News Details
Synthesis of phosphate-ester flame retardant
2017-9-26 11:35:29
Synthesis of phosphate-ester flame retardant
Synthesis scheme of phosphate flame retardants: a scheme proposed by henan university
1, the intermediate of resorcinol synthesis (phosphoryl chloride) : anhydrous aluminum chloride as catalyst, phosphorus oxychloride and resorcinol mole ratio of 6:1 is reaction temperature at 90-90 ℃, reaction time of 5 h, dosage of catalyst is 0.65% of the total amount of phosphorus oxychloride as, intermediate yield up to 96.2%.
The synthesis of 2, RDP: anhydrous aluminum chloride as catalyst, with the method of phenol continuous feeding, feeding temperature 100 ℃, the heat preservation temperature 140-160 ℃, phenol and resorcinol mole ratio was 4.2:1, the reaction time is 4 h, dosage of catalyst is 0.5% of the total intermediates, the product yield was about 85%.
3. Test procedure: a 100ml four-mouth flask with mechanical stirrer, thermometer, condenser tube and constant pressure funnel shall be installed. From above condenser pipe by CaCl2 drying tower, HCl absorption equipment, in response to add 16.0 ml bottle phosphorus oxychloride and 0.8 g anhydrous aluminium trichloride, began to stir, the ready 100 ml bottle (conical flask) triangle add 30 ml of phosphorus oxychloride and 11.0 g (0.1 mol) resorcinol, stir the resorcinol dissolved, added to the constant pressure in the funnel, began to drop in the 100 ℃ with a mixture of phosphorus oxychloride and benzodiazepines between, add finish at 100 ℃ heat preservation 5 h, began to drop overtime, rapid response, and has a huge number of HCl gas emitted by dropping speed control, the control response speed. At the beginning, the reaction liquid is transparent and transparent. As the reaction is carried out, the reaction fluid becomes lighter and lighter, and finally the light yellow is transparent or almost colorless. Triclosan was recovered from decompression distillation, and the diphenol biphenol (phosphoryl dichloride) was found.
Then distillation unit to the reaction device, add molten phenol in constant voltage funnel 40.3 g (0.42 mol), adding catalyst, began to drop in the 100 ℃ melting phenol, and never put off till tomorrow what you can, then heat up to 150 ℃ heat preservation 4 ~ 8 h h, the product obtained for yellow or colorless transparent liquid. The reaction device should be the vacuum distillation unit, which can recover the raw material of the flame retardant RDP.
Isopropylphenyl Phosphate(IPPP35) Use
The Product Is Used For Rubber Products And PVC Plastic Flame Retardant Conveyor Belt, Cable, Chloroprene Rubber, Rubber And Other Synthetic Rubber Flame Retardant Plasticizer, Isopropylphenyl Phosphate Flame Retardant IPPP35 Use Also Applies To Fabric Coating, Circuit Boards, Flooring, Textiles, PVC, Phenolic Resin, And Other Fields.
Isopropylphenyl Phosphate Flame Retardant IPPP35 Halogen-Free Phosphate Flame Retardant Plasticizer, Which Does Not Pollute The Environment Twice. It Is The Lowest In The Phosphate Species And Has The Highest Phosphorus Content. This Product Is Colorless And Transparent, Good Compatibility, The Use Of Both Flame Retardant And Plasticizer, In The Flame Retardant And Plasticizer To Play A Balance Between The Role, But Also To Make The Processing Of The Same Material And Its Physical Properties.
Use RDP coarse product 2% oxalic acid solution washing, 2% naoh aqueous solution washing twice respectively, and then washed with water to neutral, vacuum distillation and distillate, filtering pale yellow or colorless transparent viscous liquid, is the end product of flame retardants RDP.
Main ingredients: phosphorus oxychloride, analysis of pure, resorcinol, analysis of pure, phenol, analysis of pure, anhydrous aluminium trichloride, analysis of pure, anhydrous calcium chloride, analysis of pure, sodium hydroxide, analysis of pure, oxalic acid
Instrument: d-971 type infinitely variable speed governor agitator; Temperature controller; Circulating water multi-purpose vacuum pump; Constant temperature magnetic stirrer; AVARTAR 360ft-ir infrared spectrometer; TG/DTA6300 thermal analyzer.
Synthesis scheme of phosphate-ester flame retardant 2: experimental scheme proposed by nanjing normal university
Test steps: phosphorus oxychloride as 42.2 g and 42.2 g benzodiazepines added to the reaction between the bottle and add 1.2 g anhydrous aluminium chloride as catalyst, stirring and heating, heating up to 60 ℃, 6 h reaction, vacuum distillation to remove excessive phosphorus oxychloride, the system temperature down to room temperature, then add 47.1 g of phenol, heating, keep the reaction at 130 ℃, reaction 8 h, vacuum distillation to remove not reaction of phenol, the alkaline cleaning, washing, drying process of the final product is 64.6 g, yield was 90% (with resorcinol).
Conclusion: the RDP flame retardant is synthesized with trichloro phosphorus, polyphenol and phenol as raw materials without aqueous trichloride as catalyst. The optimum technological conditions of the reaction were: the ratio of triclosan and the molar ratio was 2.2:1; The dosage of aluminum chloride catalyst was 2% of the total reactant. The first step reaction temperature of 60 ℃, reaction time 6 h; The second step reaction temperature is 130 ℃, reaction time 8 h; The yield of the product reaches 90%.
