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Production method of dipropyl disulfide

A technology of dipropyl disulfide and production method, which is applied in chemical instruments and methods, thiol preparation, organic compound preparation and other directions, can solve the problems of unreasonable process design, increased operation difficulty, low product purity, etc. The effect of shortening the reaction cycle, reducing the difficulty, and simple steps

Pending Publication Date: 2022-05-06
TENGZHOU TIANSHUI BIO TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] 1) The reaction operation is carried out under normal pressure, and a large amount of organic solvent is used in the reaction process, which not only wastes money, but also increases the difficulty of operation
[0009] 2) The existing production process of dipropyl disulfide is unreasonable in process design, and the preparation method is to adopt S and Na 2 S reacts 1:1 to form Na 2 S 2 , then Na 2 S 2 React with 1-bromopropane at 1:2; since the synthesized sodium sulfide is Na 2 S 2 Mainly and containing Na 2 S, Na 2 S 3 、Na 2 S 4 etc., the components of the crude product after treatment are more complicated, and the content of the main peak is about 50%
The composition of the product is relatively complex, the product purity is low, and the aroma of the product is poor

Method used

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  • Production method of dipropyl disulfide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Synthesis of propanethiol;

[0029] 100L enamel reaction kettle, equipped with thermometer, dropping, reflux and distillation devices. Pump 25kg of water into the kettle, add 12.5kg of thiourea and 2.5kg of 1-bromopropane under stirring, heat the system, heat to reflux, add 14kg of 1-bromopropane dropwise under reflux, and control the dripping speed depending on the size of the reflux; after dropping, heat to 100°C, keep warm for 30 minutes. Add the lye made of 6kg sodium hydroxide and 25kg water to the reaction kettle dropwise, and carry out water distillation while adding dropwise. . The weight of the crude product is 8.5kg, the content is 93.2%, and the fine product is 6.4kg, and the content is 99.6%.

[0030] 2) Synthesis of dipropyl disulfide

[0031] The 100L enamel reaction kettle is equipped with a thermometer, a dripping device, and a chain control system for dripping and temperature detection. Add 50kg of water, 0.8kg of sodium hydroxide, and 15kg of p...

Embodiment 2

[0033] 1) Synthesis of propanethiol;

[0034] 200L enamel reaction kettle, equipped with thermometer, dropping, reflux and distillation devices. Pump 50kg of water into the kettle, add 25kg of thiourea and 5kg of 1-bromopropane under stirring, heat the system to reflux, add 28kg of 1-bromopropane dropwise under reflux, and control the dropping speed according to the size of the reflux; after dropping, heat to 100°C , keep warm for 30 minutes. Add the lye made of 12kg sodium hydroxide and 50kg water to the reaction kettle dropwise, and carry out water distillation while adding dropwise. . The weight of the crude product is 17kg, the content is 93.2%, and the refined product is 13kg, and the content is 99.6%.

[0035] 2) Synthesis of dipropyl disulfide;

[0036] The 200L enamel reaction kettle is equipped with a thermometer, a dripping device, and a chain control system for dripping and temperature detection. Add 100kg of water, 1.6kg of sodium hydroxide, and 30kg of propan...

Embodiment 3

[0038] 1) Synthesis of propanethiol;

[0039] 500L enamel reaction kettle, equipped with thermometer, dropping, reflux and distillation devices. Pump 125kg of water into the kettle, add 60kg of thiourea and 12.5kg of 1-bromopropane under stirring, heat the system, heat to reflux, add 70kg of 1-bromopropane dropwise under reflux, and control the dripping speed depending on the size of the reflux; after dropping, heat to 100 ℃, keep warm for 30 minutes. Add the lye made of 30kg sodium hydroxide and 125kg water to the reaction kettle dropwise, and carry out water distillation while adding dropwise. . The weight of the crude product is 42.5kg, the content is 93.2%, and the refined product is 32kg, and the content is 99.6%.

[0040] 2) Synthesis of dipropyl disulfide;

[0041]The 500L enamel reaction kettle is equipped with a thermometer, a dripping device, and a chain control system for dripping and temperature detection. Add 250kg of water, 4kg of sodium hydroxide, and 75kg ...

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Abstract

The invention discloses a production method of dipropyl disulfide, which comprises the following steps: thiourea and 1-bromopropane produce high-content propanethiol in a reflux state under the condition of taking water as a solvent, and propanethiol is oxidized by hydrogen peroxide under the alkaline condition of a sodium hydroxide aqueous solution to obtain dipropyl disulfide. No organic solvent is used for producing the propanethiol, and water is used for replacing the organic solvent, so that the method is environment-friendly and safe; by using water as a solvent and sodium hydroxide as a catalyst, the aroma quality of dipropyl disulfide obtained by directly oxidizing propanethiol with hydrogen peroxide is greatly improved, the product grade is improved, the reaction period is greatly shortened, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of food additive production, in particular to a production method of dipropyl disulfide. Background technique [0002] Dipropyl disulfide is a sulfur-containing spice. It has a pungent sulfur, onion, and garlic-like spicy aroma, with green and earthy aromas. It is used to prepare shallots, onions, garlic, vegetables, and tropical fruits. Food flavor. [0003] Dipropyl disulfide, the molecular formula is C 6 h 14 S 2 , the structural formula is as follows. [0004] CH 3 -CH 2 -CH 2 -S-S-CH 2 -CH 2 -CH 3 [0005] At present, there are relatively few reports on the synthesis of dipropyl disulfide. The current synthesis method is to add methanol to the reaction kettle, start stirring, add sodium sulfide (60%), stir to dissolve, and then raise the temperature to 60°C and then add in batches Sulfur powder, control the reaction temperature at 60°C to 70°C, and keep it warm for 1 hour. At 60°C, 1-bromop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/24C07C319/28C07C321/14C07C319/02C07C321/04
CPCC07C319/24C07C319/28C07C319/02C07C321/04C07C321/14
Inventor 张士金贾友良张翔洲李新华马兆峰
Owner TENGZHOU TIANSHUI BIO TECH CO LTD