CN109825250A - A kind of preparation method of waterproof humidity-permeant film - Google Patents
A kind of preparation method of waterproof humidity-permeant film Download PDFInfo
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- CN109825250A CN109825250A CN201910029274.6A CN201910029274A CN109825250A CN 109825250 A CN109825250 A CN 109825250A CN 201910029274 A CN201910029274 A CN 201910029274A CN 109825250 A CN109825250 A CN 109825250A
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Abstract
The invention discloses a kind of preparation methods of waterproof humidity-permeant film, belong to high polymer waterproof material technical field.Waterproof humidity-permeant film prepared by the present invention includes gluey fiber liquid, moisture absorption toughener, hot melt adhesive and polytetrafluoroethylmicroporous microporous membrane, wherein mulberry tree hide fiber internal layer is dispersed with deeper striped along longitudinal direction in gluey fiber liquid, and there is cavity structure, with more micropore, coagulating bath by absorbing moisture absorption in dipping promotes the moisture pick-up properties of gluey fiber liquid, moisture absorption toughener is prepared by introducing tetrahydrofuran segment in glycidyl azide polymer, it and gluey fiber liquid synergistic effect improve moisture permeable membrane toughness at normal temperature and moisture pick-up properties, improve the water vapour permeability and toughness of entire waterproof humidity-permeant film, waterproof humidity-permeant film prepared by the present invention is by the polytetrafluoroethylmicroporous microporous membrane of low-surface-energy to extraneous waterproof, internal layer is the moisture that hygroscopicity toughness material is can absorb inside lagging skin, with broad prospect of application.
Description
Technical field
The invention discloses a kind of preparation methods of waterproof humidity-permeant film, belong to high polymer waterproof material technical field.
Background technique
Waterproof humidity-permeant film is a kind of novel high polymer waterproof material.It with polyurethanes (TPU) be main material,
Import hydrophilic group.Film surface pore-free, therefore can windproof water repellent.Because film has hydrophilic group, conducted by moisture absorption, to have
There is the function of moisture-inhibiting.The purposes of waterproof humidity-permeant film: racing car clothes, locomotive dress, golf dress, waterproof garment, climbing boot, shower curtain, tablecloth,
Raincoat, infant bib, navigation clothes, fishing trousers, the regged, wind coat of snow, cold-proof jacket, anorak, ski glove, anorak, hunting clothes,
Surfing clothes, horsecloth, water-proof jacket, fighting uniform, lamp decoration fittings, mobile phone waterproof fitting etc..
The working principle of waterproof humidity-permeant film: film conducts moisture-inhibiting by moisture absorption.The production status of waterproof humidity-permeant film: waterproof is saturating
The technology of wet film is introduced since American-European countries earliest.About 2003 or so, domestic Ye You producer started to produce, but also
There is a certain distance.
Waterproof Breathable is the basic function of outdoor wear, and clothes Waterproof Breathable in fabric surface mainly by being bonded at present
The mode of one layer of waterproof humidity-permeant film is realized.Divide from the material used, common waterproof humidity-permeant film mainly has PTFE film, E-
PTFE film, PU film and TPU membrane etc., but all there are the following problems for these waterproof humidity-permeant films: production process needs to consume a large amount of
Non-renewable fossil resources；It can not natural degradation or natural degradation is slow in the environment；Due to material and fabric itself
Material is different, needs to be unfavorable for by sorting, removing, cleaning etc. the recycling and utilization of waste and old clothing in removal process.
Although its thickness is thicker in the prior art, there is also some environment-friendly degradable films, do not have water-proof function,
The requirement of outdoor textile material is also not achieved in strength and elasticity etc.；It is former that some only use aqueous polymer to replace
Carry out common oiliness high molecular polymer, although there is certain progress in terms of environmental protection, film itself is in biodegrade side
Face or inadequate, and its material and fabric material itself are different in removal process or is needed by sorting, removing, clear
It the complicated cumbersome technique such as washes, while can also reduce the viscosity and crystallinity of regenerated polymer, seriously affect regenerated polymer
Quality and quality.
People inevitably meet with the bad weathers such as heavy rain, severe cold in environment outdoors, and traditional dress is easily soaked and deposited by sleet
It is difficult to the defect being discharged in time in sweat, can generate and glue the senses of discomfort such as wet, cold or even frostbite etc. is caused to injure, therefore wear simultaneous
The clothes of tool waterproof and moisture-inhibiting perspiration functions, which have become, resists one of boisterous important channel.Waterproof Breathable microporous barrier is made
For the core material of waterproof and moisture-permeable function clothes, it is desirable that it is with lesser aperture, to guarantee preferable waterproofness and higher
Voidage, to guarantee higher moisture-inhibiting.The structures such as electrostatic spinning fiber film is small with its fibre diameter, aperture is small, porosity is high are excellent
Gesture has huge application potential in high performance water proof moisture-inhibiting microporous barrier manufacture field.Presently disclosed electrostatic spinning fiber base is anti-
The technology of water moisture-inhibiting microporous barrier has very much, is all that polymer solution is carried out to electrostatic spinning, preparation tunica fibrosa in aperture and
Porosity is still lower and is difficult to control, and leads to waterproofing and moisture-penetration performances lower (water pressure resistance < 40kPa, moisture-inhibiting flux <
9000g/m2/ d), to limit the application performance of electrostatic spinning fiber base waterproof humidity-permeant film.
