CN111057510A - High-moisture-permeability polyurethane hot melt adhesive and preparation method thereof - Google Patents
High-moisture-permeability polyurethane hot melt adhesive and preparation method thereof Download PDFInfo
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- CN111057510A CN111057510A CN201911423449.8A CN201911423449A CN111057510A CN 111057510 A CN111057510 A CN 111057510A CN 201911423449 A CN201911423449 A CN 201911423449A CN 111057510 A CN111057510 A CN 111057510A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
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- 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
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- 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
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- 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
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- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to a polyurethane hot melt adhesive with high moisture permeability and a preparation method thereof, wherein the polyurethane hot melt adhesive comprises the following components in parts by weight: 20-40 parts of polyester polyol, 30-60 parts of polyether polyol, 0.05-0.2 part of antioxidant, 0.01-0.1 part of catalyst and 10-30 parts of isocyanate. The high moisture-permeable polyurethane hot melt adhesive has high cohesiveness under the compounding action of polyester polyol, polyether polyol, an antioxidant, a catalyst and isocyanate, and has the moisture-permeable rate of over 85 percent, no solvent volatile matter, environmental protection and no pollution. In addition, the preparation method of the polyurethane hot melt adhesive with high moisture permeability is simple in preparation process, easy in obtaining of raw materials and equipment, and capable of realizing large-scale production.
Description
Technical Field
The invention relates to the field of hot melt adhesives, and particularly relates to a polyurethane hot melt adhesive with high moisture permeability and a preparation method thereof.
Background
The hot melt adhesive is a plastic adhesive, the physical state of which changes along with the change of temperature within a certain temperature range, and the chemical property of which is unchanged, is nontoxic and tasteless, and belongs to an environment-friendly chemical product. The product is solid, so the product is convenient to package, transport and store, and has no solvent, pollution and toxicity; and the production process is simple, the added value is high, the bonding strength is high, the speed is high, and the like. In the field of functional composite fabrics, hot melt adhesives are often used as adhesives for bonding two fabrics, such as windproof and breathable functional fabrics, but with improvement of living standard of people, people have higher requirements on outdoor clothing, such as windproof performance, moisture permeability and breathability. The PUR adhesive used in the field of the functional composite fabric at present achieves the bonding strength, but has poor moisture permeability, so that the moisture permeability of the functional composite fabric is influenced.
Therefore, how to prepare the polyurethane hot melt adhesive with high moisture permeability is a problem which needs to be solved urgently by research and development personnel.
Disclosure of Invention
The invention aims to provide a polyurethane hot melt adhesive with high moisture permeability and a preparation method thereof, aiming at the problem of poor water resistance and boiling resistance of the existing powder coating.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a high-moisture-permeability polyurethane hot melt adhesive, which comprises the following components in parts by weight:
further, the polyester polyol is polymerized by one or more of adipic acid, carbonic acid, sebacic acid, dodecanedioic acid, terephthalic acid, isophthalic acid or phthalic acid and one or more of hexanediol, butanediol, hexanediol, diethylene glycol or neopentyl glycol, and the weight-average molecular weight of the polyester polyol is 1000-5000.
Further, the polyether polyol is one or more of polyoxypropylene glycol, polytetrahydrofuran ether glycol-oxypropylene glycol and polyethylene glycol, and the weight average molecular weight is 400-2000-.
Further, the antioxidant is a hindered phenol antioxidant.
Further, the solid content of the hot melt adhesive is 100%.
Further, the content of isocyanate groups in the hot melt adhesive is 2-5%.
Further, the viscosity of the hot melt adhesive is 3000-6000cps at the temperature of 90 ℃.
The second aspect of the invention provides a preparation method of a polyurethane hot melt adhesive with high moisture permeability, which comprises the following steps:
(1) putting the molten polyester polyol, polyether polyol and antioxidant into a closed reaction container, heating to 120 ℃, stirring for 10min at 100 revolutions/min, uniformly mixing, vacuumizing to the negative pressure of 0.08-0.1MPa, and keeping for 60 min;
(2) cooling the material obtained in the step (1) to 70-80 ℃, breaking vacuum, rapidly adding isocyanate and a catalyst while stirring at 100 revolutions per minute, stirring at 150 revolutions per minute, vacuumizing to negative pressure of 0.08-0.1MPa, and then taking a test sample to detect the content and viscosity of isocyanate groups;
(3) and (3) discharging when the content of the isocyanate group of the sample to be measured in the step (2) is 2-5% and the viscosity is 3000-6000cps at the temperature of 90 ℃, and sealing and packaging to obtain the polyurethane hot melt adhesive with high moisture permeability.
