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Process for synthesis of melamine salt of pentaerythritol bis (dihydrogen phosphate)

The technology of pentaerythritol bisphosphate melamine salt and pentaerythritol is applied in the field of synthesis of pentaerythritol bisphosphate melamine salt, which can solve the problems of hindering mass transfer, heat transfer, high requirements for equipment stirring, high material viscosity, etc.

Inactive Publication Date: 2006-01-18
BC P INC CHINA NAT PETROLEUM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the reaction process, the viscosity of the material is high, and the requirements for equipment stirring are high, which hinders mass transfer and heat transfer, and is not suitable for industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 184.5 grams of polyphosphoric acid, 108.8 grams of pentaerythritol, 2.5 grams of catalyst benzoic acid, and 1,000 milliliters of toluene into a 2000 mL four-neck flask equipped with a stirrer, thermometer, water separator, and condenser, and heat up to 100-115 ° C. Hour. The solvent was distilled off at -0.095Mpa. Add 201.6 grams of melamine and 2015 milliliters of water into the four-necked bottle, raise the temperature to 100° C., and react for 2 hours. After cooling to room temperature, stop stirring, filter and wash, dry the wet product in an oven at 80-100°C, crush and pack. The product yield is 82.2%, the phosphorus content is 11.6%, and the solvent toluene recovery rate is 96%.

Embodiment 2

[0026] Add 184.5 grams of polyphosphoric acid, 108.8 grams of pentaerythritol, 2.5 grams of catalyst p-toluenesulfonic acid, and 1000 milliliters of toluene into a 2000 mL four-necked bottle equipped with a stirrer, thermometer, water separator and condenser, and heat up to 100-115 ° C. Reacted for 9 hours. Afterwards, the solvent was distilled off at -0.095 MPa. Add 201.6 grams of melamine and 1400 milliliters of water into the four-necked bottle, raise the temperature to 100°C, and react for 2 hours. After cooling down to room temperature, stop stirring, filter, wash, and dry the wet product in an oven at 80-100°C. Package. The product yield is 80.5%, the phosphorus content is 12.0%, and the solvent recovery rate is 95%.

Embodiment 3

[0028] Add 184.5 grams of polyphosphoric acid, 108.8 grams of pentaerythritol, 2.5 grams of catalyst p-toluenesulfonic acid, and 1000 milliliters of xylene into a 2000 mL four-neck flask equipped with a stirrer, thermometer, water separator and condenser, and heat up to 130-144 °C , reacted for 7 hours. The solvent xylene was distilled off at -0.095Mpa. Add 201.6 grams of melamine and 1400 milliliters of water into the four-necked bottle, raise the temperature to 100° C., and react for 2 hours. After cooling down to room temperature, stop stirring, filter, wash, dry the wet product in an oven at 80-100°C, crush and pack. The yield is 81.5%, the phosphorus content is 11.8%, and the solvent recovery rate is 95%.

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PUM

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Abstract

The present invention relates to the synthesis process of pentaerythritol diphophate melamine as phosphorus-nitrogen expansion type fire retardant. The present invention features that pentaerythritol and polyphosphate in the molar ratio of 1 to 2 are dispersed in benzene solvent in the amount one 8-9 times the weight of pentaerythritol and reacted in the presence of p-toluenesulfonic acid or benzoic acid catalyst through heating to 80-144 deg.c for 7-10 hr before decompression distillation to recover solvent and obtain ropy intermediate product; water and melamine in the weight ratio of 1 to 7-10 and with melamine / pentaerythritol molar ratio of 1 to 2 are then added for reaction of 2 hr while heating to 100 deg.c; and through further cooling naturally to room temperature, filtering, washing, stoving and crushing, the target product is obtained. The process is simple and has less environmental pollution, and the product has excellent fire retarding effect and high heat stability.

Description

technical field [0001] The invention relates to a preparation method of a phosphorus-nitrogen expansion flame retardant, in particular to a synthesis method of pentaerythritol diphosphate melamine salt. Background technique [0002] Flame retardants can be divided into inorganic flame retardants and organic flame retardants, among which organic flame retardants include halogen-containing flame retardants, and their representative brands are bromophenyl ethers, such as decabromodiphenyl ether, tetrabromobisphenol A, etc. , although the bromine-containing flame retardant meets the flame-retardant requirements of polymer materials and basically maintains the physical properties of the original resin, the toxic substances produced by the bromine-containing polymer during combustion are extremely harmful, seriously destroying the ecology and polluting the environment. With the increasing awareness of environmental protection, halogenated flame retardants are facing severe challen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6533
Inventor 刘福安姜丹蕾张锁秦张宏宇刘长清李耀先
Owner BC P INC CHINA NAT PETROLEUM CORP
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