Fire retardant in use for cellulose and fabricating method

A manufacturing method and technology for flame retardants, which are applied in the field of flame retardants and their manufacturing, can solve the problems of limiting the wide application of flame retardants, increasing product costs, and low flame retardant efficiency, and extending the flame retardant time and strengthening the flame retardant. Effect, strong flame retardant effect

Inactive Publication Date: 2005-01-12
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the manufacturing process of flame-retardant cellulose products, the addition amount of flame retardants required in the prior art is relatively large (generally more than 20% of the cellulose weight, or higher, to meet the flame-retardant requirements), in order to obtain com...

Method used

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  • Fire retardant in use for cellulose and fabricating method
  • Fire retardant in use for cellulose and fabricating method
  • Fire retardant in use for cellulose and fabricating method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) PSCl 3 Synthesis

[0041] Add 1 mole of sulfur and 0.015 mole of aluminum trichloride to a four-necked flask equipped with a thermometer, agitator, and reflux condenser, and heat up to 115°C to melt the sulfur; Quickly add 1 mole of PCl to the four-neck flask 3 , the temperature was controlled at 145° C., and the reaction was carried out for 1 hour. Finally, the reaction solution is distilled, and the fraction between 120°C is taken to obtain a colorless and transparent liquid, which is PSCl 3 ;

[0042] (2) Synthesis of 2-thio-2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane (DDSP)

[0043] Add 0.24 moles of PSCl to a four-necked flask equipped with a thermometer, a stirrer, and a reflux condenser 3and 0.24 moles of neopentyl glycol, and then added 0.05 moles of benzene, heated to 50°C to dissolve the neopentyl glycol, and then controlled the temperature at 45°C for constant temperature reaction for 1.5h. After the reaction, add 30ml of distilled water, shake w...

Embodiment 2

[0047] (1) PSCl 3 Synthesis

[0048] With embodiment 1;

[0049] (2) Synthesis of DDSP

[0050] Add 0.24 moles of PSCl to a four-necked flask equipped with a thermometer, a stirrer, and a reflux condenser 3 and 0.24 moles of neopentyl glycol, and then added 0.055 moles of benzene, heated to 50°C to dissolve the neopentyl glycol, and then controlled the temperature at 75°C for constant temperature reaction for 3 hours. After the reaction, add 30ml of distilled water, shake well and filter to separate the oil layer, and distill off benzene, and finally recrystallize the product with 0.15 mole of petroleum ether to obtain a white semi-crystalline solid, which is DDSP;

[0051] (3) Synthesis of DDPSN

[0052] Put 1 mole of DDSP after drying into a four-necked flask equipped with a thermometer, a stirrer, and a reflux condenser, and add 0.1 mole of CCl 4 , control the reaction temperature at 30°C, slowly add 0.5 mole of ethylenediamine, the reaction time is 3h, wash the reacti...

Embodiment 3

[0054] (1) PSCl 3 Synthesis

[0055] With embodiment 1;

[0056] (2) Synthesis of DDSP

[0057] Add 0.24 moles of PSCl to a four-necked flask equipped with a thermometer, a stirrer, and a reflux condenser 3 and 0.24 moles of neopentyl glycol, and then added 0.05 moles of benzene, heated to 50°C to dissolve the neopentyl glycol, and then controlled the temperature at 60°C for constant temperature reaction for 2.5 hours. After the reaction, add 30ml of distilled water, shake and filter to separate the oil layer, and distill to remove benzene, and finally recrystallize the product with 0.12 moles of petroleum ether to obtain a white semi-crystalline solid, which is DDSP;

[0058] (3) Synthesis of DDPSN

[0059] Put 1 mole of DDSP after drying into a four-necked flask equipped with a thermometer, a stirrer, and a reflux condenser, and add 0.1 mole of CCl 4 , control the reaction temperature at 25°C, slowly add 0.5 mole of ethylenediamine, the reaction time is 3h, wash the rea...

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PUM

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Abstract

The molecular formula of designed fire retardant for cellulose is C12H26O4P2S2N2 named as DDPSN. The preparing method includes reacting on trichloro-thiophosphorus with neophenyl dialcohol for 1.5-3 h. under dissolving of benzene or pyridine at 45-75 deg.C temperature, washing and distillating to remove benzene, forming DDSP by benzinum recrystallization and by drying for 24h. with airflow, reacting on drid DDSp with ethylene diamine for 3-5 hr. at 10-30 deg.C temp under dissolving of chloroform or carbon terochloride and obtaining DDPSN by ethyl ether recrystallization through 24 hr. drying with airflow.

Description

technical field [0001] The invention relates to a flame retardant and its manufacturing method technology, specifically a flame retardant containing high-efficiency flame-retardant elements phosphorus, sulfur and nitrogen and specially used for cellulose and its derivative products and its manufacturing method technology. The patent classification number is proposed to be Int.Cl 7 C09D 7 / 12. Background technique [0002] Natural cellulose fiber is the earliest fiber used by humans, and viscose fiber is also the earliest chemical cellulose fiber used. Their comfortable and excellent performance is incomparable to other fibers, and they are widely favored by consumers. But whether it is natural cellulose fibers such as cotton and hemp, or chemical cellulose fibers such as viscose, all cellulose fibers have a biggest weakness, that is, they are flammable! Flammability limits the further development and wider application of cellulose fiber products, so developing cellulose fi...

Claims

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Application Information

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IPC IPC(8): C08K5/5398C08L1/02
Inventor 程博闻任元林
Owner TIANJIN POLYTECHNIC UNIV
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