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CN103061121A - Environmental-friendly flame-retardant finishing technology of real silk or real silk cellulosic fiber interwoven fabric - Google Patents

Environmental-friendly flame-retardant finishing technology of real silk or real silk cellulosic fiber interwoven fabric Download PDF

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Publication number
CN103061121A
CN103061121A CN2013100347845A CN201310034784A CN103061121A CN 103061121 A CN103061121 A CN 103061121A CN 2013100347845 A CN2013100347845 A CN 2013100347845A CN 201310034784 A CN201310034784 A CN 201310034784A CN 103061121 A CN103061121 A CN 103061121A
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real silk
fabric
softener
fire retardant
environmental protection
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CN2013100347845A
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吴岚
余志成
王晓芳
翁艳芳
钱士明
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HIGH FASHION (CHINA) CO Ltd
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HIGH FASHION (CHINA) CO Ltd
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Abstract

The invention relates to an environmental-friendly flame-retardant finishing technology of real silk or a real silk cellulosic fiber interwoven fabric, which has the advantages that the fabric can be endowed with a good flame-retardant function by the technology, and the content of free formaldehyde in the fabric is low. According to the technical solution, the environmental-friendly flame-retardant finishing technology of the real silk or the real silk cellulosic fiber interwoven fabric comprises the following steps of: (1) preparing finishing liquid by mixing a fire retardant, a synergist DL-121, a catalyst, a softening agent and water; (2) finishing, namely soaking for twice and rolling for twice, wherein the liquid rate is 80-100%; (3) drying, wherein the temperature is 70-90 degrees centigrade, and the time is 40-180 seconds; (4) baking by a heat-setting machine, wherein the temperature is 150-170 degrees centigrade and the time is 60-240 seconds; and (5) washing, namely firstly, washing by cold water (at a temperature same as an outdoor environment temperature), and then washing by warm water at 45-55 degrees centigrade for 10 minutes.