Copyright: Zhang Jia Gang YaRui Chemical co.,Ltd
http://www.yaruichem.com
Synthesis scheme of phosphate flame retardants: a scheme proposed by henan university
1, the intermediate of resorcinol synthesis (phosphoryl chloride) : anhydrous aluminum chloride as catalyst, phosphorus oxychloride and resorcinol mole ratio of 6:1 is reaction temperature at 90-90 ℃, reaction time of 5 h, dosage of catalyst is 0.65% of the total amount of phosphorus oxychloride as, intermediate yield up to 96.2%.
The synthesis of 2, RDP: anhydrous aluminum chloride as catalyst, with the method of phenol continuous feeding, feeding temperature 100 ℃, the heat preservation temperature 140-160 ℃, phenol and resorcinol mole ratio was 4.2:1, the reaction time is 4 h, dosage of catalyst is 0.5% of the total intermediates, the product yield was about 85%.
3. Test procedure: a 100ml four-mouth flask with mechanical stirrer, thermometer, condenser tube and constant pressure funnel shall be installed. From above condenser pipe by CaCl2 drying tower, HCl absorption equipment, in response to add 16.0 ml bottle phosphorus oxychloride and 0.8 g anhydrous aluminium trichloride, began to stir, the ready 100 ml bottle (conical flask) triangle add 30 ml of phosphorus oxychloride and 11.0 g (0.1 mol) resorcinol, stir the resorcinol dissolved, added to the constant pressure in the funnel, began to drop in the 100 ℃ with a mixture of phosphorus oxychloride and benzodiazepines between, add finish at 100 ℃ heat preservation 5 h, began to drop overtime, rapid response, and has a huge number of HCl gas emitted by dropping speed control, the control response speed. At the beginning, the reaction liquid is transparent and transparent. As the reaction is carried out, the reaction fluid becomes lighter and lighter, and finally the light yellow is transparent or almost colorless. Triclosan was recovered from decompression distillation, and the diphenol biphenol (phosphoryl dichloride) was found.
Then distillation unit to the reaction device, add molten phenol in constant voltage funnel 40.3 g (0.42 mol), adding catalyst, began to drop in the 100 ℃ melting phenol, and never put off till tomorrow what you can, then heat up to 150 ℃ heat preservation 4 ~ 8 h h, the product obtained for yellow or colorless transparent liquid. The reaction device should be the vacuum distillation unit, which can recover the raw material of the flame retardant RDP.
Isopropylphenyl Phosphate(IPPP35) Use
The Product Is Used For Rubber Products And PVC Plastic Flame Retardant Conveyor Belt, Cable, Chloroprene Rubber, Rubber And Other Synthetic Rubber Flame Retardant Plasticizer, Isopropylphenyl Phosphate Flame Retardant IPPP35 Use Also Applies To Fabric Coating, Circuit Boards, Flooring, Textiles, PVC, Phenolic Resin, And Other Fields.
Isopropylphenyl Phosphate Flame Retardant IPPP35 Halogen-Free Phosphate Flame Retardant Plasticizer, Which Does Not Pollute The Environment Twice. It Is The Lowest In The Phosphate Species And Has The Highest Phosphorus Content. This Product Is Colorless And Transparent, Good Compatibility, The Use Of Both Flame Retardant And Plasticizer, In The Flame Retardant And Plasticizer To Play A Balance Between The Role, But Also To Make The Processing Of The Same Material And Its Physical Properties.
Use RDP coarse product 2% oxalic acid solution washing, 2% naoh aqueous solution washing twice respectively, and then washed with water to neutral, vacuum distillation and distillate, filtering pale yellow or colorless transparent viscous liquid, is the end product of flame retardants RDP.
Main ingredients: phosphorus oxychloride, analysis of pure, resorcinol, analysis of pure, phenol, analysis of pure, anhydrous aluminium trichloride, analysis of pure, anhydrous calcium chloride, analysis of pure, sodium hydroxide, analysis of pure, oxalic acid
Instrument: d-971 type infinitely variable speed governor agitator; Temperature controller; Circulating water multi-purpose vacuum pump; Constant temperature magnetic stirrer; AVARTAR 360ft-ir infrared spectrometer; TG/DTA6300 thermal analyzer.
Synthesis scheme of phosphate-ester flame retardant 2: experimental scheme proposed by nanjing normal university
Test steps: phosphorus oxychloride as 42.2 g and 42.2 g benzodiazepines added to the reaction between the bottle and add 1.2 g anhydrous aluminium chloride as catalyst, stirring and heating, heating up to 60 ℃, 6 h reaction, vacuum distillation to remove excessive phosphorus oxychloride, the system temperature down to room temperature, then add 47.1 g of phenol, heating, keep the reaction at 130 ℃, reaction 8 h, vacuum distillation to remove not reaction of phenol, the alkaline cleaning, washing, drying process of the final product is 64.6 g, yield was 90% (with resorcinol).
Conclusion: the RDP flame retardant is synthesized with trichloro phosphorus, polyphenol and phenol as raw materials without aqueous trichloride as catalyst. The optimum technological conditions of the reaction were: the ratio of triclosan and the molar ratio was 2.2:1; The dosage of aluminum chloride catalyst was 2% of the total reactant. The first step reaction temperature of 60 ℃, reaction time 6 h; The second step reaction temperature is 130 ℃, reaction time 8 h; The yield of the product reaches 90%.
Copyright: Zhang Jia Gang YaRui Chemical co.,Ltd
http://www.yaruichem.com
Spanish
French
Italian
Portuguese
Japanese
Korean
Arabic
Russian