CN102174211A - Polyurethane microporous water-proof and moisture permeable film prepared by using solidification method and preparation method thereof - Google Patents
Polyurethane microporous water-proof and moisture permeable film prepared by using solidification method and preparation method thereof Download PDFInfo
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- CN102174211A CN102174211A CN2011100518106A CN201110051810A CN102174211A CN 102174211 A CN102174211 A CN 102174211A CN 2011100518106 A CN2011100518106 A CN 2011100518106A CN 201110051810 A CN201110051810 A CN 201110051810A CN 102174211 A CN102174211 A CN 102174211A
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Abstract
The invention discloses a polyurethane microporous water-proof and moisture permeable film prepared by using a solidification method and a preparation method thereof. The method comprises the following steps of: firstly, preparing a wet coating working liquid and a dry direct coating working liquid; then coating the wet coating working liquid on a transfer carrier, solidifying in the aqueous solution of dimethylformamide (DMF) at mass concentration of 16-22 percent to form a film, washing, drying and coiling to obtain a polyurethane microporous film layer; coating the dry direct coating working liquid on the polyurethane microporous film layer and drying to form a protective layer; and separating the polyurethane microporous film layer and the protective layer from the transfer carrier together so as to form the polyurethane microporous water-proof and moisture permeable film. The film has a two-layer structure, wherein one layer is the polyurethane microporous layer and the other layer is the protective layer. The film structurally has a microporous form and has performances such as non-swelling, water-proofing, moisture permeability, air permeability and the like.
Description
Technical field
The present invention relates to the little porous Waterproof Breathable of a kind of freezing method urethane film and preparation method thereof.
Background technology
In recent years, mushroom development along with outdoor activity such as mountain-climbing, skiing, navigations, and some powerful departments (as army, police etc.) are to the special requirement of garment material, multiple functional Waterproof Breathable film and develop, be applied to the compound of textiles, production has the garment material of Waterproof Breathable function, is applied to functional clothing.Wherein representational product has:
1. TPU Waterproof Breathable film: TPU Waterproof Breathable film is a kind of film of homogeneous atresia, and its adopts the polyurethane elastomer with hydrophilic radical is main material, utilizes the processing of hydrostomia or blow molding process.This film water pressure resistance height (usually＞and 10000mmH2O, ISO811), saturating wet high, cheap.But its fusing point low (about 120 ℃), wet impedance is big, and low-temperature performance is bad, and the water-sprinkling processibility after compound is bad.
2. copolyether polyester film: this film also is a kind of homogeneous nonporous film, is to extrude the copolymerization film based on the fusing of polyethylene oxide and butylene terephthalate.Denaturing treatment by polyester is introduced polyether group, gives film wetting ability and control swelling.This film water pressure resistance height (usually＞and 10000mmH2O, ISO811), saturating wet high.But its price height, because atresia, wet impedance is bigger than normal, airtight.
3. PTFE film: this film is about a kind of micro-pore diameter 0.14 μ m, the function film that tetrafluoroethylene is formed through stretch processes.This film water pressure resistance height, the water vapour permeability height has ventilation property, and the product adaptation temperature range is wide.But its price height, and after wearing for a long time and washing, because greasy dirt and Action of Surfactant, hydraulic pressure descends fast, loses water-repellancy on the contrary.Because PTFE is difficult to decompose, about its environmental issue arguement is arranged always, European Union forbids that it uses on clothes.
Summary of the invention
In order to overcome above-mentioned defective, the invention provides the little porous Waterproof Breathable of a kind of freezing method urethane film and preparation method thereof, not only high water pressure resistant, height are wet thoroughly for this film, good permeability, and cost is low, and its material also is easy to degraded, environmental protection more.
