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CN109056320A - A kind of fire-retardant hydrophobic finishing method based on cotton fabric - Google Patents

A kind of fire-retardant hydrophobic finishing method based on cotton fabric Download PDF

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Publication number
CN109056320A
CN109056320A CN201810784054.XA CN201810784054A CN109056320A CN 109056320 A CN109056320 A CN 109056320A CN 201810784054 A CN201810784054 A CN 201810784054A CN 109056320 A CN109056320 A CN 109056320A
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China
Prior art keywords
fabric
finishing
coupling agent
flame
retardant
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Granted
Application number
CN201810784054.XA
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Chinese (zh)
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CN109056320B (en
Inventor
叶远丽
巫瑛
蒋春燕
李飞
李嘉
杜金梅
张璐璐
王鸿博
傅佳佳
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Jiangnan University
Swoto Protection and Technology Co Ltd
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Jiangnan University
Swoto Protection and Technology Co Ltd
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Priority to CN201810784054.XA priority Critical patent/CN109056320B/en
Publication of CN109056320A publication Critical patent/CN109056320A/en
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/50Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
    • D06M13/51Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
    • D06M13/513Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/184Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/207Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • D06M2101/06Vegetal fibres cellulosic
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10Repellency against liquids
    • D06M2200/12Hydrophobic properties
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/30Flame or heat resistance, fire retardancy properties

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

本发明公开了一种棉的阻燃疏水织物的整理方法,属于功能纺织品技术领域。本发明方法采用硅烷偶联剂改性柠檬酸及长链硅氧烷类化合物(拒水剂)处理棉织物,得到具有阻燃疏水性能的纺织品。整理方法采用传统的轧烘焙工艺,对设备要求小,属于连续化生产工艺,产品均匀性、重复性好,省时,高效。因整个整理过程都是在较温和条件下进行,焙烘时间短,织物受到的损伤小。该方法可用于棉纺织物的阻燃疏水功能整理。The invention discloses a method for finishing cotton flame-retardant and hydrophobic fabrics, belonging to the technical field of functional textiles. The method of the invention adopts the silane coupling agent to modify the citric acid and the long-chain siloxane compound (water repellent) to treat the cotton fabric, so as to obtain the textile with flame-retardant and hydrophobic properties. The finishing method adopts the traditional rolling and baking process, which requires less equipment and belongs to the continuous production process, with good product uniformity and repeatability, time-saving and high efficiency. Because the whole finishing process is carried out under relatively mild conditions, the baking time is short and the damage to the fabric is small. The method can be used for flame retardant and hydrophobic functional finishing of cotton fabrics.

Description

A kind of fire-retardant hydrophobic finishing method based on cotton fabric
Technical field
The fire-retardant hydrophobic finishing method based on cotton fabric that the present invention relates to a kind of, belongs to function textile technical field
Background technique
It is easy to be spontaneously wet out by water, be infected with the series of problems such as washing difficulty after greasy dirt, contamination currently, most fabrics exist.This leads Fabric is caused to arrange the series of problems such as time-consuming and laborious, big, the detergent pollution environment of slurry amount.Meanwhile as textile uses Amount increases sharply, and the fire incident as caused by textile is also increasing, and the mankind directly contact with textile, once burning, gently Person's skin burn, heavy then threat to life, in addition textile combustion can also generate the life that pernicious gas endangers people.As the mankind are raw The flat raising of running water, consumer propose unprecedented high request to the fire-retardant hydrophobic performance of textile fabric.Therefore, it reduces because spinning Fire incident caused by fabric burns, studies the flame-retarded technology of textile, while assigning fabric hydrophobic soil release performance energy, exploitation tool There is the textile of fire-retardant hydrophobic effect to become one of the Main way of research.The hydrophobic of fabric refers to fabric to the refusing property of resistance of water Energy.The purpose of hydrophobic finishing is the wetting for preventing water to fabric, and fabric still maintains breathable moisture permeability after arrangement.Flame-retardant textile Combustibility of the fabric in flame is exactly reduced, the rate of fire travel is slowed down, the quick self-extinguishment of fabric energy, subtracts after flame is removed Burning bring harm less.Demand domestic, on international market to the fabric with fire-retardant hydrophobic composite performance is increasing year by year Add.The advantages that cotton fabric is natural, comfortable and easy to wear, antistatic because of its feel becomes weaving one of main fabric, but pure cotton is knitted Object the disadvantages of there are inflammable easy contaminations, therefore fire-retardant hydrophobic cotton fabric is developed, it has very important significance.
