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Method for continuously synthesizing hydroquinone dihydroxyethyl ether

A technology for hydroquinone dihydroxyethyl ether and hydroquinone, which is applied in the field of continuous synthesis of hydroquinone dihydroxyethyl ether in a microchannel reactor, and can solve the problems of low reaction rate, long time consumption, complicated operation, etc. question

Inactive Publication Date: 2021-04-20
SHENYANG RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method has high yield and good product color, but the reaction rate of the process is low, the operation is complicated, and the overall time-consuming is long. The catalyst used is more expensive than the alkali catalyst. enlarge

Method used

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  • Method for continuously synthesizing hydroquinone dihydroxyethyl ether
  • Method for continuously synthesizing hydroquinone dihydroxyethyl ether
  • Method for continuously synthesizing hydroquinone dihydroxyethyl ether

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Such as figure 1 visible:

[0036] (1) Preparation of hydroquinone and ethylene oxide aqueous solution: adding 80g of hydroquinone to 950mL of water for dilution, obtaining a mass concentration of 8% aqueous solution of hydroquinone, adding sodium hydroxide to aqueous solution of hydroquinone In, wherein, the addition amount of sodium hydroxide is 2% of hydroquinone quality, heats to dissolve; Ethylene oxide is added into 500mL water and dilutes, obtains mass concentration and is 12% ethylene oxide aqueous solution, cryopreservation, to The molar ratio of hydroquinone and ethylene oxide is 1:2.1;×

[0037] (2) Adjust the pressure of the back pressure valve to 1.2MPa, raise the temperature to 80°C, preheat the pipeline and the feed pump, and then pass the hydroquinone and ethylene oxide aqueous solutions through the first and second metering advection pumps respectively Input into the microchannel reactor, the hydroquinone aqueous solution flow rate is 19mL / min, the et...

Embodiment 2

[0039] (1) Preparation of hydroquinone and ethylene oxide aqueous solution: 80g of hydroquinone is added into 550mL of water and diluted to obtain a mass concentration of 13% aqueous solution of hydroquinone, sodium hydroxide is added to aqueous solution of hydroquinone In, wherein, the addition amount of sodium hydroxide is 2% of hydroquinone quality, heats to dissolve; Ethylene oxide is added into 450mL water and dilutes, obtains mass concentration and is 14% ethylene oxide aqueous solution, cryopreservation, to The molar ratio of hydroquinone and ethylene oxide is 1:2.3;

[0040] (2) Adjust the pressure of the back pressure valve to 1.5MPa, raise the temperature to 100°C, preheat the pipeline and the feed pump, and then input hydroquinone and ethylene oxide aqueous solution into the microchannel reactor synchronously, and the hydroquinone The flow rate of the phenol aqueous solution is 18mL / min, the flow rate of the ethylene oxide aqueous solution is 15mL / min, and the react...

Embodiment 3

[0042] (1) Prepare hydroquinone and ethylene oxide aqueous solution: 80g hydroquinone is added 1300mL water and dilutes, obtains the hydroquinone aqueous solution that mass concentration is 6%, sodium hydroxide is added hydroquinone aqueous solution In, wherein, the addition amount of sodium hydroxide is 2% of hydroquinone quality, heats to dissolve; Add ethylene oxide to 600mL water and dilute, obtain mass concentration and be 10% aqueous solution of ethylene oxide, cryopreservation, to The molar ratio of hydroquinone and ethylene oxide is 1:2.2;

[0043] (2) Adjust the pressure of the back pressure valve to 1.8MPa, raise the temperature to 120°C, preheat the pipeline and the feed pump, and then input hydroquinone and ethylene oxide aqueous solution into the microchannel reactor synchronously, and the hydroquinone The flow rate of phenol aqueous solution is 17mL / min, the flow rate of ethylene oxide aqueous solution is 13mL / min, and the reaction residence time is 4min. After t...

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Abstract

The invention relates to the field of organic synthesis, in particular to a method for continuously synthesizing hydroquinone dihydroxyethyl ether by a micro-channel reactor. Hydroquinone and ethylene oxide are used as raw materials, a catalyst is added into a hydroquinone diluent, the two raw materials are controlled by a metering advection pump to be synchronously input into a micro-channel reaction system, the volume flow of hydroquinone and ethylene oxide is regulated and controlled, reaction liquid reacts in a reaction unit of a micro-channel, and hydroquinone dihydroxyethyl ether is obtained. According to the method, the hydroquinone dihydroxyethyl ether is synthesized by adopting a micro-channel continuous process, so that rapid heating can be realized, the liquid holdup is small, the safety is high, and the flammable and combustible risk of ethylene oxide with relatively high initial concentration in the rapid heating process in an intermittent process can be avoided.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for continuously synthesizing hydroquinone dihydroxyethyl ether with a microchannel reactor. Background technique [0002] Hydroquinone dihydroxyethyl ether (HQEE for short) is a symmetrical aromatic diol chain extender, which has good compatibility with 4,4'-diphenylmethane diisocyanate (MDI) prepolymer , can produce high resilience PU elastomer, compared with aliphatic diol chain extender, can significantly improve the tensile strength, tear strength, heat resistance, compression deformation, hardness and resilience performance of the product. HQEE can be used to produce cast polyurethane elastomers, reduce the sensitivity of the formulation system to equipment and process conditions, and increase the compatibility between components in the formulation system; HQEE is also used for high-performance thermoplastic polyurethane elastomers and temperature-resistant spandex...

Claims

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Application Information

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IPC IPC(8): C07C41/03C07C43/23
Inventor 刘嵩鄢冬茂明卫星边策刘冰王珂贾志远杨林涛郭林
Owner SHENYANG RES INST OF CHEM IND
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