Description

The environmental protection flame retardant finishing technique of real silk or cocoon fiber cellulose fiber MIXED FABRIC
Technical field
The present invention relates to a kind of fabric loop environment friendly flame-retardant finishing technique, the flame-proof finishing process of especially authentic silk face fabric and cocoon fiber cellulose fiber interwoven fabric.
Background technology
Fire causes great threat to human life's property, and according to the statistics of World Developed Countries, about 50% fire is caused by textiles.The survey showed that for the death by accident that fire causes: the fire that is caused by textiles and upholstery holds pride of place, and simultaneously research finds that the pernicious gas that discharges during flammable textile combustion substantially exceeds the anti-flammability textiles to the extent of injury of human body.
Real silk is natural protein fibre, can not be by obtaining the durable flame-retardant effect with the method for fire retardant co-blended spinning, can only reach fire-retardant purpose by cocoon fiber or fabric are carried out rear arrangement.But Main Problems is: can obtain good flame retardant effect though cocoon fiber or fabric are carried out rear arrangement, oxygen index (LOI) can reach more than 30; But fabric feeling is partially hard after the arrangement, and powerful decline is larger, and yellowing is serious; And free formaldehyde is up to hundreds of ppm.For the cellulose fibres such as cotton, fiber crops, viscose glue because the oxygen index of itself is just not high, with silk blend or be interwoven to contain the silk fabrics fire resistance just poorer, the ratio of occupying that contains silk fabrics such as silk/cotton, silk/fiber crops then increases year by year in the market.
Summary of the invention
The purpose of this invention is to provide the finishing technique of a kind of real silk, cocoon fiber cellulose fiber MIXED FABRIC, this technique can give fabric good anti-flaming function, and the fabric free formaldehyde content is lower.
Technical scheme provided by the invention is: the environmental protection flame retardant finishing technique of real silk or cocoon fiber cellulose fiber MIXED FABRIC, carry out successively according to the following steps:
1) configuration dressing liquid: dressing liquid is formed by fire retardant, synergist DL-121, catalyst, softener and water mixed configuration, the content of each composition is: fire retardant 280-320g/L, synergist DL-12180-110g/L, catalyst 15-25g/L, softener is 15-25g/L, and all the other are water;
2) arrangement: two soak two rolls liquid carrying rate 80-100%;
3) oven dry: temperature 70-90 ℃, time 40-180 second;
4) bake: carry out at heat setting machine, temperature 150-170 ℃, time 60-240 second;
5) washing: first cold water (water temperature is identical with outdoor environment temperature) is washed, and then 45-55 ℃ of hot water wash is 10 minutes.
Described synergist DL-121 is formed by dihydroxymethyl dihydroxy ethylene-urea, dihydroxylic alcohols, phthalic anhydride hybrid reaction; Wherein dihydroxylic alcohols is diethylene glycol (DEG) or ethylene glycol or the mixture of the two; The mol ratio of dihydroxymethyl dihydroxy ethylene-urea and dihydroxylic alcohols is 1 ︰ 1, and phthalic anhydride is 0.5~1.0% of dihydroxylic alcohols quality; 70 ± 2 ℃ of reaction temperatures, reaction time 3-4h.
Described fire retardant is the hydroxyl organophosphorous fire retardant, comprises among fire retardant HFPO, the fire retardant DM-3070 any one.
Described catalyst is the acid metal salt, comprises MgCl2, ZnCl2 and Zn(NO3) in 2 any one.
Described softener is the nonionic silicone softening agent, comprises among softener HA-011, hydrophilic silicone oil FCG, softener G-AO2 and the softener TF-442A any one.
Active ingredient in the described dihydroxymethyl dihydroxy ethylene-urea is 40~50%.
The invention has the beneficial effects as follows: because the flame-proof treatment system that has adopted organophosphorous fire retardant and synergist to form has been given full play to phosphorus-nitrogen synergy, make the fabric after the arrangement have good flame retardant effect and durability; The synergist of development also makes the fabric face free formaldehyde content reach national formaldehyde one-level limitation standard in Effective Raise fabrics flame resistance and durability, has guaranteed that effectively the user's is healthy.
The specific embodiment
Principle of the present invention is: must could not react with fabric by synergist the performance fire retardation so have covalently bound active function groups to occur with real silk or cellulose fibre on the hydroxyl organophosphorous fire retardant.Synergist can with fiber on hydroxyl, carboxyl isoreactivity group and fire retardant generation cross-linking reaction, generate ehter bond or ester bond.Synergist DL-121 of the present invention is formed by dihydroxymethyl dihydroxy ethylene-urea, dihydroxylic alcohols, phthalic anhydride hybrid reaction.
Synergist can be used as the supplier of nitrogen simultaneously, for flame-retardant system provides the nitrogen element, generates the N-P key with fire retardant, forms the N-P collaboration system.This flame-retardant system is that condensed phase plays fire retardation, and the N-P flame-retardant system has promoted the dehydration of fiber and carbonization has reduced heat decomposition temperature, has reduced imflammable gas, has increased the flame retardancy solid carbon.In addition, phosphorus-nitrogen cooperative effect has been accelerated the phosphorus acylation reaction of fiber, and the content that improves the phosphorylated fiber strengthens fire retardancy.Therefore flame retardant effect also just can be greatly improved.
