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Process and device for continuously synthesizing tribromophenol by using microreactors

A microreactor, a technology of tribromophenol, applied in the field of tribromophenol synthesis, can solve the problems affecting the increase of the production capacity of tris(tribromophenoxy)triazine, prone to side reactions, low heat utilization rate, etc. The effect of occurrence of side reactions, small liquid holding capacity and high heat exchange efficiency

Inactive Publication Date: 2021-06-15
WEIFANG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, the phenol bromination process is to add deionized water, phenol and methylene chloride into the reaction kettle, heat up and stir, and after the phenol is completely dissolved, start to add bromine and hydrogen peroxide dropwise. The dropwise addition process takes about 3 hours. Continue to react at -42°C for 3 hours. This reaction mainly has the following problems: (1) the solvent is dichloromethane, which has a low boiling point, so that the entire reaction is completed at about 40°C, and the reaction rate is slow; (2) the entire process takes time. About 6 hours, the production cycle is long, and side reactions are prone to occur, which affects the increase in production capacity of tris(tribromophenoxy)triazine; (3) Conventional kettle reaction, low heat utilization rate, high energy consumption, and bromination during the process Hydrogen, the pressure fluctuates, there is a safety hazard

Method used

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  • Process and device for continuously synthesizing tribromophenol by using microreactors

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The flow rate of the metering pump is 47 g / min, and the flow rate of the metering pump 2 6 is 29.3 g / min, and the flow rate of the metering pump three 7 is 49.6 g / min, and the flow rate of the meter pump four 8 is 19.2g / min. The heating temperature of the water bath heater 14 was 75 ° C, the ripening kettle 15 temperature was controlled at 75 ° C, cooked for 30 min, and the cooked liquid was obtained by post-treatment to obtain tribromephenols, experimental results: 32min, total reaction time, 99.1% of triophenol .

Embodiment 2

[0034] The flow rate of the metering pump is 47 g / min, and the flow rate of the metering pump 2 6 is 28.3 g / min, and the flow rate of metering pump three 7 is 48 g / min, and the flow rate of metering pump four 8 is 18.8g / min, water bath The heating temperature of the heater 14 was 75 ° C, and the ripening kettle 15 temperature was controlled at 75 ° C, cooked for 30 min, and obtained trihydraminated liquid obtained by subjected to trihydrazhen, experimental results: 32 min of total reaction time and 98.9% of tribrominol.

Embodiment 3

[0036] The flow rate of the metering pump 1 5 is 47 g / min, and the flow rate of the metering pump 2 6 is 28.9 g / min, and the flow rate of the metering pump three 7 is 49 g / min, and the flow rate of the metering pump four 8 is 19g / min, the water bath heating The heating temperature of the unit 14 was 75 ° C, the ripening kettle 15 temperature was controlled at 75 ° C, cooked for 30 min, and obtained tropic liquid was treated with tribromol after treatment: 32 min, and a total rate of total reaction time was 99.4%.

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Abstract

The invention discloses a process and a device for continuously synthesizing tribromophenol by using microreactors, belonging to the technical field of tribromophenol synthesis. The process comprises the following steps that a phenol dichloroethane solution and deionized water enter a microreactor I through a metering pump and are fully mixed, and then enter a microreactor II for a reaction with a metered bromine dichloroethane solution; after a full reaction in a microreaction pipeline I, a formed mixture enters a microreactor III to continue to react with a hydrogen peroxide solution; after a full reaction in a microreaction pipeline II, the mixture is pumped into a curing kettle; and after curing, a tribromophenol product is obtained through post-treatment. The invention also discloses a device for continuously synthesizing tribromophenol. The device comprises the microreactors and the microreaction pipelines. According to the method, a reaction rate is increased, the problems of long tribromophenol production time, incapability of continuous production, low safety performance and the like of the existing intermittent reactor are solved, and the method has an important application prospects.

Description

Technical field [0001] The present invention relates to the field of tribromol synthesis, and more particularly to a process and apparatus for continuously synthesizing tribromovallols in a microreactor. Background technique [0002] At present, the phenol bromide is added to deionized water, phenol, and dichloromethane, stirring and stirring, and then lysis of olfol is completely dissolved, and the dripping process is about 3 h and left, and after the addition is completed. 38 -42 ° C continued to react for 3 hours, the reaction mainly present the following problems: (1) The solvent uses dichloromethane, low boiling point, so that the entire reaction is completed at 40 ° C, the reaction rate is slow; (2) The whole process takes time Around 6h, long production cycle, susceptible side effects, affecting the production capacity of three (tribromobenzoxy) triazine; (3) conventional kettle reactions, low heat utilization rate, large energy consumption, and process produce bromide Hyd...

Claims

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Application Information

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IPC IPC(8): C07C37/62C07C39/27B01J19/00
CPCB01J19/0093C07C37/62C07C39/27
Inventor 王德强孙超
Owner WEIFANG UNIV OF SCI & TECH
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