CN106049055A - Preparation method of sea-island superfine fiber synthetic leather base cloth with high moisture absorption and moisture permeability - Google Patents
Preparation method of sea-island superfine fiber synthetic leather base cloth with high moisture absorption and moisture permeability Download PDFInfo
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- CN106049055A CN106049055A CN201610393907.8A CN201610393907A CN106049055A CN 106049055 A CN106049055 A CN 106049055A CN 201610393907 A CN201610393907 A CN 201610393907A CN 106049055 A CN106049055 A CN 106049055A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/18—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation
- D06M14/26—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin
- D06M14/30—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M14/34—Polyamides
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
Abstract
The invention discloses a preparation method of sea-island superfine fiber synthetic leather base cloth with high moisture absorption and moisture permeability. Sulfhydrylization sea-island superfine fiber synthetic leather base cloth is firstly prepared, then, the surface of the sulfhydrylization sea-island superfine fiber synthetic leather base cloth is modified with a vinyl collagen solution, and the sea-island superfine fiber synthetic leather base cloth is obtained. The sulfhydrylization sea-island superfine fiber synthetic leather base cloth is subjected to dipping, adsorption, padding, crosslinking, water washing and other process treatment by the aid of vinyl modified collagen, vinyl collagen can be grafted and modified in the sulfhydrylization sea-island superfine fiber synthetic leather base cloth in a covalent bond form, the moisture absorption and the moisture permeability of the sea-island superfine fiber synthetic leather base cloth are improved, and the problem of poor moisture absorption and moisture permeability of the sea-island superfine fiber synthetic leather base cloth is successfully solved. The process is simple, causes no pollution to the environment and has better economic benefits and social benefits.
Description
Technical field
The invention belongs to technical field of polymer materials, be specifically related to a kind of highly hygroscopic poisture-penetrability sea-island composite fiber and close
Become the preparation method of leather base cloth.
Background technology
Fypro active group in Sea-island Composite Fiber Synthetic Leather base fabric (ISFSLB) is little, with collagen fiber
Compare, only have its about 10%, therefore hygroscopicity and the poisture-penetrability of superfine fiber chemical leather are poor.According to data: natural leather
Crust leather vapor pervious amount 700g/ (m224h) left and right, and the vapor pervious amount of ISFSLB is only 400g/ (m224h) left and right, it is excellent
The features such as good chemical-resistant, weatherability are the most popular to people, but its poor moisture absorption water vapour permeability makes it can not be by extensively
It is applied to clothing.
The raising of the domestic water vapour permeability to Sea-island Composite Fiber Synthetic Leather base fabric has carried out a series of research, has people
The methods such as research formic acid hydrolysis, sulphuric acid hydrolysis, triethanolamine hydrolysis, protease hydrolysis and pancreatin hydrolysis, make superfine fibre close
Fypro in finished leather exposes more polar group.But excessively hydrolysis can destroy the intensity of Fypro, for asking
Obtaining more surface polar groups, somebody's research formic acid is coordinated with the carboxylic group of aluminum tannin with exposure after slightly hydrolyzing,
Phenolic hydroxyl group is modified on Fypro, reaches to increase the purpose of fiber surface polar group number.It addition, there is people successively to grind
Study carefully and superfine fiber synthetic leather base cloth has been carried out appropriateness hydrolysis, using glutaraldehyde as cross-linking agent, by polyamide-amide with sulphuric acid
(PAMAM) macromolecules cross-linking increases the water vapour permeability of superfine fiber synthetic leather base cloth on Fypro.Follow-up also use
Superfine fiber synthetic leather base cloth is modified by G0.5PAMAM-COOH and G1PAMAM-COOH.Somebody's research sulphuric acid is located in advance
Reason, using organic phosphine tanning agent FP as cross-linking agent, improves superfine fiber chemical leather on Fypro by collagen cross-linking
The poisture-penetrability of base fabric.The base fabric water vapour permeability that above method obtains has promoted, but continues to carry to modified base fabric water vapor permeability
Rise and the exploration of mechanism of modification needs further to study.
The present invention is with the pure Fypro (Nylon) study model as ISFSLB, right with vinyl collagen protein (CMA)
Fypro (Nylon-SH) after the sulfhydrylation of surface carries out grafting and modifying research, and obtains CMA grafting and modifying Fypro
(Nylon-S-CMA).On this basis, the best practice of CMA graft-polyamide fiber is applied to the grafting and modifying of ISFSLB
In research, and obtain CMA grafting and modifying ISFSLB (ISFSLB-S-CMA) product, successfully prepare a kind of highly hygroscopic poisture-penetrability
The Sea-island Composite Fiber Synthetic Leather base fabric of energy, this technique is simple, environmentally safe, has preferable economic benefit and society
Benefit.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of highly hygroscopic poisture-penetrability Sea-island Composite Fiber Synthetic Leather base fabric,
The problem improving sea-island composite fiber moisture absorption water vapour permeability difference.
The technical solution adopted in the present invention is, the system of a kind of highly hygroscopic poisture-penetrability Sea-island Composite Fiber Synthetic Leather base fabric
Preparation Method, specifically implements according to following steps:
Step 1, prepares sulfhydrylation Sea-island Composite Fiber Synthetic Leather base fabric (USFSLB-SH), standby；
Step 2, prepares vinyl collagen solution (CMA), standby；
Step 3, is placed in step 2 gained vinyl glue by step 1 gained sulfhydrylation Sea-island Composite Fiber Synthetic Leather base fabric
In former protein solution, under ultraviolet irradiation condition, carry out Fypro in Sea-island Composite Fiber Synthetic Leather base fabric (USFSLB)
Surface grafting is modified, and to obtain final product.
