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Preparation method of phosphonitrile polymeric flame retardant

A technology of polymer flame retardant and phosphazene, which is applied in the field of preparation of polymer flame retardant, can solve the problems of the influence of mechanical properties of flame retardant materials, different flame retardants, etc., and achieves extensive research and application prospects, good thermal performance effect

Inactive Publication Date: 2019-09-06
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the phosphazene flame retardants in the domestic market are limited, and they are all small molecule flame retardants. Although they have high flame retardant efficiency, they have a certain impact on the mechanical properties of flame retardant materials.
In fact, different materials have different requirements for flame retardants. At present, there is no flame retardant that is completely suitable for polyurethane in the market.

Method used

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  • Preparation method of phosphonitrile polymeric flame retardant
  • Preparation method of phosphonitrile polymeric flame retardant
  • Preparation method of phosphonitrile polymeric flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Into a 250ml three-necked flask, add 40ml of THF after dehydration and 4.32g of NaH in sequence, pass nitrogen protection, and stir magnetically throughout. Add 11.16g of ethylene glycol dropwise into the three-necked flask with a dropping funnel, and the dropping rate can be controlled at every two seconds. After the dropwise addition, the temperature was raised to 60°C, and the reaction was continued for 2 hours to obtain monosodium ethylene glycol.

[0030] Another 250ml three-neck flask was taken, and 40ml of THF after dehydration and 4.32gNaH were successively added into the three-necked flask, protected by nitrogen gas, and magnetically stirred throughout. 8.28g of ethanol was added dropwise into the three-necked flask with a dropping funnel, and the rate of addition was controlled at one drop every two seconds. After the dropwise addition, the temperature was raised to 60°C, and the reaction was continued for 2 hours to obtain sodium ethoxide.

[0031] The prep...

Embodiment 2

[0033] Add 40ml of THF and 4.32g of NaH after dehydration to a 250ml three-necked flask in sequence, and pass nitrogen gas for five minutes to remove the air in the flask, and stir magnetically throughout. Add the phenol tetrahydrofuran solution dropwise into the three-necked flask with a dropping funnel. Note that the melting point of phenol is 43°C, and it is solid at room temperature. Therefore, it is heated and dissolved in tetrahydrofuran before weighing and added dropwise. After the dropwise addition was completed, the temperature was raised to 60° C., and the reaction was continued for 2 h to obtain sodium phenoxide. Dissolve HCCP in tetrahydrofuran and add dropwise into the mixed solution of sodium phenate and monosodium ethylene glycol. The molar ratio of the reaction feed is HCCP: sodium phenate: monosodium ethylene glycol = 1:3:3. After the dropwise addition, the temperature was raised to 60° C., stirred by magnetic force, and the reaction was continued for 12 hours...

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Abstract

The invention provides a preparation method of a phosphonitrile polymeric flame retardant. According to the method, from a molecule design angle, two specific substituent groups are introduced on phosphonitrilic chloride trimer, a ring phosphonitrile derivative with polyhydroxyl is obtained, and through a polyaddition reaction of the derivative and isocyanate, the polymeric flame retardant with aphosphonitrile ring is synthesized. The phosphonitrile polymeric flame retardant is used for flame-retardant modification on materials such as polyurethane and is efficient and environmentally friendly, and the compatibility of the flame retardant and the materials is good. According to the technical scheme, aryloxy or alkoxy and ethylene glycol single sodium with different molar ratios are used as nucleophilic agents, two or more hydroxyl functional groups are introduced to the phosphonitrilic chloride trimer and further react with diisocyanate, and phosphonitrile polyurethane is synthesized.The phosphonitrile polyurethane is used as the polymeric flame retardant for modifying thermoplastic polyurethane (TPU), the LOI value of modified TPU reaches 27.7%, and the flame-retardant level reaches UL94V-0.

Description

technical field [0001] The invention discloses a method for preparing a polymer flame retardant containing a phosphazene ring. The polymer flame retardant obtained by this method has the advantages of high efficiency, low toxicity, low migration, and good system compatibility. , the loss of mechanical properties is small, and the performance is not affected. [0002] technical background [0003] Phosphazene compounds have been researched and developed for hundreds of years since they were synthesized, and have been used in a wide range of fields such as military materials in the United States. There are also applied research in various fields in China, especially in the field of flame retardancy. However, the phosphazene flame retardants in the domestic market are limited, and all of them are small molecule flame retardants. Although they have high flame retardant efficiency, they have a certain impact on the mechanical properties of flame retardant materials. In fact, dif...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/32C07F9/6593C08L75/04C08K5/5399
CPCC07F9/65815C08G18/3889C08K5/5399C08L75/04C08L2201/02C08L2205/025
Inventor 王秀芬赵章启耿婷婷周克亮韩莹李妍赵跃龙
Owner BEIJING UNIV OF CHEM TECH
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