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Star-structure fluorine-containing phosphazene flow modifier and preparation method and application thereof

A technology of flow modifier and fluorine-containing phosphazene, which is applied in the field of flow modifier, can solve the problems of no improvement in the flame retardant performance of composite materials, limited processing flow performance, large molecular weight, etc., and achieves improved processing flow performance and dispersibility. The effect of improving and reducing the viscosity of the system

Active Publication Date: 2021-02-12
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Cao Bo et al. (Simultaneous improvement of processability and toughness of highly filled MH / LLDPEcomposites by using fluorine-containing flow modifiers. Composites Part A: Applied Science and Manufacturing, 2020, 134) combined methyl methacrylate with hexafluorobutyl methacrylate The random copolymers (PMFs) prepared by free radical emulsion polymerization are used in 80wt% magnesium hydroxide filled modified linear low density polyethylene blending system, which has great influence on the processing fluidity of the system and the toughness of the formed composite material. However, the flow modifier adopts free radical emulsion polymerization, has a relatively large molecular weight (a molecular weight of more than 100,000), and has no flame-retardant elements in its molecular structure. There is basically no improvement in the flame retardant performance

Method used

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  • Star-structure fluorine-containing phosphazene flow modifier and preparation method and application thereof
  • Star-structure fluorine-containing phosphazene flow modifier and preparation method and application thereof
  • Star-structure fluorine-containing phosphazene flow modifier and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Take 3.47g of hexachlorocyclotriphosphazene, 10.64g of methylparaben and 178mL of acetone in a 250ml three-neck flask, heat to 65°C, add 11.04g of potassium carbonate and react for 72h, cool, filter with suction, and place Dry in a vacuum oven at 70°C for 24 hours to obtain 8.15 g of a white solid product, which is hexa-(4-methoxy-phenoxy)-cyclotriphosphazene, with a yield of 57.8%;

[0038] (2), take 6.76g hexa-(4-carbocarboxylate-phenoxy)-cyclotriphosphazene and 145mL of methanol into a 250mL three-necked flask equipped with a condenser tube and a magnetic stirrer, then add 23mL of deionized water, React at 60°C for 9h under stirring, after cooling, adjust the pH value to 2 with hydrochloric acid, a white precipitate precipitates out of the solution, filter it with suction, and dry it in a vacuum oven at 70°C for 6h to obtain 6.39g of a white solid product, which is hexa- (4-carboxy-phenoxy)-cyclotriphosphazene, the yield is 94.5%;

[0039] (3) Take 1.44g of hexa...

Embodiment 2

[0046] (1) Take 3.47g of hexachlorocyclotriphosphazene, 10.64g of methylparaben and 143mL of acetone in a 250ml three-neck flask, heat to 60°C, add 12.4g of potassium carbonate and react for 96h, cool, filter with suction, and place Dry in a vacuum oven at 65°C for 24 hours to obtain 8.11 g of a white solid product, which is hexa-(4-methoxy-phenoxy)-cyclotriphosphazene, with a yield of 64.4%;

[0047] (2), take 6.76g hexa-(4-methoxy-phenoxy)-cyclotriphosphazene and 144mL methanol into a 250mL three-necked flask equipped with a condenser tube and a magnetic stirrer, then add 24mL deionized water, React at 60°C for 8h under stirring, after cooling, adjust the pH value to 3 with hydrochloric acid, a white precipitate precipitates out of the solution, filter it with suction, and dry it in a vacuum oven at 60°C for 6h to obtain 6.52g of white solid product, which is hexa- (4-carboxy-phenoxy)-cyclotriphosphazene, the yield is 96.4%;

[0048] (3) Take 1.44g of hexa-(4-carboxy-phenox...

Embodiment 3

[0052] (1) Take 3.47g of hexachlorocyclotriphosphazene, 9.12g of methylparaben and 115mL of tetrahydrofuran in a 250ml three-necked flask, heat to 70°C, add 11.04g of potassium carbonate and react for 72h, cool, filter with suction, and place Dry in a vacuum oven at 65°C for 24 hours to obtain 8.23 ​​g of a white solid product, which is hexa-(4-methoxy-phenoxy)-cyclotriphosphazene, with a yield of 65.4%;

[0053] (2), take 6.76g hexa-(4-carbocarboxylate-phenoxy)-cyclotriphosphazene and 150mL of methanol into a 250mL three-necked flask equipped with a condenser tube and a magnetic stirrer, then add 25mL of deionized water, React at 70°C for 9h under stirring, after cooling, adjust the pH value to 2 with hydrochloric acid, a white precipitate precipitates out of the solution, filter it with suction, and dry it in a vacuum oven at 65°C for 6h to obtain 6.48g of a white solid product, which is hexa- (4-carboxy-phenoxy)-cyclotriphosphazene, the yield is 95.9%;

[0054] (3) Take 1....

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Abstract

The invention discloses a star-structure fluorine-containing phosphazene flow modifier and a preparation method and application thereof. The preparation method comprises the following steps: dissolving hexachlorocyclotriphosphazene and methylparaben, heating, adding potassium carbonate, continuously reacting, cooling, carrying out suction filtration, and drying to obtain a solid product hexachlorocyclotriphosphazene-(4-methyl-phenoxy)-cyclotriphosphazene; mixing the obtained product with methanol, and then adding deionized water to react to obtain hexa-(4-carboxyl-phenoxy)-cyclotriphosphazene;dissolving the obtained product, heating to 80-90 DEG C, reacting, adding a solvent, fluoroalcohol, 4-dimethylaminopyridine and triethylamine, and reacting; and carrying out suction filtration and drying to obtain the star-structure fluorine-containing phosphazene flow modifier. Compared with an existing auxiliary agent, after the star-structure fluorine-containing phosphazene flow modifier is added, the balance torque of a system is reduced by 11.3%, the notch impact strength of the composite material is improved by 21.4%, and the limit oxygen index of the composite material is improved to 65.8% from 59.4%.

Description

technical field [0001] The invention relates to a flow modifier, in particular to a star-shaped structure fluorine-containing phosphazene flow modifier and its preparation method and application. The processing fluidity of the mixed system, the toughness of the composite material and the flame retardancy. Background technique [0002] The flame retardancy and thermal conductivity of polyolefins such as polyethylene and polypropylene usually need to add up to 50wt% of inorganic particles such as magnesium hydroxide, aluminum hydroxide, aluminum oxide, silicon carbide, etc. to achieve, when the inorganic particles When the filling amount is so high, the distance between the particles becomes smaller, and the possibility of particle aggregation increases, that is, the filler particles will be more obviously agglomerated in the polyolefin matrix. At this time, the interaction force between filler particles and particles will play a dominant role. The constant frictional resist...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6593C08L23/08C08K5/5399C08K3/22
CPCC07F9/65815C08K5/5399C08K3/22C08L2201/02C08K2003/2224C08L23/0815
Inventor 赵建青曹博刘述梅朱亚明
Owner SOUTH CHINA UNIV OF TECH
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