Therefore, a kind of hygroscopicity good permeability is invented, the waterproof humidity-permeant film of good toughness leads high polymer waterproof material technology
Domain has positive effect.
Summary of the invention
Present invention mainly solves the technical issues of, for waterproof humidity-permeant film hygroscopicity poor air permeability, moisture permeable membrane support used
Carrier is mostly fluorine-containing waterproof resin, and toughness is poor, when being applied to the clothings such as cold-proof jacket, anorak, anorak, water-proof jacket, is worn
It is uncomfortable, be also unfavorable for fold defect, provide a kind of preparation method of waterproof humidity-permeant film.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of waterproof humidity-permeant film, it is characterised in that specific preparation step are as follows: by gluey fiber liquid, moisture absorption toughener
It is mixed with hot melt adhesive, after being heated to 120~150 DEG C of hot melts, is placed in vacuum air pump, is heated to 70~80 DEG C,
Controlling vacuum degree in vacuum air pump is 100~200Pa, after 3~4h of standing and defoaming, with glue point transfer compounding machine be sprayed onto two pieces it is double
To between stretch polytetrafluoroethylraw microporous membrane, is pressed, waterproof humidity-permeant film is prepared；
The specific preparation step of the gluey fiber liquid are as follows:
(1) it taking 200~230g paper mulberry bark to be put into 400~450mL sulfuric acid solution to impregnate, control soaking temperature is 50~55 DEG C,
The immersion treatment time be 1~2h, be subsequently placed in water-bath, be heated to 90~100 DEG C, into water-bath be added 100~
120mL sodium hydroxide solution, 50~60mL polyphosphoric acids sodium solution, 30~40mL sodium silicate solution, after 2~3h of boiling, filtering,
Removal filtrate obtains soda boiling mulberry skin；
(2) after the 8~10min of salt acid soak for being 10% with 150~180mL mass fraction by above-mentioned soda boiling mulberry skin, after taking out acidleach
Mulberry skin beat 30~35min with wooden mallet, and be put into baking oven after being rinsed with water 3~5 times, be heated to 100~110 DEG C,
Dry 10~12h, obtains degumming mulberry fibre；
(3) take hydroxypropyltrimethylammonium chloride chitosan with lithium bromide is that 3 ︰ 1 are mixed in mass ratio, is then dissolved in water to obtain matter
The moisture absorption coagulating bath that score is 35% is measured, the N-methylmorpholine aqueous solution that mass fraction is 30% is pressed into quality with degumming mulberry fibre
Than being mixed for 10 ︰ 1, the mixed liquor of 230~250mL is obtained, is subsequently transferred in Rotary Evaporators, and is added into Rotary Evaporators
Add 8~12mL antioxidant, is heated to 90~95 DEG C, with revolving speed 30~40min of rotary evaporation of 110~130r/min,
Obtain gluey fiber liquid；
The specific preparation step of the moisture absorption toughener are as follows:
(1) after leading to nitrogen discharge air to three-necked flask, 20~30mL 1,4-butanediol, 40~50mL boron trifluoride second is added
Ether and 30~35mL tetrahydrofuran, are stirred, and starting mixed liquor are obtained, with constant pressure funnel with the dropwise addition of 5~7mL/min
30~40mL epoxychloropropane is added dropwise into three-necked flask for rate, keeps 4~5h of ice-water bath conditioned response, then to three-necked flask
4~5mL distilled water is added, stands 5~10min, obtains reaction product；
(2) above-mentioned reaction product is poured into separatory funnel, is successively washed with the sodium carbonate liquor that distilled water and mass fraction are 30%
It washs 2~3 times, washing is placed in distilling flask, is heated to 90~100 DEG C, is distilled 3~4h, is obtained copolyether, by weight
Number meter takes copolyether, dimethyl sulfoxide, sodium azide, sodium sulfonate to be put into reaction kettle, and oil bath heating is warming up to 100~120
DEG C, 18~20h of back flow reaction is kept the temperature, moisture absorption toughener is obtained.
The hot melt adhesive is polyurethane hot melt or polyamide hot.
Gluey fiber liquid, moisture absorption toughener and the hot melt adhesive mixing mass ratio is 4 ︰, 1 ︰ 2.
The biaxial tension polytetrafluoroethylmicroporous microporous membrane aperture is 0.3~0.5 μm, with a thickness of 40~50 μm.
Sulfuric acid solution, sodium hydroxide solution, sodium polyphosphate are molten in the specific preparation step (1) of the gluey fiber liquid
Liquid, sodium silicate solution mass fraction be respectively preferably 30%, 40%, 4%, 6%.