Inventive feature also resides in,
In step 1, the detailed process of Sea-island Composite Fiber Synthetic Leather base fabric sulfhydrylation is:
Step 1.1: cut the Sea-island Composite Fiber Synthetic Leather sample cloth (about 12g ± 0.5g) of 170 × 130mm, with third
Ketone ultrasonic waves for cleaning 30min at normal temperatures, puts into immersion 1h in the NaOH solution that concentration is 10%, rushes with a large amount of water after taking-up
Wash, be subsequently placed at 50 DEG C of oven for drying；
Step 1.2: the superfine fibre after step 1.1 being processed is arranged in the mixed liquor of phosphoric acid solution and formalin,
After reacting 15h at 60 DEG C, take out and rinse with a large amount of water, dry to obtain hydroxylating Sea-island Composite Fiber Synthetic Leather base fabric for 50 DEG C
(USFSLB-OH)；
Step 1.3: hydroxylating Sea-island Composite Fiber Synthetic Leather base fabric is placed in isopropanol, then is added thereto to (3-
Mercaptopropyi) trimethyoxysilane (MPS), it is filled with nitrogen the most wherein, is placed at 70 DEG C reaction 12h, reaction knot
Take out after bundle, fully clean with isopropanol 3 times, dry in 60 DEG C of environment, obtain sulfhydrylation Sea-island Composite Fiber Synthetic Leather base
Cloth.
In step 1.2, the concentration of phosphoric acid solution is 85%, and the concentration of formalin is 37%；Phosphoric acid solution in mixed liquor
It is 1:100～2:100 with the amount ratio of formalin.
In step 1.3, hydroxylating Sea-island Composite Fiber Synthetic Leather base fabric is 12:100 (W/ with the amount ratio of isopropanol
V)；Hydroxylating Sea-island Composite Fiber Synthetic Leather base fabric is 12:0.7 with the amount ratio of (3-mercaptopropyi) trimethyoxysilane
(W/V)。
In step 2, the concrete preparation process of vinyl collagen protein is:
Weigh collagen protein to be placed in phosphate buffer solution, under the conditions of 70 DEG C ± 2 DEG C, stir 0.5～1h so that it is fully
Dissolve, obtain collagen solution；At a temperature of 40～60 DEG C, under water bath condition, methacrylic anhydride is added drop-wise to collagen protein molten
In liquid, stir 1～3h, to collagen protein dialysis treatment, obtain vinyl collagen solution (CMA).
The number-average molecular weight of collagen protein is 178580；The pH of phosphate buffer solution is 7.4, collagen protein and phosphoric acid buffer
The amount ratio of solution is 1:8～12 (w/v)；The mass concentration of methacrylic anhydride is 94%, methacrylic anhydride and collagen egg
The amount ratio of white solution is 0.1:5～2.4:5 (V/W)；Rate of addition is 1mL/min.
Dialysis treatment process is: is poured into by solution in the bag filter that trapped molecular weight is 3500D, uses deionized water conduct
Dialysis solution, at a temperature of 40 DEG C ± 2 DEG C, dialyse 24h.
In step 3, the detailed process that Fypro surface grafting is modified is:
Take light trigger and add in step 2 gained vinyl collagen solution, ultrasonic wave concussion 30min at 40 DEG C,
Mixed liquor, subsequently step 1 sulfhydrylation Sea-island Composite Fiber Synthetic Leather base fabric is put in mixed liquor supersonic vibration 0.5～
1h, rolls unnecessary collagen protein (CMA) with padding machine under the pressure of 0.3MPa, and the ultraviolet putting into a length of 365nm of ultraviolet light wave is handed over
Carrying out ultra-vioket radiation 4～6h in connection instrument, irradiation is 30～50kGy, dries, then 40 DEG C ± 2 at a temperature of 30 DEG C ± 5 DEG C
DEG C water in after ultrasonic cleaning 30min, take out, dry, to obtain final product.
Light trigger is ultraviolet initiator2959；In vinyl collagen solution, light trigger is dense
Degree is 0.005%～0.01%.
Sulfhydrylation Sea-island Composite Fiber Synthetic Leather base fabric is 1:4～5 with the mass ratio of vinyl collagen solution.
The invention has the beneficial effects as follows, utilize the collagen protein after vinyl modified that sulfhydrylation sea-island composite fiber is closed
Become leather base cloth to carry out impregnating, adsorb, pad, cross-link, after the PROCESS FOR TREATMENT such as washing, it is possible to by vinyl collagen protein and sulfhydrylation
Sea-island Composite Fiber Synthetic Leather base fabric be grafted, fiber surface formed space net structure, close covered fiber, preparation
The moisture absorption water vapour permeability of collagen protein composite modified Sea-island Composite Fiber Synthetic Leather base fabric strengthens, and improves synthetic leather base cloth
Sanitation performance, the problem successfully solving superfine fiber synthetic leather base cloth moisture absorption water vapour permeability difference, this technique is simple, to environment without
Pollute, there is preferable economic benefit and social benefit.
