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A kind of method for continuously preparing 4-(6-hydroxyhexyloxy)phenol

A technology of hydroxyhexyloxyl and phenol, which is applied in the field of continuous preparation of 4-phenol by using microreactor technology, which can solve the problems of long production cycle, cumbersome operation process and low yield

Active Publication Date: 2020-10-30
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to overcome the cumbersome operation process of preparing 4-(6-hydroxyhexyloxy)phenol in the tank reactor, the defects such as long production cycle and low yield, the invention provides a continuous preparation of 4-(6- The method of hydroxyhexyloxy)phenol not only can prepare 4-(6-hydroxyhexyloxy)phenol rapidly and efficiently, but also the process is simple and the process is easy to regulate

Method used

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  • A kind of method for continuously preparing 4-(6-hydroxyhexyloxy)phenol
  • A kind of method for continuously preparing 4-(6-hydroxyhexyloxy)phenol
  • A kind of method for continuously preparing 4-(6-hydroxyhexyloxy)phenol

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Effect test

Embodiment 1

[0019] After dissolving 3.3g hydroquinone and 1.37g 6-chloro-1-hexanol with ethanol, the volume was adjusted to 100ml to make mixed raw material 1, and then 3mol / L NaOH aqueous solution 2 was prepared. The flow rate of min is transported to the heating zone 6 in the microreactor (characteristic size: 0.4 mm) 4 by the metering pump 3, the temperature in the heating zone is controlled at 135°C, and the two materials enter the reactor from the reactor inlet 7 and 8 respectively after mixing , react in the microchannel 9, the material residence time is 5.4min, the material after the reaction enters the cooling zone 12, and the reaction is terminated by cold fluid heat exchange, and the product is collected at the outlet 13. The collected sample was transferred into a separatory funnel, extracted by n-hexane and then phase-separated. Unreacted 6-chloro-1-hexanol was present in the organic phase, and the aqueous phase was neutralized to pH=2 with hydrochloric acid. Ethanol is evapor...

Embodiment 2

[0021] Process is the same as example 1, only change the proportioning of reactant hydroquinone and 6-chloro-1-hexanol and the residence time of material: 5.5g hydroquinone and 1.37g 6-chloro-1-hexanol are mixed with ethanol After the alcohol is dissolved, the volume is adjusted to 100ml to make a mixed raw material, 3mol / L NaOH aqueous solution is used as a catalyst, and the residence time of the material is 1.5min. 100% conversion of 6-chloro-1-hexanol and 50% yield of 4-(6-hydroxyhexyloxy)phenol were obtained.

Embodiment 3

[0023] Process is the same as example 1, only change the concentration of reactant hydroquinone and 6-chloro-1-hexanol: After dissolving 16.52g hydroquinone and 6.831g 6-chloro-1-hexanol with ethanol, settle to 100ml is made into mixed raw material, and the NaOH aqueous solution of 3mol / L is used as catalyst, and the material residence time is 5min. The conversion rate of 6-chloro-1-hexanol was 100%, and the yield of 4-(6-hydroxyhexyloxy)phenol was 80%.

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Abstract

The invention discloses a method for continuously preparing 4-(6-hydroxyhexyloxy)phenol in a micro-reactor. The method comprises the following steps: dissoling hydroquinone and 6-chloro-1-hexanol in the solvent ethanol; and with an alkali aqueous solution of NaOH<-> as a catalyst, carrying out a bimolecular nucleophilic substitution reaction in the micro-reactor so as to continuously prepare 4-(6-hydroxyhexyloxy)phenol. Compared with the prior art, the method provided by the invention has the following advantages that the synthesis time of 4-(6-hydroxyhexyloxy)phenol is reduced to 10 min or less from original 20 hours; yield is increased from original 40% to 80%;continuous operation during the reaction can be realized; and integration and enlargement can be easily realized.

Description

technical field [0001] The invention relates to a synthesis method of 4-(6-hydroxyhexyloxy)phenol, in particular to a method for continuously preparing 4-(6-hydroxyhexyloxy)phenol by using microreactor technology. Background technique [0002] Optical functional films (such as cholesteric color filters, polarizers, etc.) are very important for improving the optical performance of liquid crystal displays, and it is an effective way to prepare optical functional films by photopolymerization of liquid crystal diacrylate, 4-( 6-Hydroxyhexyloxy)phenol can be used as an intermediate for synthesizing optical functional films to synthesize suitable optical functional films and improve the performance of the synthesized films. Due to the unique properties of 4-(6-hydroxyhexyloxy)phenol in optical functional membrane components, the efficient preparation of 4-(6-hydroxyhexyloxy)phenol in batches shows important practical significance and research value. [0003] The synthesis of 4-(6...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/16C07C41/34C07C43/23B01J19/00
CPCB01J19/0093C07C41/16C07C41/34C07C43/23
Inventor 陈光文李雷周峰焦凤军韩梅
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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