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Method for synthesizing monoalkyl phosphonate

A technology of alkyl phosphinic acid ester and alkyl phosphinic acid, which is applied in the field of synthesis of alkyl phosphinic acid and its esters, can solve the problems of potential safety hazards and harshness, reduce risks, reduce production costs, The effect of environmentally friendly production costs

Inactive Publication Date: 2012-02-15
JIANGSU YOUTH CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The conditions for the synthesis of this route are relatively harsh: the reaction temperature needs to reach 180-200°C. If the high temperature stays for a long time, the alkyl phosphinic acid itself is prone to disproportionation reaction to generate more complex compounds such as alkyl phosphine and alkyl phosphate. Substances, dialkyl phosphine is a highly flammable substance, which has potential safety hazards

Method used

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  • Method for synthesizing monoalkyl phosphonate
  • Method for synthesizing monoalkyl phosphonate
  • Method for synthesizing monoalkyl phosphonate

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Embodiment 1: batch hydrolysis method

[0032] Add 180g of 20% hydrochloric acid into a 500ml four-neck flask, replace with nitrogen, raise the temperature to 50-60°C, start adding 235g (2mol) of methylphosphine dichloride dropwise, and the dropping time is controlled for 1-1.5hr. The by-product hydrogen chloride produced in the dropwise addition process is absorbed with deionized water. After the dropwise addition, the temperature was kept at this temperature for 15 minutes, and then the hydrogen chloride in the system was removed by negative pressure and absorbed by deionized water to obtain 600 g of 30% hydrochloric acid in total. The residual material in the four-neck bottle was methyl hypophosphorous acid aqueous solution, 267 g was collected, the analytical content was 59.06% (TP=228876.1), and the yield was 98.57%.

Embodiment 2

[0033] Embodiment 2: continuous method

[0034] According to Example 1, an aqueous solution of methyl hypophosphorous acid was prepared.

[0035] In a 500ml overflow flask, add 250 g (content 59.75%) of the prepared methyl hypophosphorous acid aqueous solution, replace with nitrogen, heat up to 50-60 ° C, and add methyl phosphine dichloride and Deionized water. The dropping rate is controlled at 235g / hr of methylphosphine dichloride, and 144g / hr of deionized water. At the same time, the feed begins to overflow into the second-stage reaction bottle for heat preservation, and the hydrogen chloride produced by the reaction is absorbed by deionized water. Feed continuously for 5 hours, total 1175g of methylphosphine dichloride was fed, and then the two-stage materials were combined to remove hydrogen chloride in the system by negative pressure and absorbed by deionized water to obtain 2415g of 30% hydrochloric acid in total. The remaining material was an aqueous solution of met...

Embodiment 3

[0037] Preparation of ethyl phosphinic acid aqueous solution according to Example 1: The yield of ethyl phosphinic acid is 97.65%.

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Abstract

The invention provides a method for synthesizing monoalkyl phosphonate. The method is characterized in that alkyl phosphine dihalideis is taken as a raw material and performed a hydrolysis reaction to obtain alkyl phosphinic acid, the alkyl phosphinic acid is performed a dehydrated esterification reaction with a compound possessing a structure of R2-OH to obtain the alkyl phosphonate, wherein R2 is alkyl, nonsaturated alkylene or aryl. The process route for preparing by-product halogen hydride or its aqueous solution can be used as a normal industrialization production process, the esterification process reaction has mild condition and low equipment requirement to the reaction. So that the production cost is reduced and the three wastes substances are not generated basically.

Description

technical field [0001] The invention belongs to the synthesis method of alkyl phosphinic acid and its ester. Specifically, the method obtains alkyl phosphinic acid by hydrolyzing alkyl dihalide phosphine, and then esterifies to obtain alkyl phosphinate. The by-products produced by this process route are mainly hydrogen halide or its aqueous solution, which can be applied to normal industrial production processes. The reaction conditions of the esterification process are mild, and the requirements for reaction equipment are low. It not only reduces the production cost, but also produces almost no three wastes. The invention has the advantages of environmental friendliness, lower production cost and the like. Background technique [0002] In recent years, the development of organophosphorus chemistry has not only greatly enriched the content of chemistry, but also opened up a new field of organic chemistry. Organophosphorus compounds are not only good insecticides, but also...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/32
Inventor 戚明珠王东朝孔勇王宝林蒋贤梅杨凡
Owner JIANGSU YOUTH CHEM