Accompanying drawing explanation
Fig. 1 is the preparation method sulfhydrylation sea of a kind of highly hygroscopic poisture-penetrability Sea-island Composite Fiber Synthetic Leather base fabric of the present invention
The formaldehyde consumption impact on USFSLB degree of hydroxylation in island superfine fiber synthetic leather base cloth preparation process (USFSLB-SH)；
Fig. 2 is the preparation method sulfhydrylation sea of a kind of highly hygroscopic poisture-penetrability Sea-island Composite Fiber Synthetic Leather base fabric of the present invention
The MPS consumption impact on USFSLB degree of hydroxylation in island superfine fiber synthetic leather base cloth preparation process (USFSLB-SH)；
Fig. 3 be a kind of highly hygroscopic poisture-penetrability Sea-island Composite Fiber Synthetic Leather base fabric of the present invention preparation method in difference take
The impact on modified USFSLB water vapour permeability of the vinyl collagen protein of Dai Du；
Fig. 4 is that the preparation method difference of a kind of highly hygroscopic poisture-penetrability Sea-island Composite Fiber Synthetic Leather base fabric of the present invention replaces
The impact on modified USFSLB moisture pick-up properties of the degree vinyl collagen protein；
Fig. 5 is the water vapour permeability contrast of USFSLB after distinct methods is modified；
Fig. 6 is the moisture pick-up properties contrast of USFSLB after distinct methods is modified；
Fig. 7 is the preparation method difference irradiation of a kind of highly hygroscopic poisture-penetrability Sea-island Composite Fiber Synthetic Leather base fabric of the present invention
The infrared spectrum on Fypro surface under time.
Detailed description of the invention
The present invention is described in detail with detailed description of the invention below in conjunction with the accompanying drawings.
The preparation method of a kind of highly hygroscopic poisture-penetrability Sea-island Composite Fiber Synthetic Leather base fabric of the present invention, specifically according to following
Step is implemented:
Step 1, cuts the superfine fibre sample (about 12g ± 0.5g) of 170 × 130mm, with acetone ultrasound wave at normal temperatures
Clean 30min, after taking-up, put into immersion 1h in 10%NaOH solution, rinse with a large amount of water after taking-up, be placed in 50 DEG C of oven for drying,
Be placed in 85% phosphoric acid solution and formalin with volume ratio as 1:100～in the mixed solution of 2:100, at 60 DEG C react
After 15h, take out and rinse with a large amount of water, dry to obtain hydroxylating Sea-island Composite Fiber Synthetic Leather base fabric (USFSLB-OH) for 50 DEG C, will
USFSLB-OH is placed in isopropanol, then is added thereto to (3-mercaptopropyi) trimethyoxysilane (MPS), USFSLB-OH with
The mass volume ratio 12:0.7 of MPS；Then in sample cup, it is filled with nitrogen, sample cup is placed at 70 DEG C reaction 12h, reaction knot
Take out after bundle, fully clean with isopropanol 3 times, dry in 60 DEG C of baking ovens and obtain sulfhydrylation Sea-island Composite Fiber Synthetic Leather base
Cloth (USFSLB-SH).
Step 2, weighs the collagen protein that molecular mass is 178580 and is placed in phosphate buffer solution (pH 7.4), at 70 DEG C
Under the conditions of ± 2 DEG C, stir 0.5～1h so that it is fully dissolve, obtain collagen solution；Water bath condition at a temperature of 40～60 DEG C
Lower being added drop-wise in collagen solution by methacrylic anhydride, methacrylic anhydride is 0.1 with the volume mass ratio of collagen protein:
5～2.4:5 (mL/g), stir 1～3h, to collagen protein dialysis treatment, obtain vinyl collagen solution (CMA).
Step 3, take light trigger (2959) the vinyl collagen solution after step 2 dialysis is added
In, at 40 DEG C after ultrasonic wave concussion 30min mix homogeneously, step 1 gained USFSLB-SH is put into wherein, Under Ultrasonic Vibration subsequently
Dynamic 0.5～1h, under the pressure of 0.3MPa, roll unnecessary collagen protein with padding machine, put into the ultraviolet of a length of 365nm of ultraviolet light wave
Crosslinking instrument carries out ultra-vioket radiation 4～6h, dries at a temperature of 30 DEG C ± 5 DEG C, then ultrasonic cleaning in the water of 40 DEG C ± 2 DEG C
After 30min, take out, dry.
In terms of principle, the present invention will be described below:
The route of vinyl collagen solution grafting sulfhydrylation superfine fiber synthetic leather base cloth (USFSLB-SH) is concrete such as
Under: react with USFSLB-OH and (3-mercaptopropyi) trimethyoxysilane (MPS) that to obtain the fabric of island-in-sea type of surface sulfhydrylation ultra-fine
Fiber synthetic leather base cloth (USFSLB-SH).Then USFSLB-SH is put into containing certain density light trigger (2959) in vinyl collagen protein (CMA) solution (solid content 6% ± 0.5%), when 40 DEG C, ultrasonic shake
After dynamic 30min, take out and put in UV-crosslinked instrument, carry out ultraviolet light and irradiate initiation crosslinking, complete " click " reaction.Crosslinking terminates
After sample be placed in the distilled water of 40 DEG C carry out ultrasonic cleaning 30min, dry alternative after taking-up.
Utilize sulfydryl-alkene " click chemistry " method, by the USFSLB with sulfydryl and the vinyl collagen with C=C key
Albumen can carry out Radical Addition under the conditions of ultraviolet light irradiation.Light trigger causes under the conditions of ultra-vioket radiation and obtains
Primary group of free radicals, primary group of free radicals captures the hydrogen on sulfydryl-SH thus obtains sulfydryl free radical, and it is double that sulfydryl free radical runs into C=C
Key carries out Radical Addition, so that collagen protein grafting and modifying is on Fypro surface.
