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Dialkyl phosphinate as well as preparation method and application thereof

A technology of dialkyl phosphinate and dialkyl phosphinic acid, which is applied in the field of dialkyl phosphinate and its preparation, and can solve problems such as agglomeration, large specific surface area, and low flame retardancy

Active Publication Date: 2021-05-11
ZHEJIANG XINHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the dialkyl phosphinate products prepared by the general method are mostly random structures or spherical structures, with large specific surface area and low surface energy, and are prone to agglomeration in the material matrix, resulting in a decrease in the mechanical properties of the material and flame retardant performance. low level problem

Method used

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  • Dialkyl phosphinate as well as preparation method and application thereof
  • Dialkyl phosphinate as well as preparation method and application thereof
  • Dialkyl phosphinate as well as preparation method and application thereof

Examples

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preparation example Construction

[0031] like figure 1 As shown, the preparation method of dialkyl phosphinate according to one embodiment of the present invention includes the following steps S1-S2:

[0032] S1. Mix the metal salt solution, the mesoporous template agent and the alkali to carry out the metathesis reaction to obtain the template-loaded metal hydroxide. The specific surface area of ​​the mesoporous template is 100m 2 / g~450m 2 / g, the pore diameter is 1nm~10nm.

[0033] S2. Neutralizing the dialkylphosphinic acid and the metal hydroxide supported on the template to obtain a dialkylphosphinic acid salt.

[0034] The traditional preparation method uses dialkyl phosphinate and metal salt for metathesis reaction. In this process, a large amount of inorganic salt by-products will inevitably be produced, which increases the processing cost, and there is a problem that the crystal particles cannot be controlled, which leads to subsequent When used, agglomeration and precipitation are prone to occur...

Embodiment 1

[0044] With 4440g 15wt% 18 water aluminum sulfate aqueous solution and 20g mesoporous alumina (mesoporous specific surface area is 150m 2 / g, the pore diameter is 2nm) in a 10L three-necked flask for rapid stirring and dispersing and heating up, at 65°C, 2400g of 10wt% sodium hydroxide solution was added dropwise for neutralization, and the solid product was filtered and washed with water. The obtained solid product was mixed with 2500g of 30wt% diethylphosphinic acid aqueous solution and reacted at 115°C and 0.5MPa for 2h to obtain fibrous rod-shaped aluminum diethylphosphinate, the product quality was 752g, and the micrograph was as follows: figure 1 and figure 2 shown.

Embodiment 2

[0046] With 2664g 25wt% 18 water aluminum sulfate aqueous solution and 25g mesoporous aluminum phosphite (mesoporous specific surface area is 450m 2 / g, pore diameter is 10nm) in a 10L three-necked flask, stir rapidly to disperse and heat up, add dropwise 2400g of 10wt% sodium hydroxide solution to neutralize at 65°C, and the solid product is filtered and washed with water. The obtained solid product was mixed with 2500 g of 30 wt % diethylphosphinic acid aqueous solution, and then reacted at 75° C. and 0.1 MPa for 3 hours to obtain fibrous rod-shaped aluminum diethylphosphinate with a product quality of 734 g.

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Abstract

The invention relates to dialkyl phosphinate as well as a preparation method and application thereof. The preparation method comprises the following steps of: mixing a metal salt solution, a mesoporous template agent and alkali for double decomposition reaction to obtain template-loaded metal hydroxide; and carrying out a neutralization reaction on dialkyl phosphinic acid and the template-loaded metal hydroxide to obtain the dialkyl phosphinate. According to the preparation method of the dialkyl phosphinate, double decomposition reaction is performed on inorganic metal salt and alkali under the action of a mesoporous template agent to form template-loaded metal hydroxide, and then neutralization reaction is performed on the template-loaded metal hydroxide and dialkyl phosphinic acid to obtain the fiber rod-shaped dialkyl phosphinate. As the mesoporous template agent has higher heat resistance and a pore structure, the larger specific surface area is beneficial to loading of the dialkyl phosphinate in the reaction process, and meanwhile, the dialkyl phosphinate can be changed into fibrous crystals from an irregular agglomeration form.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a dialkyl phosphinate and its preparation method and application. Background technique [0002] Fire prevention is an eternal theme of human social security. Most of the polymer materials widely used in industry, agriculture and people's life are combustible and combustible in the air, and their limiting oxygen index is mostly lower than 21%. Therefore, a considerable part of the fires that have occurred in various countries in recent decades is caused by the ignition of polymer materials. Moreover, the composition of modern synthetic polymer materials is different from that of natural polymer materials. The former can produce a large amount of toxic and corrosive gaseous products and smoke during thermal cracking and combustion, so their consequences in fires are even more serious. In view of this, countries all over the world are paying great attention to the flame...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30C08K5/5313
CPCC07F9/301C08K5/5313
Inventor 应思斌章震谢自强周健祝航陈攀洪晔叶菁吴杨杨王超远
Owner ZHEJIANG XINHUA CHEM
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