CN114478991B - Super-washable waterproof moisture-permeable polyurethane resin and preparation method thereof - Google Patents
Super-washable waterproof moisture-permeable polyurethane resin and preparation method thereof Download PDFInfo
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- CN114478991B CN114478991B CN202210091637.0A CN202210091637A CN114478991B CN 114478991 B CN114478991 B CN 114478991B CN 202210091637 A CN202210091637 A CN 202210091637A CN 114478991 B CN114478991 B CN 114478991B
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- 229920005749 polyurethane resin Polymers 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229920005862 polyol Polymers 0.000 claims abstract description 47
- 150000003077 polyols Chemical class 0.000 claims abstract description 47
- 239000002994 raw material Substances 0.000 claims abstract description 36
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 30
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims abstract description 22
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims abstract description 22
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims abstract description 22
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims abstract description 19
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 12
- QFGCFKJIPBRJGM-UHFFFAOYSA-N 12-[(2-methylpropan-2-yl)oxy]-12-oxododecanoic acid Chemical compound CC(C)(C)OC(=O)CCCCCCCCCCC(O)=O QFGCFKJIPBRJGM-UHFFFAOYSA-N 0.000 claims abstract description 11
- SXFJDZNJHVPHPH-UHFFFAOYSA-N 3-methylpentane-1,5-diol Chemical compound OCCC(C)CCO SXFJDZNJHVPHPH-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 11
- 235000011037 adipic acid Nutrition 0.000 claims abstract description 11
- 239000001361 adipic acid Substances 0.000 claims abstract description 11
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229920000570 polyether Polymers 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims abstract description 9
- 239000004970 Chain extender Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims description 38
- 239000000463 material Substances 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 238000010992 reflux Methods 0.000 claims description 10
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 9
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 9
- QKIUAMUSENSFQQ-UHFFFAOYSA-N dimethylazanide Chemical compound C[N-]C QKIUAMUSENSFQQ-UHFFFAOYSA-N 0.000 claims description 6
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical group OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 claims description 6
- RLJWTAURUFQFJP-UHFFFAOYSA-N propan-2-ol;titanium Chemical group [Ti].CC(C)O.CC(C)O.CC(C)O.CC(C)O RLJWTAURUFQFJP-UHFFFAOYSA-N 0.000 claims description 6
- VXUYXOFXAQZZMF-UHFFFAOYSA-N tetraisopropyl titanate Substances CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- 230000008033 biological extinction Effects 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 19
- 239000004744 fabric Substances 0.000 abstract description 8
- 230000035699 permeability Effects 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000009545 invasion Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6603—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6607—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4018—Mixtures of compounds of group C08G18/42 with compounds of group C08G18/48
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
- C08G18/4238—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups derived from dicarboxylic acids and dialcohols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4833—Polyethers containing oxyethylene units
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/14—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes
- D06N3/146—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes characterised by the macromolecular diols used
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2203/00—Macromolecular materials of the coating layers
- D06N2203/06—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06N2203/068—Polyurethanes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2209/00—Properties of the materials
- D06N2209/12—Permeability or impermeability properties
- D06N2209/121—Permeability to gases, adsorption
- D06N2209/123—Breathable
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2209/00—Properties of the materials
- D06N2209/14—Properties of the materials having chemical properties
- D06N2209/142—Hydrophobic
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
A super water-washing resistant waterproof moisture-permeable polyurethane resin and a preparation method thereof, wherein the polyurethane resin comprises the following raw materials: primer, self-made polyol, polyether PEG, toluene, N-dimethylformamide, diphenylmethane diisocyanate, chain extender and matting powder; the self-made polyol consists of the following raw materials: adipic acid, sebacic acid, dodecanedioic acid, neopentyl glycol, 1, 4-butanediol, 3-methyl-1, 5-pentanediol and a catalyst are limited, and the specific composition of polyurethane resin, the specific composition of primer and the raw material composition of self-made polyol are limited, so that the viscosity of the finally prepared polyurethane resin is 60000-80000cps/25 ℃, the solid content is 50-51%, and the prepared fabric has strong water resistance, high water pressure resistance and good air permeability.
Description
Technical Field
The invention belongs to the field of polyurethane resin preparation, and particularly relates to a waterproof moisture-permeable polyurethane resin with super water washing resistance and a preparation method thereof.
