Hyperbranched phosphorus-containing oxygen group functionalized silicon-based resin flame retardant and preparation method thereof

A phosphorus-oxygen-functional, silicon-based resin technology, applied in the field of flame retardants, can solve the problems of flame retardant efficiency, heat resistance and water washing resistance that are not as good as bromine antimony flame retardant systems, etc.

Active Publication Date: 2021-02-26
SHANDONG TIANYI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although intumescent flame retardants have the advantages of being halogen-free, low-smoke, low-toxicity, anti-melt droplets and non-corrosive gases, they are not as good as bromine-antimony flame-retardant systems in terms of flame-retardant efficiency, heat resistance, and water-washing resistance.

Method used

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  • Hyperbranched phosphorus-containing oxygen group functionalized silicon-based resin flame retardant and preparation method thereof
  • Hyperbranched phosphorus-containing oxygen group functionalized silicon-based resin flame retardant and preparation method thereof
  • Hyperbranched phosphorus-containing oxygen group functionalized silicon-based resin flame retardant and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0043] In one embodiment of the present invention, in step (1), tetraethoxysilane is used as a silane compound having three or more condensable functional groups, and neopentyl glycol is used as a hydroxyl-containing compound. Controlling the molar ratio of condensable ethoxy functional groups in tetraethoxysilane to neopentyl glycol hydroxyl groups in the range of 1.2:1 to 4.0:1, preferably greater than 1.2:1 to 3.0:1 , more preferably in the range of 1.5:1 to 2.5:1, most preferably 2:1 into the reactor. Stirring is carried out at a high temperature of 120-180°C in the absence of catalysts and solvents, and the reaction is carried out for 5-20 hours. In order to increase the reaction rate, a catalyst such as p-toluenesulfonic acid, and a solvent such as xylene may also be used in appropriate amounts.

[0044] While not wishing to be bound by any theory, the inventors believe that tetraethoxysilane and neopentyl glycol react in the examples as represented by Scheme A below: ...

Embodiment 2

[0052] In one embodiment of the present invention, in step (1), tetraethoxysilane is used as a silane compound having three or more condensable functional groups, and neopentyl glycol and trimethylolpropane are used as hydroxyl-containing compounds. The molar ratio of the condensable ethoxy group of tetraethoxysilane to the hydroxyl group in neopentyl glycol and trimethylolpropane is controlled in the range of 1:1.2 to 1:4, preferably 1:1.4 to 1: 2.5, more preferably in the range of 1:1.5 to 1:2.0, into the reactor. In the absence of catalysts and solvents, stirring is carried out at a high temperature of 120-180° C., and the reaction is carried out for 5-20 hours. In order to increase the reaction rate, catalysts (such as p-toluenesulfonic acid) and solvents (such as xylene) can also be used in appropriate amounts.

[0053] Although not wishing to be bound by any theory, the inventors believe that tetraethoxysilane reacts with neopentyl glycol and pentaerythritol according t...

Embodiment 3

[0061] Step (1) Add 208.33g (1.00mol) of tetraethoxysilane and 374.94g (3.60mol) of neopentyl glycol to four ports equipped with thermometer, top stirrer, gas inlet and distillation device at room temperature in the flask. The reaction was carried out under the protection of a stream of anhydrous nitrogen introduced through the gas inlet of the reactor. The reaction mixture was then heated to 115°C and maintained at this temperature until distillate distilled from the reaction mixture. Heating was continued and the temperature of the reaction mixture was gradually increased to 180° C. until the ethanol was distilled off completely. In this way, hyperbranched polysiloxanes containing hydroxyl groups are obtained.

[0062] Step (2) Weigh 613.32g (1.60mol) of phosphorus oxychloride and place it in a constant pressure dropper, install it on the three-necked flask containing hydroxyl-containing hyperbranched polysiloxane obtained in step 3, and pour it into the three-necked flask...

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Abstract

The invention discloses a hyperbranched phosphorus-containing oxygen group functionalized silicon-based resin flame retardant, which is provided with a branched silicon atom-containing molecular skeleton and a phosphorus-containing oxygen group chemically bonded to the silicon atom of the molecular skeleton. The phosphorus-containing oxygen group functionalized silicon-based resin is obtained by (1) reacting a silane compound having three or more condensable functional groups with at least one hydroxyl group-containing compound to form a branched silicon-based resin, and (2) introducing a phosphorus-containing oxygen group to the silicon-based resin to obtain the hyperbranched phosphorus-containing oxygen group functionalized silicon-based resin flame retardant. A flame-retardant polymer composition containing the flame retardant is high in carbon forming rate, high in oxygen index and good in flame-retardant effect.

Description

technical field [0001] The invention belongs to the technical field of flame retardants, and relates to a hyperbranched phosphorus-containing oxygen functionalized silicon-based resin flame retardant and a preparation method thereof. Background technique [0002] Polymer materials have excellent characteristics such as light weight, good chemical stability, and easy processing, and have become important matrix materials in the fields of aerospace, transportation, electrical and electronics, and building materials. However, most polymer materials are flammable materials, so polymer materials not only provide convenience, but also increase great safety hazards. Fire is one of the major disasters that threaten public safety, causing a large number of casualties and huge economic losses every year. From January to October 2017 alone, a total of 219,000 fires were reported across the country, 1,065 people were killed, 679 people were injured, and 2.62 billion yuan of direct prop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/395C08G77/04C08G77/06C08L83/08
CPCC08G77/395C08G77/04C08G77/06C08L83/08C08L2201/02
Inventor 汪少锋崔剑光
Owner SHANDONG TIANYI CHEM
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