The mass fraction of hydrochloric acid is preferably 10% in the specific preparation step (2) of the gluey fiber liquid.
Hydroxypropyltrimethylammonium chloride chitosan and lithium bromide are mixed in the specific preparation step (3) of the gluey fiber liquid
Conjunction mass ratio is 3 ︰ 1.
Antioxidant is butylated hydroxy anisole, dibutyl hydroxyl in the specific preparation step (3) of the gluey fiber liquid
One kind of base toluene, tert-butylhydroquinone, propylgallate.
Reaction need to carry out under the conditions of ice-water bath in the specific preparation step (1) of the moisture absorption toughener.
In the specific preparation step (2) of the moisture absorption toughener when preparation moisture absorption toughener according to parts by weight, each group
Dividing raw material is 50~70 parts of copolyethers, 20~30 parts of dimethyl sulfoxides, 5~8 parts of sodium azide, 2~3 parts of sodium sulfonates.
The beneficial effects of the present invention are:
(1) present invention using paper mulberry bark as raw material, after acidleach is handled, be put into sodium hydroxide solution, polyphosphoric acids sodium solution and
In the mixed liquor of sodium silicate solution, soda boiling mulberry skin is obtained by filtration after water-bath boiling, after soda boiling mulberry skin again acidleach neutralization, passes through
Wooden mallet beats, degumming mulberry fibre is prepared in washing and drying, and degumming mulberry fibre is mixed with N-methylmorpholine aqueous solution and is put
Enter in Rotary Evaporators, add oil-soluble inhibitor, rotary evaporation obtains gluey fiber liquid, and gluey fiber liquid, moisture absorption are increased
Tough dose is shifted compounding machine two pieces of polytetrafluoroethylmicroporous microporous membranes of bonding by glue point with after pumping deaeration after hot melt adhesive composite hot melt,
Pressing obtains waterproof humidity-permeant film, and mulberry tree hide fiber internal layer is dispersed with deeper striped along longitudinal direction in the present invention, and has cavity structure,
With more micropore, fiber micropore diastole after vitriol lixiviation, in soda boiling processing, polyphosphoric acids sodium solution can integrate fiber
The metal ion of plain surrounding medium, and the gap at the coarse position of mulberry fibre can be filled up with hydroxy combining in paper mulberry bark cellulose,
In order to combine hydroxypropyltrimethylammonium chloride chitosan and lithium bromide in moisture absorption coagulating bath infiltration, be conducive to promote gluey fiber
The moisture pick-up properties of liquid, mulberry fibre is after N-methylmorpholine aqueous solution is processed, and the molecular weight of fiber reduces, and sodium metasilicate is molten
Liquid is capable of forming colloidal sol in soda boiling degumming and penetrates into fibrous inside, when dissolution prepares gluey fiber liquid, protects in mulberry fibre
The fibrous reticular structure in portion is not destroyed, and important composition substance of the gluey fiber liquid as the middle layer of waterproof humidity-permeant film, can
To significantly improve the water vapour permeability and toughness of entire waterproof humidity-permeant film；
(2) present invention is added dropwise under the conditions of ice-water bath using 1,4-butanediol, boron trifluoride ether and tetrahydrofuran as starting material
Epoxychloropropane reaction a period of time, obtains reaction product, is total to by washing, distilling to obtain tetrahydrofuran/epoxychloropropane
Polyethers, by tetrahydrofuran/epoxychloropropane copolyether, sodium azide, dimethyl sulfoxide Hybrid Heating, back flow reaction is inhaled
Wet toughener, for the present invention using 1,4-butanediol as initiator, boron trifluoride ether is catalyst, by cation ring-opening polymerization,
Tetrahydrofuran and epoxychloropropane polymerization are generated into tetrahydrofuran/epoxychloropropane copolyether, add sodium azide to fold
Tetrahydrofuran/epoxychloropropane copolyether is nitrogenized, obtains moisture absorption toughener, this moisture absorption toughener is tetrahydrofuran/poly- folded
The copolyether of nitrogen glycidol ether, wherein tetrahydrofuran is a kind of water-miscible compound, its polarity is extremely strong, in humidity
It can be sucked inside moisture permeable membrane by the micropore of polytetrafluoroethylene (PTFE), moisture absorption by water-setting vapour knot in moisture-inhibiting film surface in higher air
The main chain section of toughener is tetrahydrofuran, and tetrahydrofuran segment is more in moisture permeable membrane, and glass transition temperature is lower, tetrahydro furan
The epoxychloropropane residue segment that segment of muttering carries is more so that the glass transition temperature of copolyether can reduce, this be by
In the introducing-(CH in main chain section2)4O- segment, flexibility improve, and glycidyl azide polymer segment is folded due to having on side chain
Nitrogen groups hinder the flexibility of main chain section, in this way can be by introducing tetrahydrofuran segment in glycidyl azide polymer
Moisture permeable membrane toughness at normal temperature and moisture pick-up properties are improved, there is broad prospect of application.