The present invention also utilizes poisture-penetrability and hygroscopicity to test the moisture absorption poisture-penetrability utilizing the modified base fabric of the inventive method
Can, wherein:
(1) water vapour permeability of modified Sea-island Composite Fiber Synthetic Leather base fabric is expressed by static rate of perviousness, specifically surveys
Examination process is: take the sample of Φ 55mm, then carries out air regulation in sample is placed on climatic chamber, air conditioning method according to
QB/T 3812.12-1999 regulation is carried out, and the condition of regulation is: temperature 20 DEG C ± 2 DEG C, relative humidity 65% ± 2%, base fabric
When weight alternation amount is less than 0.25%, can think and reach balance.Air regulation takes 30mL distilled water in test cup after terminating
In, put sample and rubber washer successively, then aluminium lid is tightened, weigh moisture vapor transmission cup gross mass, and record data.Then thoroughly
Wet cup is put in the exsiccator having relative density to be 1.84g/mL concentrated sulphuric acid, again weighs after standing 24h.
In formula:
SWVT static state rate of perviousness, unit is the every 10 square centimeters of 24 hours [mg/10cm of milligram224h] or gram every
Square metre hour [g/m2·24h]
The difference of fit twice weighing of the same test group of Δ m, unit is (mg)；
The difference of fit twice weighing of the same test group of Δ m' blank sample, unit is (mg)；Do not do blank assay
Time, Δ m'=0.
A efficiency test area (10cm2), unit is square centimeter (cm2)；
T test period, unit is 24 hours (24h).
(2) modified Sea-island Composite Fiber Synthetic Leather base fabric moisture absorption performance measures: liquid core suction speed is to characterize to knit
Thing moisture absorption and lead the leading indicator of wet ability.Sampling: cutting length and be not less than 250mm, the long cloth of width about 30mm is as examination
Sample.Put it into 20 DEG C before test, after the climatic chamber hollow controlled atmosphere joint 24h of relative humidity 65%, carry out liquid core suction speed
Mensuration.
Measure: sample is hung up, in the beaker that bottom 15mm immerses containing mixing test solution, observe and metering liquid
Time, unit, s used by 30mm height is risen along sample from liquid level.I.e. being measured by liquid core suction speed, liquid passes through capillary
Pipe effect, the liquid core suction height that the unit interval reaches on textile material.
Embodiment 1
Step 1, cuts the super superfine fibre sample (about 12g ± 0.5g) of 170 × 130mm, the most ultrasonic with acetone
Ripple cleans 30min, puts into immersion 1h in 10%NaOH solution after taking-up, rinses with a large amount of water after taking-up, is placed in 50 DEG C of baking ovens and dries
Dry, it is placed in phosphoric acid solution and the formalin mixed solution with volume ratio as 1:100 of 85%, after reacting 15h at 60 DEG C,
Taking out and rinse with a large amount of water, 50 DEG C of drying obtain hydroxylating superfine fibre (USFSLB-OH), are put by the superfine fibre after hydroxylating
In the sample cup of 100mL isopropanol, add 0.7mLMPS, then in sample cup, be filled with nitrogen, sample cup is placed in 70 DEG C
Lower reaction 12h, reaction is taken out after terminating, is fully cleaned with isopropanol 3 times, dries and obtain sulfhydrylation fabric of island-in-sea type in 60 DEG C of baking ovens
Superfine fiber synthetic leather base cloth.
Step 2, weighs the collagen protein 5.0g that several equal molecular mass is 178580, is placed in 50mL phosphate buffer solution (pH
7.4), in, 0.5h is stirred so that it is fully dissolve, obtain collagen solution；By 0.1mL methyl under water bath condition at a temperature of 40 DEG C
Acrylic anhydride is added drop-wise in gained collagen solution with 1mL/min speed, stirs 2h, obtains vinyl collagen solution；Will
Vinyl collagen solution is placed in the bag filter of molecular size range 3500D, with deionized water as dialysis solution, 40 DEG C of temperature
Dialyse under degree 24h, vinyl collagen protein (CMA) that substitution value is 15%.
Step 3, is 0.005% by light trigger concentration in CMA solution, weigh light trigger (
2959) add in the vinyl collagen solution after step 2 dialysis, at 40 DEG C after ultrasonic wave concussion 30min mix homogeneously,
Putting into wherein by step 1 gained USFSLB-SH, supersonic vibration 0.5h subsequently, it is unnecessary to roll with padding machine under the pressure of 0.3MPa
Collagen protein, puts in the UV-crosslinked instrument of a length of 365nm of ultraviolet light wave and carries out ultra-vioket radiation 4h, dries at a temperature of 30 DEG C,
Then, in the water of 40 DEG C after ultrasonic cleaning 30min, take out, dry.
Embodiment 2
Step 1, cuts the super superfine fibre sample (about 12g ± 0.5g) of 170 × 130mm, the most ultrasonic with acetone
Ripple cleans 30min, puts into immersion 1h in 10%NaOH solution after taking-up, rinses with a large amount of water after taking-up, is placed in 50 DEG C of baking ovens and dries
Dry, it is placed in phosphoric acid solution and the formalin mixed solution with volume ratio as 2:100 of 85%, after reacting 15h at 60 DEG C,
Taking out and rinse with a large amount of water, 50 DEG C of drying obtain hydroxylating superfine fibre (USFSLB-OH), are put by the superfine fibre after hydroxylating
In the sample cup of 100mL isopropanol, add 0.7mLMPS, then in sample cup, be filled with nitrogen, sample cup is placed in 70 DEG C
Lower reaction 12h, reaction is taken out after terminating, is fully cleaned with isopropanol 3 times, dries and obtain sulfhydrylation fabric of island-in-sea type in 60 DEG C of baking ovens
Superfine fiber synthetic leather base cloth.
