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Quaternary phosphonium sulfonate fire retardant and synthesis method and use thereof

A quaternary phosphonium sulfonate and a synthesis method are applied in the field of refractory materials to achieve the effects of high yield, good chemical and thermal properties, and preventing dripping

Active Publication Date: 2014-07-23
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This flame retardant can combine the advantages of organophosphorus flame retardants and sulfonate flame retardants to exert the phosphorus-sulfur synergistic flame retardant effect, and has excellent flame retardant effect when applied to polymers such as polycarbonate. not reported

Method used

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  • Quaternary phosphonium sulfonate fire retardant and synthesis method and use thereof
  • Quaternary phosphonium sulfonate fire retardant and synthesis method and use thereof
  • Quaternary phosphonium sulfonate fire retardant and synthesis method and use thereof

Examples

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Embodiment 1

[0034] 1.1 Synthesis of sulfonate (IV) (R 1 = R 2 = )

[0035] Add sodium hydride (0.12mol) to the two-necked flask, and add N 2 protective gas. Then add an appropriate amount of tetrahydrofuran. Alcohol (II) (0.1 mol) was added dropwise in an ice-water bath, and magnetically stirred for about 10 minutes at room temperature. Dissolve sulfonyl chloride (III) (0.1 mol) in an appropriate amount of tetrahydrofuran, add it dropwise to the above reaction system in an ice-water bath, and react at room temperature for about 12 hours to obtain sulfonate IV. Yield about 78%.

[0036] 1.2 Synthesis of quaternary phosphonium sulfonate flame retardant (I)

[0037] Sulfonate (IV) (0.1mol) and triphenylphosphine (V) (0.067mol) were dissolved in an appropriate amount of toluene, added to a round-bottomed flask, under N 2 Protected and heated to reflux at about 85°C for 10h. Cool to room temperature, remove toluene by rotary evaporation, wash the reaction system with diethyl ether,...

Embodiment 2

[0056] 2.1 Synthesis of sulfonate (IV) (R 1 = R 2 = )

[0057] Add sodium hydride (0.12mol) to the two-necked flask, and add N 2 protective gas. Then add an appropriate amount of tetrahydrofuran. Alcohol (II) (0.1 mol) was added dropwise in an ice-water bath, and magnetically stirred for about 10 minutes at room temperature. Sulfonyl chloride (III) (0.12mol) was dissolved in an appropriate amount of tetrahydrofuran, and added dropwise to the above reaction system in an ice-water bath, and reacted for about 12 hours at room temperature to obtain sulfonate IV. Yield about 73%.

[0058] 2.2 Synthesis of quaternary phosphonium sulfonate flame retardant (I)

[0059] Dissolve sulfonate (IV) (0.1mol) and triphenylphosphine (V) (0.1mol) in an appropriate amount of xylene, add them to a round bottom flask, and place under N 2 Protected and heated to reflux at about 140°C for 10h. Cool to room temperature, add an appropriate amount of petroleum ether to precipitate a solid, ...

Embodiment 3

[0073] 3.1 Synthesis of sulfonate (IV) (R 1 = R 2 = )

[0074] Add sodium hydride (0.12mol) to the two-necked flask, and add N 2 protective gas. Then add an appropriate amount of tetrahydrofuran. Alcohol (II) (0.1 mol) was added dropwise in an ice-water bath, and magnetically stirred for about 10 minutes at room temperature. Dissolve sulfonyl chloride III (0.15 mol) in an appropriate amount of tetrahydrofuran, add it dropwise to the above reaction system in an ice-water bath, and react for about 12 hours at room temperature to obtain sulfonate (IV). Yield about 75%.

[0075] 3.2 Synthesis of quaternary phosphonium sulfonate flame retardant (I)

[0076] Dissolve sulfonate (IV) (0.1mol) and triphenylphosphine (V) (0.1mol) in an appropriate amount of xylene, add them to a round bottom flask, and place under N 2 Protected and heated to reflux at about 145°C for 12 hours. Cool to room temperature, add an appropriate amount of petroleum ether to precipitate a solid, let ...

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Abstract

The invention provides a quaternary phosphonium sulfonate fire retardant and a synthesis method and use thereof. The structural general formula of the fire retardant is as shown in a formula (I) in the specification, wherein R1 and R2 are one of C1-C24 alkyl, C2-C24 alkenyl, C3-C24 cycloalkyl, C4-C24 aryl, and C4-C24 substituted aromatic of which the substituent group contains N, O or P. The fire retardant is prepared from sulfonyl chloride, alcohol, an organic phosphorus compound and the like as raw materials by reaction in two steps. The synthesis condition is mild, operation is simple and convenient, and yield is high. Meanwhile, the fire retardant has good heat stability, and has good flame retardant efficiency when being applied to a plurality of polymers, UL-94 of the obtained PC fire-retardant composite material achieves the V-0 grade, UL-94 of the obtained POE fire-retardant composite material achieves V-2 grade, and meanwhile, good chemical and thermal properties are kept.

Description

technical field [0001] The invention belongs to the field of refractory materials, and in particular relates to a quaternary phosphonium sulfonate flame retardant and its synthesis method and application. Background technique [0002] At present, halogen-containing flame retardants are widely used organic flame retardants and have excellent flame-retardant properties. However, when a fire occurs, halogen-containing flame retardants will release a large amount of smoke and toxic hydrogen halide gas, causing secondary hazards. . With the promulgation of the RoHs and WEEE directives promulgated by the European Union, the application of organic halogen-containing flame retardants in the fields of electronic and electrical equipment has been subject to many restrictions. Therefore, the development of high-efficiency halogen-free flame retardants has become a very important topic. [0003] Most organophosphorus flame retardants have the characteristics of low smoke, halogen-free...

Claims

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Application Information

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IPC IPC(8): C07F9/54C07C309/29C07C303/32C08K5/50C08L69/00C08L23/02
Inventor 侯世杰张勇健江平开
Owner SHANGHAI JIAO TONG UNIV
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