CN102633977B - Waterproof moisture-permeable coating adhesive and preparation method and application thereof - Google Patents
Waterproof moisture-permeable coating adhesive and preparation method and application thereof Download PDFInfo
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- CN102633977B CN102633977B CN2012101363323A CN201210136332A CN102633977B CN 102633977 B CN102633977 B CN 102633977B CN 2012101363323 A CN2012101363323 A CN 2012101363323A CN 201210136332 A CN201210136332 A CN 201210136332A CN 102633977 B CN102633977 B CN 102633977B
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Abstract
The invention discloses waterproof moisture-permeable coating adhesive and preparation method and application thereof. The method comprises the following steps of: dehydrating polyether diol, and adding diisocyanate and hydrophilic monomer for pre-polymerization; adding a crosslinking monomer for crosslinking and a chain extender for chain extension; grafting with long-chain saturated fatty alcohol; neutralizing through a neutralizer; and emulsifying and removing solvent to obtain a kind of waterproof moisture-permeable coating adhesive which is used for the coating finish of cotton, terylene and chinlon fabric. According to the invention, by adopting long-chain saturated fatty alcohol modified waterborne polyurethane with relatively strong hydrophobicity, the waterproof perforamnce of a polyurethane film can be remarkably improved; and meanwhile, polyether diol is used as a soft monomer, the micro-phase separation degree with the hard-chain segment in polyurethane molecule is high, and the moisture permeability of the polyurethane film can be improved. The raw materials of the waterproof moisture-permeable coating adhesive disclosed by the invention are widely available, cheap and harmless to the environment, and the product has high cost performance; and moreover, the preparation technology is simple, easy to control and suitable for industrial production.
Description
Technical field
The present invention relates to a kind of Waterproof Breathable coating adhesive arranged for fabric coating and synthetic, be specifically related to a kind of Waterproof Breathable coating adhesive for cotton, terylene and polyamide fabric top finish.
Background technology
Waterproof moisture permeating fabric is a kind of function textile that 20 century 70s grow up mid-term, is widely used in the fields such as military affairs, physical culture, medical science.Waterproof Breathable refers to that polymeric film or coating do not allow the liquid infiltration such as water droplet, but can make water vapor freely see through, and reaches the purpose of Waterproof Breathable.Waterproof Breathable coating adhesive for textiles is mainly polyurethanes at present, is divided into two kinds of solvent borne polyurethane and aqueous polyurethanes.Because of with an organic solvent, (as: toluene, dimethylbenzene etc.) are restricted solvent borne polyurethane Waterproof Breathable coating adhesive; The waterproof of aqueous polyurethane Waterproof Breathable coating adhesive and water vapour permeability are desirable not enough.
In recent years, the investigator introduces the fluorochemicals with utmost point low surface energy in urethane by the method for grafting or blend both at home and abroad, document " dodecafluoroheptyl methacrylate modified aqueous polyurethane " (Zheng Feilong etc., the 7th phase of " coatings industry " 39 volumes) in, a kind of employing dodecafluoroheptyl methacrylate modified aqueous polyurethane is disclosed, improved the method for the water-repellancy of polyurethane film, the long fluorocarbon chain hard degradation of its use, larger to environmental hazard, its use finally can be restricted.Document " study on the modification of short-chain fluorine-containing acrylate to aqueous polyurethane " (Zhou Weiyan etc., the 2nd phase of " Chinese sizing agent " 19 volumes) in, adopt the trifluoroethyl methacrylate modified aqueous polyurethane, the cotton that the fluorochemical urethane obtained (FPU) emulsion was processed has water resistance preferably, but the synthesis technique complexity of fluorochemical monomer and production process are controlled difficulty, domestic also do not have scale operation, main dependence import, price is higher, and this has seriously hindered popularization and the use of the aqueous polyurethane Waterproof Breathable coating adhesive of high water resistance.
