Preparation of low polyphosphate

A technology of oligomeric phosphate and monoalkyl dichlorophosphate, which is applied in the field of improvement of the preparation method of oligomeric phosphate, can solve the problems of low phosphorus content of diphosphate, poor flame retardant effect, etc. Simple operation, less corrosive effect

Inactive Publication Date: 2008-10-29
JIANGSU YOKE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the product can be used as a flame retardant, because of the raw materials fatty alcohol and diethylene glycol, the phosphorus content of the obtained diphosphate is low, and the flame retardant effect is poor, and because of its large molecular weight, it is solid at room temperature, so Can only be used in plastics, not suitable for use in polyurethane

Method used

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  • Preparation of low polyphosphate
  • Preparation of low polyphosphate
  • Preparation of low polyphosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1: drop into 1mol phosphorus oxychloride, 3 ‰ carbon tetrachloride catalysts in four-necked flask, turn on stirring, drip 1mol ethylene glycol from separatory funnel, control temperature 20 ± 10 ℃, drop rate is controlled at 2-3h, absorb the HCl gas generated during the dropwise addition with water, and keep stirring at 20-25°C after the dropwise addition, and the reaction ends when no HCl gas is released. Continue to stir for another half an hour, then add about 2 mol of absolute ethanol (excessive amount) dropwise, control the dropwise addition within 2-3 hours, absorb the released HCl gas with water, after the dropwise addition, continue to react until no HCl gas is released, continue to stir for half a day Hour ends. Using the same method as ordinary flame retardants, after pickling, alkali washing, water washing and distillation, a light yellow viscous liquid is obtained. Liquid chromatography analysis showed that its molecular weight was 1250, its phos...

Embodiment 2

[0024] Embodiment 2: drop into 1mol phosphorus oxychloride, 3‰AlCl in four-necked flask 3 Catalyst, turn on the stirring, add 1.8mol of absolute ethanol dropwise from the separatory funnel, control the temperature at 20-30°C, add dropwise for 2-3h, and absorb the HCl gas released during the dropwise addition with water. When no HCl gas is released, the reaction is complete. Continue to stir at this temperature for half an hour, then add 1 mol of ethylene glycol dropwise to it, keep dropping at 20-25°C for about 2.5 hours, and absorb the released HCl gas with water. When no HCl gas was released, the reaction ended, and after stirring for 1 hour, post-treatment was carried out. After acid washing, alkali washing, water washing and distillation, viscous liquid is obtained. Liquid chromatography analysis shows that its molecular weight is 1315, its phosphorus content is 18.7%, and its hydroxyl value is 19.

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Abstract

The invention relates to an improved preparation method of an oligomeric phosphate ester, and is characterized in that the method comprises the steps of: obtaining dichloro-monoalkyl phosphate ester monomer through the reaction of phosphorus oxychloride and a monohydric alcohol performing the polymerization of the dichloro-monoalkyl phosphate ester monomer with a dihydric alcohol, and blocking end with a monohydric alcohol. Compared with the prior art, the inventive preparation method has the advantages of easily accessible raw materials, low corrosiveness, low cost (reducing cost by about 50%), no dangerous chemicals as raw materials, good safety, synthesis under relatively low temperature and low pressure, simple process, high production safety factor, simple equipment and operation, and no pollution in production process. The produced hydrogen chloride during reaction can be directly used in production of polyaluminum chloride.

Description

technical field [0001] The invention relates to a phosphorus-containing halogen-free flame retardant, in particular to the improvement of the preparation method of oligophosphate. Background technique [0002] With the improvement of environmental protection requirements, halogen-free flame retardants have been paid attention to. For example, the additive-type halogen-free flame retardants DMMP and GEEP used in polyurethane foam have good flame retardant effect in polyurethane foam, but their molecular weight is small and volatile, and they can migrate after a long time in the foam, causing The flame retardancy of the foam decreases. Oligomeric phosphate contains hydroxyl groups in its molecular structure, which can react with the foaming material and be combined into the foam molecular structure without migration, decomposition, or core burning. It is an additive reactive flame retardant, and it has certain polymerization properties. High degree, high content, no halogen,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/11C09K21/12
Inventor 沈琦周乐群吴仁铭
Owner JIANGSU YOKE TECH
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