Specific embodiment
It takes 200~230g paper mulberry bark to be put into the sulfuric acid solution that 400~450mL mass fraction is 30% to impregnate, control is impregnated
Temperature is 50~55 DEG C, and the immersion treatment time is 1~2h, is subsequently placed in water-bath, is heated to 90~100 DEG C, Xiang Shui
The sodium hydroxide solution that 100~120mL mass fraction is 40% is added in bath, the poly phosphorus that 50~60mL mass fraction is 4%
Acid sodium solution, the sodium silicate solution that 30~40mL mass fraction is 6%, after 2~3h of boiling, filtering, removal filtrate obtains soda boiling mulberry
Skin；Mulberry after the 8~10min of salt acid soak for being 10% with 150~180mL mass fraction by above-mentioned soda boiling mulberry skin, after taking out acidleach
Skin beats 30~35min with wooden mallet, and is put into baking oven after being rinsed with water 3~5 times, is heated to 100~110 DEG C, drying
10~12h obtains degumming mulberry fibre；Take hydroxypropyltrimethylammonium chloride chitosan with lithium bromide is that 3 ︰ 1 are mixed in mass ratio,
Then be dissolved in water to obtain the moisture absorption coagulating bath that mass fraction is 35%, by mass fraction be 30% N-methylmorpholine aqueous solution with
Degumming mulberry fibre is 10 ︰ 1 mixing in mass ratio, obtains the mixed liquor of 230~250mL, is subsequently transferred in Rotary Evaporators,
And 8~12mL propylgallate is added into Rotary Evaporators, 90~95 DEG C are heated to, with 110~130r/min's
Revolving speed 30~40min of rotary evaporation obtains gluey fiber liquid；After leading to nitrogen discharge air to three-necked flask, 20~30mL is added
1,4-butanediol, 40~50mL boron trifluoride ether and 30~35mL tetrahydrofuran, are placed in ice-water bath, obtain starting mixing
30~40mL epoxychloropropane is added dropwise into three-necked flask with constant pressure funnel with the drop rate of 5~7mL/min for liquid, protects
Ice-water bath 4~5h of conditioned response is held, then 4~5mL distilled water is added to three-necked flask, 5~10min is stood, obtains reaction product；
Above-mentioned reaction product is poured into separatory funnel, successively washs 2~3 with the sodium carbonate liquor that distilled water and mass fraction are 30%
Secondary, washing is placed in distilling flask, is heated to 90~100 DEG C, is distilled 3~4h, is obtained copolyether, in parts by weight
Meter, takes 50~70 parts of copolyethers, 20~30 parts of dimethyl sulfoxides, 5~8 parts of sodium azide, 2~3 parts of sodium sulfonates to be put into reaction kettle
In, oil bath heating is warming up to 100~120 DEG C, keeps the temperature 18~20h of back flow reaction, obtains moisture absorption toughener；First by gluey fiber
Liquid, moisture absorption toughener are that 4 ︰, 1 ︰ 2 is mixed with hot melt adhesive in mass ratio, after being heated to 120~150 DEG C of hot melts, are placed in vacuum
In air exhauster, 70~80 DEG C are heated to, controlling vacuum degree in vacuum air pump is 100~200Pa, 3~4h of standing and defoaming
Afterwards, it is sprayed between two pieces of biaxial tension polytetrafluoroethylmicroporous microporous membranes with glue point transfer compounding machine, is pressed, be prepared anti-
Water moisture permeable membrane, the biaxial tension polytetrafluoroethylmicroporous microporous membrane aperture is 0.3~0.5 μm, with a thickness of 40~50 μm, described
Hot melt adhesive be polyurethane hot melt or polyamide hot.
Hot melt adhesive are as follows: polyurethane hot melt antioxidant are as follows: butylated hydroxy anisole glue fiber liquid the preparation method comprises the following steps:
It takes 200g paper mulberry bark to be put into the sulfuric acid solution that 400mL mass fraction is 30% to impregnate, control soaking temperature is 50 DEG C, at immersion
The reason time is 1h, is subsequently placed in water-bath, is heated to 90 DEG C, and it is 40% that 100mL mass fraction is added into water-bath
The sodium silicate solution that polyphosphoric acids sodium solution that sodium hydroxide solution, 50mL mass fraction are 4%, 30mL mass fraction are 6% steams
After boiling 2h, filtering, removal filtrate obtains soda boiling mulberry skin；The salt acid soak for being 10% with 150mL mass fraction by above-mentioned soda boiling mulberry skin
After 8min, the mulberry skin after taking out acidleach beats 30min with wooden mallet, and is put into baking oven after being rinsed with water 3 times, is heated to
100 DEG C, dry 10h obtains degumming mulberry fibre；Take hydroxypropyltrimethylammonium chloride chitosan and lithium bromide is 3 ︰ in mass ratio
1 mixing is then dissolved in water to obtain the moisture absorption coagulating bath that mass fraction is 35%, the N-methylmorpholine water for being 30% by mass fraction
Solution is that 10 ︰ 1 are mixed with degumming mulberry fibre in mass ratio, obtains the mixed liquor of 230mL, is subsequently transferred to Rotary Evaporators
In, and 8mL butylated hydroxy anisole is added into Rotary Evaporators, 90 DEG C are heated to, is rotated with the revolving speed of 110r/min
30min is evaporated, gluey fiber liquid is obtained.