The fire-retardant hydrophobic finishing of textile generally uses top finish, but the fabric feeling of top finish is poor, airtight And durability is poor.With the exploitation of new technology, the technologies such as plasma, electron radiation are applied, but these new technologies by Its industrial application is limited in the cost problem of the inhomogeneities of running product, poor repeatability and equipment.
Summary of the invention
The fire-retardant hydrophobic finishing method based on cotton fabric that the invention discloses a kind of is to utilize silane coupler modified lemon Acid and long-chain type siloxane water repellent handle fabric, obtain the cotton fabric with fire-retardant hydrophobic function.
The method of the invention the following steps are included:
Step (1) silane coupler modified Citric Acid Finishing: amino silicane coupling agent is hydrolyzed first, then by citric acid It is slowly dropped in amino silicane coupling agent hydrolyzate and obtains silane coupler modified Citric Acid Finishing liquid, then cotton fabric is added Into the dilution of silane coupler modified Citric Acid Finishing liquid, using rolling baking process finish fabric.
Step (2) long-chain type siloxane water repellent arranges: will be after the processing of silane coupler modified Citric Acid Finishing liquid Fabric be impregnated into long-chain type siloxane water repellent, using padding baking technique.
Described hydrolyze amino silicane coupling agent is to take water as a solvent, using hydrochloric acid as catalyst, concentration of hydrochloric acid 0.05g/L ~0.1g/L, the content of amino silicane coupling agent is 150-250g/L in gained amino silicane coupling agent hydrolyzate.
The Citric Acid Dosage is 150-200g/L amino silicane coupling agent hydrolyzate.
The concentration of silane coupler modified citric acid is 50-100g/L in the dilution.
The long-chain type siloxane water repellent processing cotton fabric is the long-chain type siloxane water repellent using dehydrated alcohol as solvent Dosage is 15-35g/L, and using hydrochloric acid as catalyst, concentration of hydrochloric acid is 0.01g/L~0.05g/L, will be changed by silane coupling agent Treated that fabric is immersed for property Citric Acid Finishing liquid.The long-chain type siloxane water repellent can select commercialization is siliceous to have Machine water repellent compound.The long-chain type siloxane water repellent is octyl trimethoxy silane, ruthenium trimethoxysilane, dodecane The mixing of one or more of base trimethoxy silane, tetradecyltrimethoxysilane or hexadecyl trimethoxy silane Object.
It is to roll extra processing with padding machine after dipping 1-5min using baking process finish fabric is rolled in the step (1) Liquid, pick-up 80-120%, 80-120 DEG C bakes 3-5min, then bakes 3-5min for 150-180 DEG C.
Using baking technique is padded in the step (2), it is to roll extra treatment fluid with padding machine after dipping 1-5min, rolls remaining Rate is 80-100%, and 60-90 DEG C bakes 3-5min, then bakes 3-5min for 120-150 DEG C.
Beneficial effects of the present invention: this method can be used for the fire-retardant hydrophobic finishing of all cotton fabrics, have the advantage that
1. product uniformity, reproducible, at low cost.Using traditional dyeing and finishing technology, to equipment without particular/special requirement, simultaneously Since using padding process, final products have good uniform in effect.