Step 2, weighs the collagen protein 5.0g that several equal molecular mass is 178580, is placed in 50mL phosphate buffer solution (pH
7.4), in, 0.5h is stirred so that it is fully dissolve, obtain collagen solution；By 0.3mL methyl under water bath condition at a temperature of 40 DEG C
Acrylic anhydride is added drop-wise in gained collagen solution with 1mL/min speed, stirs 3h, obtains modified collagen solution；
Modified collagen solution is placed in the bag filter of molecular size range 3500D, with deionized water as dialysis solution, 40
At a temperature of DEG C dialyse 24h, vinyl collagen protein (CMA) that substitution value is 50%.
Step 3, by light trigger concentration in CMA solution be 0.006% weigh light trigger (
2959) adding in the vinyl collagen solution after step 2 dialysis, ultrasonic wave concussion 30min at 40 DEG C, with step 1
USFSLB-SH uniformly mixes, subsequently supersonic vibration 0.5h, rolls unnecessary collagen protein with padding machine, put under the pressure of 0.3MPa
Enter in the UV-crosslinked instrument of a length of 365nm of ultraviolet light wave and carry out ultra-vioket radiation 6h, dry at a temperature of 30 DEG C, then at 40 DEG C
In water after ultrasonic cleaning 30min, take out, dry.
Embodiment 3
Step 1, cuts the super superfine fibre sample (about 12g ± 0.5g) of 170 × 130mm, the most ultrasonic with acetone
Ripple cleans 30min, puts into immersion 1h in 10%NaOH solution after taking-up, rinses with a large amount of water after taking-up, is placed in 50 DEG C of baking ovens and dries
Dry, it is placed in phosphoric acid solution and the formalin mixed solution with volume ratio as 1.5:100 of 85%, at 60 DEG C, reacts 15h
After, to take out and rinse with a large amount of water, 50 DEG C of drying obtain hydroxylating superfine fibre (USFSLB-OH), by the ultra-fine fibre after hydroxylating
Dimension is placed in the sample cup of 100mL isopropanol, adds 0.7mLMPS, is then filled with nitrogen in sample cup, is placed in by sample cup
Reacting 12h at 70 DEG C, reaction is taken out after terminating, and fully cleans with isopropanol 3 times, dries and obtain sulfhydrylation sea in 60 DEG C of baking ovens
Island superfine fiber synthetic leather base cloth.
Step 2, weighs the collagen protein 5.0g that several equal molecular mass is 178580, is placed in 50mL phosphate buffer solution (pH
7.4), in, 0.5h is stirred so that it is fully dissolve, obtain collagen solution；By 1.2mL methyl under water bath condition at a temperature of 40 DEG C
Acrylic anhydride is added drop-wise in gained collagen solution with 1mL/min speed, stirs 1h, obtains modified collagen solution；
Modified collagen solution is placed in the bag filter of molecular size range 3500D, with deionized water as dialysis solution, 40
At a temperature of DEG C dialyse 24h, vinyl collagen protein (CMA) that substitution value is 73%.
Step 3, by light trigger concentration in CMA solution be 0.01% weigh light trigger (2959)
Add in the vinyl collagen solution after step 2 dialysis, at 40 DEG C after ultrasonic wave concussion 30min, by step 1 gained
USFSLB-SH puts into wherein, subsequently supersonic vibration 0.5h, rolls unnecessary collagen protein with padding machine, put under the pressure of 0.3MPa
Enter in the UV-crosslinked instrument of a length of 365nm of ultraviolet light wave and carry out ultra-vioket radiation 4h, dry at a temperature of 30 DEG C, then at 40 DEG C
In water after ultrasonic cleaning 30min, take out, dry.
Embodiment 4
Step 1, cuts the super superfine fibre sample (about 12g ± 0.5g) of 170 × 130mm, the most ultrasonic with acetone
Ripple cleans 30min, puts into immersion 1h in 10%NaOH solution after taking-up, rinses with a large amount of water after taking-up, is placed in 50 DEG C of baking ovens and dries
Dry, it is placed in phosphoric acid solution and the formalin mixed solution with volume ratio as 1:100 of 85%, after reacting 15h at 60 DEG C,
Taking out and rinse with a large amount of water, 50 DEG C of drying obtain hydroxylating superfine fibre (USFSLB-OH), are put by the superfine fibre after hydroxylating
In the sample cup of 100mL isopropanol, add 0.7mLMPS, then in sample cup, be filled with nitrogen, sample cup is placed in 70 DEG C
Lower reaction 12h, reaction is taken out after terminating, is fully cleaned with isopropanol 3 times, dries and obtain sulfhydrylation fabric of island-in-sea type in 60 DEG C of baking ovens
Superfine fiber synthetic leather base cloth.
Step 2, weighs the collagen protein 5.0g that several equal molecular mass is 178580, is placed in 50mL phosphate buffer solution (pH
7.4), in, 0.5h is stirred so that it is fully dissolve, obtain collagen solution；By 1.8mL methyl under water bath condition at a temperature of 40 DEG C
Acrylic anhydride is added drop-wise in gained collagen solution with 1mL/min speed, stirs 2h, obtains modified collagen solution；
Modified collagen solution is placed in the bag filter of molecular size range 3500D, with deionized water as dialysis solution, 40
At a temperature of DEG C dialyse 24h, vinyl collagen protein (CMA) that substitution value is 83%.
Step 3, taking light trigger concentration in CMA solution is 0.006%.Weigh light trigger (
2959) add in the vinyl collagen solution after step 2 dialysis, at 40 DEG C after ultrasonic wave concussion 30min, by step 1
Gained USFSLB-SH puts into wherein, subsequently supersonic vibration 0.5h, rolls unnecessary collagen egg with padding machine under the pressure of 0.3MPa
In vain, put in the UV-crosslinked instrument of a length of 365nm of ultraviolet light wave and carry out ultra-vioket radiation 5h, dry at a temperature of 30 DEG C, then exist
In the water of 40 DEG C after ultrasonic cleaning 30min, take out, dry.
