Continuous preparation process of phosphate flame retardant based on micro-channel reactor

A technology of microchannel reactor and preparation process, which is applied in chemical/physical/physical chemical reactors, phosphorus organic compounds, chemical instruments and methods, etc., and can solve the problems of high raw material input cost, incomplete reaction, and great pollution impact, etc. problem, to achieve the effects of short diffusion time, short reaction time and simple process flow

Pending Publication Date: 2020-12-04
扬州晨化新材料股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Due to the incomplete reaction of the above-mentioned traditional flame retardant preparation process, the molar ratio of phosphorus oxychloride to epoxy compound in actual production is 1:3.1-3.3, or even higher, the input cost of raw materials is too high, and the raw materials are all highly corrosive Non-toxic, flammable and explosive substances, low safety, long reaction time, many side reactions, low yield
[0007] In addition, the current domestic industrial production methods basically require water washing. The acid value of the product after water washing is relatively high, the flash point is not too high, and the quality is worse after thermal storage reaction. Treatment equipment for treatment, the cost is too high, and can not be completely treated, phosphorus-containing wastewater through infiltration and evaporation has a great impact on the pollution of the surrounding environment

Method used

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  • Continuous preparation process of phosphate flame retardant based on micro-channel reactor
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] At room temperature, put 4.8mol of catalyst titanium tetrachloride and 1000mol of phosphorus oxychloride into the mixing raw material preparation tank and mix, and at the same time put 3000mol of propylene oxide into the epoxy compound metering tank.

[0034] The materials in the above two metering tanks were continuously poured into the microchannel reactor for reaction. The temperature in the reactor was maintained at 61° C., the pressure was 0.46 MPa, and the residence time was 10 minutes. TCPP was obtained by continuous discharge. The acid value of the product is 0.06mgKOH / g, and the yield is 99.92%.

Embodiment 2

[0036] At normal temperature, put 4.4mol of catalyst titanium tetrachloride and 1000mol of phosphorus oxychloride into the mixing raw material preparation tank and mix, and at the same time put 3006mol of propylene oxide into the epoxy compound metering tank.

[0037] The materials in the above two metering tanks were continuously poured into the microchannel reactor for reaction. The temperature in the reactor was maintained at 66° C., the pressure was 0.47 MPa, and the residence time was 9 minutes. TCPP was obtained by continuous discharge. The acid value of the product is 0.05mgKOH / g, and the yield is 99.93%.

Embodiment 3

[0039] At normal temperature, 3.1 mol of catalyst anhydrous tin tetrachloride and 1000 mol of phosphorus oxychloride are injected into the mixed raw material preparation tank for mixing, and at the same time, 3009 mol of propylene oxide is injected into the epoxy compound metering tank.

[0040] The materials in the above two metering tanks were continuously pumped into the microchannel reactor for reaction. The temperature in the reactor was maintained at 73° C., the pressure was 0.48 MPa, and the residence time was 9 minutes. TCPP was obtained by continuous discharge. The acid value of the product is 0.08mgKOH / g, and the yield is 99.93%.

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Abstract

The invention relates to a continuous preparation process of a phosphate flame retardant based on a micro-channel reactor, and belongs to the technical field of phosphorus-based flame retardant preparation. The process comprises the steps of mixing a catalyst and phosphorus oxychloride to obtain a mixed raw material, and respectively pumping the mixed raw material and an epoxy compound into the micro-channel reactor to perform continuous reaction, thereby obtaining the phosphorus-based flame retardant. According to the method, the mixed raw materials are directly introduced into the micro-channel reactor for reaction, the equipment is simple, the operation is convenient, continuous production can be achieved, the quality is stable, the yield is high, energy consumption is low, and safety is good.

Description

technical field [0001] The invention relates to the technical field of preparation of phosphorus-based flame retardants, in particular to the production technology of organic phosphorus flame retardants. Background technique [0002] With the development of social economy, due to the needs of fire safety in electronic and electrical materials, automobiles, high-rise buildings, transportation (high-speed rail, aircraft) and other fields, the materials used must be flame-retardant, so as to reduce the occurrence of fires and protect people's lives. Property safety, and the most common flame retardants are TCEP, TCPP and TDCP, all of which are additive flame retardants, easy to use, cheap, and have great market competitiveness. [0003] Tris (2-chloroethyl) phosphate, referred to as TCEP. It can be used in the production of polyurethane soft foam and hard foam. It has the functions of improving water resistance, cold resistance, antistatic property and soft hand feeling. Gene...

Claims

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Application Information

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IPC IPC(8): C07F9/09B01J19/00
CPCC07F9/091B01J19/0093
Inventor 郝银房连顺董晓红
Owner 扬州晨化新材料股份有限公司
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