Catalytic synthesizing method of hexa chloro cyclotripolyphosphazene

A technology for hexachlorocyclotripolyphosphazene and a synthesis method, which is applied in chemical instruments and methods, compounds of elements of Group 5/15 of the periodic table, catalysts for physical/chemical processes, etc., can solve the problem of hexachlorocyclotripolyphosphazene High production cost, limited application scope, complicated operation, etc., to achieve the effect of low cost, shortened response time and simple operation

Inactive Publication Date: 2006-10-25
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Stocks, H.N.Am.Chem J., 1897, 19:782; Allcock, H.R, Chem.Eng, News, 1985, 63(11):22; J.Emsleg and P.B.Udy.J.Chem.soc 1997, (5 ): 768 etc. have reported the synthesis of hexachlorocyclotriphosphazene, but their reaction time is generally 10~20h, the operation is complicated, and the yield is generally 50~75%, resulting in the production cost of hexachlorocyclotriphosphazene is too high, so that the application range is limited

Method used

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  • Catalytic synthesizing method of hexa chloro cyclotripolyphosphazene
  • Catalytic synthesizing method of hexa chloro cyclotripolyphosphazene
  • Catalytic synthesizing method of hexa chloro cyclotripolyphosphazene

Examples

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Embodiment 1

[0029] Embodiment 1: 0.1200mol ammonium chloride, 0.0017mol magnesium chloride and 0.0050mol pyridine are added in the reaction kettle, add 110ml chlorobenzene heating and dissolving, reflux; Under reflux state, add 0.1000mol phosphorus pentachloride 5~10 times, Complete the addition within 2 hours; then continue to reflux for 3 hours, the system turns light yellow-green; stop heating, cool to room temperature, filter out unreacted ammonium chloride, and then distill chlorobenzene; add 56ml of petroleum ether to the residue and heat under reflux for extraction 0.5~1h, cooling, filtering, distilling petroleum ether to obtain orange or white crystals, recrystallization or sublimation with n-heptane to obtain pure white crystal product hexachlorocyclotrimeric phosphazene, the yield is 88%, and the melting point is 111 ~113°C, 31 P(DMSO): 20.5ppm.

Embodiment 2

[0030] Example 2: Add 0.1200mol of ammonium chloride, 0.0017mol of cobalt chloride and 0.0050mol of pyridine into the reactor, add 110ml of chlorobenzene to heat and dissolve, and reflux; under reflux, add 0.1000mol of pentachloride in 5 to 10 times Add phosphorus within 2 hours; then continue to reflux for 5 hours, the system turns light yellow-green; stop heating, cool to room temperature, filter out unreacted ammonium chloride, and then distill chlorobenzene; add 56ml of petroleum ether to the residue and heat Reflux extraction for 0.5-1h, cooling, filtering, and distilling petroleum ether to obtain orange or white crystals, recrystallization or sublimation with n-heptane to obtain pure white crystal product hexachlorocyclotrimeric phosphazene, the yield rate is 83%, the melting point 111~113℃, 31 P(DMSO): 20.5ppm.

Embodiment 3

[0031] Example 3: Add 0.1200mol ammonium chloride, 0.0017mol zinc chloride and 0.0050mol pyridine into the reaction kettle, add 110ml chlorobenzene to heat and dissolve, and reflux; in the reflux state, add 0.1000mol pentachloride in 5 to 10 times Add phosphorus within 2 hours; then continue to reflux for 5 hours, the system turns light yellow-green; stop heating, cool to room temperature, filter out unreacted ammonium chloride, then distill chlorobenzene, add 56ml of petroleum ether to the residue and heat Reflux extraction for 0.5-1h, cooling, filtering, and distilling petroleum ether to obtain orange or white crystals, recrystallization or sublimation with n-heptane to obtain pure white crystal product hexachlorocyclotrimeric phosphazene, the yield rate is 83%, the melting point 111~113℃, 31 P(DMSO): 20.5ppm.

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Abstract

This invention discloses hexachloro ring trimerization phosphonitrile catalysis synthesis method. 1.1-1.5mol ammonium chloride, complex catalyst made uo by 0.012-0.022mol metal compound and 0.030-0.070mol pyridine substance are added into reaction kettle, and then 1000-1300 ml chlorobenzene is added and heated to dissolve. 1mol phosphoric chloride is added at back flow state, then 1 mol phosphoric chloride is added and continue back flow 3-5 hours, then stoped and cooled down to room temperature, and filter off unreacted ammonium chloride and distill out chlorobenzene. 550-600ml petroleum ether is added into residual, then they are heated back flow and extracting for 0.5 to 1 hours, then they are cooled down and filtrated, distilled petroleum ether, finally the crystal is recrystallized and sublimed by normal heptane, and pure white srystal hexachloro ring trimerization phosphonitrile is got. The catalysis synthesis method in this invention uses special complex catalyst, that is metal compound and pyridine or its alkyl substitute to shorten reaction time to 3-5 hours, and improves yield to 80-90 percent, its operation is simple, so is worth extending.

Description

Technical field: [0001] The invention relates to a synthesis method of a compound, in particular to a catalytic synthesis method of hexachlorocyclotrimeric phosphazene, belonging to the field of chemical synthesis. Background technique: [0002] Hexachlorocyclotripolyphosphazene, as an organic synthesis intermediate with multiple substituted active chlorine atoms, can generate compounds with multiple uses such as new high-efficiency flame retardants, side chain liquid crystals, special rubbers and electronic materials, etc. Because of its unique performance and broad application prospects, it has attracted much attention. Stocks, H.N.Am.Chem J., 1897, 19:782; Allcock, H.R, Chem.Eng, News, 1985, 63(11):22; J.Emsleg and P.B.Udy.J.Chem.soc 1997, (5 ): 768 etc. have reported the synthesis of hexachlorocyclotriphosphazene, but their reaction time is generally 10~20h, the operation is complicated, and the yield is generally 50~75%, which causes the production cost of hexachlorocy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6593B01J31/02B01J31/26
Inventor 赵玉芬叶勇鞠志宇廖新成邹如意屈凌波
Owner ZHENGZHOU UNIV
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