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Synthetic method of 6(4-hydroxyl ethyoxyl) cyclotriphophazene

A technology of hydroxyethoxy and hexachlorocyclotriphosphazene, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve problems such as low yield, and achieve the reaction yield. High-rate, simple post-processing effects

Inactive Publication Date: 2012-11-07
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the yield of this method is low, traces it to its reason, may be because the hydroxyl group in the ethylene glycol monosodium molecule has certain reactivity, easily five-membered ring-forming reaction or bimolecular phosphazene ring coupling take place on the same phosphorus atom. A large number of by-products are produced in the reaction

Method used

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  • Synthetic method of 6(4-hydroxyl ethyoxyl) cyclotriphophazene
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  • Synthetic method of 6(4-hydroxyl ethyoxyl) cyclotriphophazene

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Effect test

Embodiment 1

[0024] (1) Synthesis of six (4-methoxyethoxy) cyclotriphosphazene

[0025] Add 300ml of tetrahydrofuran and 149.28g of sodium hydride (50%?) into a 1L three-necked reaction flask, then add 50ml of tetrahydrofuran solution containing 157.78g of methoxyethanol dropwise to the reaction flask under stirring at a temperature of 20°C to 30°C, After dropping, react at a temperature of 30° C. for 30 minutes. Then the temperature was lowered to 5°C, and 100ml of a tetrahydrofuran solution dissolved with 100g of hexachlorocyclotriphosphazene was added dropwise to the reaction flask, and reacted at a temperature of 50°C for 30h after the drop was completed. Filter the reaction solution, and evaporate the tetrahydrofuran in the obtained filtrate under reduced pressure to obtain a light yellow turbid viscous liquid, then add 150ml of dichloromethane to the liquid, wash the above liquid with distilled water until the water phase is neutral, separate the organic phase, reduce Dichloromethan...

Embodiment 2

[0046] (1) Synthesis of six (4-methoxyethoxy) cyclotriphosphazene

[0047] Add 300ml of tetrahydrofuran and 129.60g of sodium hydride (50%) into a 1L three-necked reaction flask, then add dropwise 50ml of tetrahydrofuran solution containing 164.35g of methoxyethanol to the reaction flask under stirring at a temperature of 20°C to 30°C, dropwise After completion, react at a temperature of 30° C. for 45 minutes. Then the temperature was lowered to 5°C, and 100ml of a tetrahydrofuran solution dissolved with 100g of hexachlorocyclotriphosphazene was added dropwise to the reaction flask, and reacted at a temperature of 50°C for 30h after the dropping was completed. After the reaction was completed, filter the reaction solution, distill off the tetrahydrofuran in the resulting filtrate under reduced pressure to obtain a light yellow turbid viscous liquid, then add 150ml of dichloromethane to the liquid, wash the above liquid with distilled water until the water phase is neutral, sep...

Embodiment 3

[0051] (1) Synthesis of six (4-methoxyethoxy) cyclotriphosphazene

[0052] Add 300ml of tetrahydrofuran and 129.60g of sodium hydride (50%) into a 1L three-necked reaction flask, then add dropwise 50ml of tetrahydrofuran solution containing 164.35g of methoxyethanol to the reaction flask under stirring at a temperature of 20°C to 30°C, dropwise After completion, react at a temperature of 35° C. for 40 minutes. Then the temperature was lowered to 0°C, and 100ml of tetrahydrofuran solution in which 100g of hexachlorocyclotriphosphazene was dissolved was added dropwise to the reaction flask, and reacted at 60°C for 24 hours after dropping. After the reaction was completed, filter the reaction solution, distill off the tetrahydrofuran in the resulting filtrate under reduced pressure to obtain a light yellow turbid viscous liquid, then add 150ml of dichloromethane to the liquid, wash the above liquid with distilled water until the water phase is neutral, separate the organic phase...

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Abstract

The invention discloses a synthetic method of 6(4-hydroxyl ethyoxyl) cyclotriphophazene. The method includes the following steps: (1) enabling methyl cellosolve and sodium hydride to react to obtain methyl sodium ethoxide, adding a tetrahydrofuran solution of hexachlorocyclotriphosphazene, reacting for 30min-45min at the temperature of 20 DEG C-35 DEG C, filtering, removing solvent by steaming, extracting, washing and conducting reduced pressure distillation to obtain 6(4-methoxyl ethyoxyl) cyclotriphophazene; (2) enabling the 6(4-methoxyl ethyoxyl) cyclotriphophazene and iodotrimethylsilane to react for 30h-40h at the temperature of 25 DEG C-35 DEG C under the condition of stirring, adding a methanol solution of sodium hydroxide, reacting for 6h-8h at the temperature of 15-30 DEG C under the condition of stirring, filtering, and conducting reduced pressure removing of the solvent by steaming to obtain the 6(4-hydroxyl ethyoxyl) cyclotriphophazene. The synthetic method of the 6(4-hydroxyl ethyoxyl) cyclotriphophazene is high in reacting yield and is mainly used for synthesis of the 6(4-hydroxyl ethyoxyl) cyclotriphophazene.

Description

technical field [0001] The invention relates to a method for synthesizing hexa(4-hydroxyethoxy)cyclotriphosphazene, belonging to the field of chemical synthesis. Background technique [0002] The cyclotriphosphazene structure can provide good heat resistance and superior flame retardancy, and has attracted much attention in the research fields of fire resistance, flame retardant materials and special polymer materials. Hexa(4-hydroxyethoxy)cyclotriphosphazene is a special aliphatic cyclotriphosphazene derivative, because it contains six active hydroxyl groups in its structure, it can usually be used as a modification of heat-resistant and flame-retardant polyurethane materials Agents and polyhydroxy initiators for the preparation of six-armed star polymers. [0003] Hexa(4-hydroxyethoxy)cyclotriphosphazene can be obtained by substitution reaction of hexachlorocyclotriphosphazene and sodium alkoxide. For example, Jaeger R.D. et al. "Poly(organophosphazene)s and related comp...

Claims

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Application Information

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IPC IPC(8): C07F9/6593
Inventor 肖啸甘孝贤葛忠学刘庆黄小梧汪伟
Owner XIAN MODERN CHEM RES INST
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