Moisture absorption toughener the preparation method comprises the following steps: to three-necked flask lead to nitrogen discharge air after, be added 20mL Isosorbide-5-Nitrae-fourth two
Alcohol, 40mL boron trifluoride ether and 30mL tetrahydrofuran, are placed in ice-water bath, obtain starting mixed liquor, use constant pressure funnel
With the drop rate of 5mL/min, the dropwise addition 30mL epoxychloropropane into three-necked flask, holding ice-water bath conditioned response 4h, then to
4mL distilled water is added in three-necked flask, stands 5min, obtains reaction product；Above-mentioned reaction product is poured into separatory funnel, successively
It is washed 2 times with the sodium carbonate liquor that distilled water and mass fraction are 30%, washing is placed in distilling flask, is heated to 90
DEG C, 3h is distilled, copolyether is obtained, according to parts by weight, takes 50 parts of copolyethers, 20 parts of dimethyl sulfoxides, 5 parts of sodium azide, 2 parts
Sodium sulfonate is put into reaction kettle, and oil bath heating is warming up to 100 DEG C, is kept the temperature back flow reaction 18h, is obtained moisture absorption toughener.
Waterproof humidity-permeant film the preparation method comprises the following steps: first by gluey fiber liquid, moisture absorption toughener and polyurethane hot melt press quality
Than being placed in vacuum air pump after being heated to 120 DEG C of hot melts for 4 ︰, 1 ︰ 2 mixing, 70 DEG C are heated to, vacuum is controlled
Vacuum degree is 100Pa in air exhauster, after standing and defoaming 3h, is sprayed onto two blocks of biaxial tension polytetrafluoroethylene (PTFE) with glue point transfer compounding machine
It between microporous membrane, is pressed, waterproof humidity-permeant film is prepared.
Hot melt adhesive are as follows: stabilization of polyamide hot melt adhesive agent are as follows: dibutyl hydroxy toluene glue fiber liquid the preparation method comprises the following steps:
It takes 220g paper mulberry bark to be put into the sulfuric acid solution that 420mL mass fraction is 30% to impregnate, control soaking temperature is 52 DEG C, at immersion
The reason time is 1.5h, is subsequently placed in water-bath, is heated to 95 DEG C, and it is 40% that 110mL mass fraction is added into water-bath
Sodium hydroxide solution, 55mL mass fraction be 4% polyphosphoric acids sodium solution, 35mL mass fraction be 6% sodium silicate solution,
After boiling 2.5h, filtering, removal filtrate obtains soda boiling mulberry skin；The hydrochloric acid for being 10% with 170mL mass fraction by above-mentioned soda boiling mulberry skin
After impregnating 9min, the mulberry skin after taking out acidleach beats 32min with wooden mallet, and is put into baking oven after being rinsed with water 4 times, heat temperature raising
To 105 DEG C, dry 11h obtains degumming mulberry fibre；The hydroxypropyltrimethylammonium chloride chitosan is taken to be in mass ratio with lithium bromide
3 ︰ 1 mixing is then dissolved in water to obtain the moisture absorption coagulating bath that mass fraction is 35%, the N-methylmorpholine for being 30% by mass fraction
Aqueous solution is that 10 ︰ 1 are mixed with degumming mulberry fibre in mass ratio, obtains the mixed liquor of 210mL, is subsequently transferred to Rotary Evaporators
In, and 10mL dibutyl hydroxy toluene is added into Rotary Evaporators, 92 DEG C are heated to, is rotated with the revolving speed of 120r/min
35min is evaporated, gluey fiber liquid is obtained.
Moisture absorption toughener the preparation method comprises the following steps: to three-necked flask lead to nitrogen discharge air after, be added 25mL Isosorbide-5-Nitrae-fourth two
Alcohol, 45mL boron trifluoride ether and 32mL tetrahydrofuran, are placed in ice-water bath, obtain starting mixed liquor, use constant pressure funnel
With the drop rate of 6mL/min, 35mL epoxychloropropane is added dropwise into three-necked flask, keeps ice-water bath conditioned response 4.5h, then
4mL distilled water is added to three-necked flask, stands 7min, obtains reaction product；Above-mentioned reaction product is poured into separatory funnel, according to
The secondary sodium carbonate liquor for being 30% with distilled water and mass fraction washs 2 times, and washing is placed in distilling flask, is heated to
95 DEG C, 3.5h is distilled, copolyether is obtained, according to parts by weight, takes 60 parts of copolyethers, 25 parts of dimethyl sulfoxides, 7 parts of Azides
Sodium, 2 parts of sodium sulfonates are put into reaction kettle, and oil bath heating is warming up to 110 DEG C, are kept the temperature back flow reaction 19h, are obtained moisture absorption toughener.