Background
The waterproof moisture-permeable fabric is a fabric which can only penetrate water molecules and cannot penetrate water, integrates the functions of water resistance, moisture permeability, wind resistance and heat preservation, can resist the invasion of rainwater and wind-cold, can discharge sweat of a human body, ensures the dryness and warmth of the human body, and is a preferred fabric for sportswear, casual wear and clothing with special functions.
However, although the polyurethane resin produced in the prior art has moisture permeability and good initial water pressure resistance, the water pressure resistance after a few times of water washing is excessively large, and the water pressure resistance of the common moisture permeable waterproof polyurethane resin before water washing is more than 10200mm 2 O, after 3 times of water washing, the water pressure is less than 5000mm.H 2 O; after washing for 5 times, the water pressure resistance is less than 2000mm.H 2 O, thus losing the original properties, is to be further improved.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a waterproof and moisture-permeable polyurethane resin with super water washing resistance, and also aims to provide a method for preparing the polyurethane resin.
The invention adopts the following technical scheme:
a super water-washing resistant waterproof moisture-permeable polyurethane resin is composed of the following raw materials in parts by weight: 50 parts of a base material, 10 parts of self-made polyol, 10-30 parts of polyether PEG, 30-40 parts of toluene, 10-30 parts of N, N-dimethylformamide, 3-9 parts of diphenylmethane diisocyanate, 3-4 parts of a chain extender and 3-5 parts of matting powder;
the self-made polyol consists of the following raw materials in parts by weight: 14.6 parts of adipic acid, 20 parts of sebacic acid, 22.8 parts of dodecanedioic acid, 13 parts of neopentyl glycol, 11 parts of 1, 4-butanediol, 18.25 parts of 3-methyl-1, 5-pentanediol and 0.05 part of catalyst.
Further, the base material consists of the following raw materials in parts by weight: 10-50 parts of self-made polyol, 18-25 parts of dimethyl carbonate, 15 parts of N, N-dimethylamide, 5-7 parts of liquefied MDI and 0.03 part of silane coupling agent.
Further, the molecular weight of the homemade polyol of the primer is 1000.
Further, the molecular weight of the self-made polyol is 2000.
Further, the chain extender is 1, 6-hexanediol.
Further, the catalyst is tetraisopropyl titanate.
A preparation method of super water-washing-resistant waterproof moisture-permeable polyurethane resin comprises the following steps:
step one, preparing self-made polyol and a base material according to the raw material composition of the self-made polyol and the base material respectively;
sequentially adding a base material, self-made polyol, polyether PEG, toluene, N-dimethylamide, diphenylmethane diisocyanate and a chain extender into a four-neck flask with a thermometer, a reflux condenser tube, a stirring rod and a dropping funnel according to the proportion of each raw material, heating to 80-85 ℃, controlling the stirring speed to 600r/min, stirring and reacting for 3h, heating the reaction temperature to 90 ℃, keeping the temperature constant for 2h, controlling the stirring speed to 700r/min, and reacting for 2h; then controlling the reaction temperature at 80-90 ℃, adding extinction powder, and continuing stirring and reacting until the viscosity of the obtained polyurethane resin is 60000-80000cps/25 ℃ and the solid content is 30-31%.
Further, in the first step, the preparation method of the primer is as follows: sequentially adding self-made polyol, dimethyl carbonate, N-dimethyl amide, liquefied MDI and a silane coupling agent according to the proportion of the raw materials into a four-neck flask provided with a thermometer, a reflux condenser tube, a stirring rod and a dropping funnel, heating to 80-85 ℃, controlling the stirring speed to 600r/min, stirring and reacting for 3h, heating the reaction temperature to 90 ℃, keeping the temperature constant for 2h, controlling the stirring speed to 700r/min, and reacting for 2h; then the reaction temperature is controlled at 80-90 ℃, and stirring reaction is continued until the viscosity of the obtained backing material is 60000-80000cps/25 ℃ and the solid content is 50-51%.
Further, in the first step, the preparation method of the self-made polyol is as follows: adding adipic acid, sebacic acid, dodecanedioic acid, neopentyl glycol, 1, 4-butanediol, 3-methyl-1, 5-pentanediol and a catalyst in turn according to the proportion of the raw materials into a four-neck flask provided with a thermometer, a reflux condenser tube, a stirring rod and a dropping funnel, stirring and polycondensing for 2 hours at 130-140 ℃, heating to 210 ℃, and vacuum decompressing to obtain self-made polyol, wherein the acid value is controlled to be 0.1-0.5mgKOH/g, and the viscosity is controlled to be 400-500cps/75 ℃.
