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Diphenolic acid-based polyphosphate ester flame retardant containing DOPO structure and preparation method of flame retardant

A technology of bisphenolic acid-based polyphosphate and polyphosphate, applied in the field of polyphosphate and its preparation, can solve the problems of low flame retardant efficiency, toxic gas, poor thermal stability, etc. The effect of beneficial combustion performance and complex structural design

Inactive Publication Date: 2017-05-24
NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the halogen-based flame retardant system based on gas phase flame retardant has a good flame retardant effect, it releases toxic and corrosive gases during combustion, which poses great hidden dangers to humans and the environment, and has been gradually restricted. or prohibit the use of
Compared with halogenated flame retardants, inorganic flame retardants based on endothermic flame retardants and intumescent flame retardants based on condensed phase flame retardants are environmentally friendly "green" flame retardants recognized by the scientific and industrial circles. agent, but this type of flame retardant often requires a higher addition amount (inorganic type is usually not less than 40wt%, phosphorus-containing type is not less than 30wt%) to make the material achieve the expected flame retardant effect, and the flame retardant efficiency is low. It will also lead to greater damage to the mechanical properties and processing properties of the material; at the same time, poor thermal stability and low decomposition temperature will cause difficulties in the processing and recycling of flame-retardant polymers

Method used

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  • Diphenolic acid-based polyphosphate ester flame retardant containing DOPO structure and preparation method of flame retardant
  • Diphenolic acid-based polyphosphate ester flame retardant containing DOPO structure and preparation method of flame retardant
  • Diphenolic acid-based polyphosphate ester flame retardant containing DOPO structure and preparation method of flame retardant

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 28.6 g of bisphenolic acid (DPA; 4,4-di(4-hydroxyphenyl)pentanoic acid, CAS No. 126-00-1) and 9,10-dihydro-9-oxa- 10-phosphaphenanthrene-10-hydroxymethyl-10-oxide (ODOPM) 24.6g, concentrated sulfuric acid 5g, DMF 100mL. Protected by nitrogen gas, the reaction was refluxed for 40 hours under mechanical stirring. During this period, part of the azeotrope of DMF and water was distilled off five times, and then a corresponding volume of DMF was added to finally obtain a yellow transparent solution. The solvent was removed by rotary evaporation to obtain a crude product.

[0034] The crude product was added to deionized water at 100 °C to remove impurities. TLC was used to track until there was no bisphenolic acid in the upper layer of water, and then the product was filtered and vacuum-dried at 80° C. for 10 hours. Monomer (II) is obtained. (That 1 H NMR and FTIR spectra are attached figure 1 )

[0035] Synthesis of polyphosphate (Ⅲ): Add 25.7 g of monomer (II) a...

Embodiment 2

[0041] Add 28.6g of bisphenolic acid, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-hydroxymethyl-10-oxide (ODOPM) 22g, concentrated sulfuric acid 5.5g, DMF100mL, under nitrogen protection, reflux reaction for 35 hours under mechanical stirring. During this period, part of the azeotrope of DMF and water was distilled off seven times, and then a corresponding volume of DMF was added to obtain a yellow transparent solution. The solvent was removed by rotary evaporation to obtain a crude product.

[0042]The crude product was added into deionized water at 100°C for purification. TLC was used to track until there was no bisphenolic acid in the upper layer of water, and then the product was filtered and vacuum-dried at 80° C. for 10 hours. Monomer (II) is obtained.

[0043] Synthesis of polyphosphate (IV): Add 25.7 g of monomer (II) and 110 mL of ethyl acetate into a 250 mL three-necked flask, and flush with nitrogen gas for 10 minutes. Slowly raise the temperature to 40°C. Slo...

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Abstract

The invention provides a diphenolic acid-based polyphosphate ester flame retardant containing a DOPO structure and a preparation method of the flame retardant. The prepared polyphosphate ester is high in phosphorus content, a good flame retarding effect can be achieved when the adding amount of the flame retardant is lower than 12 wt%, the using amount is far less than that of a traditional phosphorous flame retardant, and the efficient, green and environment-friendly flame retardant is obtained. The flame retardant has the advantages that compared with a condensed phase flame retardant group, the DOPO structure is more excellent in heat resistance, can play a flame retarding role in a gas phase and has a good flame retarding effect on epoxy; by considering that PLA is degraded in the processing process due to the end phosphate ester group, the phosphate ester group is enclosed by two benzene ring, and therefore the final mechanical property destruction degree of the material is greatly decreased; the structural general formula of the flame retardant is shown as the formula (I) in the description, wherein n is 3-20, and the R group is a phenyl group or phenoxy group.

Description

technical field [0001] The invention relates to a polyphosphate and a preparation method thereof. This type of polyphosphate can be used as an efficient flame retardant in the field of flame retardancy, in particular to a bisphenolic acid-based polyphosphate flame retardant containing a DOPO structure and its preparation method. Background technique [0002] At present, the basic research and application development of flame retardant materials at home and abroad are very active. Although the halogen-based flame retardant system based on gas phase flame retardant has a good flame retardant effect, it releases toxic and corrosive gases during combustion, which poses great hidden dangers to humans and the environment, and has been gradually restricted. or prohibited. Compared with halogenated flame retardants, inorganic flame retardants based on endothermic flame retardants and intumescent flame retardants based on condensed phase flame retardants are environmentally friendl...

Claims

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Application Information

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IPC IPC(8): C08G79/04C08L67/04C08L85/02
Inventor 井健张艳方征平
Owner NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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