Embodiment 5
Step 1, cuts the super superfine fibre sample (about 12g ± 0.5g) of 170 × 130mm, the most ultrasonic with acetone
Ripple cleans 30min, puts into immersion 1h in 10%NaOH solution after taking-up, rinses with a large amount of water after taking-up, is placed in 50 DEG C of baking ovens and dries
Dry, it is placed in phosphoric acid solution and the formalin mixed solution with volume ratio as 1:100 of 85%, after reacting 15h at 60 DEG C,
Taking out and rinse with a large amount of water, 50 DEG C of drying obtain hydroxylating superfine fibre (USFSLB-OH), are put by the superfine fibre after hydroxylating
In the sample cup of 100mL isopropanol, add 0.7mLMPS, then in sample cup, be filled with nitrogen, sample cup is placed in 70 DEG C
Lower reaction 12h, reaction is taken out after terminating, is fully cleaned with isopropanol 3 times, dries and obtain sulfhydrylation fabric of island-in-sea type in 60 DEG C of baking ovens
Superfine fiber synthetic leather base cloth.
Step 2, weighs the collagen protein 5.0g that several equal molecular mass is 178580, is placed in 50mL phosphate buffer solution (pH
7.4), in, 0.5h is stirred so that it is fully dissolve, obtain collagen solution；By 1.5mL methyl under water bath condition at a temperature of 40 DEG C
Acrylic anhydride is added drop-wise in gained collagen solution with 1mL/min speed, stirs 2h, obtains modified collagen solution；
Modified collagen solution is placed in the bag filter of molecular size range 3500D, with deionized water as dialysis solution, 40
At a temperature of DEG C dialyse 24h, vinyl collagen protein (CMA) that substitution value is 79%.
Step 3, by light trigger concentration in CMA solution be 0.01% weigh light trigger (2959)
Add in the vinyl collagen solution after step 2 dialysis, at 40 DEG C after ultrasonic wave concussion 30min mix homogeneously, will step
Rapid 1 gained USFSLB-SH puts into wherein, and supersonic vibration 0.5h subsequently rolls unnecessary collagen with padding machine under the pressure of 0.3MPa
Albumen, puts in the UV-crosslinked instrument of a length of 365nm of ultraviolet light wave and carries out ultra-vioket radiation 4h, dries, then at a temperature of 30 DEG C
In the water of 40 DEG C after ultrasonic cleaning 30min, take out, dry.
As it is shown in figure 1, along with in the increase USFSLB of formaldehyde consumption, hydroxyl quantity is in increase, when formaldehyde consumption is 100mL
Time, the hydroxyl quantity in USFSLB is close to maximum.When being further continued for increasing formaldehyde consumption, the hydroxyl quantity in USFSLB is the most no longer
Increase, tend to constant.I.e. formaldehyde consumption is 100mL, and measured absorbance is 0.5909, calculates and modifies on 12gUSFSLB
There are about the hydroxyl of 0.1335mmol.Fig. 2 is the impact on USFSLB sulfhydrylation degree of the consumption of MPS.As shown in Figure 2, along with
The increase of MPS consumption, in USFSLB, sulfydryl quantity is increasing, when MPS consumption is between 0.5～0.7mL, the mercapto in USFSLB
Base content is most.MPS consumption about 0.5～0.7mL, the absorbance of its correspondence is 0.704～0.707, calculates 12gUSFSLB
On modify the sulfydryl that there are about 0.902～0.9145mmol.Because 12gUSFSLB-OH surface hydroxyl number is about 0.1335mmol,
Speculating that on USFSLB, the reaction mol ratio (SH/OH) of sulfydryl and hydroxyl is 8:1～9:1, i.e. 1 hydroxyl connects 8～9 mercaptos
Base.
Fig. 3 is the impact on the static rate of perviousness (SWVT) of USFSLB-S-CMA of the substitution value of CMA.It can be seen that
The static rate of perviousness of USFSLB-S-CMA reduces afterwards along with the increase of substitution value first increases.The USFSLB-when substitution value is 50%
The static water vapour permeability of S-CMA preferably (2221.5g/m224h), with the USFSLB (1554.7g/m of unmodified224h) compare
Relatively SWVT value improves 43%.This is because, along with the increase of vinyl collagen protein substitution value, the C=C quantity on strand
The most, under the conditions of ultraviolet irradiation, the sulfydryl (-SH) on USFSLB-SH surface and the reaction of unsaturated C=C key addition polymerization
Efficiency is the highest, and the collagen protein amount of USFSLB-SH surface grafting crosslinking is the most, and the substantial amounts of hydrophilic group on collagen protein makes
The water vapour permeability of USFSLB gets a promotion.But, when the substitution value of CMA is increasing, and the water vapour permeability of USFSLB-S-CMA is anti-
And reduce.This is possibly due to, on the one hand, the detection of static water vapour permeability is to measure USFSLB-S-under uniform temperature humidity
The weight that CMA steam in 24h passes through and discharges.And the absorption energy that the CMA film being attached to around Fypro is to water
Power is very strong, and comparatively speaking, it is the strongest that vapour molecule is possessed ability by it.So after steam is quickly absorbed,
Not the fastest discharging in a large number, therefore the weight of poisture-penetrability detection assembly does not significantly reduce, thus causes
The value change of SWVT is inconspicuous.On the other hand, the poisture-penetrability of fabric is that a small amount of gaseous state moisture of evaporation is because of the water steaming inside and outside fabric
Draught head and to external diffusion and migrate to outer space by interfibrous space.So poisture-penetrability may depend primarily on material
Microcellular structure, next to that the quantity of polar group.Therefore the biggest when the substitution value of CMA, on collagen molecules chain C=C
Key gets more and more, and the sulfydryl on USFSLB-SH surface improves further with C=C key reaction efficiency, vinyl collagen protein simultaneously
Between the contact probability of C=C key also increase, be also cross-linked with each other between collagen protein reaction, generates continuous print network structure, causes
The amount of the collagen protein being grafted on fiber surface increases, and occupies original fibre gap, causes the moisture-inhibiting of USFSLB-S-CMA
Hydraulic performance decline.
