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Polyphosphoester containing fluorine and silicon as well as preparation method and application thereof

A technology of silicon polyphosphate and cyclic phosphate, which is applied in the field of organic flame retardant materials, can solve the problems of poor compatibility, inability to expand the application fields of flame retardants and polymer materials, and single function, so as to reduce surface energy, Improve the protective effect and enhance the effect of the carbon layer structure

Active Publication Date: 2017-05-31
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most flame retardants still have the defect of poor compatibility with the matrix resin, and the function of the flame retardant to modify the matrix is ​​single, which cannot expand the application fields of flame retardants and polymer materials.

Method used

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  • Polyphosphoester containing fluorine and silicon as well as preparation method and application thereof
  • Polyphosphoester containing fluorine and silicon as well as preparation method and application thereof
  • Polyphosphoester containing fluorine and silicon as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Add 8.00g (9.14mmol) aminopropyl cage polysilsesquioxane (NH 2 -POSS), 1.12g (11.06mmol) triethylamine and 25mL dichloromethane, then slowly drop 1.96g (13.75mmol) 2-chloro-2-oxo-1,3,2-dioxaphosphine Pentane, reacted at room temperature for 8 hours; then filtered to remove triethylamine hydrochloride, repeatedly quenched the obtained filtrate with water, took the organic phase and dried it with anhydrous magnesium sulfate, filtered it with suction, and rotary evaporated to remove the solvent to obtain a silicon-containing cyclic phosphate monomer.

[0034] (2) Take 6.08g (6.20mmol) of the silicon-containing cyclic phosphate monomer obtained in step (1) in a single-mouth bottle, add 13.60mg (0.10mmol) tetrafluoropropanol, 20.00mg (0.04mmol) isooctanoic acid sulfide Tin and 10mL tetrahydrofuran, heated up to 80°C, reacted for 6h, after the reaction was completed, the solvent was spin-dried to obtain fluorine-containing silicon polyphosphate (such as figure 1 shown)....

Embodiment 2

[0039] (1) The synthesis of silicon-containing cyclic phosphate monomer is the same as in Example 1.

[0040] (2) The synthesis of fluorine-containing silicon polyphosphate is the same as in Example 1.

[0041] (3) Weigh 20g of epoxy resin prepolymer and heat up to 90°C, add 6.26g of fluorine-containing silicon polyphosphate obtained in step (2), stir until the mixture is uniform and transparent, add 5.05g of DDM until completely dissolved, Pour it into an aluminum mold, cure at 120°C for 4 hours, at 140°C for 2 hours, and at 180°C for 2 hours to obtain a flame-retardant epoxy resin.

[0042] According to GB / T 2406-2009, the oxygen index of the above-mentioned flame-retardant epoxy resin is 33.1%.

[0043] According to GB / T 30693-2014, the water contact angle of the above-mentioned flame-retardant epoxy resin is 90.5°.

Embodiment 3

[0045] (1) The preparation of the silicon-containing cyclic phosphate monomer is the same as in Example 1.

[0046] (2) Take 6.08g (6.20mmol) of the silicon-containing cyclic phosphate monomer obtained in step (1) in a one-mouth bottle, add 24.41mg (0.10mmol) of 3,5-bis(trifluoromethyl)benzyl alcohol, 20.00 mg (0.04 mmol) of stannous isooctanoate and 10 mL of tetrahydrofuran were heated up to 80°C and reacted for 6 hours. After the reaction, the solvent was spin-dried to obtain fluorine-containing silicon polyphosphate.

[0047] (3) Weigh 20g of epoxy resin prepolymer and raise the temperature to 90°C, add 2.78g of fluorine-containing silicon polyphosphate obtained in step (2), stir until it is uniform and transparent, then add 5.05g of DDM until completely dissolved, Then pour it into an aluminum mold, cure at 120°C for 4 hours, at 140°C for 2 hours, and at 180°C for 2 hours to obtain a flame-retardant epoxy resin.

[0048] According to GB / T 2406-2009, the oxygen index of th...

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Abstract

The invention discloses a polyphosphoester containing fluorine and silicon as well as a preparation method and an application thereof. The chemical formula structure of the polyphosphoester containing fluorine and silicon is expressed as a formula which is shown in description, wherein R1 is selected from a chemical formula which is shown in description, a chemical formula which is shown in description or a chemical formula which is shown in description; R2 is selected from a chemical formula which is shown in description or a chemical formula which is shown in description; n is 10-100. According to the polyphosphoester containing fluorine and silicon, phosphorus, fluorine and silicon elements are used for resisting flame; the phosphorus element is capable of catalyzing a system to form a phosphorus-enriched carbon layer, so that the effect of a protection layer is achieved, and thus the further decomposition of epoxy resin is prevented; silicon-containing epoxy resin can form a carbon layer containing silicon dioxide in the combustion process, so that the carbon layer structure is enhanced, and thus the protection effect of the carbon layer is further improved; through introduction of the fluorine element, the heat stability of the epoxy resin can be improved, so that the flame resistance of the system is improved.

Description

technical field [0001] The invention belongs to the technical field of organic flame-retardant materials, and in particular relates to a fluorine-containing silicon polyphosphate and a preparation method and application thereof. Background technique [0002] Most polymer materials are flammable, and many fires are caused by the combustion of polymer materials, which brings great harm to people's lives. In order to improve the flame retardant properties of polymer materials, the application of flame retardants has also been on the rise. A highly efficient flame retardant is prepared to improve the flame retardant properties of materials, or to endow materials with new materials while improving flame retardant properties. Performance research is still a challenging subject. [0003] CN201410680503.8 discloses a phosphorus-silicon composite flame retardant, which utilizes caged heptaphenyltrisiliconphosphorussilsesquioxane to be applied to the flame retardancy of silicone rubb...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/04C08G77/42C08G77/395C08L63/00C08L85/02
CPCC08G77/395C08G77/42C08G79/04C08L63/00C08L2201/02C08L85/02C08G59/5033C07F9/2458C08G77/26C08G77/24C08G77/80C08G77/30C08K5/17C08K5/5313C08L83/08C08K5/0066C07F9/098C08G59/245C08G59/4071C08G59/56C08G77/46
Inventor 戴李宗陈婷刘诚王世成陈国荣袁丛辉许一婷曾碧榕罗伟昂何凯斌
Owner XIAMEN UNIV
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