Waterproof humidity-permeant film the preparation method comprises the following steps: first by gluey fiber liquid, moisture absorption toughener and polyamide hot press quality
Than being placed in vacuum air pump after being heated to 140 DEG C of hot melts for 4 ︰, 1 ︰ 2 mixing, 75 DEG C are heated to, vacuum is controlled
Vacuum degree is 150Pa in air exhauster, after standing and defoaming 3.5h, is sprayed onto two pieces of biaxial tension polytetrafluoroethyl-nes with glue point transfer compounding machine
It between alkene microporous membrane, is pressed, waterproof humidity-permeant film, the biaxial tension polytetrafluoroethylmicroporous microporous membrane hole is prepared
Diameter is 0.4 μm, with a thickness of 45 μm, and the hot melt adhesive is polyurethane hot melt or polyamide hot.
Hot melt adhesive are as follows: polyurethane hot melt antioxidant are as follows: propylgallate glue fiber liquid the preparation method comprises the following steps: taking
230g paper mulberry bark, which is put into the sulfuric acid solution that 450mL mass fraction is 30%, impregnates, and control soaking temperature is 55 DEG C, immersion treatment
Time is 2h, is subsequently placed in water-bath, is heated to 100 DEG C, and it is 40% that 120mL mass fraction is added into water-bath
The sodium silicate solution that polyphosphoric acids sodium solution that sodium hydroxide solution, 60mL mass fraction are 4%, 40mL mass fraction are 6% steams
After boiling 3h, filtering, removal filtrate obtains soda boiling mulberry skin；The salt acid soak for being 10% with 180mL mass fraction by above-mentioned soda boiling mulberry skin
After 10min, the mulberry skin after taking out acidleach beats 35min with wooden mallet, and is put into baking oven after being rinsed with water 3~5 times, heat temperature raising
To 110 DEG C, dry 12h obtains degumming mulberry fibre；The hydroxypropyltrimethylammonium chloride chitosan is taken to be in mass ratio with lithium bromide
3 ︰ 1 mixing is then dissolved in water to obtain the moisture absorption coagulating bath that mass fraction is 35%, the N-methylmorpholine for being 30% by mass fraction
Aqueous solution is that 10 ︰ 1 are mixed with degumming mulberry fibre in mass ratio, obtains the mixed liquor of 250mL, is subsequently transferred to Rotary Evaporators
In, and 12mL propylgallate is added into Rotary Evaporators, 95 DEG C are heated to, is rotated and is steamed with the revolving speed of 130r/min
40min is sent out, gluey fiber liquid is obtained.
Moisture absorption toughener the preparation method comprises the following steps: to three-necked flask lead to nitrogen discharge air after, be added 30mL Isosorbide-5-Nitrae-fourth two
Alcohol, 50mL boron trifluoride ether and 35mL tetrahydrofuran, are placed in ice-water bath, obtain starting mixed liquor, use constant pressure funnel
With the drop rate of 7mL/min, the dropwise addition 40mL epoxychloropropane into three-necked flask, holding ice-water bath conditioned response 5h, then to
5mL distilled water is added in three-necked flask, stands 10min, obtains reaction product；Above-mentioned reaction product is poured into separatory funnel, according to
The secondary sodium carbonate liquor for being 30% with distilled water and mass fraction washs 3 times, and washing is placed in distilling flask, is heated to
100 DEG C, distill 4h, obtain copolyether, according to parts by weight, take 70 parts of copolyethers, 30 parts of dimethyl sulfoxides, 8 parts of sodium azide,
3 parts of sodium sulfonates are put into reaction kettle, and oil bath heating is warming up to 120 DEG C, are kept the temperature back flow reaction 20h, are obtained moisture absorption toughener.
Waterproof humidity-permeant film the preparation method comprises the following steps: first by gluey fiber liquid, moisture absorption toughener and polyurethane hot melt press quality
Than being placed in vacuum air pump after being heated to 150 DEG C of hot melts for 4 ︰, 1 ︰ 2 mixing, 80 DEG C are heated to, vacuum is controlled
Vacuum degree is 200Pa in air exhauster, after standing and defoaming 4h, is sprayed onto two blocks of biaxial tension polytetrafluoroethylene (PTFE) with glue point transfer compounding machine
It between microporous membrane, is pressed, waterproof humidity-permeant film, the biaxial tension polytetrafluoroethylmicroporous microporous membrane aperture is prepared
For 0.5 μm, with a thickness of 50 μm, the hot melt adhesive is polyurethane hot melt or polyamide hot.