Fig. 4 is the impact on the liquid core suction speed (LWR) of USFSLB-S-CMA of the CMA substitution value.Shown in figure, along with
The increase of CMA substitution value, the LWR of USFSLB-S-CMA is increasing sharply, when substitution value is 73%, the liquid of USFSLB-S-CMA
Body wicking rate is up to 0.597mm/s.Increase compared with the liquid core suction speed (0.085mm/s) of the USFSLB of unmodified
602.4%.When substitution value is 50%, the maximum (2221.5g/m of the static poisture-penetrability of USFSLB-S-CMA224h), but liquid
Body wicking rate is not maximum (0.364mm/s).Find that the big poisture-penetrability on the contrary of substitution value is poor, but hygroscopicity is fine.Experiment is
Verified, the amount of the collagen protein that CMA that substitution value is big is grafted in the fibre is the most, and substitution value is that the CMA of 73% is at fiber
The amount of the collagen protein of upper grafting is more than the CMA that substitution value is 50%.This explanation USFSLB-S-CMA hygroscopicity promote with
How many collagen protein amounts has relation, i.e. the collagen protein amount of fiber surface grafting is the most, and the hygroscopicity of USFSLB-S-CMA is more
Good.This is possibly due to, and the hygroscopicity of fabric is that the most of gaseous state moisture of evaporation fiber surface in fabric condenses into liquid
A large amount of sweat that state water and human body are discharged suck fabric with aqueous water, then are diffused into fabric face evaporation discharge.Simultaneously
Polar group on collagen protein has affinity to hydrone, and when there being aqueous water, collagen protein amount is the most, accordingly parent
Aqueous group is the most, and its water absorbing properties is the strongest, thus the moisture pick-up properties showed is the best.Therefore conclude that the moisture absorption of USFSLB
Property depends primarily on the quantity of the polar group inside it.
Fig. 5 and 6 is poisture-penetrability (SWVT) and the hygroscopicity (LWR) of the USFSLB under different modifying method respectively.For not
Same method of modifying, USFSLB surface hydroxylation (USFSLB-OH), surface sulfhydrylation (USFSLB-SH), CMA coat modification
USFSLB (USFSLB/CMA) and CMA grafting and modifying USFSLB (USFSLB-S-CMA) compares poisture-penetrability and the hygroscopicity of its maximum
Contrast is as illustrated in Figures 5 and 6.Compared with the USFSLB of unmodified, the SWVT of USFSLB-OH improves 28.7%, and LWR improves
208.2%；The SWVT of USFSLB-SH improves 14.4%, and LWR but reduces 67%；The SWVT of USFSLB/CMA improves
32.6%, LWR improve about 477.7%；The SWVT of USFSLB-S-CMA improves 43%, and LWR improves 602.4%.SWVT
Mainly reflect the water vapour permeability of material, and LWR reflects the moisture pick-up properties of material.USFSLB is modified at vinyl collagen protein
During find, the moisture absorption water vapour permeability of USFSLB/CMA and USFSLB-S-CMA all has a distinct increment, and USFSLB-S-
The moisture absorption poisture-penetrability of CMA is better than USFSLB/CMA.
Fig. 7 is the sulfhydrylation Fypro infrared spectrum without collagen protein grafting and modifying, and in figure, b, c, d are purple respectively
The infrared spectrum of the collagen protein grafting and modifying sulfhydrylation polyamide of gained under outer photoirradiation time 3h, 4h, 5h.In Fig. 7-a,
3296cm-1The peak at place is the stretching vibration peak of N-H in polyamide molecule, along with the increase of exposure time, when exposure time reaches 4h
Time (such as Fig. 7-c), peak shape herein broadens, this is because a part of CMA and sulfydryl react and be grafted to Fypro
Surface, in CMA, the existence of substantial amounts of N-H there occurs hydrogen bond association so that peak shape broadens.When exposure time reaches 5h
(such as Fig. 7-d), respectively at 3232cm-1And 3340cm-1Place occurs in that two big Bao Feng, and this is from secondary acyl in collagen protein
The stretching vibration peak of N-H (containing hydrogen bond) on amine and primary amide, further, since the depositing of relatively large number of primary amine in collagen protein
, it is at lower wave number district 900cm-1～650cm-1Between have peak, this is N-H out-of-plane deformation vibration peak, but due to by hydrogen bond
Impact, peak shape is dispersed.Thus proving, vinyl collagen protein C=C and sulfydryl react and are successfully grafted to polyamide
On fiber surface.
Claims (10)
1. the preparation method of a highly hygroscopic poisture-penetrability Sea-island Composite Fiber Synthetic Leather base fabric, it is characterised in that specifically according to
Following steps are implemented:
Step 1, prepares sulfhydrylation Sea-island Composite Fiber Synthetic Leather base fabric, standby；
Step 2, prepares vinyl collagen solution, standby；
Step 3, is placed in step 2 gained vinyl collagen egg by step 1 gained sulfhydrylation Sea-island Composite Fiber Synthetic Leather base fabric
In white solution, under ultraviolet irradiation condition, carry out Fypro surface grafting in Sea-island Composite Fiber Synthetic Leather base fabric repair
Decorations, to obtain final product.