2. reaction condition is relatively mild, pH is controlled between 5~6, avoids common process high temperature, highly basic, strong acid condition Fabric strength caused by lower declines.Cotton fabric ingredient is cellulose fibre, the β-D glucose of cellulose remain based structures make its intolerant to Acid, oxidant etc., therefore the scission of link of glycosidic bond, fabric intensity decline occur under high temperature, strong acid, highly basic for cotton.The silicon that the present invention uses The coupling agent modified citric acid of alkane and long-chain type siloxane water repellent are organized in and react compared in benign environment, small to fabric damage, can The good non-ironing fire-retardant hydrophobic function of fabric is assigned, fabric whiteness variation is unobvious after arrangement.
3. the present invention combines silane coupler modified citric acid and long-chain type siloxane water repellent finishing of cotton textiles.Silane is even Join agent containing there are two types of different chemically active functional groups: one kind is that hydrolyzable groups can also be mutual between group after hydrolyzing Reaction generates complicated space network;Another kind of is the functional groups such as amino or epoxy group, living with certain reaction Property, but it more difficult is reacted with the hydroxyl of cotton fiber.Citric acid belongs to polynary acid reagent, can be used as the crosslinking of amino etc. with hydroxyl Agent uses ,-the NH with amino silicane coupling agent2Crosslinking arranges amino silicane coupling agent to fabric surface as cotton fabric Fire retardant, to improve the flame retardant property of cotton fabric.At the same time, it is the function of silanol that amino silicane coupling agent, which also has hydrolyzable, Group can be crosslinked and generate reticular structure, further increase the durability of flame retardant effect, and assign fabric certain ironing-free performance.It is long Chain type siloxane water repellent contains the alkane chain with low-surface-energy, can be effectively reduced fabric surface energy, has fabric Good water repellent effect, and fabrics feel soft after arrangement.Long-chain type siloxane water repellent is used alone to arrange, fabric only has Medium water-wash resistance is first arranged with silane coupler modified citric acid, the silanol structure of long-chain type siloxane water repellent It can be combined well with amino silicane coupling agent, the two is used in conjunction with and can prepare the cotton with fire-retardant hydrophobic complex function and knit Object improves water-wash resistance.
4. the present invention uses padding process, entire arrangement process is carried out under the conditions of partial neutral, and it is short to bake the time, instead Mild condition is answered, the damage that fabric is subject to is small.Therefore, the present invention has great social and economic implications.
Specific embodiment
For the cloth of not flame retardant effect, meeting sustained combustion (i.e. after flame time is big) after flame is left, is gone back after open fire Glow (and the inflammable index) for loseing flame is had, after flame time is usually indicated with a period of time is greater than;For Cloth with flame retardant property, after leaving flame, can stop within the cracking time burn (afterflame and smoldering time are short), afterflame and Smoldering time is usually indicated with a period of time is less than.
Control sample 1 (without any finishing of cotton textiles)
Fabric: plain weave pure cotton fabric (40S × 40S/133*72), is raw cotton, and material both without hydrophobic effect does not have yet in this There is flame retardant effect.
Cotton fabric is not collated, and Static water contact angles are 0 °;According to AATCC22-2010 testing standard, imitated without waterproof Fruit.Water droplet penetration time ﹤ 0.5s, hydrophily are strong;According to national standard GB_T 5455-1997 textile combustion performance test normal beam technique Standard, fabric after flame time ﹥ 10s, smoldering time ﹥ 25s, flammability are strong.
Product is after 20 washings, 0 ° of the static contact angle of fabric, fabric after flame time ﹥ 10s, smoldering time ﹥ 25s, combustion Burning property is strong.
Control sample 2 (only with aminosilane coupling agent modifying citric acid treatment)
Silane coupler modified citric acid treatment:
Silane coupling agent hydrolysis (concentration containing amino silicane coupling agent is 150g/L, and hydrochloric acid is catalyst, and water is solvent) → Modified Citric Acid (citric acid concentration 150g/L) → fabric impregnates silane coupler modified citrate diluent (50g/L) 5- 10min → second dipping and rolling (pick-up 80%) → 80 DEG C of preliminary drying 3min → 150 DEG C bake 3min.
