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.