As can be seen from the above description of the present invention, compared with the prior art, the present invention has the following beneficial effects: the invention limits the specific composition of polyurethane resin, the specific composition of primer and the raw material composition of self-made polyol, so that the viscosity of the finally prepared polyurethane resin is 60000-80000cps/25 ℃, the solid content is 50-51%, and the prepared fabric has strong water resistance, high water pressure resistance and good air permeability.
Detailed Description
The invention is further described below by means of specific embodiments.
A super water-washing resistant waterproof moisture-permeable polyurethane resin is composed of the following raw materials in parts by weight: 50 parts of base material, 10 parts of self-made polyol, 10-30 parts of polyether PEG, 30-40 parts of toluene, 10-30 parts of N, N-dimethylformamide, 3-9 parts of diphenylmethane diisocyanate, 3-4 parts of 1, 6-hexanediol and 3-5 parts of matting powder.
The self-made polyol consists of the following raw materials in parts by weight: 14.6 parts of adipic acid, 20 parts of sebacic acid, 22.8 parts of dodecanedioic acid, 13 parts of neopentyl glycol, 11 parts of 1, 4-butanediol, 18.25 parts of 3-methyl-1, 5-pentanediol and 0.05 part of tetraisopropyl titanate.
The bottom material consists of the following raw materials in parts by weight: 10-50 parts of self-made polyol, 18-25 parts of dimethyl carbonate, 15 parts of N, N-dimethylamide, 5-7 parts of liquefied MDI and 0.03 part of silane coupling agent.
Wherein the molecular weight of the self-made polyol in the base material is 1000; the molecular weight of the self-made polyol in the polyurethane resin is 2000; the molecular weight of the polyether PEG was 2000.
A preparation method of super water-washing-resistant waterproof moisture-permeable polyurethane resin comprises the following steps:
step one, preparing self-made polyol and a base material according to the raw material composition of the self-made polyol and the base material respectively;
sequentially adding a base material, self-made polyol 2000, polyether PEG, toluene, N-dimethyl amide, diphenylmethane diisocyanate and a chain extender into a four-neck flask with a thermometer, a reflux condenser tube, a stirring rod and a dropping funnel according to the proportion of each raw material, heating to 80-85 ℃, controlling the stirring speed to 600r/min, stirring and reacting for 3h, heating the reaction temperature to 90 ℃, keeping the temperature constant for 2h, controlling the stirring speed to 700r/min, and reacting for 2h; then controlling the reaction temperature at 80-90 ℃, adding extinction powder, and continuing stirring and reacting until the viscosity of the obtained polyurethane resin is 60000-80000cps/25 ℃ and the solid content is 30-31%.
In the first step, the preparation method of the bottom material comprises the following steps: sequentially adding self-made polyol, dimethyl carbonate, N-dimethyl amide, liquefied MDI and a silane coupling agent according to the proportion of the raw materials into a four-neck flask provided with a thermometer, a reflux condenser tube, a stirring rod and a dropping funnel, heating to 80-85 ℃, controlling the stirring speed to 600r/min, stirring and reacting for 3h, heating the reaction temperature to 90 ℃, keeping the temperature constant for 2h, controlling the stirring speed to 700r/min, and reacting for 2h; then the reaction temperature is controlled at 80-90 ℃, and stirring reaction is continued until the viscosity of the obtained backing material is 60000-80000cps/25 ℃ and the solid content is 50-51%.
The preparation method of the self-made polyol with the molecular weight of 1000 comprises the following steps: adding adipic acid, sebacic acid, dodecanedioic acid, neopentyl glycol, 1, 4-butanediol, 3-methyl-1, 5-pentanediol and a catalyst in turn according to the proportion of the raw materials into a four-neck flask provided with a thermometer, a reflux condenser tube, a stirring rod and a dropping funnel, stirring and polycondensing for 2 hours at 130-140 ℃, heating to 210 ℃, and vacuum decompressing to obtain self-made polyol, wherein the acid value is controlled to be 0.1-0.5mgKOH/g, and the viscosity is controlled to be 400-500cps/75 ℃.
The preparation method of the self-made polyol with the molecular weight of 2000 comprises the following steps: adding adipic acid, sebacic acid, dodecanedioic acid, neopentyl glycol, 1, 4-butanediol, 3-methyl-1, 5-pentanediol and a catalyst in turn according to the proportion of the raw materials into a four-neck flask provided with a thermometer, a reflux condenser tube, a stirring rod and a dropping funnel, stirring and polycondensing for 2 hours at 130-140 ℃, heating to 210 ℃, and vacuum decompressing to obtain self-made polyol, wherein the acid value is controlled to be 0.1-0.5mgKOH/g, and the viscosity is controlled to be 500-600cps/75 ℃.