After cotton fabric is collated, 40 ° of Static water contact angles ﹤, water droplet gradually permeates;According to AATCC22-2010 test mark Standard, waterproof effect almost without.Water droplet penetration time ﹤ 2s, hydrophily is strong, does not have hydrophobicity;According to national standard GB_T 5455- 1997 textile combustion performance test normal beam technique standards, fabric after flame time ﹤ 5s, smoldering time ﹤ 10s have certain anti-flammability.
Product is after 20 washings, 0 ° of the static contact angle of fabric, fabric after flame time ﹤ 8s, and smoldering time ﹤ 12s has Certain anti-flammability.
The present invention only has certain flame retardant effect compared with without finishing of cotton textiles (control sample 1) fire-retardant hydrophobic effect, but Without hydrophobic effect, fabric after flame time ﹤ 5s, smoldering time ﹤ 10s, breaking strength, which is lost, to be reduced and (is lower than 20%).
Control sample 3 (arranges) only with long-chain type siloxane water repellent
Fabric: plain weave pure cotton fabric (40S × 40S/133*72)
Long-chain type siloxane water repellent arranges:
Cotton fabric dipping long-chain type siloxane water repellent (hexadecyl trimethoxy silane 30g/L, hydrochloric acid are catalyst, Dehydrated alcohol is solvent) 5min → second dipping and rolling (pick-up 80%) → 80 DEG C of preliminary drying 3min → 120 DEG C bake 5min.
After cotton fabric is collated, Static water contact angles are 130 degree;According to AATCC22-2010 testing standard, waterproof effect Reach 90 points or more.Water droplet is impermeable, and hydrophobicity is strong;It is vertical according to national standard GB_T 5455-1997 textile combustion performance test Method standard, fabric after flame time ﹥ 10s, smoldering time ﹥ 20s, flammability are strong.
Product is after 20 washings, and 110 ± 5 ° of the static contact angle of fabric, durability is medium, fabric after flame time ﹥ 10s, Smoldering time ﹥ 25s, flammability are strong.
Compared with without the fire-retardant hydrophobic effect of finishing of cotton textiles (control sample 1-2), hydrophobic effect significantly increases the present invention, but There is no flame retardant effect, fabric smoldering time reduces unobvious, breaking strength loss reduction (being lower than 20%).
Embodiment 1
Fabric: plain weave pure cotton fabric (40S × 40S/133*72)
1) silane coupler modified citric acid treatment:
Silane coupling agent hydrolysis (concentration containing amino silicane coupling agent is 150g/L, and hydrochloric acid is catalyst, and water is solvent) → Modified Citric Acid (citric acid concentration 150g/L) → fabric impregnates silane coupler modified citrate diluent (50g/L) 5- 10min → second dipping and rolling (pick-up 80%) → 80 DEG C of preliminary drying 3min → 150 DEG C bake 3min.
2) long-chain type siloxane water repellent arranges:
Cotton fabric impregnates long-chain type siloxane water repellent, and (ruthenium trimethoxysilane 20g/L, hydrochloric acid is catalyst, anhydrous Ethyl alcohol is solvent) 5min → second dipping and rolling (pick-up 90%) → 80 DEG C of preliminary drying 3min → 120 DEG C bake 5min.
After cotton fabric is collated, Static water contact angles are 115 degree;According to AATCC22-2005 testing standard, waterproof effect Reach 90 points or more.Cotton fabric is after silane coupler modified citric acid treatment, fabric after flame time ﹤ 5s, smoldering time drop Low is < 8s, and has good anti-wrinkle effect, and less, textile finishing effect is preferable for ultimate strength loss.
Product is after 20 washings, and 105 ± 5 ° of fabric static contact angle, fabric after flame time ﹤ 6s, smoldering time < 10s, Fabrics flame resistance hydrophobic effect is still preferable, has good durability.