The fabric decomposition temperature reduces after the flame-proof treatment, and the more breeze of corresponding formation, breeze itself are firing-difficult matter matter, can heat insulation, oxygen barrier, be unfavorable for that gas conducts heat to material surface.Containing when silk fabrics is burnt after the flame-proof treatment forms thin and fine and close, smooth continuous carbon layer, and is difficult for subsiding and dripping; Can well cover matrix surface, play the effect of insulation wall, can effectively stop heat to be propagated to base material, stop the diffusion of imflammable gas and the transmission of free radical, stop the further burning of matrix, thereby obtain good flame retardant effect.
Embodiment 1
Real silk element crepe-back satin (100% real silk), redness
Technological process
Fabric is prepared
Figure BDA00002785101200031
Configuration dressing liquid → padding finishing liquid (two soak two rolls pick-up 85%) → preliminary drying (70 ℃, 3min) → bake → cold wash → hot water wash (50 ℃, 10min) → cold wash → oven dry
A. add water 40L in the charging basket, add successively fire retardant HFPO 29Kg, synergist DL-121 9Kg, catalyst MgCl 21.8Kg, softener HA-011 1.5Kg, need stir simultaneously; Adding water to total liquid measure is 100L again.
B. add dressing liquid in the setting machine groove, fabric padding finishing liquid is adjusted and is rolled rod pressure, and making the fabric liquid carrying rate is 85-90%.80 ± 5 ℃ of bake out temperatures, 2.5 minutes time, rolling is waited to bake.
C. baking temperature is 160 ± 5 ℃, time 3-4 minute, send washing after the rolling.
D. dye jigger water inlet 350L walks 4 roads, draining; The 350L of intaking again is warming up to 50 ± 2 ℃, walks 6 roads, draining; Cold flow washing, on roll out cylinder and send the blanket oven dry.
Synergist DL-121 in the present embodiment is formed by dihydroxymethyl dihydroxy ethylene-urea, diethylene glycol (DEG) and phthalic anhydride synthesis under normal pressure; Wherein the mol ratio of dihydroxymethyl dihydroxy ethylene-urea and diethylene glycol (DEG) is 1 ︰ 1, and phthalic anhydride is 0.5% of diethylene glycol (DEG) quality; 70 ± 2 ℃ of reaction temperatures, reaction time 3h.
Embodiment 2
Silk flosssilk wadding herringbone * (containing real silk 55.5%), shallow coffee look
Technological process
Fabric is prepared
Figure BDA00002785101200032
Configuration dressing liquid → padding finishing liquid (two soak two rolls pick-up 100%) → preliminary drying (90 ℃, 3min) → bake → cold wash → hot water wash (50 ℃, 10min) → cold wash → oven dry
A. add water 40L in the charging basket, add successively fire retardant DM-3070 30.5Kg, synergist DL-121 10Kg, catalyst Z nCl 22Kg, hydrophilic silicone oil FCG 2.5Kg need stir simultaneously; Adding water to total liquid measure is 100L again.
B. add dressing liquid in the setting machine groove, fabric padding finishing liquid is adjusted and is rolled rod pressure, and making the fabric liquid carrying rate is 95-100%.75 ± 5 ℃ of bake out temperatures, 3 minutes time, rolling is waited to bake.
C. baking temperature is 165 ± 5 ℃, time 2-3 minute, send washing after the rolling.
D. dye jigger water inlet 350L walks 4 roads, draining; The 350L of intaking again is warming up to 50 ± 2 ℃, walks 6 roads, draining; Cold flow washing, on roll out cylinder and send the setting machine oven dry.
Synergist DL-121 in the present embodiment is formed by dihydroxymethyl dihydroxy ethylene-urea, ethylene glycol and phthalic anhydride synthesis under normal pressure; Wherein the mol ratio of dihydroxymethyl dihydroxy ethylene-urea and ethylene glycol is 1 ︰ 1, and phthalic anhydride is 1.0% of quality of glycol; 70 ± 2 ℃ of reaction temperatures, reaction time 4h.
Embodiment 3
The numb silk fabric of silk ((containing real silk 54.6%), yellow green
Technological process
Fabric is prepared
Figure BDA00002785101200041
Configuration dressing liquid → padding finishing liquid (two soak two rolls pick-up 95%) → preliminary drying (80 ℃, 3min) → bake → cold wash → hot water wash (50 ℃, 10min) → cold wash → oven dry
A. add water 40L in the charging basket, add successively fire retardant HFPO 32Kg, synergist DL-121 11Kg, catalyst Z n(NO 3) 22.5Kg, softener TF-442A 2Kg, need stir simultaneously; Adding water to total liquid measure is 100L again.
B. add dressing liquid in the setting machine groove, fabric padding finishing liquid is adjusted and is rolled rod pressure, and making the fabric liquid carrying rate is 93-97%.85 ± 5 ℃ of bake out temperatures, 2.5 minutes time, rolling is waited to bake.
C. baking temperature is 165 ± 5 ℃, time 2-3 minute, send washing after the rolling.
D. dye jigger water inlet 350L walks 4 roads, draining; The 350L of intaking again is warming up to 50 ± 2 ℃, walks 6 roads, draining; Cold flow washing, on roll out cylinder and send the setting machine oven dry.
Synergist DL-121 in the present embodiment is formed by dihydroxymethyl dihydroxy ethylene-urea, dihydroxylic alcohols and phthalic anhydride synthesis under normal pressure; Wherein dihydroxylic alcohols is 1 ︰, 1 mixture of diethylene glycol (DEG) and ethylene glycol; The mol ratio of dihydroxymethyl dihydroxy ethylene-urea and dihydroxylic alcohols is 1 ︰ 1, and phthalic anhydride is 0.8% of dihydroxylic alcohols quality; 70 ± 2 ℃ of reaction temperatures, reaction time 3.5h.
Sample before and after the arrangement detects through Shandong Province textile product quality supervision and test test center, and testing result is as follows:
Figure BDA00002785101200051

