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Preparation method of cyclic phosphonate flame retardant

A cyclic phosphonate and flame retardant technology, which is applied in flame retardant fibers, chemical instruments and methods, compounds of elements of Group 5/15 of the periodic table, etc., which can solve the problems of catalyst pollution and long reaction time.

Inactive Publication Date: 2020-07-07
青岛长荣化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The technical problem to be solved in the present invention is to provide a fast-response, halogen-free catalyst preparation method to meet Higher and higher flame retardant requirements for fabrics

Method used

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  • Preparation method of cyclic phosphonate flame retardant
  • Preparation method of cyclic phosphonate flame retardant
  • Preparation method of cyclic phosphonate flame retardant

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Transesterification: Add 745g of trimethyl phosphite and 201g of trimethylolpropane to a 1000mL four-necked flask equipped with a magnetic stirrer, atmospheric distillation device (with packed column) and a thermometer, and heat to 80-120°C , Distillation and separation of by-product methanol while reacting, the column top temperature of the extracted methanol fraction is 63-65°C, and the reaction distillation is 4h to obtain the transesterification product;

[0038] Rearrangement: replace the packing column with a reflux condenser, so that the reaction distillation unit becomes a reflux reaction unit. Add 6g of catalyst methyl p-toluenesulfonate into the reactor, stir, heat to 170-180°C, keep warm for 2h to obtain the crude product;

[0039] Distillation under reduced pressure: transfer the crude product to a rotary evaporator, evaporate at a vacuum degree of 0.095-0.1MPa, and an oil bath temperature of 190-200°C, collect and obtain 390g of dimethyl methylphosphonate, ...

Embodiment 2

[0041] Transesterification: Add 558g of trimethyl phosphite and 201g of trimethylolpropane into a 1000mL four-neck flask equipped with a magnetic stirrer, atmospheric distillation device (with packed column) and a thermometer, and heat to 80-120°C , distill and separate the by-product methanol while reacting, the column top temperature of the extracted methanol fraction is 63-65°C, and the reaction distillation is 3h to obtain the transesterification product;

[0042] Rearrangement: replace the packing column with a reflux condenser, so that the reaction distillation unit becomes a reflux reaction unit. Add 5g of catalyst methyl benzenesulfonate into the reactor, stir, heat to 170-180°C, keep warm for 3 hours to obtain the crude product;

[0043] Distillation under reduced pressure: transfer the crude product to a rotary evaporator, evaporate at a vacuum degree of 0.095-0.10MPa, and an oil bath temperature of 180-190°C, collect and obtain 204g of dimethyl methylphosphonate, an...

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Abstract

The invention discloses a preparation method of a cyclic phosphonate flame retardant, which relates to the technical field of organic phosphorus flame retardant synthesis. The method comprises the following steps of taking trimethylolpropane and trimethyl phosphite as raw materials with the feed mole ratio of 1: 2-4, selecting methyl benzenesulfonate or methyl p-toluenesulfonate as a catalyst, controlling proper process parameters such as catalyst quantity, temperature, time and the like, and carrying out transesterification and rearrangement reaction to obtain the phosphonate flame retardantwith a cyclic structure and the byproduct dimethyl methylphosphonate flame retardant. The method provided by the invention has the advantages of few raw material varieties, easy source, low cost, rapid reaction, high efficiency, environment-friendly process, energy conservation and consumption reduction; the product prepared by the method is the same as the product prepared by the existing method,but the production period is shortened by 2 / 3-3 / 4, the production capacity is greatly improved, and the method is suitable for industrial production.

Description

[0001] 1 technical field [0002] The invention relates to a method for preparing a phosphonate flame retardant, in particular to a method for preparing a phosphonate flame retardant with a ring structure, and belongs to the technical field of organic phosphorus flame retardant synthesis. [0003] 2 background technology [0004] Cyclic phosphonate, that is, methyl phosphonate of trimethylolpropane, including monocyclic ester P2, bicyclic ester P3 and mixed cyclic ester (P2+P3), CAS registration numbers are 41203-81-0, 42595 respectively -45-9 and 170836-68-7, the most widely used products are mixed cyclic esters (P2+P3) mainly monocyclic ester P2, of which monocyclic ester P2 has two isomers, the content of And more than 90%, the appearance is a colorless to light yellow viscous liquid, containing more than 20.5% phosphorus. It was first successfully developed by Mobil Oil Company in the early 1970s (US3789091, 1974-01-29). [0005] As a flame retardant, cyclic phosphonate i...

Claims

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Application Information

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IPC IPC(8): C07F9/6574D06M13/288D06M101/32
CPCC07F9/657181D06M13/288D06M2101/32D06M2200/30
Inventor 韩忠山韩明序杨松慧
Owner 青岛长荣化工科技有限公司
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