The present invention for the technical scheme that solves its technical problem and adopt is: the preparation method of the little porous Waterproof Breathable of a kind of freezing method urethane film, and it may further comprise the steps:
1. prepare the direct coating working fluid of wet type coating working fluid and dry type respectively, wherein, described wet type coating working fluid comprises the component of following mass fraction:
Polyether(poly)urethane resin: 100;
Flow agent: 0.5-2;
Release agent: 0.5-2;
Bridging agent: 0.5-8;
Dimethyl formamide: 20-50;
Mill base: 3-15;
The direct coating working fluid of described dry type comprises the component of following mass fraction:
Waterproof moisture-penetrating urethane resin: 100
Mill base: 3-15;
Toluene (TOL): 10-40;
Methyl ethyl ketone (MEK): 10-40;
Wherein, 100% modulus of described polyether(poly)urethane resin is 60-120kg/cm
2
100% modulus of described waterproof moisture-penetrating urethane resin is 30-80kg/cm
2
2. wet type coating working fluid is coated on the transfer vector, and be freezing film in dimethyl formamide (the be called for short DMF) aqueous solution of 16-22% in mass concentration, washing then, dry rolling promptly obtains the little porous film layer of urethane;
3. the direct coating working fluid of dry type is coated on the little porous membrane of above-mentioned urethane, and dry, form protective layer;
4. little porous film layer of above-mentioned urethane and protective layer are separated from described transfer vector together, promptly formed the little porous Waterproof Breathable of urethane film.
As a further improvement on the present invention, the viscosity of described wet type coating working fluid is 3500-4500cps/25 ℃, and the viscosity of the direct coating working fluid of described dry type is 1000-1500cps/25 ℃.
As a further improvement on the present invention, described step 2. in the coating thickness of wet type coating working fluid be: 0.10-0.30mm, glue spread is 80-240g/m
2
As a further improvement on the present invention, described step 2. in the curing condition of wet type coating working fluid be to solidify 8-15min under 25 ℃.
As a further improvement on the present invention, the described step 2. washing condition of wet type coating working fluid is under 60-80 ℃ temperature, and every 5min extruding is once pushed 3-20 time.
As a further improvement on the present invention, described step 2. the drying conditions of wet type coating working fluid be at 100-150 ℃ of following dry 10-20min.
As a further improvement on the present invention, described step 3. in the glue spread of the direct coating working fluid of dry type be 40-50g/m
2
As a further improvement on the present invention, described step 3. in the drying conditions of the direct coating working fluid of dry type be: dry 3-5min under 100 ℃, 120 ℃, 140 ℃ condition respectively.
As a further improvement on the present invention, described transfer vector is the PET film.
In addition, the present invention also provides the little porous Waterproof Breathable of a kind of coacervation urethane film, and described film is a double-layer structure, and one deck is the little porous layer of urethane, and another layer is a protective layer.
The present invention at first uses a kind of polyether-type PU slurry of full DMF system, form working fluid to be coated according to certain prescription, it is coated on the PET film, enter concentration and be in the DMF aqueous solution between the 16-22%, this moment, water diluted or extraction from the coated membrane surface with DMF, when water and DMF when face carries out bidirectional diffusion, urethane changes PU-DMF-H into by the dissolved state in DMF
2The gel state of O, and from DMF solution, separate, solution originally becomes two-phase (muddiness) by single-phase (clarification), has taken place to be separated.Bidirectional diffusion is proceeded, in gel phase, produced the precipitation of solid PU, the liquid that takes off of solid PU shrinks, make and produced the micropore that is full of the DMF aqueous solution in the coated membrane, hole wall is a solid polyurethane, in washing afterwards, the drying course, remove the DMF aqueous solution, promptly stay the micropore of the no DMF aqueous solution.The little porous of urethane this moment forms, and water vapour permeability is also corresponding to be set up, but water-repellancy is still unstable.For this reason, need on the little porous layer of this PU, directly be coated with the PU resin that one deck has the Waterproof Breathable function again, form the PU protective layer.Thereby form the little porous Waterproof Breathable of a kind of wet type freezing method urethane film of indication of the present invention, also the film of visible indication of the present invention is bilayer structure (seeing accompanying drawing 1).
