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Preparing method of temporary soluble type viscose microcapsule flame retardant

A technology of viscose fiber and microcapsules, which is applied in the field of preparation of temporarily soluble viscose fiber microcapsule flame retardants, can solve problems such as re-aggregation and impact on viscose fibers, and achieve improved flame retardant efficiency and flame retardant effect Good, simple preparation steps

Inactive Publication Date: 2016-06-08
JIANGSU SHIKONG COATING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention: Aiming at the fact that the current viscose fiber flame retardants will produce glue lumps during the mixing and dispersing treatment, and re-agglomeration will occur in a short time, thus affecting the spinnability of viscose fibers. Through the introduction of hydrophilic groups, the capsule flame retardant will disperse evenly when it encounters water and adhere to the viscose fiber during use, and then it will solidify when it comes out of the water to effectively disperse, thus avoiding the occurrence of glue in the spinning process. Block and re-agglomeration phenomenon, improve the spinnability of viscose fiber, and improve the flame retardancy of flame retardant

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0018] First, add 23g of 4,4-diaminobenzanilide and 60mL of deionized water to the four-neck flask in turn, stir and mix for 15 minutes, then continue to add 10mL of 30% hydrochloric acid solution, stir and mix, and heat in a water bath at 95°C React for 45 minutes; after the reaction is completed, stop heating and let stand to cool to 30°C, continue to add 22mL of 30% sodium hydroxide solution and 7.7g of sodium carbonate, stir and mix for 15min, then add 25mL of toluene, then heat to boiling, Insulate for 3 hours; after the boiling is completed, stop heating and cool to 30°C, add 13mL of benzamide dropwise, after the dropwise addition is completed, stir and mix for 30 minutes, adjust the pH to 7.0 with 30% sodium hydroxide solution , rotary evaporated to dryness, collected crystals, and prepared crystals; then in parts by weight, weighed 35 parts of dimethyl methylphosphonate, 20 parts of mass concentration were 15% hydrochloric acid, 5 parts of sorbitan fatty acid Esters, 1...

example 2

[0021] First, add 22g of 4,4-diaminobenzanilide and 55mL of deionized water to the four-neck flask in sequence, stir and mix for 10 minutes, then continue to add 5mL of 30% hydrochloric acid solution, stir and mix, and place in a water bath at 90°C for heating React for 30 minutes; after the reaction is completed, stop heating and let stand to cool to 20°C, continue to add 20mL of 30% sodium hydroxide solution and 7.5g of sodium carbonate, stir and mix for 10min, then add 20mL of toluene, then heat to boiling, Insulate for 2 hours; after the boiling is completed, stop heating and cool to 20°C, add 11 mL of benzamide dropwise, after the dropwise addition is completed, stir and mix for 25 minutes, adjust the pH to 7.0 with 30% sodium hydroxide solution , rotary evaporated to dryness, collected crystals, and prepared crystals; then in parts by weight, weighed 15 parts of dimethyl methylphosphonate, 25 parts of mass concentration were 15% hydrochloric acid, 10 parts of sorbitan fat...

example 3

[0024]First, add 22g of 4,4-diaminobenzanilide and 57mL of deionized water to the four-neck flask in turn, stir and mix for 12 minutes, then continue to add 7mL of 30% hydrochloric acid solution, stir and mix, and heat in a water bath at 92°C React for 40 minutes; after the reaction is complete, stop heating and let stand to cool to 25°C, continue to add 21mL of 30% sodium hydroxide solution and 7.6g of sodium carbonate, stir and mix for 12min, then add 22mL of toluene, then heat to boiling, Insulate for 2 hours; after the boiling is completed, stop heating and cool to 25°C, add 12mL of benzamide dropwise, after the dropwise addition is completed, stir and mix for 27min, adjust the pH to 7.0 with 30% sodium hydroxide solution , rotary evaporated to dryness, collected crystals, and prepared crystals; then in parts by weight, weighed 20 parts of dimethyl methylphosphonate, 20 parts of mass concentration were 15% hydrochloric acid, 10 parts of sorbitan fatty acid Esters, 15 parts...

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PUM

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Abstract

The invention relates to a preparing method of a temporary soluble type viscose microcapsule flame retardant and belongs to the technical field of flame retardant preparation. According to the method, at first, 4,4'-diamino benzanilide and deionized water are stirred and mixed, hydrochloric acid is added, the mixture is subjected to a water-bath heating reaction and cooled, a sodium hydroxide solution and sodium carbonate continue to be added, after stirring and mixing are carried out, toluene is added, then heating is carried out, heat is preserved, after cooling is carried out, benzamide is added dropwise, the mixture is stirred and mixed, after a pH value is adjusted to 7.0, the mixture is evaporated in a rotary mode to be dried, and the mixture is collected and crystallized to prepare a temporary soluble product; the temporary soluble product is mixed with substances like dimethyl methyl phosphonic acid ester to prepare a temporary solution, the temporary solution is mixed with cyclohexane, subjected to ultrasonic oscullating, placed into a polyvinyl alcohol solution, stirred, mixed, and filtered in a suction mode, and filter cakes are collected, washed and dried to obtain the flame retardant. The phenomena of rubber block generation and reunion in the spinning process are avoided, and a spinning property of viscose is improved; meanwhile, the flame-retardant effect is good, and flame-retardant efficiency is improved by 8-12%.

Description

technical field [0001] The invention relates to a preparation method of a temporarily soluble viscose fiber microcapsule flame retardant, belonging to the technical field of flame retardant preparation. Background technique [0002] Fire prevention is an eternal theme of human social security. Most of the polymer materials widely used in industry, agriculture and people's life are combustible and combustible in the air, and their limiting oxygen index is mostly lower than 20%. Therefore, a considerable part of the fires that have occurred in various countries in recent decades has been caused by the ignition of polymer materials. Moreover, the composition of modern synthetic polymer materials is different from that of natural polymer materials. The former can produce a large amount of smoke and dust of toxic and corrosive gaseous products during pyrolysis and combustion, so their consequences in fires are even more serious. The domestic research on flame-retardant viscose ...

Claims

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Application Information

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IPC IPC(8): D01F2/08
CPCD01F2/08
Inventor 陈明生薛红娟高力群
Owner JIANGSU SHIKONG COATING
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