Example 1
A super water-washing resistant waterproof moisture-permeable polyurethane resin is composed of the following raw materials in parts by weight: 50 parts of base material, 10 parts of self-made polyol, 10 parts of polyether PEG, 30 parts of toluene, 30 parts of N, N-dimethylformamide, 3 parts of diphenylmethane diisocyanate, 4 parts of 1, 6-hexanediol and 3 parts of matting powder.
The self-made polyol consists of the following raw materials in parts by weight: 14.6 parts of adipic acid, 20 parts of sebacic acid, 22.8 parts of dodecanedioic acid, 13 parts of neopentyl glycol, 11 parts of 1, 4-butanediol, 18.25 parts of 3-methyl-1, 5-pentanediol and 0.05 part of tetraisopropyl titanate.
The bottom material consists of the following raw materials in parts by weight: 10 parts of self-made polyol, 25 parts of dimethyl carbonate, 15 parts of N, N-dimethylamide, 7 parts of liquefied MDI and 0.03 part of silane coupling agent.
Example 2
A super water-washing resistant waterproof moisture-permeable polyurethane resin is composed of the following raw materials in parts by weight: 50 parts of base material, 10 parts of self-made polyol, 30 parts of polyether PEG, 40 parts of toluene, 10 parts of N, N-dimethylformamide, 9 parts of diphenylmethane diisocyanate, 3 parts of 1, 6-hexanediol and 5 parts of matting powder.
The self-made polyol consists of the following raw materials in parts by weight: 14.6 parts of adipic acid, 20 parts of sebacic acid, 22.8 parts of dodecanedioic acid, 13 parts of neopentyl glycol, 11 parts of 1, 4-butanediol, 18.25 parts of 3-methyl-1, 5-pentanediol and 0.05 part of tetraisopropyl titanate.
The bottom material consists of the following raw materials in parts by weight: 50 parts of self-made polyol, 18 parts of dimethyl carbonate, 15 parts of N, N-dimethylamide, 5 parts of liquefied MDI and 0.03 part of silane coupling agent.
Example 3
A super water-washing resistant waterproof moisture-permeable polyurethane resin is composed of the following raw materials in parts by weight: 50 parts of base material, 10 parts of self-made polyol, 20 parts of polyether PEG, 35 parts of toluene, 20 parts of N, N-dimethylformamide, 5 parts of diphenylmethane diisocyanate, 3.5 parts of 1, 6-hexanediol and 4 parts of matting powder.
The self-made polyol consists of the following raw materials in parts by weight: 14.6 parts of adipic acid, 20 parts of sebacic acid, 22.8 parts of dodecanedioic acid, 13 parts of neopentyl glycol, 11 parts of 1, 4-butanediol, 18.25 parts of 3-methyl-1, 5-pentanediol and 0.05 part of tetraisopropyl titanate.
The bottom material consists of the following raw materials in parts by weight: 350 parts of self-made polyol, 22 parts of dimethyl carbonate, 15 parts of N, N-dimethylamide, 6 parts of liquefied MDI and 0.03 part of silane coupling agent.
The polyurethane resin distributions obtained in examples 1 to 3 were coated on a fabric, dried to form sample 1, sample 2 and sample 3, respectively, and samples 1 to 3 were tested with commercially available water-wash-resistant waterproof moisture-permeable fabrics in the prior art, to obtain the following data:
as can be seen from the table, the specific composition of the polyurethane resin, the specific composition of the primer and the raw material composition of the self-made polyol are limited, so that the viscosity of the finally prepared polyurethane resin is 60000-80000cps/25 ℃, the solid content is 50-51%, and the prepared fabric has strong water resistance, high water pressure resistance and good air permeability.
The foregoing description is only illustrative of the preferred embodiments of the present invention and is not to be construed as limiting the scope of the invention, i.e., the invention is not to be limited to the details of the claims and the description, but rather is to cover all modifications which are within the scope of the invention.