The invention has the beneficial effects as follows:
1. high hydraulic pressure, height are wet thoroughly, and ventilation property is arranged.Water pressure resistance (ISO811)＞5000mmH
2O; Vapor transfer rate (JIS L1099A1)＞5000g/m
2.24hr; Ventilation property (ASTM D737) 0.5cm
3/ cm
2.sec.Satisfy most of application scenarios.
2. have little vesicular structure, wet impedance is little.
3. cost is lower than the PTFE film, and every index is lower than the PTFE film, but also can satisfy former PTFE film portion market demand.
4. have not swelling property, film surface intensity is good.
5. be higher than the compound of textiles and PTFE film with the compound back of textiles stripping strength.
6. the film of indication of the present invention uses polyurethane material, and molecular structure simple (carbon C, hydrogen H, oxygen O, nitrogen N) does not have air pollution problems inherent during the incinerator burning, and material is subjected to humidity and microbial process, 3-5 natural decomposition when soil is buried.
Description of drawings
Fig. 1 is a structural representation of the present invention;
Fig. 2 is the structural representation of a side composite spinning lining of film of the present invention;
Fig. 3 is the structural representation of the both sides composite spinning lining of film of the present invention.
Embodiment
The preparation method of the little porous Waterproof Breathable of a kind of freezing method urethane film, it may further comprise the steps:
1. prepare the direct coating working fluid of wet type coating working fluid and dry type respectively, wherein, the direct coating working fluid of described wet type coating working fluid and dry type comprises the component of mass fraction as shown in Table 1 respectively; The direct coating working fluid of described dry type comprises the component of following mass fraction;
Wherein, 100% modulus of described polyether(poly)urethane resin is 60-120kg/cm
2
100% modulus of described waterproof moisture-penetrating urethane resin is 30-80kg/cm
2
2. wet type coating working fluid is coated on the transfer vector, and be freezing film in dimethyl formamide (the be called for short DMF) aqueous solution of 16-22% in mass concentration, washing then, dry rolling promptly obtains the little porous film layer of urethane;
3. the direct coating working fluid of dry type is coated on the little porous membrane of above-mentioned urethane, and dry, form protective layer;
4. little porous film layer of above-mentioned urethane and protective layer are separated from described transfer vector together, promptly formed the little porous Waterproof Breathable of urethane film.
The viscosity of described wet type coating working fluid is 3500-4500cps/25 ℃, and the viscosity of the direct coating working fluid of described dry type is 1000-1500cps/25 ℃.
The described step 2. coating thickness of middle wet type coating working fluid is: 0.10-0.30mm, glue spread is 80-240g/m
2
The described step 2. curing condition of middle wet type coating working fluid is to solidify 8-15min under 25 ℃.
The described step 2. washing condition of wet type coating working fluid is under 60-80 ℃ temperature, and every 5min extruding is once pushed 3-20 time.
The described step 2. drying conditions of wet type coating working fluid is dry 10-20min under 100-150 ℃.
The described step 3. glue spread of the middle direct coating working fluid of dry type is 40-50g/m
2
Described step 3. in the drying conditions of the direct coating working fluid of dry type be: dry 3-5min under 100 ℃, 120 ℃, 140 ℃ condition respectively.
Described transfer vector is the PET film.
A kind of little porous Waterproof Breathable of urethane film by above-mentioned freezing method preparation, this film is a double-layer structure, and one deck is the little porous layer 1 of urethane, and another layer is a protective layer 2, sees Fig. 1; In addition, this film one side can compound again last layer weaving face fabric 3, forms the polyurethane textile composite material, sees accompanying drawing 2; Can also form another kind of polyurethane textile composite material at the compound one deck weaving face fabric 3 of the two sides of this film difference, see accompanying drawing 3.