Comparative example 1: it is essentially identical with the preparation method of example 2, it has only the difference is that lacking gluey fiber liquid.
Comparative example 2: it is essentially identical with the preparation method of example 2, it has only the difference is that lacking moisture absorption toughener.
Comparative example 3: the waterproof humidity-permeant film of Shanghai company production.
The test of moisture-inhibiting flux is detected using steam penetrating capacity analyzer；Water pressure resistance test uses water pressure resistance testing machine
It is detected；
Toughness test carries out tensile strength and tensile strength test by GBT10004 standard.
Table 1: moisture permeable membrane performance measurement result
| Test item | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Moisture-inhibiting flux (g/m2D) | 16215 | 16230 | 16250 | 11320 | 11350 | 11355 |
| Water pressure resistance (kPa) | 129 | 130 | 132 | 90 | 80 | 92 |
| Tensile strength (MPa) | 48.5 | 48.7 | 48.9 | 34.8 | 32.5 | 35.6 |
| Tensile strength (MPa) | 40 | 41 | 42 | 32 | 30 | 33 |
In summary, the moisture-inhibiting flux of waterproof humidity-permeant film of the invention is high as can be seen from Table 1, and water pressure resistance is high, sucting wet air permeability
Good, tensile strength is high, and tensile strength is high, and good toughness has broad application prospects.
The foregoing is merely preferred modes of the invention, are not intended to limit the invention, all in spirit and original of the invention
Within then, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of waterproof humidity-permeant film, it is characterised in that specific preparation step are as follows:
Gluey fiber liquid, moisture absorption toughener are mixed with hot melt adhesive, after being heated to 120~150 DEG C of hot melts, are placed in vacuum pumping
In mechanism of qi, it is heated to 70~80 DEG C, controlling vacuum degree in vacuum air pump is 100~200Pa, after 3~4h of standing and defoaming,
It is sprayed between two pieces of biaxial tension polytetrafluoroethylmicroporous microporous membranes with glue point transfer compounding machine, is pressed, waterproof is prepared
Moisture permeable membrane；
The specific preparation step of the gluey fiber liquid are as follows:
(1) it taking 200~230g paper mulberry bark to be put into 400~450mL sulfuric acid solution to impregnate, control soaking temperature is 50~55 DEG C,
The immersion treatment time be 1~2h, be subsequently placed in water-bath, be heated to 90~100 DEG C, into water-bath be added 100~
120mL sodium hydroxide solution, 50~60mL polyphosphoric acids sodium solution, 30~40mL sodium silicate solution, after 2~3h of boiling, filtering,
Removal filtrate obtains soda boiling mulberry skin；
(2) after the 8~10min of salt acid soak for being 10% with 150~180mL mass fraction by above-mentioned soda boiling mulberry skin, after taking out acidleach
Mulberry skin beat 30~35min with wooden mallet, and be put into baking oven after being rinsed with water 3~5 times, be heated to 100~110 DEG C,
Dry 10~12h, obtains degumming mulberry fibre；
(3) take hydroxypropyltrimethylammonium chloride chitosan with lithium bromide is that 3 ︰ 1 are mixed in mass ratio, is then dissolved in water to obtain matter
The moisture absorption coagulating bath that score is 35% is measured, the N-methylmorpholine aqueous solution that mass fraction is 30% is pressed into quality with degumming mulberry fibre
Than being mixed for 10 ︰ 1, the mixed liquor of 230~250mL is obtained, is subsequently transferred in Rotary Evaporators, and is added into Rotary Evaporators
Add 8~12mL antioxidant, is heated to 90~95 DEG C, with revolving speed 30~40min of rotary evaporation of 110~130r/min,
Obtain gluey fiber liquid；
The specific preparation step of the moisture absorption toughener are as follows:
(1) after leading to nitrogen discharge air to three-necked flask, 20~30mL1,4- butanediol, 40~50mL boron trifluoride ether is added
It with 30~35mL tetrahydrofuran, is stirred, obtains starting mixed liquor, with constant pressure funnel with the dropwise addition speed of 5~7mL/min
30~40mL epoxychloropropane is added dropwise into three-necked flask for rate, keeps 4~5h of ice-water bath conditioned response, then add to three-necked flask
Enter 4~5mL distilled water, stands 5~10min, obtain reaction product；
(2) above-mentioned reaction product is poured into separatory funnel, is successively washed with the sodium carbonate liquor that distilled water and mass fraction are 30%
It washs 2~3 times, washing is placed in distilling flask, is heated to 90~100 DEG C, is distilled 3~4h, is obtained copolyether, by weight
Number meter takes copolyether, dimethyl sulfoxide, sodium azide, sodium sulfonate to be put into reaction kettle, and oil bath heating is warming up to 100~120
DEG C, 18~20h of back flow reaction is kept the temperature, moisture absorption toughener is obtained.
2. a kind of preparation method of waterproof humidity-permeant film according to claim 1, it is characterised in that: the hot melt adhesive is poly-
Urethane hot melt adhesive or polyamide hot.