Fabric after present invention arrangement, water drop static contact angle increase, and fabric smoldering time reduces, and fabric has well Anti-wrinkle effect, breaking strength loss reduces (be lower than 20%), and the decline of fabrics flame resistance hydrophobic effect is unobvious after washing.
The fire-retardant hydrophobic effect repeatability of product: the cotton fabric arranged by embodiment 1 arranges, every time in batches by 10 times The fluctuation range of the Static water contact angles of arrangement be 115 ± 5 °, fabric after flame time ﹤ 5s, smoldering time < 8s, by data it is found that Handle the reproducible of fabric effects.
The fire-retardant hydrophobic effect uniformity of product: the range of any 5 points of measurements Static water contact angles is 115 on fabric after arrangement ± 5 °, there is not water droplet penetration phenomenon in product;Any 5 pieces of cloth specimens of fabric test its flame retardant effect, after flame time drop after arrangement Low, smoldering time is 8 ± 1s, by data it is found that processing fabric effects uniformity is good.
Embodiment 2
Fabric: plain weave pure cotton fabric (40S × 40S/133*72)
1) silane coupler modified citric acid treatment:
Silane coupling agent hydrolysis (concentration containing amino silicane coupling agent is 180g/L, and hydrochloric acid is catalyst, and water is solvent) → Modified Citric Acid (citric acid concentration 180g/L) → fabric impregnates silane coupler modified citrate diluent (70g/L) 5- 10min → second dipping and rolling (pick-up 100%) → 90 DEG C of preliminary drying 3min → 160 DEG C bake 3min.
2) long-chain type siloxane water repellent arranges:
Cotton fabric dipping long-chain type siloxane water repellent (dodecyltrimethoxysilane 20g/L, hydrochloric acid are catalyst, Dehydrated alcohol is solvent) 5min → second dipping and rolling (pick-up 90%) → 80 DEG C of preliminary drying 3min → 130 DEG C bake 5min.
2) long-chain type siloxane water repellent arranges: 20g/L
Impregnate 5min long-chain type siloxane water repellent → second dipping and rolling (pick-up 80%) → 80 DEG C preliminary drying 3min → 120 DEG C Bake 5min.
After cotton fabric is collated, Static water contact angles are 120 degree;According to AATCC22-2005 testing standard, waterproof effect Reach 90 points or more.Cotton fabric is after silane coupler modified citric acid treatment, fabric after flame time ﹤ 3s, smoldering time drop Low < 4s, and there is good anti-wrinkle effect, less, textile finishing effect is preferable for ultimate strength loss.
Product is after 20 washings, and 115 ± 5 ° of fabric static contact angle, fabric after flame time ﹤ 5s, smoldering time < 8s is knitted The fire-retardant hydrophobic effect of object is still preferable, has good durability.
Fabric after present invention arrangement, water drop static contact angle increase, and fabric smoldering time reduces, and fabric has well Anti-wrinkle effect, breaking strength loss reduces (be lower than 20%), and the decline of fabrics flame resistance hydrophobic effect is unobvious after washing.
The fire-retardant hydrophobic effect repeatability of product: the cotton fabric arranged by embodiment 2 arranges, every time in batches by 10 times The range of the Static water contact angles of arrangement is 120 ± 5 °, fabric after flame time ﹤ 3s, smoldering time < 4s, by data it is found that processing Fabric effects are reproducible.
The fire-retardant hydrophobic effect uniformity of product: the range of any 5 points of measurements Static water contact angles is 120 on fabric after arrangement ± 5 °, there is not water droplet penetration phenomenon in product;Any 5 pieces of cloth specimens of fabric test its flame retardant effect, after flame time drop after arrangement It is low, smoldering time < 4s, by data it is found that processing fabric effects uniformity is good.
