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Polysiloxane fire retardant containing nitrogen, phosphorus and silicon, and preparation method thereof

A technology of polysiloxane and flame retardant, which is applied in the field of polysiloxane flame retardant and its preparation, can solve problems such as complex synthesis steps, and achieve the goal of improving crosslinking strength, good flame retardant effect, and high yield Effect

Active Publication Date: 2017-05-24
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The siloxane production method is reasonably designed and the yield is high, but the synthesis steps are slightly complicated and many factors need to be controlled

Method used

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  • Polysiloxane fire retardant containing nitrogen, phosphorus and silicon, and preparation method thereof
  • Polysiloxane fire retardant containing nitrogen, phosphorus and silicon, and preparation method thereof
  • Polysiloxane fire retardant containing nitrogen, phosphorus and silicon, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Mix 5 parts of poly(methylhydrogensiloxane-dimethylsiloxane copolymer), 6*10 -5 Parts of Karstdet catalyst and 50 parts of isopropanol were added to a four-necked flask equipped with a reflux condenser, a thermometer, magnetic stirring, and an inert atmosphere, and the temperature was raised to 70°C and then stirred at a constant temperature for 15 minutes; after the temperature was raised to 100°C, the 15 parts of isocyanate propyltriethoxysilane and 15 parts of isopropanol in the pressure funnel were added dropwise into the four-necked flask, and the constant temperature reaction was continued for 6 hours; within 2 hours, 35 parts of allyl triethoxysilane in the constant pressure funnel Glycidyl ether and 20 parts of isopropanol were added dropwise in a four-necked flask, and the constant temperature reaction was continued for 6 hours; the solvent and unreacted substances were removed by distillation under reduced pressure to obtain the flame retardant intermediate API...

Embodiment 2

[0061] 10 parts of 1,3,5,7-tetramethylcyclotetrasiloxane, 4*10 -5 Parts of Speier catalyst and 60 parts of toluene solvent were added to a four-necked flask equipped with a reflux condenser, a thermometer, magnetic stirring, and an inert atmosphere, and the temperature was raised to 70°C and then stirred at a constant temperature for 10 minutes; after the temperature was raised to 95°C, the 10 parts of isocyanate propyltriethoxysilane and 15 parts of toluene in the funnel were added dropwise into the four-necked flask, and the reaction was continued at constant temperature for 8 hours; within 2 hours, 30 parts of allyl glycidyl ether in the constant pressure funnel Add 35 parts of toluene dropwise in a four-neck flask, continue the constant temperature reaction for 7h; remove the solvent and unreacted substances by distillation under reduced pressure to obtain the flame retardant intermediate API; all the flame retardant intermediate API obtained in the previous step , 35 part...

Embodiment 3

[0063] Mix 6 parts of polymethylhydrogen siloxane, 7*10 -5Parts of Speier catalyst and 70 parts of toluene solvent were added to a four-necked flask equipped with a reflux condenser, a thermometer, magnetic stirring, and an inert atmosphere, and the temperature was raised to 70°C and then stirred at a constant temperature for 10 minutes; after the temperature was raised to 100°C, the 10 parts of 3-isocyanatopropyl trimethoxysilane and 15 parts of toluene in the funnel were added dropwise into the four-necked flask, and the constant temperature reaction was continued for 7 hours; 50 parts of allyl glycidyl ether in the constant pressure funnel were added within 3 hours Add 20 parts of toluene dropwise in a four-neck flask, continue the constant temperature reaction for 5h; remove the solvent and unreacted substances by distillation under reduced pressure to obtain the flame retardant intermediate API; all the flame retardant intermediate API obtained in the previous step , 30 p...

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Abstract

The invention discloses a polysiloxane fire retardant containing nitrogen, phosphorus and silicon, and a preparation method thereof. The polysiloxane fire retardant is prepared through utilizing mutual reaction of hydrogen-containing silicone oil, allyl glycidyl ether, isocyanate silane and a phosphorus-containing active matter in a solvent. The fire retardant has a certain degree of polymerization, organic groups such as a benzene ring and longer -Si-O-Si- main chain are contained in a molecule, the fire retardant has favorable hydrophobicity, a contact angle reaches 118 degrees, and the compatibility of the fire retardant and a high polymer can be remarkably improved; the fire retardant is rich in carbon, nitrogen, phosphorus and silicon elements so as to have a synergistic flame retardant effect of various flame retardant elements, a high carbonization ability, and high flame retardant efficiency; the fire retardant has higher heat stability, and can meet the processing requirement of the high polymer; the polysiloxane fire retardant is rich in -Si-O-CH2CH3 group, and can be used as a modifying agent to modify other substances so as to obtain a functional fire retardant.

Description

technical field [0001] The invention relates to a polysiloxane flame retardant containing nitrogen, phosphorus and silicon and a preparation method thereof, belonging to the technical field of flame retardant preparation. Background technique [0002] In contemporary life, fire is one of the main disasters that generally threaten public safety and social development among various disasters. The main cause of fire is the spread of fire caused by flammable materials. Failure to impart flame retardancy to these flammable items will increase the spread of fire and release flammable gases and toxic fumes during combustion. Therefore, in order to reduce fire hazards and damage caused by fire, flame retardancy has become one of the important performance requirements of material properties. Since fire safety is closely related to people's living standards, with the improvement of people's living standards, the demand for flame retardants will continue to increase. [0003] In rec...

Claims

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Application Information

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IPC IPC(8): C08G77/395C08G77/388C08G77/30C08G77/26C08L83/08
CPCC08G77/26C08G77/30C08G77/388C08G77/395C08L83/08C08L2201/02C08L2201/08
Inventor 晏泓赵智垒高向华李生虎王远航张乃恩
Owner TAIYUAN UNIV OF TECH
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