Compared with the prior art, the invention has the following advantages:
the high moisture-permeable polyurethane hot melt adhesive has high cohesiveness under the compounding action of polyester polyol, polyether polyol, an antioxidant, a catalyst and isocyanate, and has the moisture-permeable rate of over 85 percent, no solvent volatile matter, environmental protection and no pollution. In addition, the preparation method of the polyurethane hot melt adhesive with high moisture permeability is simple in preparation process, easy in obtaining of raw materials and equipment, and capable of realizing large-scale production.
Detailed Description
The present invention will be described in detail and specifically with reference to the following examples to facilitate better understanding of the present invention, but the following examples do not limit the scope of the present invention.
In the embodiment of the invention, the related performance test of the high-moisture-permeability polyurethane hot melt adhesive adopts the following method:
1. apparent viscosity detection
Viscosity is a viscous property of liquid which generates internal friction between molecules when flowing, and the viscosity is expressed by viscosity and is used for characterizing a resistance factor related to the liquid property. Has a unit of Pa.s and is characterized in that the area of the two blocks is 1m2The plate (2) is immersed in a liquid at a distance of 1m, and when a shear stress of 1N is applied to the plate so that the relative velocity between the plates becomes 1m/s, the viscosity of the liquid becomes 1 pas, and 1000 mPas becomes 1000 cps.
The apparent viscosity was measured using a Brookfield DV-II viscometer as follows:
(1) sample preparation: directly taken with a specified container, should be uniform without bubbles, and the amount is at 2/3.
(2) The method comprises the following operation steps:
s1: the same sample should be selected with the same rotor and rotation speed, so that the reading is within 20-80% of the dial;
s2: placing the container containing the sample into a heating sleeve, balancing the temperature of the sample with the test temperature, and keeping the temperature of the sample uniform;
s3: vertically immersing the rotor into the center of the sample, and enabling the liquid level to reach the rotor liquid level mark line (a protective frame is arranged);
s4: starting the rotational viscometer to read the reading when the pointer is unchanged on the disk during rotation;
s5: each sample was assayed in triplicate.
2. Detection of isocyanate group (NCO) content
The isocyanate group is reacted with excessive di-n-butylamine to produce urea, and the excessive di-n-butylamine is titrated by hydrochloric acid to quantitatively calculate the content of the isocyanate. The specific test method is as follows:
(1) weighing 3.5-6.5g of prepolymer, putting the prepolymer into a dried flask, adding 25mL of anhydrous toluene, covering the flask with a bottle cap, and shaking to completely dissolve the sample;
(2) 20mL of a di-n-butylamine solution (wherein the di-n-butylamine solution is obtained by adding 338mL of di-n-butylamine diluted to 1000mL with dried toluene in a volumetric flask) by a pipette;
(3) adding 100mL of anhydrous isopropanol;
(4) 0.5mL of bromophenol blue solution is used as an indicator, and 1.0N hydrochloric acid solution is used for titration until the yellow end point (wherein, the bromophenol blue solution is specifically prepared by taking 0.1g of bromophenol blue, adding 1.5mL of 1N NaOH solution, and diluting to 1000mL by using distilled water).
(5) A blank test was performed to calculate the NCO content, as follows:
3. hydrostatic pressure resistance
The resistance to water penetration through a fabric is expressed in terms of the hydrostatic pressure experienced by the fabric. One side of the sample was subjected to a continuously rising water pressure under standard atmospheric conditions until three points of water penetration were reached, at which time the pressure was recorded. The specific test method was referenced to AATCC 127-.
4. Moisture permeability
The mass of water vapor passing vertically through the sample per unit area for a predetermined time under the condition of keeping a predetermined temperature and humidity on both sides of the sample. Specific test methods refer to ASTM E96.
