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A kind of metal oxide catalyzes the method for synthesizing polyethylene glycol phosphonate

A technology of poly(ethylene glycol methylphosphonate) and dimethyl methylphosphonate, which is applied in the direction of fireproof coatings, etc., can solve the problems of long synthesis reaction time, many by-products, expensive catalysts, etc., so as to avoid the utilization rate of atoms Low, reduce the generation of by-products, the effect of low cost

Active Publication Date: 2021-01-01
NORTHEAST FORESTRY UNIVERSITY
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Problems solved by technology

[0003] The purpose of the present invention is to solve the problems of long synthesis reaction time, expensive catalyst and many by-products of the current polymethylphosphonate flame retardant, and to provide a metal oxide catalyzed synthesis of polymethylphosphonate Preparation method of ester

Method used

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specific Embodiment approach 1

[0009] Specific embodiment 1: This embodiment describes a method for metal oxide catalyzed synthesis of polyethylene glycol methyl phosphonate, the method steps are as follows: metal oxide, dimethyl methyl phosphonate and ethyl Diols are evenly mixed to obtain a heterogeneous mixture, and the mixture is added to a three-necked flask, and a stirring bar is added to it, and the three-necked flask is placed on an electromagnetic heating mantle with a temperature of 160°C to 170°C, and the temperature is stirred and distilled After 2h to 4h, filter to obtain polyethylene glycol methylphosphonate.

specific Embodiment approach 2

[0010] Specific embodiment two: the method for the synthesis of polymethylphosphonate catalyzed by a metal oxide described in specific embodiment one, wherein the metal oxide is zinc oxide, aluminum oxide, cerium oxide, titanium oxide, One of tin oxide, bismuth oxide and gallium oxide.

specific Embodiment approach 3

[0011] Specific embodiment three: a method for metal oxide catalyzed synthesis of polyethylene glycol methyl phosphonate described in specific embodiment one, the metal oxide, dimethyl methyl phosphonate and ethylene glycol The amount ratio of substances is (0.02-0.05): 1: (1.1-1.2).

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Abstract

The invention relates to a method for synthesizing poly(oxy-1,2-ethanediyl)methylphosphonate through catalysis by virtue of a metallic oxide and belongs to the technical field of preparation of flameretardants. The method comprises the following steps: uniformly mixing the metallic oxide, dimethyl methylphosphorate and ethylene glycol to obtain a heterogeneous mixture, adding the mixture into a three-necked flask, adding stirrers into the three-necked flask, placing the three-necked flask on an electromagnetic heating jacket at the temperature of 160-170 DEG C, stirring at constant temperature, distilling for 2-4 hours, and filtering, so that the poly(oxy-1,2-ethanediyl)methylphosphonate is obtained. The method provided by the invention has the advantages that reaction time is greatly shortened, reaction can be finished within 2-4 hours, the reaction time is almost the same compared with an equivalent excellent ionic liquid catalyst, but cost is lower, and catalytic conditions are milder. In the industry, the ionic liquid catalyst needs to carry out intermittent operation by adopting a kettle type reaction system, and the metallic oxide can carry out continuous operation, so thatproduction efficiency of industrial production of poly(oxy-1,2-ethanediyl)methylphosphonate is improved, and economic benefit is further improved.

Description

technical field [0001] The invention belongs to the technical field of preparation of flame retardants, and in particular relates to a method for synthesizing poly(ethylene glycol methylphosphonate) catalyzed by metal oxides. Background technique [0002] Poly(ethylene glycol methylphosphonate) is used as a flame retardant in the flame retardant industry. It has the advantages of high phosphorus content and good flame retardant effect. The catalytic synthesis of dimethyl methylphosphonate and ethylene glycol to generate polyethylene glycol methylphosphonate by transesterification is catalyzed by ionic liquid catalysts. Although ionic liquids have many advantages, there are also some shortcomings. : The synthetic process of ionic liquid catalyst is loaded down with trivial details and complicated, needs to use organic solvent in synthesis, can produce waste water, not only can make the production cost of ionic liquid catalyst greatly increase, and also pollute environment, do...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G79/04C09K21/14
CPCC08G79/04C09K21/14
Inventor 姜大伟肖博申茜姜瑞婷王莹刘理鑫李佳家
Owner NORTHEAST FORESTRY UNIVERSITY
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