3. a kind of preparation method of waterproof humidity-permeant film according to claim 1, it is characterised in that: the gluey fiber
Liquid, moisture absorption toughener and hot melt adhesive mixing mass ratio are 4 ︰, 1 ︰ 2.
4. a kind of preparation method of waterproof humidity-permeant film according to claim 1, it is characterised in that: described is two-way
Stretch polytetrafluoroethylraw microporous membrane aperture is 0.3~0.5 μm, with a thickness of 40~50 μm.
5. a kind of preparation method of waterproof humidity-permeant film according to claim 1, it is characterised in that: the gluey fiber liquid
Specific preparation step (1) in sulfuric acid solution, sodium hydroxide solution, polyphosphoric acids sodium solution, sodium silicate solution mass fraction
It is respectively preferably 30%, 40%, 4%, 6%.
6. a kind of preparation method of waterproof humidity-permeant film according to claim 1, it is characterised in that: the gluey fiber liquid
Specific preparation step (2) in the mass fraction of hydrochloric acid be preferably 10%.
7. a kind of preparation method of waterproof humidity-permeant film according to claim 1, it is characterised in that: the gluey fiber liquid
Specific preparation step (3) in hydroxypropyltrimethylammonium chloride chitosan and lithium bromide mixing mass ratio be 3 ︰ 1.
8. a kind of preparation method of waterproof humidity-permeant film according to claim 1, it is characterised in that: the gluey fiber liquid
Specific preparation step (3) in antioxidant be butylated hydroxy anisole, dibutyl hydroxy toluene, tert-butylhydroquinone, do not have
One kind of propyl galate.
9. a kind of preparation method of waterproof humidity-permeant film according to claim 1, it is characterised in that: the moisture absorption toughener
Specific preparation step (1) in reaction need to be carried out under the conditions of ice-water bath.
10. a kind of preparation method of waterproof humidity-permeant film according to claim 1, it is characterised in that: the moisture absorption toughening
In the specific preparation step (2) of agent when preparation moisture absorption toughener according to parts by weight, each component raw material be 50~70 parts of copolyethers,
20~30 parts of dimethyl sulfoxides, 5~8 parts of sodium azide, 2~3 parts of sodium sulfonates.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111409341A (en) * | 2020-02-21 | 2020-07-14 | 杭州路先非织造股份有限公司 | Medical mask material based on spunlace nonwoven material and preparation method thereof |
| CN111409342A (en) * | 2020-02-21 | 2020-07-14 | 杭州路先非织造股份有限公司 | Protective clothing material based on spunlace nonwoven material and preparation method thereof |
| CN112724857A (en) * | 2020-12-21 | 2021-04-30 | 南京玻璃纤维研究设计院有限公司 | Waterproof material with unidirectional moisture conduction and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2015054888A (en) * | 2013-09-11 | 2015-03-23 | 日東電工株式会社 | Adhesive tape |
| CN108103605A (en) * | 2017-12-18 | 2018-06-01 | 常州达奥新材料科技有限公司 | A kind of preparation method of toughening antibacterial mulberry fibre |
| CN108973301A (en) * | 2018-07-11 | 2018-12-11 | 黄勇 | A kind of preparation method of waterproof moisture permeating fabric |
-
2019
- 2019-01-12 CN CN201910029274.6A patent/CN109825250A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2015054888A (en) * | 2013-09-11 | 2015-03-23 | 日東電工株式会社 | Adhesive tape |
| CN108103605A (en) * | 2017-12-18 | 2018-06-01 | 常州达奥新材料科技有限公司 | A kind of preparation method of toughening antibacterial mulberry fibre |
| CN108973301A (en) * | 2018-07-11 | 2018-12-11 | 黄勇 | A kind of preparation method of waterproof moisture permeating fabric |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111409341A (en) * | 2020-02-21 | 2020-07-14 | 杭州路先非织造股份有限公司 | Medical mask material based on spunlace nonwoven material and preparation method thereof |
| CN111409342A (en) * | 2020-02-21 | 2020-07-14 | 杭州路先非织造股份有限公司 | Protective clothing material based on spunlace nonwoven material and preparation method thereof |
| CN111409341B (en) * | 2020-02-21 | 2022-12-23 | 杭州路先非织造股份有限公司 | Medical mask material based on spunlace nonwoven material and preparation method thereof |
| CN111409342B (en) * | 2020-02-21 | 2022-12-27 | 杭州路先非织造股份有限公司 | Protective clothing material based on spunlace nonwoven material and preparation method thereof |
| CN112724857A (en) * | 2020-12-21 | 2021-04-30 | 南京玻璃纤维研究设计院有限公司 | Waterproof material with unidirectional moisture conduction and preparation method thereof |
| CN112724857B (en) * | 2020-12-21 | 2022-07-26 | 南京玻璃纤维研究设计院有限公司 | Waterproof material with unidirectional moisture conduction and preparation method thereof |
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