Example 1
A preparation method of a polyurethane hot melt adhesive with high moisture permeability comprises the following steps:
weighing 25 parts of polyester polyol, 50 parts of polyether polyol, 0.05 part of hindered phenol antioxidant, 0.01 part of catalyst and 24.94 parts of isocyanate according to the component proportion; wherein the polyester polyol is polymerized by one or more of adipic acid, carbonic acid, sebacic acid, dodecanedioic acid, terephthalic acid, isophthalic acid or phthalic acid and one or more of hexanediol, butanediol, hexanediol, diethylene glycol or neopentyl alcohol, and the weight-average molecular weight of the polyester polyol is 1000-5000-;
putting the polyester polyol, the polyether polyol and the hindered phenol antioxidant which are melted into liquid into a closed reaction container, heating to 120 ℃, stirring for 10min at 100 r/min, uniformly mixing, vacuumizing to the negative pressure of 0.08-0.1MPa, and keeping for 60 min;
cooling the materials to 70-80 ℃, breaking vacuum, rapidly adding the isocyanate and the catalyst while stirring at 100 r/min, stirring at 150 r/min, vacuumizing to negative pressure of 0.08-0.1MPa, and then taking a test sample to detect the content and viscosity of the isocyanate group; and when the content of the isocyanate group of the sample to be measured is 2-5% and the viscosity is 3000-6000cps at 90 ℃, discharging, sealing and packaging to obtain the high-moisture-permeability polyurethane hot melt adhesive.
Example 2
A preparation method of a polyurethane hot melt adhesive with high moisture permeability comprises the following steps:
weighing 20 parts of polyester polyol, 55 parts of polyether polyol, 0.05 part of hindered phenol antioxidant, 0.01 part of catalyst and 24.94 parts of isocyanate according to the component proportion; wherein the polyester polyol is polymerized by one or more of adipic acid, carbonic acid, sebacic acid, dodecanedioic acid, terephthalic acid, isophthalic acid or phthalic acid and one or more of hexanediol, butanediol, hexanediol, diethylene glycol or neopentyl alcohol, and the weight-average molecular weight of the polyester polyol is 1000-5000-;
putting the polyester polyol, the polyether polyol and the hindered phenol antioxidant which are melted into liquid into a closed reaction container, heating to 120 ℃, stirring for 10min at 100 r/min, uniformly mixing, vacuumizing to the negative pressure of 0.08-0.1MPa, and keeping for 60 min;
cooling the materials to 70-80 ℃, breaking vacuum, rapidly adding the isocyanate and the catalyst while stirring at 100 r/min, stirring at 150 r/min, vacuumizing to negative pressure of 0.08-0.1MPa, and then taking a test sample to detect the content and viscosity of the isocyanate group; and when the content of the isocyanate group of the sample to be measured is 2-5% and the viscosity is 3000-6000cps at 90 ℃, discharging, sealing and packaging to obtain the high-moisture-permeability polyurethane hot melt adhesive.
Example 3
A preparation method of a polyurethane hot melt adhesive with high moisture permeability comprises the following steps:
weighing 30 parts of polyester polyol, 45 parts of polyether polyol, 0.15 part of hindered phenol antioxidant, 0.05 part of catalyst and 28 parts of isocyanate according to the component proportion; wherein the polyester polyol is polymerized by one or more of adipic acid, carbonic acid, sebacic acid, dodecanedioic acid, terephthalic acid, isophthalic acid or phthalic acid and one or more of hexanediol, butanediol, hexanediol, diethylene glycol or neopentyl alcohol, and the weight-average molecular weight of the polyester polyol is 1000-5000-;
putting the polyester polyol, the polyether polyol and the hindered phenol antioxidant which are melted into liquid into a closed reaction container, heating to 120 ℃, stirring for 10min at 100 r/min, uniformly mixing, vacuumizing to the negative pressure of 0.08-0.1MPa, and keeping for 60 min;
cooling the materials to 70-80 ℃, breaking vacuum, rapidly adding the isocyanate and the catalyst while stirring at 100 r/min, stirring at 150 r/min, vacuumizing to negative pressure of 0.08-0.1MPa, and then taking a test sample to detect the content and viscosity of the isocyanate group; and when the content of the isocyanate group of the sample to be measured is 2-5% and the viscosity is 3000-6000cps at 90 ℃, discharging, sealing and packaging to obtain the high-moisture-permeability polyurethane hot melt adhesive.
The high moisture-permeable polyurethane hot melt adhesives prepared in examples 1-3 were subjected to performance tests, and the experimental results are shown in table 1.
