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Method for preparing 2, 3-epoxy-1, 4-butanediol by using micro-channel reactor

A microchannel reactor, epoxy-based technology, applied in chemical instruments and methods, chemical/physical/physical-chemical reactors, chemical/physical/physical-chemical processes, etc., can solve the problem of shortening reaction time, high labor intensity, increasing Safety and other issues, to achieve the effect of shortening the response time, overcoming the labor intensity, and increasing the safety

Inactive Publication Date: 2021-06-29
SHANGHAI CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The purpose of the present invention is to provide a method for preparing 2,3-epoxy-1,4-butanediol using a microchannel reactor, the reaction efficiency is significantly improved, the reaction time is greatly shortened, and the possible failure of the tank reaction is avoided. The risk of explosion caused by product polymerization or hydrogen peroxide accumulation increases safety, reduces production costs, facilitates control of the production process, and overcomes the shortcomings of traditional production such as high labor intensity, long production cycle, and low product quality.

Method used

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  • Method for preparing 2, 3-epoxy-1, 4-butanediol by using micro-channel reactor

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Effect test

Embodiment 1

[0036]Prepare 1,4-butenediol and phosphotungstic heteropoly acid into a mixed solution of 1,4-butenediol / phosphotungstic heteropoly acid, and the concentration of 1,4-butenediol in the mixed solution is 1.5mol / L, the molar ratio of 1,4-butenediol and phosphotungstic heteropoly acid is 1:0.07, and then 1,4-butenediol / phosphotungstic heteropoly acid mixed solution and 30% hydrogen peroxide solution are respectively The flow rate of 20ml / min and 5ml / min is pumped into the mixing module in the T1 area of ​​the microchannel reactor. After mixing, it enters the first temperature zone for pre-heating. The temperature is set at 30°C and the residence time is 8s. The epoxidation reaction is carried out in the zone, the reaction temperature is 60°C, and the reaction time is 60s. After the reaction is completed, the reaction solution is input into the mixing module of the T2 zone, and then the catalase solution is pumped into the mixing module of the T2 zone, and the catalase solution is...

Embodiment 2

[0038] Prepare 1,4-butenediol and phosphotungstic heteropoly acid into 1,4-butenediol / phosphotungstic heteropoly acid mixed solution, the concentration of 1,4-butenediol in the mixed solution is 1.0mol / L, the molar ratio of 1,4-butenediol and phosphotungstic heteropoly acid is 1:0.05, and then 1,4-butenediol / phosphotungstic heteropoly acid mixed solution and 25% hydrogen peroxide solution are respectively The flow rate of 24ml / min and 4ml / min is pumped into the mixing module in the T1 area of ​​the microchannel reactor. After mixing, it enters the first temperature zone for pre-heating. The temperature is set at 35°C and the residence time is 10s. zone for epoxidation reaction, the reaction temperature is 75°C, and the reaction time is 45s. After the reaction is completed, the reaction solution is input into the mixing module of the T2 zone, and then the catalase solution is pumped into the mixing module of the T2 zone, and the catalase solution is put into The amount is 0.2 ...

Embodiment 3

[0040] Prepare 1,4-butenediol and phosphotungstic heteropoly acid into a mixed solution of 1,4-butenediol / phosphotungstic heteropoly acid, and the concentration of 1,4-butenediol in the mixed solution is 2.0mol / L, the molar ratio of 1,4-butenediol and phosphotungstic heteropoly acid is 1:0.2, and then 1,4-butenediol / phosphotungstic heteropoly acid mixed solution and 25% hydrogen peroxide solution are respectively The flow rate of 30ml / min and 7.5ml / min is pumped into the mixing module in the T1 area of ​​the microchannel reactor. After mixing, it enters the first temperature zone for pre-heating. The temperature is set at 25°C and the residence time is 10s. The epoxidation reaction is carried out in the temperature zone, the reaction temperature is 85°C, and the reaction time is 30s. After the reaction is completed, the reaction solution is input into the mixing module of the T2 zone, and then the catalase solution is pumped into the mixing module of the T2 zone, and the catal...

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Abstract

A method for preparing 2, 3-epoxy-1, 4-butanediol by using a micro-channel reactor comprises the following steps: preparing 1, 4-butylene glycol and a catalyst into a mixed solution according to a certain proportion, then respectively inputting the mixed solution and a hydrogen peroxide solution into the micro-channel reactor, fully mixing, pre-heating the mixed material in a first temperature zone of the micro-channel reactor, and pre-heating at a second temperature zone of the micro-channel reactor, feeding into a second temperature zone for epoxidation reaction, adding a hydrogen peroxide decomposer solution into the reaction liquid flowing out of the second temperature zone to remove redundant hydrogen peroxide, and continuously extracting and concentrating the obtained product liquid by using an ester organic solvent to obtain the product 2, 3-epoxy-1, 4-butanediol. By utilizing the method, the reaction efficiency can be obviously improved, the reaction time is greatly shortened, the risk of explosion caused by product polymerization, hydrogen peroxide aggregation and the like possibly occurring in kettle type reaction is avoided, the production process is convenient to control, the production cost is reduced, and the defects of high labor intensity, long production period, low product quality and the like in traditional production are overcome.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method for preparing 2,3-epoxy-1,4-butanediol using a microchannel reactor. Background technique [0002] 1,2,4-Butanetriol (BT) is a colorless, odorless, transparent, water-soluble viscous syrupy polyol, and 1,2,4-Butanetriol sold in the market is usually straw yellow to brown Viscous liquid, with sweet taste, non-toxic. BT is an important organic synthesis intermediate, widely used in military industry, medicine, tobacco, cosmetics, papermaking, agriculture and polymer materials and other fields. Its nitro compound (BTTN) is a good energetic plasticizer, which can replace nitroglycerin as NEPE propellant and high-energy, high-tech propellant. The property is smaller than that of nitroglycerin, and mixed with other energetic plasticizers, it can significantly improve the low-temperature mechanical properties of nitrocellulose-based gunpowder. BT can be...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/14C07D301/12B01J19/00
CPCC07D303/14C07D301/12B01J19/0093
Inventor 张传好周励纪招君
Owner SHANGHAI CHEM REAGENT RES INST