Summary of the invention
The purpose of this invention is to provide a kind of high performance-price ratio, for Waterproof Breathable coating adhesive of the top finish of cotton, terylene and polyamide fibre textiles and preparation method thereof, the requirement of high water-repellancy, high vapor transfer rate can be met, environmental friendliness, requirement with low cost can be met again.
For achieving the above object, the technical solution used in the present invention is:
Principle of the present invention is: adopt a kind ofly to have than strong-hydrophobicity and low-cost long-chain saturated fatty alcohol modified aqueous polyurethane Waterproof Breathable coating adhesive, in long-chain saturated fatty alcohol molecule, an end is long chain alkane, there is stronger hydrophobic performance, can improve the water resistance of polyurethane film, the other end is hydroxyl (OH), can react with the isocyanate group (NCO) in polyurethane molecular; Simultaneously, adopt polyoxyethylene glycol or polypropylene glycol as soft monomer, utilize them in polyurethane molecular, can improve with the feature of hard segment generation microphase-separated the water vapour permeability of polyurethane film.Long-chain saturated fatty alcohol, polyoxyethylene glycol and polypropylene glycol wide material sources, low price, can be used in the synthetic high aqueous polyurethane Waterproof Breathable coating adhesive of cost performance.
The present invention compared with the existing technology, has following advantage:
(1) one aspect of the present invention adopts and has the long-chain saturated fatty alcohol modified aqueous polyurethane than strong-hydrophobicity, can improve by a relatively large margin the water resistance of polyurethane film; On the other hand, the employing polyether Glycols is soft monomer, high with the microphase separation degree of hard segment in polyurethane molecular, can improve the water vapour permeability of polyurethane film.
(2) the present invention adopts polyether Glycols, long-chain saturated fatty alcohol wide material sources, low price, and environment is safe from harm, synthetic aqueous polyurethane Waterproof Breathable coating adhesive cost performance is high.
(3) technique of the present invention simple, be easy to control, be applicable to suitability for industrialized production.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1:
Adopt the raw material of the present embodiment synthetic method to comprise:
1. polyether Glycols: the polyoxyethylene glycol 0.1mol that molecular weight is 1000;
2. vulcabond: isophorone diisocyanate 0.3mol;
3. hydrophilic monomer: N, N-dimethylol propionic acid 0.05mol;
4. cross-linking monomer: TriMethylolPropane(TMP) 0.05mol;
5. chainextender: BDO 0.05mol;
6. long-chain saturated fatty alcohol: stearyl alcohol 0.05mol;
7. neutralizing agent: triethylamine 0.05mol;
8. solvent: acetone appropriate (for the viscosity of conditioned reaction system); Deionized water appropriate (being 25%～30% for the solid content of adjusting product).
The concrete steps of synthetic method are:
(1) polyether Glycols dehydration; Be specially: the polyoxyethylene glycol that is 1000 by molecular weight adds in flask, under 90 ℃, is evacuated down to 0.1MPa, processes and within 3 hours, sloughs moisture.
(2) add vulcabond, hydrophilic monomer pre-polymerization; Be specially: by isophorone diisocyanate, N, N-dimethylol propionic acid and 0.033g dibutyl tin laurate add in above-mentioned flask, open and stir and condensation reflux device, are warming up to 85 ℃ under nitrogen protection, insulation reaction 4 hours.
(3) add cross-linking monomer crosslinked; Be specially: add the TriMethylolPropane(TMP) insulation reaction 1 hour under 85 ℃.
(4) add the chainextender chain extension; Be specially: add the BDO insulation reaction 1 hour under 85 ℃, according to reaction system viscosity, become large situation, suitably add acetone to reduce viscosity.
(5) add the grafting of long-chain saturated fatty alcohol; Be specially: add the stearyl alcohol insulation reaction 1 hour under 85 ℃, according to reaction system viscosity, become large situation, suitably add acetone to reduce viscosity.
(6) add the neutralizing agent neutralization; Be specially: be cooled to 50 ℃ and add triethylamine, insulation reaction 0.5 hour.