Embodiment 3
Fabric: plain weave pure cotton fabric (40S × 40S/133*72)
1) silane coupler modified citric acid treatment:
Silane coupling agent hydrolysis (concentration containing amino silicane coupling agent is 200g/L, and hydrochloric acid is catalyst, and water is solvent) → Modified Citric Acid (citric acid concentration 180g/L) → fabric impregnates silane coupler modified citrate diluent (90g/L) 5- 10min → second dipping and rolling (pick-up 90%) → 90 DEG C of preliminary drying 3min → 150 DEG C bake 3min.
2) long-chain type siloxane water repellent arranges:
Cotton fabric dipping long-chain type siloxane water repellent (hexadecyl trimethoxy silane 30g/L, hydrochloric acid are catalyst, Dehydrated alcohol is solvent) 5min → second dipping and rolling (pick-up 80%) → 90 DEG C of preliminary drying 3min → 130 DEG C bake 5min.
After cotton fabric is collated, Static water contact angles are 135 degree;According to AATCC22-2005 testing standard, waterproof effect Reach 90 points or more.Cotton fabric is after silane coupler modified citric acid treatment, and fabric after flame time is almost nil, when glowing Between < 1s, and there is good anti-wrinkle effect, less, textile finishing effect is preferable for ultimate strength loss.
Product is after 20 washings, and 130 ± 5 ° of fabric static contact angle, fabric after flame time ﹤ 1s, smoldering time < 3s is knitted The fire-retardant hydrophobic effect of object is still preferable, has good durability.
Fabric after present invention arrangement, water drop static contact angle increase, and fabric smoldering time reduces and is intended to zero, and knits Object has good anti-wrinkle effect, and breaking strength loss reduces and (is lower than 20%), and fabrics flame resistance hydrophobic effect declines not after washing Obviously.
The fire-retardant hydrophobic effect repeatability of product: the cotton fabric arranged by embodiment 3 arranges, every time in batches by 10 times The range of the Static water contact angles of arrangement is 135 ± 5 °, and fabric after flame time is almost nil, smoldering time < 1s, can by data Know, processing fabric effects are reproducible.
The fire-retardant hydrophobic effect uniformity of product: the range of any 5 points of measurements Static water contact angles is 135 on fabric after arrangement ± 5 °, there is not water droplet penetration phenomenon in product;Any 5 pieces of cloth specimens of fabric test its flame retardant effect, after flame time drop after arrangement It is low, smoldering time < 1s, by data it is found that processing fabric effects uniformity is good.
Embodiment 4
Fabric: plain weave pure cotton fabric (40S × 40S/133*72)
1) silane coupler modified citric acid treatment:
Silane coupling agent hydrolysis (concentration containing amino silicane coupling agent is 200g/L, and hydrochloric acid is catalyst, and water is solvent) → Modified Citric Acid (citric acid concentration 180g/L) → fabric impregnates silane coupler modified citrate diluent (90g/L) 5- 10min → second dipping and rolling (pick-up 90%) → 0 DEG C of preliminary drying 3min → 150 DEG C bake 3min.
2) long-chain type siloxane water repellent arranges:
Cotton fabric dipping long-chain type siloxane water repellent (hexadecyl trimethoxy silane 50g/L, hydrochloric acid are catalyst, Dehydrated alcohol is solvent) 5min → second dipping and rolling (pick-up 90%) → 70 DEG C of preliminary drying 3min → 130 DEG C bake 5min.
After cotton fabric is collated, Static water contact angles are 130 degree;According to AATCC22-2005 testing standard, waterproof effect Reach 90 points or more, but water repellent excessive concentration, fabric hydrophobic effect can be made to be declined instead.Cotton fabric is even by silane After joining the processing of agent Modified Citric Acid, fabric after flame time is almost nil, smoldering time drop < 1s, and has good crease-resistant effect Fruit, less, textile finishing effect is preferable for ultimate strength loss.
Product is after 20 washings, and 125 ± 5 ° of fabric static contact angle, fabric after flame time ﹤ 1s smoldering time < 3s is knitted The fire-retardant hydrophobic effect of object is still preferable, has good durability.
