Synthetic method for rubber cross-linking agent cyclohexanone peroxide

A technology of cyclohexanone peroxide and synthesis method, which is applied in the field of organic synthesis, can solve problems such as endangering the health of production operators and environmental pollution, and achieve the effects of prolonging the service life of equipment, reducing the risk factor, and improving the reaction yield

Inactive Publication Date: 2018-07-03
CHENGDU WEI ER BO DUN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, hydrochloric acid as a reaction raw material will endanger the health of production operators and also cause pollution to the environment

Method used

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  • Synthetic method for rubber cross-linking agent cyclohexanone peroxide

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Experimental program
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Effect test

Embodiment 1

[0016] The synthetic method of rubber crosslinking agent cyclohexanone peroxide comprises the steps:

[0017] A: Add 2mol cyclohexene in the reaction vessel, 800ml mass fraction is 40% potassium nitrate solution, control the solution temperature to 15°C, control the stirring speed to 210rpm, add 4mol mass fraction to be 30% 1,2-propanediol solution, 4mol four For lead acetate, add 4mol mass fraction of 40% methyl tert-butyl ether solution in 2 times within 30 minutes, and continue to react for 80 minutes;

[0018] B: Then add 4mol nickel oxalate powder, control the stirring speed to 290rpm, continue to react at 120rpm, react for 2h, lower the temperature to 5°C, add 1.3L of 10% sodium sulfate solution by mass fraction, separate the layers of the solution, separate the oil layer, and use the mass fraction Wash with 60% hexane solution for 30 minutes, recrystallize in 70% butyl ether solution, and dehydrate with anhydrous sodium sulfate dehydrating agent to obtain 480.684 g of f...

Embodiment 2

[0020] The synthetic method of rubber crosslinking agent cyclohexanone peroxide comprises the steps:

[0021] A: Add 2mol cyclohexene in the reaction vessel, 800ml mass fraction is 43% potassium nitrate solution, control the solution temperature to 18°C, control the stirring speed at 220rpm, add 5mol mass fraction to be 33% 1,2-propanediol solution, 5mol four For lead acetate, add 5mol mass fraction of 44% methyl tert-butyl ether solution in 3 times within 40 minutes, and continue to react for 100 minutes;

[0022] B: Then add 5mol nickel oxalate powder, control the stirring speed to 310rpm, continue to react at 140rpm, react for 2.5h, lower the temperature to 7°C, add 1.3L of 13% sodium sulfate solution, the solution is separated, the oil layer is separated, and the Wash with 63% hexane solution for 40 minutes, recrystallize in 73% butyl ether solution, and dehydrate with anhydrous sodium sulfate dehydrating agent to obtain 481.668 g of finished cyclohexanone peroxide with a ...

Embodiment 3

[0024] The synthetic method of rubber crosslinking agent cyclohexanone peroxide comprises the steps:

[0025] A: Add 2mol cyclohexene in the reaction vessel, 800ml mass fraction is 47% potassium nitrate solution, control the solution temperature to 22°C, control the stirring speed to 230rpm, add 6mol mass fraction to be 36% 1,2-propanediol solution, 6mol four For lead acetate, add 6mol mass fraction of 47% methyl tert-butyl ether solution in 4 times within 50 minutes, and continue to react for 120 minutes;

[0026] B: Then add 6mol of nickel oxalate powder, control the stirring speed to 320rpm, continue to react at 160rpm, react for 3h, lower the temperature to 9°C, add 1.3L of 16% sodium sulfate solution by mass fraction, separate the layers of the solution, separate the oil layer, and use the mass fraction Wash with 65% hexane solution for 50 minutes, recrystallize in 76% butyl ether solution, and dehydrate with anhydrous sodium sulfate dehydrating agent to obtain 483.144 g ...

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Abstract

The invention discloses a synthetic method for the rubber cross-linking agent cyclohexanone peroxide. The synthetic method comprises the following steps: adding cyclohexene and a potassium nitrate solution into a reaction vessel, controlling a solution temperature to be 15-22 DEG C, controlling a stirring speed to be 210-230 rpm, adding a 1,2-propanediol solution and lead tetraacetate, adding a methyl tert-butyl ether solution in batches within 30-50 min, and continuing a reaction for 80-120 min; and adding nickel oxalate powder, controlling the stirring speed to be 290-330 rpm, continuing a reaction for 2-3 h, lowering the temperature to 5-9 DEG C, adding a sodium sulfate solution, subjecting the solution to layering to separate an oil layer, carrying out washing with a hexane solution for 30-50 min, then carrying out recrystallization in a butyl ether solution, and carrying out dehydration with a dehydrating agent so as to obtain the finished cyclohexanone peroxide.

Description

technical field [0001] The invention relates to a method for preparing organic matter, belonging to the field of organic synthesis, in particular to a method for synthesizing a rubber crosslinking agent cyclohexanone peroxide. Background technique [0002] Cyclohexanone peroxide is mainly used in combination with a reducing agent to form a redox initiation system, which is used as a crosslinking and curing initiator for unsaturated polyester adhesives. Most of the existing synthetic methods use cyclohexanone, hydrogen peroxide, and hydrochloric acid as reactants. The reaction raw material cyclohexanone has anesthesia and stimulation. . In severe cases, shock, coma, convulsions of limbs, pulmonary edema may occur, and finally death due to respiratory failure. Cyclohexanone liquid is irritating to the skin; eye contact may cause corneal damage, and long-term repeated contact may cause dermatitis. Cyclohexanone is flammable and has an explosion hazard. Therefore, adopting c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C407/00C07C409/22
CPCC07C407/00C07C409/22
Inventor 廖如佴
Owner CHENGDU WEI ER BO DUN TECH CO LTD
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