Preparation method of polyphosphoester

A technology of polyphosphate and phosphorus oxychloride, which is applied in the field of polyphosphate preparation, can solve problems such as the method of reducing the formation of acid phosphate, and achieve the effects of low toxicity, lower production costs, and less side reactions

Inactive Publication Date: 2019-07-30
HUAIHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Also this patent does not mention the method of reducing the formation of acidic phosphate

Method used

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  • Preparation method of polyphosphoester
  • Preparation method of polyphosphoester
  • Preparation method of polyphosphoester

Examples

Experimental program
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Embodiment 1

[0031] Embodiment 1, a kind of preparation method of polyphosphate: obtain polyphosphate by one-step method of phosphorus oxychloride, dialkylphenol and hydroquinone, end-capping by phenol at last; The general formula of dialkylphenol is as formula I show:

[0032]

[0033] In formula I: the R 1 , R 2 selected from 2,3-dialkylphenol, 2,4-dialkylphenol, 2,5-dialkylphenol or 2,6-dialkylphenol.

[0034] The method first generates monomeric monophenyl ester from phosphorus oxychloride and dialkylphenol, then polymerizes hydroquinone to obtain a polyphospholipid intermediate, and then caps it with phenol; the degree of polymerization is 1-20; phosphorus oxychloride The molar ratio of dialkylphenol to dialkylphenol is 0.5:1; the molar ratio of hydroquinone to phosphorus oxychloride is 0.8:1.

[0035] The catalyst used in the reaction is AlCl 3 , the consumption of catalyst is 0.05% of dialkylphenol mass. The solvent used in the reaction is carbon tetrachloride. The solvent ...

Embodiment 2

[0036] Embodiment 2, a kind of preparation method of polyphosphate: obtain polyphosphate by one-step method of phosphorus oxychloride, dialkylphenol and hydroquinone, end-capping by phenol at last; The general formula of dialkylphenol is as formula I show:

[0037]

[0038] In formula I: R 1 , R 2 for the same or different linear C 1 -C 5 -alkyl.

[0039] The R 1 , R 2selected from 2,3-dialkylphenol, 2,4-dialkylphenol, 2,5-dialkylphenol or 2,6-dialkylphenol.

[0040] The method first generates monomeric monophenyl ester from phosphorus oxychloride and dialkylphenol, then polymerizes hydroquinone to obtain a polyphospholipid intermediate, and then caps it with phenol; the degree of polymerization is 1-20; phosphorus oxychloride The molar ratio of dialkylphenol to dialkylphenol is 1.5:1; the molar ratio of hydroquinone to phosphorus oxychloride is 5:1.

[0041] The catalyst used in the reaction is MgCl 2 . The amount of catalyst used is 1% of the mass of dialkylphen...

Embodiment 3

[0042] Embodiment 3, a kind of preparation method of polyphosphate: obtain polyphosphate by one-step method of phosphorus oxychloride, dialkylphenol and hydroquinone, end-capping by phenol at last; The general formula of dialkylphenol is as formula I show:

[0043]

[0044] In formula I: R 1 , R 2 for the same or different linear C 1 -C 5 -alkyl.

[0045] The R 1 , R 2 selected from 2,3-dialkylphenol, 2,4-dialkylphenol, 2,5-dialkylphenol or 2,6-dialkylphenol.

[0046] The method first generates monomer monophenyl ester from phosphorus oxychloride and dialkylphenol, then polymerizes polyphospholipid intermediate by hydroquinone, and then caps it with phenol; the degree of polymerization is 15; phosphorus oxychloride and dialkylphenol The molar ratio of alkylphenol is 1:1; the molar ratio of hydroquinone and phosphorus oxychloride is 2:1.

[0047] The catalyst used in the reaction is a Lewis acid catalyst. Described Lewis acid catalyst is ZnCl 2 . The amount of cat...

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Abstract

The invention relates to a preparation method of polyphosphoester. According to the method, phosphorus oxychloride, dialkyl phenol and hydroquinone are prepared into polyphosphoester through a one-step method, and finally the polyphosphoester is terminated by using phenol. The method includes the steps that the phosphorus oxychloride and the dialkyl phenol are used for generating monomer monophenyl ester, then polymerization is conducted through the hydroquinone to obtain a poly-phospholipid intermediate, and the intermediate is terminated by using phenol. The polymerization degree is 1-20. The method is carried out at normal pressure according to synthesis conditions, the process is simple, the safety coefficient is high, and the polyphosphoester is wide in application range, can serve asa solid flame retardant, has the advantages of being resistant to volatilization, migration and radiation, high in heat resistance, good in compatibility, low in toxicity and durable in flame retardant effect, can serve as a plasticizer for materials, and has the advantages of being high in toughness, small in brittleness and capable of improving the mechanical properties such as material notch impact strength.

Description

technical field [0001] The invention relates to a preparation method of a flame retardant, in particular to a preparation method of polyphosphate. Background technique [0002] With the progress of society, people pay more and more attention to environmental protection, especially strict requirements for the chemical industry, which need to achieve safety, environmental protection, energy saving and emission reduction, etc. Therefore, products with low safety factor, heavy pollution and complex production process Look for alternative products or process improvements. There are many reports on the preparation methods of phosphate esters. Most monophosphate esters are liquids. Because of their small molecular weight, high vapor pressure, low decomposition temperature, easy precipitation, and poor thermal stability, they are easy to volatilize and decompose during plastic processing, making plastics The mechanical properties of the product are greatly affected. All of these h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/04
CPCC08G79/04
Inventor 武宝萍安红高树刚刘大鹏张斐然马观奇
Owner HUAIHAI INST OF TECH
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