Fabric after present invention arrangement, water drop static contact angle increase, and fabric smoldering time reduces and is intended to zero, and knits Object has good anti-wrinkle effect, and breaking strength loss reduces and (is lower than 20%), and fabrics flame resistance hydrophobic effect declines not after washing Obviously.
The fire-retardant hydrophobic effect repeatability of product: the cotton fabric arranged by embodiment 4 arranges, every time in batches by 10 times The range of the Static water contact angles of arrangement is 130 ± 5 °, and fabric after flame time is almost nil, smoldering time < 1s, can by data Know, processing fabric effects are reproducible.
The fire-retardant hydrophobic effect uniformity of product: the range of any 5 points of measurements Static water contact angles is 130 on fabric after arrangement ± 5 °, there is not water droplet penetration phenomenon in product;Any 5 pieces of cloth specimens of fabric test its flame retardant effect after arrangement, when fabric afterflame Between almost nil, smoldering time < 1s, by data it is found that processing fabric effects uniformity it is good.
Although the present invention has been described by way of example and in terms of the preferred embodiments, it is not intended to limit the invention, any to be familiar with this skill The people of art can do various change and modification, therefore protection model of the invention without departing from the spirit and scope of the present invention Enclosing subject to the definition of the claims.

Claims (10)

1.一种棉织物的阻燃疏水整理方法,其特征在于,利用硅烷偶联剂改性柠檬酸及长链硅氧烷类拒水剂处理棉织物,得到具有阻燃疏水功能的棉织物。1. A method for flame-retardant and hydrophobic finishing of cotton fabrics, characterized in that, utilizing silane coupling agent to modify citric acid and long-chain siloxane water-repellent agents to process cotton fabrics to obtain cotton fabrics with flame-retardant and hydrophobic functions. 2.根据权利要求1所述的一种棉织物的阻燃疏水整理方法,其特征在于,包括以下步骤:2. the flame-retardant hydrophobic finishing method of a kind of cotton fabric according to claim 1, is characterized in that, comprises the following steps: 步骤(1)硅烷偶联剂改性柠檬酸整理:首先将氨基硅烷偶联剂水解,然后将柠檬酸滴加到氨基硅烷偶联剂水解液中获得硅烷偶联剂改性柠檬酸整理液,再将棉织物加入到硅烷偶联剂改性柠檬酸整理液中,采用轧烘焙工艺整理棉织物;Step (1) Silane coupling agent-modified citric acid finishing: firstly, the aminosilane coupling agent is hydrolyzed, and then citric acid is added dropwise to the aminosilane coupling agent hydrolyzate to obtain the silane coupling agent-modified citric acid finishing solution, Then the cotton fabric is added to the citric acid finishing solution modified by silane coupling agent, and the cotton fabric is finished by rolling and baking process; 步骤(2)长链硅氧烷类拒水剂整理:将经过硅烷偶联剂改性柠檬酸整理液处理后的织物浸渍到长链硅氧烷类拒水剂中,采用浸轧烘工艺。Step (2) Finishing with long-chain siloxane water-repellent agent: dipping the fabric treated with silane coupling agent-modified citric acid finishing solution into long-chain siloxane-type water-repellent agent, and adopting a pad-drying process. 3.根据权利要求2所述的一种棉织物的阻燃疏水整理方法,其特征在于,所述将氨基硅烷偶联剂水解是以水为溶剂,以盐酸为催化剂,盐酸浓度为0.05g/L~0.1g/L,所得氨基硅烷偶联剂水解液中氨基硅烷偶联剂的含量为150-250g/L。