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Phosphate type liquid alicyclic olefin compound and its preparation method

A cycloaliphatic and phosphate ester technology, which is applied in the direction of phosphorus organic compounds, can solve the problems of thermal and mechanical performance degradation of materials

Inactive Publication Date: 2003-12-03
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the problems of dispersion and interfacial compatibility between flame retardants and substrates, adding a large amount of flame retardants will inevitably lead to a large decline in the thermal and mechanical properties of the material

Method used

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  • Phosphate type liquid alicyclic olefin compound and its preparation method

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Experimental program
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Effect test

Embodiment 1

[0023] 250 milliliters of four-necked flasks are equipped with thermometer, mechanical stirring, dropping funnel, nitrogen conduit, add 3-cyclohexenol 29.4g (0.30mol), 31.8g (0.315mol) triethylamine, 32ml benzene, mechanical stirring simultaneously with Cool down to -4°C in an ice-salt bath; add phosphorus oxychloride dropwise, and control the rate of addition so that the temperature of the reaction system does not rise above 5°C; to 80°C and keep warm for 2 hours. Cool down to room temperature, add 30ml of deionized water; transfer to a separatory funnel, let it stand, and separate the water phase; wash twice with 25ml of 2% sodium hydroxide solution; then wash twice with deionized water, and separate the water phase; Dry with anhydrous magnesium sulfate; remove the solvent under reduced pressure to obtain 3-cyclohexenol phosphate as a colorless transparent liquid. Separation by column chromatography yielded 19.3 g of the product. Yield 57%.

[0024] IR (KBr): 1018cm -1 (...

Embodiment 2

[0027] 250 milliliters of four-necked flasks are equipped with thermometer, mechanical stirring, dropping funnel, nitrogen conduit, add 3-cyclopentenol 25.2g (0.30mol), 31.8g (0.315mol) triethylamine, 32ml benzene, mechanical stirring simultaneously with Cool down to -6°C in an ice-salt bath; add phosphorus oxychloride dropwise, and control the rate of addition so that the temperature of the reaction system does not rise above 5°C; to 80°C and keep warm for 2 hours. Cool down to room temperature, add 30ml of deionized water; transfer to a separatory funnel, let it stand, and separate the water phase; wash twice with 25ml of 5% sodium hydroxide solution; then wash twice with deionized water, and separate the water phase; Dry with anhydrous magnesium sulfate; remove the solvent under reduced pressure to obtain 3-cyclopentenol phosphate as a colorless transparent liquid. Separation by column chromatography yielded 16.6 g of the product. Yield 56%.

[0028] IR (KBr): 1021cm -1...

Embodiment 3

[0031] 250 milliliters of four-necked flasks are equipped with thermometer, mechanical stirring, dropping funnel, nitrogen conduit, add 2-cyclopentenol 25.2g (0.30mol), 31.8g (0.315mol) triethylamine, 32m toluene, mechanical stirring simultaneously with Cool down to -5°C in an ice-salt bath; add phosphorus oxychloride dropwise, and control the rate of addition so that the temperature of the reaction system does not rise above 5°C; To 70°C, keep warm for 1.5 hours. Cool down to room temperature, add 30ml of deionized water; transfer to a separatory funnel, let it stand, and separate the water phase; wash twice with 25ml of 5% sodium hydroxide solution; then wash twice with deionized water, and separate the water phase; Dry with anhydrous sodium sulfate; remove the solvent under reduced pressure to obtain 3-cyclopentenol phosphate as a colorless transparent liquid. Column chromatography. 15.9 g of product were obtained. Yield 54%.

[0032] IR (KBr): 1012cm -1 (P-O); 1258 (P...

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Abstract

A phosphate-type alicyclic olefine compound in the form of liquid is prepared through proportioning alicyclic olefine alkoxide, phosphorus trioxyhalide and alamine, preparing the organic solution of alicyclic olefine alkoxide and alamine, dropping the phosphorus trioxyhalide to the said organic solution, heating to 50-80 deg.c, reaction for 0.5-2, and purifying.

Description

Technical field: [0001] The invention relates to an alicyclic olefin compound and a preparation method thereof, in particular to a phosphate-type alicyclic olefin compound and a preparation method thereof. Background technique: [0002] Alicyclic olefins are a class of compounds that are widely studied and used. Alicyclic olefins can be used as monomers for ring polymerization and ring copolymerization to obtain molten ring polymer systems (J. Polym. Sci.: Part A-1, 1967, 5, 1827-1844); they can also be used as intermediates Olefin resins are prepared by olefination (U.S. Pat. 4849532 and JP Patent 05032647A). It can also be oxidized with peroxyacid to generate cycloaliphatic epoxy compounds. The synthesis method can be synthesized from phenol or hydroquinone (GE.Pat.1099733 and U.S.Pat.2848426), and can also use butadiene and acrolein or crotonaldehyde as starting materials, through diene addition, etc. Reaction to obtain esters or etherifications of alicyclic diolefins ...

Claims

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Application Information

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IPC IPC(8): C07F9/09
Inventor 巩方玲赵云峰陶志强王忠刚余云照
Owner INST OF CHEM CHINESE ACAD OF SCI