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Micro-channel reaction equipment and preparation method of halogen-free organophosphorus flame retardant

A microchannel reaction and equipment technology, applied in organic chemistry, chemical instruments and methods, chemical/physical/physical chemical reactors, etc., can solve the problems of consumption of phosphorus oxychloride, prolongation of reaction cycle, side reactions, etc., to achieve Effects of increased purity and production efficiency, improved reaction efficiency, and easy operation

Active Publication Date: 2020-11-06
NANTONG JIANGSHAN AGROCHEM & CHEM LIMITED LIABILITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process takes a long time and consumes a lot of energy, prolonging the reaction cycle
In the traditional kettle reaction process, paddle stirring is used, and there is a "back-mixing" phenomenon in the reaction process. The existence of excess air will cause many side reactions, and the product phosphorus oxychloride will be consumed

Method used

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  • Micro-channel reaction equipment and preparation method of halogen-free organophosphorus flame retardant
  • Micro-channel reaction equipment and preparation method of halogen-free organophosphorus flame retardant
  • Micro-channel reaction equipment and preparation method of halogen-free organophosphorus flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Embodiment 1, take by weighing 1.5g titanium tetrachloride and join in the 150g phosphorus oxychloride bottle, take by weighing 378g isooctyl alcohol in the second bottle, with diaphragm pump at 15g / min, with Hanbang pump at 37.8g / min speed, into the module of the microchannel reactor, the temperature of the reaction module is set to 40 ℃, after passing through 5 reaction modules, it is collected in a closed container, and after alkali washing, water washing, steam distillation and filtration, the content of 99.8%, yield 94%.

Embodiment 2

[0052] Embodiment 2, take by weighing 1.5g titanium tetrachloride and join in the 150g phosphorus oxychloride bottle, take by weighing 382g isooctyl alcohol in the second bottle, use diaphragm pump at 20g / min, use Hanbang pump at 50.93g / min speed, into the module of the microchannel reactor, the temperature of the reaction module is set to 60 ℃, after passing through 5 reaction modules, it is collected in a closed container, and after alkali washing, water washing, steam distillation and filtration, the content of 99.7%, yield 98.5%.

Embodiment 3

[0053] Embodiment 3, get 1.5g titanium tetrachloride and join in the 150g phosphorus oxychloride bottle, take by weighing 390g isooctyl alcohol in the second bottle, with diaphragm pump at 30g / min, with Hanbang pump at 78 g / min The speed of min is injected into the module of the microchannel reactor, and the temperature of the reaction module is set at 70°C. After passing through 5 reaction modules, it is collected in a closed container, washed with alkali, washed with water, steam distilled, filtered, and the content is 99.5 %, yield 96.5%.

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Abstract

The invention provides micro-channel reaction equipment. According to the heart-shaped structure module of the micro-channel reactor, an inverted-omega-shaped blending groove is arranged in the heart-shaped structure module; the blending groove is provided with an everted opening part, a narrower neck binding part and a larger lung part. When the equipment is used for preparing a halogen-free organophosphorus flame retardant, phosphorus oxychloride and isooctyl alcohol or ethylene glycol monoether are made to enter the pre-cooling module of a micro-channel reactor through a metering pump, thepre-cooled materials enter the heart-shaped reaction module and stay in the blending groove for a short time, and a reaction liquid is discharged after passing through the reaction module. According to the micro-channel reactor disclosed by the invention, the materials are more fully mixed in the blending groove in the reactor, and therefore, reaction efficiency is greatly improved, the reaction time is shortened, and almost no side reaction exists.

Description

technical field [0001] The invention belongs to the preparation technology of a microchannel reactor and a halogen-free organic phosphorus flame retardant. Background technique [0002] There are two common halogen-free organophosphorus flame retardants: [0003] 1. Tri-isooctyl phosphate (TOP), the molecular formula is C 24 h 51 o 4 P, the relative molecular mass is 434.62, the structural formula is as follows: [0004] [0005] As a flame retardant, plasticizer, and extractant, triisooctyl phosphate is widely used in chemical production, and its most important use is in the production of hydrogen peroxide. [0006] For traditional tri-isooctyl phosphate, the holding temperature is about 80 degrees, the reaction time is 6-7 hours, and the ratio of raw materials is 3.5:1. During the preparation of triisooctyl phosphate, a large amount of hydrogen chloride gas will be produced. Hydrogen chloride will react with isooctyl alcohol to generate chloroisooctane, which will ...

Claims

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Application Information

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IPC IPC(8): B01J19/00C07F9/11
CPCB01J19/0093B01J19/0053C07F9/11
Inventor 于春红秦欢朱建华殷日祥刘谜陈芸芸
Owner NANTONG JIANGSHAN AGROCHEM & CHEM LIMITED LIABILITY
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