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Synthesis technology of halogen-free high-poly type phosphate flame retardant

A synthesis process, phosphate ester technology, applied in the field of polymer synthesis process, can solve the problems of low flame retardant efficiency of flame retardants, impossibility of large-scale industrial production, and complicated preparation steps, and achieve heat and ultraviolet stability, reaction The process is convenient and the flame retardant effect is good

Active Publication Date: 2014-09-17
应急管理部四川消防研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its disadvantage is that all reactions can only be carried out in three-necked bottles, and only small sample tests can be carried out in the laboratory. The preparation steps are complicated, and large-scale industrial production is not possible, and the flame retardant efficiency of the obtained flame retardant is not high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] 1) Put 1 part of phosphorus oxychloride, 1.8 parts of ammonia water, 0.5 parts of phosphorus pentoxide, 1.0 parts of pentaerythritol, and 1.8 parts of melamine in a reaction kettle, raise the temperature to 60 ° C within half an hour, pressurize to 0.7 MPa, and continue to heat up Temperature was maintained at 115°C for 5 hours, the obtained product was cooled to room temperature, washed with dichloromethane three times, and vacuum-dried at room temperature to constant weight to obtain an intermediate.

[0010] 2) Put the intermediate obtained in step 1), 1 part of diammonium hydrogen phosphate, 3.5 parts of polyvinyl alcohol, 0.7 parts of urea, and 3.8 parts of 201 type polyether polyol into the reaction kettle, raise the temperature to 55 ° C, and add 0.2 parts Initiator, pressurize to 0.7MPa, continue to heat up to 105°C and keep it warm for 2h, after the reaction is completed, cool with water, filter, wash the product with distilled water until there are no chloride ...

Embodiment 2

[0012] 1) Put 1 part of phosphorus oxychloride, 1.35 parts of ammonia water, 1.25 parts of phosphorus pentoxide, 2 parts of pentaerythritol, and 1.2 parts of melamine in a reaction kettle, heat up to 85°C in half an hour, pressurize to 0.4MPa, and continue to heat up to 145°C and heat preservation for 6.5h. After the reaction, the obtained product was cooled to room temperature, washed with dichloromethane three times, and vacuum-dried at room temperature to constant weight to obtain an intermediate.

[0013] 2) Put the intermediate obtained in step 1), 1.75 parts of diammonium hydrogen phosphate, 2.5 parts of polyvinyl alcohol, 1.7 parts of urea, and 2.35 parts of 201 type polyether polyol in a reaction kettle, raise the temperature to 80 °C, and add 0.35 parts of initiator part, pressurize to 0.4MPa, continue to heat up to 115°C and keep it warm for 3h, after the reaction is completed, cool with water, filter, wash with distilled water until there are no chloride ions, and va...

Embodiment 3

[0015] 1) Put 1 part of phosphorus oxychloride, 0.9 parts of ammonia water, 2.0 parts of phosphorus pentoxide, 3.0 parts of pentaerythritol, and 0.6 parts of melamine in a reaction kettle, raise the temperature to 75 ° C within half an hour, pressurize to 0.6 MPa, and continue to heat up Temperature was maintained at 130°C for 8 hours, the resulting product was cooled to room temperature, washed three times with dichloromethane, and vacuum-dried at room temperature to constant weight to obtain an intermediate.

[0016] 2) Put the intermediate obtained in step 1), 2.5 parts of diammonium hydrogen phosphate, 0.5 parts of polyvinyl alcohol, 2.6 parts of urea, and 0.9 parts of 201-type polyether polyol in a reaction kettle, raise the temperature to 68°C, and add 0.5 parts of initiator Parts, pressurized to 0.5MPa, continue to heat up to 125°C and keep it warm for 1h, after the reaction is completed, cool with water, filter, wash with distilled water until there are no chloride ions...

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Abstract

The invention provides a synthesis technology of halogen-free high-poly type phosphate flame retardant, which comprises the steps of: carrying out reaction in a high pressure reaction kettle to generate intermediate by taking phosphorus oxychloride, ammonia water, phosphorus pentoxide, pentaerythritol and melamine as raw materials; 2) carrying out a reaction on the intermediate and diammonium hydrogen phosphate, polyvinyl alcohol, urea as well as 201type polyether polyol in the presence of an initiator; and finally, obtaining the product. The technology can be used for synthesizing high-poly type phosphate under the conditions of high temperature and high pressure; compared with the traditional high-temperature atmospheric technology, the synthesis technology improves the yield by more than 50%; the synthesis technology is simple in technology and convenient in control of the reaction process; and the obtained halogen-free high-poly type phosphate flame retardant is non-toxic, has the smoke suppression function, and is non-corroding, stable for heat and ultraviolet ray and good in flame retardant effect, thus being mainly used as high polymer material flame retardant.

Description

technical field [0001] The invention relates to a synthesis process of a polymer, in particular to a synthesis process of a halogen-free high polyphosphate flame retardant. Background technique [0002] At present, the development of flame retardants in the world shows the trend of non-halogenated, composite, harmless or low-harm and low-smoke. Polyphosphate flame retardant is one of the phosphorus-nitrogen flame retardants developed rapidly in recent years. It has excellent flame retardant effect, good compatibility with polymers, water resistance, solvent resistance, smokeless and low toxicity. , good dispersion, long-lasting flame retardant performance, compared with traditional halogen flame retardants and inorganic flame retardants, phosphorus nitrogen flame retardants are non-toxic, smoke suppression, non-corrosive, stable to heat and ultraviolet rays, flame retardant Good effect and other advantages. Chinese patent CN 101328269A discloses a preparation method of a p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G79/04C08L85/02
Inventor 王新钢张泽江刘军军李风李利君
Owner 应急管理部四川消防研究所
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