3. the flame-retardant hydrophobic finishing method of a kind of cotton fabric according to claim 2, it is characterized in that, described aminosilane coupling agent is hydrolyzed with water as solvent, with hydrochloric acid as catalyst, hydrochloric acid concentration is 0.05g/ L-0.1g/L, the aminosilane coupling agent content in the obtained aminosilane coupling agent hydrolyzate is 150-250g/L. 4.根据权利要求2或3所述的一种棉织物的阻燃疏水整理方法,其特征在于,所述柠檬酸用量为150-200g/L氨基硅烷偶联剂水解液。4. A method for flame-retardant and hydrophobic finishing of cotton fabrics according to claim 2 or 3, characterized in that the amount of said citric acid is 150-200 g/L aminosilane coupling agent hydrolyzate. 5.根据权利要求2或3所述的一种棉织物的阻燃疏水整理方法,其特征在于,将硅烷偶联剂改性柠檬酸整理液稀释得到稀释液后,用于整理棉织物,所述稀释液中硅烷偶联剂改性柠檬酸的浓度为50-100g/L。5. according to claim 2 or 3 described a kind of flame-retardant hydrophobic finishing method of cotton fabric, it is characterized in that, after diluting silane coupling agent modified citric acid finishing liquid to obtain diluent, be used for finishing cotton fabric, so The concentration of the silane coupling agent modified citric acid in the diluent is 50-100g/L. 6.根据权利要求1~5任一所述的一种棉织物的阻燃疏水整理方法,其特征在于,所述长链硅氧烷类拒水剂处理棉织物是以无水乙醇为溶剂,长链硅氧烷类拒水剂用量为15-35g/L,以盐酸为催化剂,盐酸浓度为0.01g/L~0.05g/L,将将经过硅烷偶联剂改性柠檬酸整理液处理后的织物浸入其中。6. A method for flame-retardant and hydrophobic finishing of cotton fabric according to any one of claims 1 to 5, wherein the long-chain siloxane water-repellent agent is used to treat cotton fabric with absolute ethanol as a solvent, The dosage of long-chain siloxane water-repellent agent is 15-35g/L, using hydrochloric acid as catalyst, the concentration of hydrochloric acid is 0.01g/L-0.05g/L, after the citric acid finishing solution modified by silane coupling agent is used The fabric is immersed in it. 7.根据权利要求1或6所述的一种棉织物的阻燃疏水整理方法,其特征在于,所述长链硅氧烷类拒水剂为含硅有机拒水化合物,包括:辛基三甲氧基硅烷、癸基三甲氧基硅烷、十二烷基三甲氧基硅烷、十四烷基三甲氧基硅烷或十六烷基三甲氧基硅烷中的一种或几种的混合物。7. A method for flame-retardant and hydrophobic finishing of cotton fabrics according to claim 1 or 6, wherein the long-chain siloxane water-repellent agent is a silicon-containing organic water-repellent compound, comprising: octyl trimethyl One or a mixture of oxysilane, decyltrimethoxysilane, dodecyltrimethoxysilane, tetradecyltrimethoxysilane or hexadecyltrimethoxysilane. 8.根据权利要求1~7任一所述的一种棉织物的阻燃疏水整理方法,其特征在于,所述硅烷偶联剂采用带氨基的硅氧烷化合物,包括:3-氨丙基三甲氧基硅烷、3-氨丙基三乙氧基硅烷、N-(β-氨乙基)-γ-氨丙基三甲氧基硅烷、N-(β-氨乙基)-γ-氨丙基甲基二乙氧基硅烷。8. A method for flame-retardant and hydrophobic finishing of cotton fabric according to any one of claims 1-7, characterized in that the silane coupling agent is a siloxane compound with amino groups, including: 3-aminopropyl Trimethoxysilane, 3-aminopropyltriethoxysilane, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, N-(β-aminoethyl)-γ-aminopropyl Methyldiethoxysilane. 9.应用权利要求1~8任一所述方法制备得到的棉织物。9. The cotton fabric prepared by applying the method according to any one of claims 1 to 8. 10.应用权利要求9所述的棉织物制备得到的特种防护服。10. the special protective clothing prepared by using the cotton fabric according to claim 9.
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