TABLE 1
| Test items | Example 1 | Example 2 | Example 3 |
| Viscosity (90 ℃ C.)/cps | 4700 | 4300 | 4800 |
| NCO％ | 2.8 | 2.6 | 2.9 |
| Hydrostatic pressure resistance | 6.7kPa | 6.9kPa | 6.4kPa |
| Moisture permeability | 85％ | 87％ | 83％ |
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (8)
1. The polyurethane hot melt adhesive with high moisture permeability is characterized by comprising the following components in parts by weight:
2. the highly moisture-permeable polyurethane hot melt adhesive according to claim 1, wherein the polyester polyol is polymerized from one or more of adipic acid, carbonic acid, sebacic acid, dodecanedioic acid, terephthalic acid, isophthalic acid or phthalic acid and one or more of hexanediol, butanediol, hexanediol, diethylene glycol or neopentyl alcohol, and has a weight-average molecular weight of 1000-5000.
3. The highly moisture-permeable polyurethane hot melt adhesive as claimed in claim 1, wherein the polyether polyol is one or more of polyoxypropylene glycol, polytetrahydrofuran ether glycol-oxypropylene glycol and polyethylene glycol, and the weight average molecular weight is 400-2000-.
4. The highly moisture-permeable polyurethane hot melt adhesive according to claim 1, wherein the antioxidant is a hindered phenol antioxidant.
5. The highly moisture-permeable polyurethane hot melt adhesive according to claim 1, wherein the solid content of the hot melt adhesive is 100%.
6. The highly moisture-permeable polyurethane hot melt adhesive according to claim 1, wherein the isocyanate group content of the hot melt adhesive is 2-5%.
7. The highly moisture-permeable polyurethane hot melt adhesive according to claim 1, wherein the viscosity of the hot melt adhesive is 3000-6000cps at 90 ℃.
8. The preparation method of the polyurethane hot melt adhesive with high moisture permeability according to any one of claims 1 to 7, which is characterized by comprising the following steps:
(1) putting the molten polyester polyol, polyether polyol and antioxidant into a closed reaction container, heating to 120 ℃, stirring for 10min at 100 revolutions/min, uniformly mixing, vacuumizing to the negative pressure of 0.08-0.1MPa, and keeping for 60 min;
(2) cooling the material obtained in the step (1) to 70-80 ℃, breaking vacuum, rapidly adding isocyanate and a catalyst while stirring at 100 revolutions per minute, stirring at 150 revolutions per minute, vacuumizing to negative pressure of 0.08-0.1MPa, and then taking a test sample to detect the content and viscosity of isocyanate groups;
(3) and (3) discharging when the content of the isocyanate group of the sample to be measured in the step (2) is 2-5% and the viscosity is 3000-6000cps at the temperature of 90 ℃, and sealing and packaging to obtain the polyurethane hot melt adhesive with high moisture permeability.
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| CN201911423449.8A CN111057510A (en) | 2019-12-31 | 2019-12-31 | High-moisture-permeability polyurethane hot melt adhesive and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112980386A (en) * | 2021-02-05 | 2021-06-18 | 华威粘结材料（上海）股份有限公司 | Polyurethane moisture-curing hot melt adhesive as well as preparation method and application thereof |
| CN114478991A (en) * | 2022-01-26 | 2022-05-13 | 泉州新华福合成材料有限公司 | Super-washable waterproof moisture-permeable polyurethane resin and preparation method thereof |
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| CN108641662A (en) * | 2018-05-11 | 2018-10-12 | 美瑞新材料股份有限公司 | A kind of low softening point Waterproof Breathable TPU hot melt adhesive and preparation method thereof |
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2019
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112980386A (en) * | 2021-02-05 | 2021-06-18 | 华威粘结材料（上海）股份有限公司 | Polyurethane moisture-curing hot melt adhesive as well as preparation method and application thereof |
| CN112980386B (en) * | 2021-02-05 | 2023-01-10 | 华威粘结材料（上海）股份有限公司 | Polyurethane moisture-curing hot melt adhesive and preparation method and application thereof |
| CN114478991A (en) * | 2022-01-26 | 2022-05-13 | 泉州新华福合成材料有限公司 | Super-washable waterproof moisture-permeable polyurethane resin and preparation method thereof |
| CN114478991B (en) * | 2022-01-26 | 2023-10-31 | 泉州新华福合成材料有限公司 | Super-washable waterproof moisture-permeable polyurethane resin and preparation method thereof |
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