(7) emulsification; Be specially: be cooled to room temperature, add appropriate amount of deionized water, high-speed stirring emulsification 0.5 hour, make the product of emulsus.
(8) remove and reclaim solvent.Be evacuated down to 0.1MPa under 60 ℃, process 0.5 hour, slough and reclaim acetone, obtain the emulsion of Waterproof Breathable coating adhesive.
Resulting emulsion is product.This product is the emulsion of milky white colour band gold-tinted, and testing its solid content is that 29%, pH is 7.1.Get this emulsion, use the thickening material thickening, arrangement is on cotton, terylene and polyamide fabric, test its waterproofing and moisture-penetration performances according to " GB/T 4744-1997 textile fabric water permeability resistance is measured hydrostatic test " and " GB/T 12704,2-2009 textile fabric water vapour permeability test method part 2: method of evaporation " as shown in table 1:
Waterproofing and moisture-penetration performances after table 1. cotton/terylene/polyamide fabric arranges
| Fabric types | Resistance to hydrostatic pressure (KPa) | Vapor transfer rate (g/m 2·24h） |
| Cotton fabric | 313 | 3900 |
| Polyester piece good | 335 | 3740 |
| Polyamide fabric | 282 | 4310 |
Embodiment 2:
Adopt the raw material of the present embodiment synthetic method to comprise:
1. polyether Glycols: the polyoxyethylene glycol 0.1mol that molecular weight is 3000.
2. vulcabond: tolylene diisocyanate 0.45mol.
3. hydrophilic monomer: N, N-dimethylolpropionic acid 0.1mol.
4. cross-linking monomer: TriMethylolPropane(TMP) 0.1mol.
5. chainextender: glycol ether 0.05mol.
6. long-chain saturated fatty alcohol: lauryl alcohol 0.1mol.
7. neutralizing agent: triethylamine 0.12mol.
8. solvent: butanone appropriate (for the viscosity of conditioned reaction system); Deionized water appropriate (being 25%～30% for the solid content of regulating product).
The concrete steps of synthetic method are:
(1) polyether Glycols dehydration; Be specially: the polyoxyethylene glycol that is 3000 by molecular weight adds in flask, under 110 ℃, is evacuated down to 0.1MPa, processes and within 2 hours, sloughs moisture.
(2) add vulcabond, hydrophilic monomer pre-polymerization; Be specially: by tolylene diisocyanate, N, N-dimethylolpropionic acid and 0.038g dibutyl tin laurate add in above-mentioned flask, open and stir and condensation reflux device, are warming up to 70 ℃ under nitrogen protection, insulation reaction 5 hours.
(3) add cross-linking monomer crosslinked; Be specially: add the TriMethylolPropane(TMP) insulation reaction 2 hours under 70 ℃.
(4) add the chainextender chain extension; Be specially: add the glycol ether insulation reaction 2 hours under 70 ℃, according to reaction system viscosity, become large situation, suitably add butanone to reduce viscosity.
(5) add the grafting of long-chain saturated fatty alcohol; Be specially: add the lauryl alcohol insulation reaction 2 hours under 70 ℃, according to reaction system viscosity, become large situation, suitably add butanone to reduce viscosity.
(6) add the neutralizing agent neutralization; Be specially: be cooled to 40 ℃ and add triethylamine, insulation reaction 1 hour.
(7) emulsification; Be specially: be cooled to room temperature, add appropriate amount of deionized water high-speed stirring emulsification 1 hour, make the product of emulsus.
(8) remove and reclaim solvent.Be evacuated down to 0.1MPa under 70 ℃, process 1 hour, slough and reclaim butanone, obtain the emulsion of Waterproof Breathable coating adhesive.
