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Organic silicon compound containing phosphorus and its preparing method

An organosilicon compound and siloxane technology, applied in the field of phosphorus-containing organosilicon compounds and their preparation, can solve the problems of inability to prepare additive flame retardants and the like

Inactive Publication Date: 2007-04-11
CHANGZHOU BAYI CABLE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The introduction of the above-mentioned reactivity is only suitable for the preparation of intrinsic flame retardant materials, and cannot be used for the preparation of additive flame retardants.

Method used

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  • Organic silicon compound containing phosphorus and its preparing method
  • Organic silicon compound containing phosphorus and its preparing method
  • Organic silicon compound containing phosphorus and its preparing method

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Add 216g (1mol) of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (solid) and 132g (1mol) of vinyldimethoxysiloxane (liquid) to three In the neck flask, stir, heat and dissolve, control the temperature at 105°C, continue to add 36g (2mol) H after reflux reaction for 12 hours 2 O, 1.12g (0.02mol) potassium hydroxide, the temperature was kept at 100°C, reacted for 10 hours, decompressed to remove water and the methanol produced by the reaction for 3 hours, and cooled to obtain 297g of light yellow viscous liquid, which was the reaction product A Base-[2-(9-oxa-10-phosphaphenanthrene-10-oxide)-ethyl]-dihydroxysilane with a yield of 92.8%.

[0028] Fig. 1 is the infrared spectrogram of methyl-[2-(9-oxa-10-phosphaphenanthrene-10-oxide)-ethyl]-dihydroxysilane; FTIR (KBr, cm -1 ): 3421(OH), 3064(C-H in phenyl group), 2800-3000(CH 2 , CH 3 ), 1595(phenyl group), 1477(P-phenyl), 1410(P-CH 2 -of aliphatic), 1206 (P=O), 1004-1117 (Si-O-Si), 911 (P-O-phenyl)

[0029] Fig. ...

Embodiment 2

[0032] Add 216g (1mol) of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (solid) and 191g (1mol) of vinyltriethoxysiloxane (liquid) to three In the flask, stir, heat to dissolve, control the temperature to 160°C, and continue to add 36g (2mol) H after reflux reaction for 12 hours 20, 1.12g (0.02mol) potassium hydroxide, the temperature is maintained at 100 ℃, reacted for 10 hours, removed water under reduced pressure and the low-boiling point small molecule ethanol generated by the reaction for 4 hours, cooled to obtain 305g of light yellow viscous liquid, which is The reaction product [2-(9-oxa-10-phosphaphenanthrene-10-oxide)-ethyl]-trihydroxysilane has a yield of 94.7%.

Embodiment 3

[0034] Methyl-[2-(9-oxa-10-phosphaphenanthrene-10-oxide)-ethyl]-dihydroxysilane 160g obtained by Example 1, 20.6g N-(β-aminoethyl) -α-Aminopropylmethyldimethoxysilane, 3.6g H 2 O and 0.12g potassium hydroxide were added in the three-necked flask, heated and dissolved, stirred, controlled temperature was 100°C, reacted for 24 hours, removed water under reduced pressure and the low-boiling point small molecule methanol generated by the reaction for 8 hours, cooled to obtain Phosphorus-containing polysiloxane 157g, yield 94.0%.

[0035] The obtained phosphorus-containing polysiloxane 21g, polycarbonate (PC) 34.3g, acrylonitrile-butadiene-styrene terpolymer (ABS) 14.7g are put into internal mixer and mix evenly, knead The temperature is 210°C, the mixing time is 6 minutes, and the flame-retardant PC / ABS alloy is obtained. The oxygen index is 27.2, which reaches the UL-94V-0 level, and a relatively high carbon formation rate is obtained at 800°C (in nitrogen: 16.7%; in air: 14.3%...

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Abstract

The present invention discloses one kind of organosilicon compound containing phosphorus and its preparation process, and the compound contains two fire-retarding elements, Si and P, and hydroxyl groups and may be used as the reaction type fire-retarding intermediate. The materials 9, 10-dihydro-9-oxo-10-phosphaphenanthryl-10-oxide (DOPO) and siloxane containing C-C double bond are heated to produce addition reaction, and water and catalyst are then added to hydrolyze alkoxy radical to prepare the organosilicon compound containing phosphorus and hydroxyl groups. The organosilicon compound containing phosphorus and hydroxyl groups is superior to DOPO in that it contains several functional groups and thus may be polycondensated with other substance to prepare macromolecular fire retardant.

Description

Technical field: [0001] The present invention relates to an organic compound and its preparation method, in particular to a phosphorus-containing organosilicon compound and its preparation method. The compound contains two flame-retardant elements, silicon and phosphorus, and contains multiple hydroxyl groups. It can be used as a reactive type Flame retardant intermediate. 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 increasin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6571
Inventor 仲含芳江平开韦平汪根林张军吴丹
Owner CHANGZHOU BAYI CABLE
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