The component and the mass fraction thereof of 1.-7. middle wet type coating working fluid of table 1: embodiment and the direct coating working fluid of dry type
Claims (10)
1. the preparation method of the little porous Waterproof Breathable of a freezing method urethane film is characterized in that it may further comprise the steps:
1. prepare the direct coating working fluid of wet type coating working fluid and dry type respectively, wherein, described wet type coating working fluid comprises the component of following mass fraction:
Polyether(poly)urethane resin: 100;
Flow agent: 0.5-2;
Release agent: 0.5-2;
Bridging agent: 0.5-8;
Dimethyl formamide: 20-50;
Mill base: 3-15;
The direct coating working fluid of described dry type comprises the component of following mass fraction:
Waterproof moisture-penetrating urethane resin: 100
Mill base: 3-15;
Toluene (TOL): 10-40;
Methyl ethyl ketone (MEK): 10-40;
Wherein, 100% modulus of described polyether(poly)urethane resin is 60-120kg/cm
2
100% modulus of described waterproof moisture-penetrating urethane resin is 30-80kg/cm
2
2. wet type coating working fluid is coated on the transfer vector, and be freezing film in dimethyl formamide (the be called for short DMF) aqueous solution of 16-22% in mass concentration, washing then, dry rolling promptly obtains the little porous film layer of urethane;
3. the direct coating working fluid of dry type is coated on the little porous membrane of above-mentioned urethane, and dry, form protective layer;
4. little porous film layer of above-mentioned urethane and protective layer are separated from described transfer vector together, promptly formed the little porous Waterproof Breathable of urethane film.
2. the preparation method of the little porous Waterproof Breathable of freezing method urethane according to claim 1 film, it is characterized in that: the viscosity of described wet type coating working fluid is 3500-4500cps/25 ℃, and the viscosity of the direct coating working fluid of described dry type is 1000-1500cps/25 ℃.
3. the preparation method of the little porous Waterproof Breathable of freezing method urethane according to claim 1 film is characterized in that: the described step 2. coating thickness of middle wet type coating working fluid is: 0.10-0.30mm, glue spread is 80-240g/m
2
4. the preparation method of the little porous Waterproof Breathable of freezing method urethane according to claim 1 film is characterized in that: the described step 2. curing condition of middle wet type coating working fluid is to solidify 8-15min under 25 ℃.
5. the preparation method of the little porous Waterproof Breathable of freezing method urethane according to claim 1 film is characterized in that: the described step 2. washing condition of wet type coating working fluid is under 60-80 ℃ temperature, and every 5min extruding is once pushed 3-20 time.
6. the preparation method of the little porous Waterproof Breathable of freezing method urethane according to claim 1 film is characterized in that: the described step 2. drying conditions of wet type coating working fluid is dry 10-20min under 100-150 ℃.
7. the preparation method of the little porous Waterproof Breathable of freezing method urethane according to claim 1 film is characterized in that: the described step 3. glue spread of the middle direct coating working fluid of dry type is 40-50g/m
2
8. the preparation method of the little porous Waterproof Breathable of freezing method urethane according to claim 1 film is characterized in that: described step 3. in the drying conditions of the direct coating working fluid of dry type be: dry 3-5min under 100 ℃, 120 ℃, 140 ℃ condition respectively.
9. the preparation method of the little porous Waterproof Breathable of freezing method urethane according to claim 1 film, it is characterized in that: described transfer vector is the PET film.
10. one kind as according to the little porous Waterproof Breathable of the urethane film of each described freezing method preparation in the claim 1 to 8, it is characterized in that: described film is a double-layer structure, and one deck is the little porous layer of urethane (1), and another layer is protective layer (2).