Resulting emulsion is product.This product is translucent flaxen emulsion, and testing its solid content is that 27%, pH is 7.5.Get this emulsion, use the thickening material thickening, arrangement is on cotton, terylene and polyamide fabric, test its waterproofing and moisture-penetration performances according to " GB/T 4744-1997 textile fabric water permeability resistance is measured hydrostatic test " and " GB/T 12704,2-2009 textile fabric water vapour permeability test method part 2: method of evaporation " as shown in table 2:
Waterproofing and moisture-penetration performances after table 2. cotton/terylene/polyamide fabric arranges
| Fabric types | Resistance to hydrostatic pressure (KPa) | Vapor transfer rate (g/m 2·24h） |
| Cotton fabric | 256 | 4260 |
| Polyester piece good | 292 | 4030 |
| Polyamide fabric | 330 | 3890 |
Embodiment 3:
Adopt the raw material of the present embodiment synthetic method to comprise:
1. polyether Glycols: the polypropylene glycol 0.1mol that molecular weight is 1000.
2. vulcabond: 1,6-hexamethylene-diisocyanate 0.55mol.
3. hydrophilic monomer: N, N-dimethylol propionic acid 0.15mol.
4. cross-linking monomer: TriMethylolPropane(TMP) 0.1mol.
5. chainextender: neopentyl glycol 0.1mol.
6. long-chain saturated fatty alcohol: hexadecanol 0.1mol.
7. neutralizing agent: triethylamine 0.1mol.
8. solvent: 1-Methyl-2-Pyrrolidone appropriate (for the viscosity of conditioned reaction system); Deionized water appropriate (being 25%～30% for the solid content of regulating product).
The concrete steps of synthetic method are:
(1) polyether Glycols dehydration; Be specially: the polypropylene glycol that is 1000 by molecular weight adds in flask, under 90 ℃, is evacuated down to 0.1MPa, processes and within 3 hours, sloughs moisture.
(2) add vulcabond, hydrophilic monomer pre-polymerization; Be specially: by 1,6-hexamethylene-diisocyanate, N, N-dimethylol propionic acid and 0.020g dibutyl tin laurate add in above-mentioned flask, open and stir and condensation reflux device, are warming up to 80 ℃ under nitrogen protection, insulation reaction 4 hours.
(3) add cross-linking monomer crosslinked; Be specially: add the TriMethylolPropane(TMP) insulation reaction 1 hour under 80 ℃.
(4) add the chainextender chain extension; Be specially: add the neopentyl glycol insulation reaction 1 hour under 80 ℃, according to reaction system viscosity, become large situation, suitably add 1-Methyl-2-Pyrrolidone to reduce viscosity.
(5) add the grafting of long-chain saturated fatty alcohol; Be specially: add the hexadecanol insulation reaction 1 hour under 80 ℃, according to reaction system viscosity, become large situation, suitably add 1-Methyl-2-Pyrrolidone to reduce viscosity.
(6) add the neutralizing agent neutralization; Be specially: be cooled to 40 ℃ and add triethylamine, insulation reaction 0.5 hour.
(7) emulsification; Be specially: be cooled to room temperature, add a certain amount of deionized water high-speed stirring emulsification 1 hour, make the product of emulsus.
(8) remove and reclaim solvent.Be evacuated down to 0.09MPa under 70 ℃, process 1 hour, slough and reclaim 1-Methyl-2-Pyrrolidone, obtain the emulsion of Waterproof Breathable coating adhesive.
Resulting emulsion is product.This product is translucent milky emulsion, and testing its solid content is that 30%, pH is 7.2.Get this emulsion, use the thickening material thickening, arrangement is on cotton, terylene and polyamide fabric, test its waterproofing and moisture-penetration performances according to " GB/T 4744-1997 textile fabric water permeability resistance is measured hydrostatic test " and " GB/T 12704,2-2009 textile fabric water vapour permeability test method part 2: method of evaporation " as shown in table 3:
Waterproofing and moisture-penetration performances after table 3. cotton/terylene/polyamide fabric arranges
| Fabric types | Resistance to hydrostatic pressure (KPa) | Vapor transfer rate (g/m 2·24h） |
| Cotton fabric | 276 | 4200 |
| Polyester piece good | 295 | 3750 |
| Polyamide fabric | 316 | 3260 |
Embodiment 4:
Adopt the raw material of the present embodiment synthetic method to comprise:
1. polyether Glycols: the polypropylene glycol 0.1mol that molecular weight is 3000.