Claims (3)
1. A super water-washing resistant waterproof moisture-permeable polyurethane resin is characterized in that: the material consists of the following raw materials in parts by weight: 50 parts of base material, 10 parts of self-made polyol with the molecular weight of 2000, 10-30 parts of polyether PEG, 30-40 parts of toluene, 10-30 parts of N, N-dimethylformamide, 3-9 parts of diphenylmethane diisocyanate, 3-4 parts of chain extender and 3-5 parts of extinction powder;
the self-made polyol with the molecular weight of 2000 comprises the following raw materials in parts by weight: 14.6 parts of adipic acid, 20 parts of sebacic acid, 22.8 parts of dodecanedioic acid, 13 parts of neopentyl glycol, 11 parts of 1, 4-butanediol, 18.25 parts of 3-methyl-1, 5-pentanediol and 0.05 part of catalyst;
the bottom material consists of the following raw materials in parts by weight: 10-50 parts of self-made polyol with molecular weight of 1000, 18-25 parts of dimethyl carbonate, 15 parts of N, N-dimethylamide, 5-7 parts of liquefied MDI and 0.03 part of silane coupling agent;
the preparation method of the self-made polyol with the molecular weight of 1000 comprises the following steps: sequentially adding adipic acid, sebacic acid, dodecanedioic acid, neopentyl glycol, 1, 4-butanediol, 3-methyl-1, 5-pentanediol and a catalyst according to the proportion of each raw material in a four-neck flask provided with a thermometer, a reflux condenser tube, a stirring rod and a dropping funnel, stirring and polycondensing for 2 hours at 130-140 ℃, heating to 210 ℃, and vacuum decompressing to obtain self-made polyol, wherein the acid value is controlled to be 0.1-0.5mgKOH/g, and the viscosity is controlled to be 400-500cps/75 ℃;
the preparation method of the base material comprises the following steps: sequentially adding self-made polyol with the molecular weight of 1000, dimethyl carbonate, N-dimethyl amide, liquefied MDI and silane coupling agent according to the proportion of each raw material into a four-neck flask provided with a thermometer, a reflux condenser tube, a stirring rod and a dropping funnel, heating to 80-85 ℃, controlling the stirring speed to 600r/min, stirring and reacting for 3h, heating the reaction temperature to 90 ℃, keeping the temperature constant for 2h, controlling the stirring speed to 700r/min, and reacting for 2h; then controlling the reaction temperature at 80-90 ℃, and continuing stirring and reacting until the viscosity of the obtained backing material is 60000-80000cps/25 ℃ and the solid content is 50-51%;
the preparation method of the super water-washing-resistant waterproof moisture-permeable polyurethane resin comprises the following steps:
step one, preparing self-made polyol and a base material according to the raw material composition of the self-made polyol and the base material respectively;
sequentially adding a base material, self-made polyol, polyether PEG, toluene, N-dimethylamide, diphenylmethane diisocyanate and a chain extender into a four-neck flask with a thermometer, a reflux condenser tube, a stirring rod and a dropping funnel according to the proportion of each raw material, heating to 80-85 ℃, controlling the stirring speed to 600r/min, stirring and reacting for 3h, heating the reaction temperature to 90 ℃, keeping the temperature constant for 2h, controlling the stirring speed to 700r/min, and reacting for 2h; then controlling the reaction temperature at 80-90 ℃, adding extinction powder, and continuing stirring and reacting until the viscosity of the obtained polyurethane resin is 60000-80000cps/25 ℃ and the solid content is 30-31%.
2. The ultra-water-washable waterproof moisture-permeable polyurethane resin of claim 1, wherein: the chain extender is 1, 6-hexanediol.
3. The ultra-water-washable waterproof moisture-permeable polyurethane resin of claim 1, wherein: the catalyst is tetraisopropyl titanate.
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| CN111057510A (en) * | 2019-12-31 | 2020-04-24 | 华威粘结材料（上海）股份有限公司 | High-moisture-permeability polyurethane hot melt adhesive and preparation method thereof |
| CN111690360A (en) * | 2020-06-22 | 2020-09-22 | 万华化学（北京）有限公司 | Reactive moisture-curing polyurethane hot melt adhesive and preparation method thereof |
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| US5869593A (en) * | 1991-07-01 | 1999-02-09 | H. B. Fuller Licensing & Financing, Inc. | High moisture vapor transmission hot melt moisture cure polyurethane adhesive |
| JPH11302356A (en) * | 1998-04-23 | 1999-11-02 | Kuraray Co Ltd | Production of polyurethane |
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| CN111057510A (en) * | 2019-12-31 | 2020-04-24 | 华威粘结材料（上海）股份有限公司 | High-moisture-permeability polyurethane hot melt adhesive and preparation method thereof |
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