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Macromolecular flame retardant, preparation method and application thereof

A technology of flame retardants and macromolecules, used in the preparation and application of flame retardants, can solve problems such as performance loss, complex process, and large reaction steric hindrance

Active Publication Date: 2021-05-18
湖南美莱珀科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It solves the problems of large steric hindrance and poor reactivity in the polymerization reaction of DOPO derivatives in the prior art
[0008] The high-molecular-weight phosphonate polymer prepared by the present invention can also be used alone as an additive flame retardant without further polymerization and application, which solves the problems of performance loss and process complexity caused by intrinsic flame-retardant polymer materials, and overcomes the Small molecule added flame retardants are easy to migrate and not durable, which is an ideal choice for flexible preparation of flame retardant materials

Method used

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  • Macromolecular flame retardant, preparation method and application thereof
  • Macromolecular flame retardant, preparation method and application thereof
  • Macromolecular flame retardant, preparation method and application thereof

Examples

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Embodiment 1

[0060] A preparation method of a macromolecular flame retardant, comprising the steps of:

[0061] (1) Substance A and substance B are added in thionyl chloride respectively, wherein, the amount of substance of thionyl chloride is 3.4 times of the sum of the amount of substance of substance A and substance B, respectively heating Reflux for 0.5 hours, then evaporate to dryness thionyl chloride to obtain the acid chloride of A and the acid chloride of B respectively; wherein, substance A is [(6-oxo-6H-dibenzo[c,e][1,2 ]oxaphosphorin-6-yl)methyl]succinic acid, substance B is HOOC-COOH;

[0062] (2) Mix the acid chloride of A, the acid chloride of B, substance C, substance D, and a catalyst to react, control the reaction temperature to 220°C, and the reaction time is 16 hours, and obtain a macromolecular flame retardant after cooling; Among them, substance C is α,α'-bis(6-oxo-6H-dibenzo[c,e][1,2]oxaphosphorin-6-yl)-1,4-benzenedimethanol , the substance D is D-1, the catalyst is...

Embodiment 2

[0066] A preparation method of a macromolecular flame retardant, comprising the steps of:

[0067] (1) Substance A and substance B are added in thionyl chloride respectively, wherein, the amount of substance of thionyl chloride is 3.1 times of the sum of the amount of substance of substance A and substance B, respectively heating Reflux for 1 hour, then evaporate to dryness thionyl chloride, obtain the acid chloride of A and the acid chloride of B respectively; Wherein, material A is [(6-oxo-6H-dibenzo[c,e][1,2 ]oxaphosphorin-6-yl)methyl]succinic acid, substance B is HOOC(CH 2 ) 4 COOH;

[0068] (2) Mix the acid chloride of A, the acid chloride of B, substance C, substance D and the catalyst to react, control the reaction temperature to 180°C, and the reaction time is 24 hours, and obtain a macromolecular flame retardant after cooling; Among them, substance C is α,α'-bis(6-oxo-6H-dibenzo[c,e][1,2]oxaphosphorin-6-yl)-1,4-benzenedimethanol , the substance D is D-2, and the c...

Embodiment 3

[0071] A preparation method of a macromolecular flame retardant, comprising the steps of:

[0072] (1) Substance A and substance B are added in thionyl chloride respectively, wherein, the amount of substance of thionyl chloride is 9.4 times of the sum of the amount of substance of substance A and substance B, respectively heating Reflux for 5 hours, then evaporate to dryness thionyl chloride, obtain the acid chloride of A and the acid chloride of B respectively; Wherein, material A is [(6-oxo-6H-dibenzo[c,e][1,2 ]oxaphosphorin-6-yl)methyl]succinic acid, substance B is

[0073] (2) react after mixing the acid chloride of A, the acid chloride of B, substance C, substance D and the catalyst, control the reaction temperature to 200°C, and the reaction time is 20 hours, and obtain the macromolecular flame retardant after cooling; Among them, substance C is α,α'-bis(6-oxo-6H-dibenzo[c,e][1,2]oxaphosphorin-6-yl)-1,4-benzenedimethanol , the substance D is D-3, and the catalyst is ...

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PUM

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Abstract

The invention relates to a macromolecular flame retardant, a preparation method and application thereof. The preparation method comprises the following steps: firstly, performing acylating chlorination on a compound with dicarboxyl, and then promoting a polymerization reaction by using a special catalyst. According to the invention, aromatic hydrocarbon diol with a DOPO structure and dibasic acid are adopted to synthesize a phosphonate ester polymer with high thermal stability and a macromolecular structure, and a method for solving the problem that a phosphaphenanthrene derivative is large in reaction steric hindrance and difficult to polymerize to obtain a high-molecular-weight polymer is developed; the flame retardant disclosed by the invention can be independently used as an additive flame retardant, so that the problems of performance loss and process complexity caused by intrinsic flame retardance can be avoided, the defect that micromolecule additive flame retardance is not durable can be overcome, and the flame retardant is an ideal choice for flexible preparation of flame-retardant materials; and the flame retardant cannot be separated out to the surface along with thermal cracking of a matrix, and a cross-linked high polymer network can be formed in the matrix to hinder overflow of flammable volatile matter, so that the total combustion heat release amount and the heat release rate peak value are reduced, and the flame retardant effect is achieved.

Description

technical field [0001] The invention belongs to the technical field of flame retardant preparation and application, and relates to a macromolecular flame retardant and its preparation method and application. Background technique [0002] Phosphophenanthrene (DOPO) derivative flame retardant is a kind of flame retardant with good flame retardant effect, economical and environmental protection, which is in line with the future development of flame retardant industry. Through exploration, it is found that some phosphaphenanthrene derivatives, such as DDP and DOPO-HQ, have certain reactivity due to the presence of carboxyl or hydroxyl groups on their molecules, and can undergo esterification reactions to introduce DOPO groups into macromolecular segments. [0003] Document 1 (A Novel Phosphorus-Containing Poly(ethylene terephthalate) Nanocomposite with Both Flame Retardancy and Anti-Dripping Effects[J].Macromolecular Materials and Engineering,2006,291(6):638-645.), the researche...

Claims

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Application Information

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IPC IPC(8): C08G63/692C08L23/06C08L23/12C08L27/06C08L55/02C08L69/00C08L77/02C08L77/06C08L53/02C08L101/00C08L75/04C08L67/02
CPCC08G63/6926C08L23/06C08L23/12C08L27/06C08L55/02C08L69/00C08L77/02C08L77/06C08L53/02C08L53/025C08L101/00C08L75/04C08L2201/02C08L2207/066C08L2207/062C08L2205/03C08L67/02Y02P20/52
Inventor 彭治汉赵勇帅郭承鑫姬贵晨陈帅李颖颖彭志宏彭治权
Owner 湖南美莱珀科技发展有限公司
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