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| CN 201110051810 CN102174211B (en) | 2011-03-04 | 2011-03-04 | Polyurethane microporous water-proof and moisture permeable film prepared by using solidification method and preparation method thereof |
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| CN 201110051810 CN102174211B (en) | 2011-03-04 | 2011-03-04 | Polyurethane microporous water-proof and moisture permeable film prepared by using solidification method and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104141239A (en) * | 2013-05-10 | 2014-11-12 | 昆山协孚人造皮有限公司 | Wet waterproof moisture-permeable leather production method |
| CN105111490A (en) * | 2015-08-06 | 2015-12-02 | 武汉纺织大学 | High-strength, high-modulus, high-elastic polyurethane film preparation method |
| CN106079497A (en) * | 2016-08-19 | 2016-11-09 | 昆山华富新材料股份有限公司 | Salting out method prepares the method for microporous polyurethane thin film |
| CN108822528A (en) * | 2018-07-09 | 2018-11-16 | 江苏阳光股份有限公司 | A kind of preparation method of warming-type wool fabric |
| CN110183717A (en) * | 2019-05-24 | 2019-08-30 | 嘉兴德永纺织品有限公司 | A kind of production technology of wet process microporous membrane |
| CN110644246A (en) * | 2019-09-16 | 2020-01-03 | 安徽安利材料科技股份有限公司 | Polyurethane synthetic leather for moisture-absorbing and breathable shoe lining and preparation method thereof |
| CN111019169A (en) * | 2019-12-24 | 2020-04-17 | 吴江市汉塔纺织整理有限公司 | Microporous milk silk film, film coating method and film coating machine |
| CN112341591A (en) * | 2020-10-27 | 2021-02-09 | 上海伊纯实业有限公司 | Polyurethane material and preparation method and application thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104141239A (en) * | 2013-05-10 | 2014-11-12 | 昆山协孚人造皮有限公司 | Wet waterproof moisture-permeable leather production method |
| CN104141239B (en) * | 2013-05-10 | 2016-05-18 | 昆山协孚人造皮有限公司 | Wet method Water-proof artificial leather production method |
| CN105111490A (en) * | 2015-08-06 | 2015-12-02 | 武汉纺织大学 | High-strength, high-modulus, high-elastic polyurethane film preparation method |
| CN105111490B (en) * | 2015-08-06 | 2018-02-06 | 武汉纺织大学 | A kind of preparation method of high-strength and high-modulus highly-elastic urethane film |
| CN106079497A (en) * | 2016-08-19 | 2016-11-09 | 昆山华富新材料股份有限公司 | Salting out method prepares the method for microporous polyurethane thin film |
| CN106079497B (en) * | 2016-08-19 | 2018-06-19 | 昆山华富新材料股份有限公司 | The method that salting out method prepares microporous polyurethane film |
| CN108822528A (en) * | 2018-07-09 | 2018-11-16 | 江苏阳光股份有限公司 | A kind of preparation method of warming-type wool fabric |
| CN110183717A (en) * | 2019-05-24 | 2019-08-30 | 嘉兴德永纺织品有限公司 | A kind of production technology of wet process microporous membrane |
| CN110644246A (en) * | 2019-09-16 | 2020-01-03 | 安徽安利材料科技股份有限公司 | Polyurethane synthetic leather for moisture-absorbing and breathable shoe lining and preparation method thereof |
| CN110644246B (en) * | 2019-09-16 | 2022-04-05 | 安徽安利材料科技股份有限公司 | Polyurethane synthetic leather for moisture-absorbing and breathable shoe lining and preparation method thereof |
| CN111019169A (en) * | 2019-12-24 | 2020-04-17 | 吴江市汉塔纺织整理有限公司 | Microporous milk silk film, film coating method and film coating machine |
| CN112341591A (en) * | 2020-10-27 | 2021-02-09 | 上海伊纯实业有限公司 | Polyurethane material and preparation method and application thereof |
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Effective date of registration: 20150915 Address after: 225700, Jiangsu, Taizhou province Xinghua city west suburb industrial concentration area Patentee after: Jiangsu Tangola polymeric materials Co Ltd Address before: 215337, Jiangsu Province, Suzhou City, Kunshan Province Zhou Town, Long Jing Jing Road No. 588 Patentee before: Kunshan Huarich Synthetic Leather Co., Ltd. |