation of the filtrate and washing liquid of Example 2 to completely dissolve 270g of dry product M at 57°C;

[0044] 2) Add cyclohexylamine dropwise while stirring, the molar ratio of cyclohexylamine to dry product M is 1:1.05;

[0045] 3) After 151.1g of cyclohexylamine has been added dropwise, isopropanol is used to prepare 10% hydrogen peroxide by mass to volume; 10% by mass hydrogen peroxide is added dropwise to the reaction system to the end of the reaction;

[0046] 4) Add one drop of ammonium sulfate, one drop of starch solution, one drop of potassium iodide reagent on the drip plate, and add 1-2 of the reaction solution dropwise to the above mixture. If it turns blue, it means the end p...

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Abstract

Belonging to the field of fine chemicals, the invention discloses a novel environment-friendly production method of an accelerant CBS without production of waste salt and wastewater. The method includes the steps of: 1) dissolving a dry product M at 40-65DEG C by an organic solvent; 2) adding cyclohexylamine dropwise under stirring, and keeping the molar ratio of cyclohexylamine to the dry productM at 1:1.0-1.3; 3) adding hydrogen peroxide diluted by an organic solvent dropwise to a reaction end point; and 4) then performing stirring for 20-60min, and conducting cooling, filtering, washing and drying to obtain the finished product CBS. The method provided by the invention uses the organic solvent to dilute hydrogen peroxide, employs hydrogen peroxide diluted by the organic solvent to carry out oxidation reaction, and the product yield and quality both reach ideal effects; and the organic solvents can be recycled, no waste salt or waste water is generated, the cost is low, the processis simple, the operation is easy, and industrial production can be realized completely, therefore the method is a novel clean and environment-friendly process, and has remarkable environmental benefits and economic benefits.

Description

Technical field [0001] The invention relates to the field of fine chemicals, and particularly relates to a new environmentally friendly production method of the accelerator CBS that does not produce waste salt wastewater. Background technique [0002] At present, the main production processes for the production of rubber vulcanization accelerator CBS at home and abroad are sodium hypochlorite method and sodium hypochlorite and hydrogen peroxide mixed oxidation method. [0003] Due to the use of raw material chlorine, the sodium hypochlorite method has serious safety hazards and produces a large amount of high-salt wastewater. The COD of the wastewater is about 30,000 mg / L, which is difficult to treat and faces the situation of elimination. [0004] The mixed oxidation method uses 70% hydrogen peroxide in the early stage and 30% sodium hypochlorite in the later stage to find the end point. Although the waste salt is reduced by about 60% in the whole process, waste salt is still produc...

Claims

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Application Information

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IPC IPC(8): C07D277/80
CPCC07D277/80
Inventor 方雪山周福朋朱国旭李硕张玉柱李英举
Owner SHANDONG SUNSINE CHEM
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