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

A technology of microchannel reaction and organic phosphorus, which is applied in organic chemistry, chemical instruments and methods, chemical/physical/physical chemical reactors, etc., can solve the problems of consumption of product phosphorus oxychloride, extended reaction cycle, and long time consumption. Achieve the effects of no amplification effect, shortened reaction cycle, and high mass and heat transfer efficiency

Active Publication Date: 2022-07-15
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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  • Microchannel reaction equipment and preparation method of halogen-free organophosphorus flame retardant
  • Microchannel reaction equipment and preparation method of halogen-free organophosphorus flame retardant
  • Microchannel reaction equipment and preparation method of halogen-free organophosphorus flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Embodiment 1, weigh 1.5g titanium tetrachloride and join in 150g phosphorus oxychloride bottle, take 378g isooctanol in the second bottle, use diaphragm pump to 15g / min, use Hanbang pump to 37.8g The speed of / min was injected into the module of the microchannel reactor, and the temperature of the reaction module was set to 40 °C. After 5 reaction modules, it was collected into a closed container, and subjected to alkali washing, water washing, steam distillation, and filtration. 99.8%, yield 94%.

Embodiment 2

[0052] Embodiment 2, weigh 1.5g titanium tetrachloride and join in 150g phosphorus oxychloride bottle, take 382g isooctanol in the second bottle, use diaphragm pump at 20g / min, use Hanbang pump at 50.93 g The speed of / min was injected into the module of the microchannel reactor. The temperature of the reaction module was set to 60 °C. After 5 reaction modules, it was collected into a closed container, and subjected to alkali washing, water washing, steam distillation, and filtration. 99.7%, yield 98.5%.

Embodiment 3

[0053] Embodiment 3, get 1.5g titanium tetrachloride and join in 150g phosphorus oxychloride bottle, take 390g isooctanol in the second bottle, use diaphragm pump at 30g / min, use Hanbang pump at 78g / min. The speed of min is injected into the module of the microchannel reactor, the temperature of the reaction module is set to 70 °C, after 5 reaction modules, it is collected in a closed container, and after alkali washing, water washing, steam distillation, and filtration, the content is 99.5 %, the yield is 96.5%.

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Abstract

The invention provides a micro-channel reaction device, a module of the micro-channel reactor "heart-shaped" structure, with an inverted Ω-shaped blending tank inside the heart-shaped, and the blending tank has an everted opening and a narrower Bundle neck, larger lungs. When the equipment is used for the preparation of halogen-free organophosphorus flame retardants, phosphorus oxychloride and isooctanol or ethylene glycol monoether are respectively fed into the pre-cooling module of the micro-channel reactor through a metering pump, and the pre-cooled materials Enter the heart-shaped reaction module, and stay in the mixing tank for a short time, and the reaction solution is discharged after passing through the reaction module. The micro-channel reactor of the present invention enables the materials to be mixed more fully in the blending tank inside the reactor, the reaction efficiency is greatly improved, the reaction time is reduced, and there are almost no side reactions.

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] Common halogen-free organophosphorus flame retardants are as follows: [0003] 1. Triisooctyl 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 triisooctyl phosphate, the holding temperature is about 80 degrees, the reaction time is 6-7h, 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 generated. Hydrogen chloride will react with isooctyl alcohol to generate chloroisooctane, which will react ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J19/00C07F9/11
CPCB01J19/0093B01J19/0053C07F9/11
Inventor 孟长春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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