Claims (6)

1. the environmental protection flame retardant finishing technique of real silk or cocoon fiber cellulose fiber MIXED FABRIC, carry out successively according to the following steps:
1) configuration dressing liquid: dressing liquid is formed by fire retardant, synergist DL-121, catalyst, softener and water mixed configuration, the content of each composition is: fire retardant 280-320g/L, synergist DL-12180-110g/L, catalyst 15-25g/L, softener is 15-25g/L, and all the other are water;
2) arrangement: two soak two rolls liquid carrying rate 80-100%;
3) oven dry: temperature 70-90 ℃, time 40-180 second;
4) bake: carry out at heat setting machine, temperature 150-170 ℃, time 60-240 second;
5) washing: first cold wash, then 45-55 ℃ of hot water wash is 10 minutes.
2. the environmental protection flame retardant finishing technique of real silk according to claim 1 or cocoon fiber cellulose fiber MIXED FABRIC, it is characterized in that: described synergist DL-121 is formed by dihydroxymethyl dihydroxy ethylene-urea, dihydroxylic alcohols, phthalic anhydride hybrid reaction; Wherein dihydroxylic alcohols is diethylene glycol (DEG) or ethylene glycol or the mixture of the two; The mol ratio of dihydroxymethyl dihydroxy ethylene-urea and dihydroxylic alcohols is 1 ︰ 1, and phthalic anhydride is 0.5~1.0% of dihydroxylic alcohols quality; 70 ± 2 ℃ of reaction temperatures, reaction time 3-4h.
3. the environmental protection flame retardant finishing technique of real silk according to claim 2 or cocoon fiber cellulose fiber MIXED FABRIC, it is characterized in that: described fire retardant is the hydroxyl organophosphorous fire retardant, comprises among fire retardant HFPO, the fire retardant DM-3070 any one.
4. the environmental protection flame retardant finishing technique of real silk according to claim 3 or cocoon fiber cellulose fiber MIXED FABRIC, it is characterized in that: described catalyst is the acid metal salt, comprises MgCl2, ZnCl2 and Zn(NO3) in 2 any one.
5. the environmental protection flame retardant finishing technique of real silk according to claim 4 or cocoon fiber cellulose fiber MIXED FABRIC, it is characterized in that: described softener is the nonionic silicone softening agent, comprises among softener HA-011, hydrophilic silicone oil FCG, softener G-AO2 and the softener TF-442A any one.
6. the environmental protection flame retardant finishing technique of real silk according to claim 5 or cocoon fiber cellulose fiber MIXED FABRIC, it is characterized in that: the active ingredient in the described dihydroxymethyl dihydroxy ethylene-urea is 40~50%.
CN2013100347845A 2013-01-28 2013-01-28 Environmental-friendly flame-retardant finishing technology of real silk or real silk cellulosic fiber interwoven fabric Pending CN103061121A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104562665A (en) * 2014-12-29 2015-04-29 无锡蚕魅科技有限公司 Preparation method of acid-alkali resistant flame-retardant silk
CN105713162A (en) * 2015-09-30 2016-06-29 齐齐哈尔大学 1,2-Propylene glycol etherification modified DMDHEU resin and synthetic method thereof
CN106758169A (en) * 2016-12-14 2017-05-31 江苏华佳控股集团有限公司 A kind of method for sorting of anti-flammability real silk fabric and its application
CN107254773A (en) * 2017-06-27 2017-10-17 太仓市玛雅针织有限公司 A kind of preparation method of anti-flammability fabric
CN107326671A (en) * 2017-06-26 2017-11-07 苏州威尔德工贸有限公司 A kind of silk fiber antiflaming finishing agent
CN108193345A (en) * 2018-03-07 2018-06-22 芜湖航飞科技股份有限公司 A kind of self-rolling woven high temperature casing and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
刘蕊平等: "真丝织物低甲醛阻燃整理工艺及机理研究", 《浙江理工大学学报》 *
游甜甜等: "DMDHEU树脂改性工艺研究", 《南通大学学报(自然科学版)》 *

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104562665A (en) * 2014-12-29 2015-04-29 无锡蚕魅科技有限公司 Preparation method of acid-alkali resistant flame-retardant silk
CN104562665B (en) * 2014-12-29 2016-08-17 无锡蚕魅科技有限公司 A kind of preparation method of acid and alkali-resistance flame-retardant silk
CN105713162A (en) * 2015-09-30 2016-06-29 齐齐哈尔大学 1,2-Propylene glycol etherification modified DMDHEU resin and synthetic method thereof
CN105713162B (en) * 2015-09-30 2018-01-09 齐齐哈尔大学 1,2 propane diols are etherified modified DMDHEU resin and its synthetic method
CN106758169A (en) * 2016-12-14 2017-05-31 江苏华佳控股集团有限公司 A kind of method for sorting of anti-flammability real silk fabric and its application
CN106758169B (en) * 2016-12-14 2019-02-26 江苏华佳控股集团有限公司 A kind of finishing method of flame-retardant silk fabric and its application
CN107326671A (en) * 2017-06-26 2017-11-07 苏州威尔德工贸有限公司 A kind of silk fiber antiflaming finishing agent
CN107254773A (en) * 2017-06-27 2017-10-17 太仓市玛雅针织有限公司 A kind of preparation method of anti-flammability fabric
CN108193345A (en) * 2018-03-07 2018-06-22 芜湖航飞科技股份有限公司 A kind of self-rolling woven high temperature casing and preparation method thereof

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Application publication date: 20130424