The preparation method of a kind of highly hygroscopic poisture-penetrability Sea-island Composite Fiber Synthetic Leather base fabric the most according to claim 1,
It is characterized in that, in step 1, the detailed process of Sea-island Composite Fiber Synthetic Leather base fabric sulfhydrylation is:
Step 1.1: cut the Sea-island Composite Fiber Synthetic Leather sample cloth of 170 × 130mm, clear with acetone ultrasound wave at normal temperatures
Wash 30min, put into immersion 1h in the NaOH solution that concentration is 10% after taking-up, rinse with a large amount of water, be subsequently placed at 50 DEG C of baking ovens
Dry；
Step 1.2: the superfine fibre after step 1.1 being processed is arranged in the mixed liquor of phosphoric acid solution and formalin, 60
After reacting 15h at DEG C, take out and rinse with a large amount of water, dry to obtain hydroxylating Sea-island Composite Fiber Synthetic Leather base fabric for 50 DEG C；
Step 1.3: hydroxylating Sea-island Composite Fiber Synthetic Leather base fabric is placed in isopropanol, then is added thereto to (3-sulfydryl
Propyl group) trimethyoxysilane, it is filled with nitrogen the most wherein, is placed at 70 DEG C reaction 12h, reaction is taken out after terminating,
Fully clean with isopropanol 3 times, dry in 60 DEG C of environment, obtain sulfhydrylation Sea-island Composite Fiber Synthetic Leather base fabric.
The preparation method of a kind of highly hygroscopic poisture-penetrability Sea-island Composite Fiber Synthetic Leather base fabric the most according to claim 2,
It is characterized in that, in step 1.2, the concentration of phosphoric acid solution is 85%, and the concentration of formalin is 37%；In mixed liquor, phosphoric acid is molten
Liquid is 1:100～2:100 with the amount ratio of formalin.
The preparation method of a kind of highly hygroscopic poisture-penetrability Sea-island Composite Fiber Synthetic Leather base fabric the most according to claim 2,
It is characterized in that, in step 1.3, hydroxylating Sea-island Composite Fiber Synthetic Leather base fabric is 12:100 with the amount ratio of isopropanol；
Hydroxylating Sea-island Composite Fiber Synthetic Leather base fabric is 12:0.7 with the amount ratio of (3-mercaptopropyi) trimethyoxysilane.
The preparation method of a kind of highly hygroscopic poisture-penetrability Sea-island Composite Fiber Synthetic Leather base fabric the most according to claim 1,
It is characterized in that, in step 2, the concrete preparation process of vinyl collagen protein is:
Weigh collagen protein to be placed in phosphate buffer solution, under the conditions of 70 DEG C ± 2 DEG C, stir 0.5～1h so that it is the most molten
Solve, obtain collagen solution；At a temperature of 40～60 DEG C, under water bath condition, methacrylic anhydride is added drop-wise to collagen solution
In, stir 1～3h, to collagen protein dialysis treatment, obtain vinyl collagen solution.
The preparation method of a kind of highly hygroscopic poisture-penetrability Sea-island Composite Fiber Synthetic Leather base fabric the most according to claim 5,
It is characterized in that, the number-average molecular weight of described collagen protein is 178580；The pH of phosphate buffer solution is 7.4, collagen protein with
The amount ratio of phosphate buffer solution is 1:8～12；The mass concentration of methacrylic anhydride is 94%, methacrylic anhydride and collagen
The amount ratio of protein solution is 0.1:5～2.4:5；Rate of addition is 1mL/min.
The preparation method of a kind of highly hygroscopic poisture-penetrability Sea-island Composite Fiber Synthetic Leather base fabric the most according to claim 5,
It is characterized in that, dialysis treatment process is: is poured into by solution in the bag filter that trapped molecular weight is 3500D, uses deionized water
As dialysis solution, at a temperature of 40 DEG C ± 2 DEG C, dialyse 24h.
The preparation method of a kind of highly hygroscopic poisture-penetrability Sea-island Composite Fiber Synthetic Leather base fabric the most according to claim 1,
It is characterized in that, in step 3, the detailed process that Fypro surface grafting is modified is:
Take light trigger and add in step 2 gained vinyl collagen solution, ultrasonic wave concussion 30min at 40 DEG C, obtain mixed
Close liquid, subsequently step 1 sulfhydrylation Sea-island Composite Fiber Synthetic Leather base fabric is put into supersonic vibration 0.5～1h in mixed liquor,
Roll unnecessary collagen protein with padding machine under the pressure of 0.3MPa, put in the UV-crosslinked instrument of a length of 365nm of ultraviolet light wave and carry out
Ultra-vioket radiation 4～6h, dries at a temperature of 30 DEG C ± 5 DEG C, then in the water of 40 DEG C ± 2 DEG C after ultrasonic cleaning 30min, takes
Go out, dry, to obtain final product.
The preparation method of a kind of highly hygroscopic poisture-penetrability Sea-island Composite Fiber Synthetic Leather base fabric the most according to claim 8,
It is characterized in that, described light trigger is ultraviolet initiator2959；In vinyl collagen solution, light draws
The concentration sending out agent is 0.005%～0.01%.
The preparation method of a kind of highly hygroscopic poisture-penetrability Sea-island Composite Fiber Synthetic Leather base fabric the most according to claim 8,
It is characterized in that, described sulfhydrylation Sea-island Composite Fiber Synthetic Leather base fabric is 1 with the mass ratio of vinyl collagen solution:
4～5.
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