2. vulcabond: ditolyl methane vulcabond 0.45mol.
3. hydrophilic monomer: N, N-dimethylolpropionic acid 0.1mol.
4. cross-linking monomer: TriMethylolPropane(TMP) 0.1 mol.
5. chainextender: BDO 0.05mol.
6. long-chain saturated fatty alcohol: stearyl alcohol 0.1mol.
7. neutralizing agent: triethylamine 0.12mol.
8. solvent: acetone appropriate (for the viscosity of conditioned reaction system); Deionized water appropriate (being 25%～30% for the solid content of regulating product).
The concrete steps of this synthetic method are:
(1) polyether Glycols dehydration; Be specially: the polypropylene glycol that is 3000 by molecular weight adds in flask, under 90 ℃, is evacuated down to 0.1MPa, processes and within 3 hours, sloughs moisture.
(2) add vulcabond, hydrophilic monomer pre-polymerization; Be specially: by ditolyl methane vulcabond, N, N-dimethylolpropionic acid and 0.083g dibutyl tin laurate add in above-mentioned flask, open and stir and condensation reflux device, are warming up to 75 ℃ under nitrogen protection, insulation reaction 4 hours.
(3) add cross-linking monomer crosslinked; Be specially: add the TriMethylolPropane(TMP) insulation reaction 2 hours under 75 ℃.
(4) add the chainextender chain extension; Be specially: add the BDO insulation reaction 1 hour under 75 ℃, according to reaction system viscosity, become large situation, suitably add acetone to reduce viscosity.
(5) add the grafting of long-chain saturated fatty alcohol; Be specially: add the stearyl alcohol insulation reaction 2 hours under 75 ℃, according to reaction system viscosity, become large situation, suitably add acetone to reduce viscosity.
(6) add the neutralizing agent neutralization; Be specially: be cooled to 45 ℃ and add triethylamine, insulation reaction 0.5 hour.
(7) emulsification; Be specially: be cooled to room temperature, add a certain amount of deionized water high-speed stirring emulsification 1 hour, make the product of emulsus.
(8) remove and reclaim solvent.Be evacuated down to 0.1MPa under 60 ℃, process 1 hour, slough and reclaim acetone, obtain the emulsion of Waterproof Breathable coating adhesive.
Resulting emulsion is product.This product is translucent milky emulsion, and testing its solid content is that 28%, pH is 7.4.Get this emulsion, use the thickening material thickening, arrangement is on cotton, terylene and polyamide fabric, test its waterproofing and moisture-penetration performances according to " GB/T 4744-1997 textile fabric water permeability resistance is measured hydrostatic test " and " GB/T 12704,2-2009 textile fabric water vapour permeability test method part 2: method of evaporation " as shown in table 4:
Waterproofing and moisture-penetration performances after table 5. cotton/terylene/polyamide fabric arranges
| Fabric types | Resistance to hydrostatic pressure (KPa) | Vapor transfer rate (g/m 2·24h） |
| Cotton fabric | 296 | 4420 |
| Polyester piece good | 313 | 4310 |
| Polyamide fabric | 322 | 3920 |
Claims (7)
1. the preparation method of a Waterproof Breathable coating adhesive is characterized in that:
Raw material for the preparation of described Waterproof Breathable coating adhesive comprises: polyether Glycols, vulcabond, hydrophilic monomer, cross-linking monomer, chainextender, neutralizing agent, catalyzer, long-chain saturated fatty alcohol;
Described polyether Glycols is selected from polyoxyethylene glycol, the polypropylene glycol that molecular weight is 1000～3000;
Described vulcabond is selected from isophorone diisocyanate, tolylene diisocyanate, diphenylmethanediisocyanate, 2,6-vulcabond methylhexanoic acid ester, 1,6-hexamethylene-diisocyanate;
Described hydrophilic monomer is selected from N, N-dimethylol propionic acid, N, N-dimethylolpropionic acid;
