Phosphorus containing siloxane and process for preparing same

A technology of polysiloxane and dihydroxysiloxane, which is applied in the field of side chain phosphorus-containing polysiloxane and its preparation, and can solve problems such as uneven distribution

Inactive Publication Date: 2005-06-29
凌庆平
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to synthesize a phosphorus-containing polysiloxane containing both phosphorus and silicon, and connect the three elements of the intumescent flame retardant with the organosilicon group through chemical bonds to prepare

Method used

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  • Phosphorus containing siloxane and process for preparing same
  • Phosphorus containing siloxane and process for preparing same
  • Phosphorus containing siloxane and process for preparing same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (a) Weigh 1 mol of neopentyl glycol, add it into 300 ml of chloroform, stir and raise the temperature to dissolve. Then control the temperature at 0°C, and add 1 mol of phosphorus oxychloride dropwise. After the phosphorus oxychloride was added dropwise, the temperature was raised to 20°C and kept at this temperature for 4 hours. Chloroform was removed, and the product obtained was treated with benzene, CCl 4 , washed with absolute ethanol three times respectively, and dried in an oven at 80° C. for about 10 hours to obtain a phosphorus oxychloride compound. attached figure 1 It is the infrared spectrogram of phosphorus oxychloride compound: FTIR (KBr, cm -1 ): 2896~2975 (-CH 2 -, -CH 3 ); 1304 (P=O); 1000-1100 (P-O-C); 540 (P-Cl).

[0037] (b) Weigh 1 mol of amino-containing siloxane (r=3, q=2), add 2 mol of water, 0.01 mol of potassium hydroxide, heat up to 80-100°C, keep the temperature at constant temperature for 12 hours under the protection of nitrogen, and ...

Embodiment 2

[0041] (a) Weigh 1 mol of neopentyl glycol, add it into 300 ml of chloroform, stir and raise the temperature to dissolve. Then control the temperature at 0°C, and add 1 mol of phosphorus oxychloride dropwise. After the phosphorus oxychloride was added dropwise, the temperature was raised to 20°C and kept at this temperature for 4 hours. Chloroform was removed, and the obtained product was washed three times with absolute ethanol, and placed in an oven at 80° C. for about 10 hours to obtain a phosphorus oxychloride compound.

[0042] (b) Weigh 1 mol of amino-containing siloxane (r=3, q=2), add 2 mol of water, 0.01 mol of potassium hydroxide, heat up to 80-100°C, keep the temperature at constant temperature for 12 hours under the protection of nitrogen, and remove the water , to obtain the hydrolysis product of aminosilane.

[0043] (c) Weigh the hydrolyzate of 0.5mol aminosilane and 0.5mol of α, ω-dihydroxydimethylsiloxane (R1, R2 are both CH 3 ) and 0.5mol of another α, ω-d...

Embodiment 3

[0046] According to Example 1, 30 g of the phosphorus-containing polysiloxane flame retardant and 70 g of polypropylene were put into an internal mixer and mixed uniformly at a mixing temperature of 170° C. for 8 minutes to obtain a flame-retardant polypropylene. Its oxygen index is 27.0, and a very high char formation rate is obtained at 800°C (in nitrogen: 27%; in air: 12%; in oxygen: 13%).

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Abstract

The invention has supplied phosphor containing shown as follows and its preparing method. Use phosphorus oxychloride and diatomic alcohol as the raw material to prepare phosphoryl chloride compound; meanwhile, use poly-polysiloxane containing amino and hydroxyl siloxane with low molecular weight to generate poly-polysiloxane containing amino; then dissolve the two compounds generated in organic solvent synthesize to be poly-polysiloxane containing p with temperaturing rising. The invention can be used as flame retardant which contains several elements like Si, P and N for polyolefin, polyacrylic acid, ABS, nylon, cellulose or polyvinyl alcohol. R1 and R2 are separately chosen from CH3 or C6H5, R3 from (CH2)r or (CH2)rNH(CH2)q, R4 and R5 seperately from H, CH3 or C2H5.

Description

Technical field: [0001] The invention relates to a flame-retardant organosilicon polymer material and a preparation method thereof, in particular to side chain phosphorus-containing polysiloxane and a preparation method thereof. Background technique: [0002] Organosilicon compounds have good biocompatibility, gas permeability and low surface energy, and their research scope is very wide; while the research on phosphorus-containing compounds mainly focuses on biology and flame retardancy. What these two elements have in common is that both can be used to improve the flame retardant effect of polymers. In previous studies, they often appeared as different flame retardant compounds. With the improvement of the flame retardant performance requirements of materials, flame retardant compounds containing a single element are increasingly unable to meet the application requirements. The development of flame retardant compounds has gradually focused on compounds that use multiple ...

Claims

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Application Information

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IPC IPC(8): C08G77/30
Inventor 李强江平开韦平
Owner 凌庆平
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