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Polymeric intumescent flame retardant and preparation method thereof

An intumescent flame retardant, polymeric technology, applied in the field of polymeric intumescent flame retardants and preparations, can solve the problems of poor matrix compatibility, poor thermal stability, low molecular weight, etc., and achieve stable reaction, high molecular weight, The effect of simple preparation process

Inactive Publication Date: 2018-12-28
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a polymeric intumescent flame retardant and its preparation method in order to solve the problems of low relative molecular weight, large addition amount, poor compatibility with the matrix and poor thermal stability in the existing intumescent flame retardants.

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  • Polymeric intumescent flame retardant and preparation method thereof
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  • Polymeric intumescent flame retardant and preparation method thereof

Examples

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Embodiment 1

[0024] A polymeric intumescent flame retardant, the structural formula is:

[0025]

[0026] Wherein the degree of polymerization n is an integer between 5-200.

[0027] A kind of preparation method of polymerization type intumescent flame retardant, concrete steps are as follows:

[0028] Weigh 10.2g (0.075mol) of pentaerythritol in a 250mL four-neck flask, add 34.5g (0.225mol) of freshly distilled phosphorus oxychloride and 50mL of anhydrous acetonitrile, connect the thermometer, mechanical stirrer, condenser tube and tail gas absorption device. Under a nitrogen atmosphere, mix at room temperature until the system is stable, then slowly raise the temperature to 80° C., and react until no HCl gas is released (reaction ends). Cool to room temperature, filter the obtained precipitate with suction, wash several times with dichloromethane, acetone or chloroform, and dry in vacuum at 80°C for 12 hours to obtain 20.9 g of a white powdery solid intermediate, which is spirocycli...

Embodiment 2

[0032] A polymeric intumescent flame retardant, the structural formula is:

[0033]

[0034] Wherein the degree of polymerization n is an integer between 5-200.

[0035] A kind of preparation method of polymerization type intumescent flame retardant, concrete steps are as follows:

[0036] Weigh 13.6g (0.1mol) of pentaerythritol in a 250mL four-neck flask, add 53.6g (0.35mol) of freshly distilled phosphorus oxychloride and 70mL of anhydrous acetonitrile, connect the thermometer, mechanical stirrer, condenser tube and tail gas absorption device. Under a nitrogen atmosphere, mix at room temperature until the system is stable, then slowly raise the temperature to 80° C., and react until no HCl gas is released (reaction ends). Cool to room temperature, filter the obtained precipitate with suction, wash several times with dichloromethane, acetone or chloroform, and dry in vacuum at 80°C for 12 hours to obtain 27.9 g of a white powdery solid intermediate, which is spirocyclic p...

Embodiment 3

[0039] A polymeric intumescent flame retardant, the structural formula is:

[0040]

[0041] Wherein the degree of polymerization n is an integer between 5-200.

[0042] A kind of preparation method of polymerization type intumescent flame retardant, concrete steps are as follows:

[0043] Weigh 20.4g (0.15mol) of pentaerythritol in a 500mL four-neck flask, add 91.8g (0.6mol) of freshly distilled phosphorus oxychloride and 90mL of toluene, and connect the thermometer, mechanical stirrer, condenser and tail gas absorption device . Under a nitrogen atmosphere, mix at room temperature until the system is stable, then slowly raise the temperature to 105° C., and react until no HCl gas is released (reaction ends). Cool to room temperature, filter the obtained precipitate with suction, wash several times with dichloromethane, acetone or chloroform, and dry in vacuum at 80°C for 12 hours to obtain 41.9 g of a white powdery solid intermediate, which is spirocyclic phosphate dichl...

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Abstract

The invention relates to a polymeric intumescent flame retardant and a preparation method thereof and belongs to the technical field of phosphorus-containing flame retardants. The structural formula is as shown in the description. In the formula, the polymerization degree n is an integer of 5-200. The preparation method comprises the following steps: adding pentaerythritol and just distilled phosphorus oxychloride into a solvent A under inert gas shielding, mixing at a room temperature until the system is stabilized, slowly raising the temperature until no hydrogen chloride gas is released, washing, performing suction filtration, and drying to obtain an intermediate spironophosphoryl dichloride; adding 2-imidazolidinone into a solvent B, stirring until the solution is clarified and transparent, adding the intermediate spironophosphoryl dichloride, stirring until the system is uniformly mixed, reacting at a temperature of 50 DEG C for 2 hours, adding an acid-binding agent, washing afterreaction completion, performing suction filtration, and drying, thereby obtaining the polymeric intumescent flame retardant. The polymeric intumescent flame retardant provided by the invention is high in molecular weight, narrow in molecular weight distribution and excellent in compatibility with the matrix, and has excellent heat stability and high flame-retardant efficiency.

Description

technical field [0001] The invention relates to a polymeric intumescent flame retardant and a preparation method thereof, belonging to the technical field of phosphorus-containing flame retardants. Background technique [0002] Materials treated with halogenated flame retardants release a large amount of toxic and corrosive gases when burned, posing a huge threat to the environment and life safety. The successive issuance of WEEE, RoHS, EuP and other directives has made halogenated flame retardants face Unprecedented challenges. Phosphorus-based flame retardants have high flame retardant efficiency, but there is a serious problem of plasticizing materials; nitrogen-based flame retardants have the advantages of low toxicity and low corrosion, but they have poor dispersion in polymers and low flame retardant efficiency. high. Combining the advantages of phosphorus and nitrogen, intumescent flame retardants can be prepared, which have become a hot research topic due to their ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/04C08L85/02C08L63/00
CPCC08G79/04C08L63/00C08L85/02C08L2201/02C08L2201/08
Inventor 刘吉平阮方王银杰
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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