Described cross-linking monomer is TriMethylolPropane(TMP);
Described chainextender is BDO, glycol ether, neopentyl glycol;
Described neutralizing agent is triethylamine;
Described catalyzer is dibutyl tin laurate;
Described long-chain saturated fatty alcohol is selected from lauryl alcohol, tetradecyl alcohol, hexadecanol and stearyl alcohol;
The ratio of the amount of substance between polyether Glycols, vulcabond, hydrophilic monomer, cross-linking monomer, chainextender is: 1:3.0～5.5:0.5～1.5:0.5～1.0:0.5～1.0;
The ratio of the amount of substance of neutralizing agent and hydrophilic monomer is 1.0～1.2:1;
The ratio of the amount of substance of long-chain saturated fatty alcohol and cross-linking monomer is 1:1;
The consumption of catalyzer is 0.01%～0.02% of polyether Glycols and vulcabond total mass;
The step for preparing described Waterproof Breathable coating adhesive comprises:
(1) polyether Glycols is added in reaction vessel, under 90～110 ℃, be evacuated to 0.09～0.1MPa, processed 2～3 hours;
(2) vulcabond, hydrophilic monomer and catalyzer are joined in the polyether Glycols after dehydration, open and stir and condensation reflux unit, be warming up to 70～85 ℃ under nitrogen protection, insulation reaction 4～5 hours;
(3) add the cross-linking monomer insulation reaction 1～2 hour under 70～85 ℃;
(4) add the chainextender insulation reaction 1～2 hour under 70～85 ℃, suitably add organic solvent to control viscosity;
(5) add the long-chain saturated fatty alcohol under 70～85 ℃, insulation reaction 1～2 hour, suitably add organic solvent to control viscosity;
(6) add neutralizing agent under 40～50 ℃, insulation reaction 0.5～1 hour;
(7) suitably add at ambient temperature deionized water to control solid content, through high-speed stirring emulsification 0.5～1 hour, make the product of emulsus;
(8) under the condition that is 0.09～0.1Mpa 60～70 ℃ and vacuum tightness, process the product 0.5～1 hour of emulsus, remove and reclaim solvent, obtain the Waterproof Breathable coating adhesive.
2. the preparation method of a kind of Waterproof Breathable coating adhesive according to claim 1, it is characterized in that: the total amount of substance of hydroxyl-OH of polyether Glycols monomer, hydrophilic monomer, cross-linking monomer, chainextender monomer and long-chain saturated fatty alcohol monomer with the ratio of the amount of substance of the isocyanate group-NCO of diisocyanate monomer is: 1:1.
3. the preparation method of a kind of Waterproof Breathable coating adhesive according to claim 1 is characterized in that: the molecular weight of described polyoxyethylene glycol is a kind of in 1000,1500,2000,3000.
4. the preparation method of a kind of Waterproof Breathable coating adhesive according to claim 1 is characterized in that: the molecular weight of described polypropylene glycol is a kind of in 1000,1500,2000,3000.
5. the preparation method of a kind of Waterproof Breathable coating adhesive according to claim 1 is characterized in that: described organic solvent is a kind of in benzene,toluene,xylene, acetone, butanone, 1-Methyl-2-Pyrrolidone, DMF.
6. adopt the Waterproof Breathable coating adhesive of the method acquisition of claim 1.
7. Waterproof Breathable coating adhesive claimed in claim 6, for the top finish of cotton, terylene and polyamide fibre textiles.
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| CN101709197A (en) * | 2009-11-20 | 2010-05-19 | 广州市纺织工业研究所 | Temperature-sensitive hydrophilic cross-linking crystal type polyurethane coating agent, preparation method thereof and application thereof |
| CN102168379B (en) * | 2011-03-11 | 2013-03-06 | 上腾新材料科技（苏州）有限公司 | Polyurethane polymer material with high water pressure resistance and high moisture permeability |
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