CN108048020B - Single-component moisture-curing reaction type polyurethane hot melt adhesive and preparation method thereof - Google Patents

Single-component moisture-curing reaction type polyurethane hot melt adhesive and preparation method thereof Download PDF

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CN108048020B
CN108048020B CN201711500644.7A CN201711500644A CN108048020B CN 108048020 B CN108048020 B CN 108048020B CN 201711500644 A CN201711500644 A CN 201711500644A CN 108048020 B CN108048020 B CN 108048020B
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adipic acid
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陈余国
赵叶宝
薛晓金
汪忠敏
何建国
陈一帆
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Zhejiang Huafeng New Material Co ltd
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04Polyurethanes
    • C09J175/06Polyurethanes from polyesters
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30Low-molecular-weight compounds
    • C08G18/36Hydroxylated esters of higher fatty acids
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/4009Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
    • C08G18/4072Mixtures of compounds of group C08G18/63 with other macromolecular compounds
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/42Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/4205Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups
    • C08G18/4208Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups containing aromatic groups
    • C08G18/4211Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups containing aromatic groups derived from aromatic dicarboxylic acids and dialcohols
    • C08G18/4216Polycondensates having carboxylic or carbonic ester groups in the main chain containing cyclic groups containing aromatic groups derived from aromatic dicarboxylic acids and dialcohols from mixtures or combinations of aromatic dicarboxylic acids and aliphatic dicarboxylic acids and dialcohols
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    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/63Block or graft polymers obtained by polymerising compounds having carbon-to-carbon double bonds on to polymers
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    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6633Compounds of group C08G18/42
    • C08G18/6662Compounds of group C08G18/42 with compounds of group C08G18/36 or hydroxylated esters of higher fatty acids of C08G18/38
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2170/00Compositions for adhesives
    • C08G2170/20Compositions for hot melt adhesives

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  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
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  • Adhesives Or Adhesive Processes (AREA)
  • Polyurethanes Or Polyureas (AREA)

Abstract

The invention discloses a single-component moisture-curing reaction type polyurethane hot melt adhesive and a preparation method thereof, wherein the single-component moisture-curing reaction type polyurethane hot melt adhesive is a reaction product of grafted polyester polyol, poly adipic acid-aromatic acid-glycol ester glycol, poly adipic acid-aromatic acid-1, 4-butanediol ester glycol, castor oil, an antioxidant, isocyanate, a catalyst and a stabilizer. The invention does not use tackifying resin, and the product bonded by the product has high peel strength and good hand feeling.

Description

Single-component moisture-curing reaction type polyurethane hot melt adhesive and preparation method thereof
Technical Field
The invention relates to a single-component moisture-curing reaction type polyurethane hot melt adhesive and a preparation method thereof.
Background
The polyurethane adhesive is an adhesive containing carbamate (-NHCOO-) or isocyanate (-NCO) in a molecular chain, and has excellent chemical adhesive force with materials containing active hydrogen, such as porous materials of foam plastics, wood, leather, fabric, paper, ceramic and the like, and materials with smooth surfaces of metal, glass, rubber, plastic and the like. With the stricter environmental requirements, the traditional organic solvent adhesives are gradually eliminated, and the development of hot melt and water-based adhesives is shifted. Therefore, the vigorous development of environmentally friendly hot melt and water-based polyurethane adhesives is the main development trend in the polyurethane adhesive industry in China.
The moisture-curing reaction type adhesive is one of hot-melt polyurethane adhesives, has the characteristics of low-temperature hot melting, easy coating, good wettability, room-temperature curing, good heat resistance and the like, and is recently popular in the industry. The Chinese patent application with the application number of 200810047234.6 discloses a preparation method of a moisture-curing reaction type polyurethane hot melt adhesive for shoes, which utilizes hydroxyl-terminated liquid rubber, polyether polyol, toluene diisocyanate, trimethylolpropane, tackifying resin and a catalyst to prepare the hot melt adhesive so as to improve the hydrolysis resistance and physical properties of the hot melt adhesive. The Chinese patent application with the application number of 201110423062.X discloses a moisture-curing silane-modified polyurethane hot melt adhesive and a preparation method thereof, wherein silane-modified polyurethane, tackifying resin, a plasticizer, a viscosity reducing auxiliary agent, an organic silicon auxiliary agent, an inorganic filler, an antioxidant and an ultraviolet absorber are used for preparing a hot melt adhesive, and the adhesive property of the hot melt adhesive is improved. The Chinese patent application with the application number of 201410623780.5 discloses a moisture-curing polyurethane hot melt adhesive with long skinning time and a preparation method thereof. The Chinese patent application with the application number of 201510821013.X discloses a preparation method of a modified moisture-curing polyurethane hot melt adhesive, wherein pentaerythritol diacrylate is used to modify the traditional moisture-curing polyurethane hot melt adhesive to obtain a satisfactory initial adhesion. The modification of moisture-curing polyurethane hot melt adhesives is continuously carried out, but unfortunately, the modified moisture-curing polyurethane hot melt adhesives still use tackifying resins which often affect the hand feeling and the peeling strength of adhesive products after being used, so that the application of the moisture-curing polyurethane hot melt adhesives is limited to a certain extent.
Disclosure of Invention
The invention aims to provide a single-component moisture-curing reaction type polyurethane hot melt adhesive without using tackifying resin and a preparation method thereof, so as to solve the problems in the prior art.
The single-component moisture-curing reaction type polyurethane hot melt adhesive is a reaction product of grafted polyester polyol, poly adipic acid-aromatic acid-glycol ester diol, poly adipic acid-aromatic acid-1, 4-butanediol ester diol, castor oil, an antioxidant, isocyanate, a catalyst and a stabilizer;
the single-component moisture-curing reaction type polyurethane hot melt adhesive comprises the following raw materials in percentage by weight:
Figure BSA0000157162010000021
the NCO content of the single-component moisture-curing reaction type polyurethane hot melt adhesive is 2.0-3.0%.
Preferably, the first and second liquid crystal materials are,
the single-component moisture-curing reaction type polyurethane hot melt adhesive comprises the following raw materials in percentage by weight:
Figure BSA0000157162010000022
the NCO content of the single-component moisture-curing reaction type polyurethane hot melt adhesive is 2.3% -2.7%.
The isocyanate is one or more of diphenylmethane diisocyanate, carbodiimide modified diisocyanate, toluene diisocyanate and polymethylene polyphenyl isocyanate;
the grafted polyester polyol is styrene grafted poly adipic acid polyester polyol;
the styrene grafted poly adipic acid polyester polyol is styrene grafted poly adipic acid ethylene glycol-1, 4-butanediol glycol ester diol, the number average molecular weight is 1500-3000, and the solid content is 15-35%;
the number average molecular weight of the poly adipic acid-aromatic acid-glycol ester is 1000-3000; preferably, the molar ratio of adipic acid to aromatic acid in the poly adipic acid-aromatic acid-ethylene glycol ester glycol is 3: 1-10: 1;
the number average molecular weight of the poly adipic acid-aromatic acid-1, 4-butanediol ester diol is 2000-5000, and preferably, the molar ratio of adipic acid to aromatic acid in the poly adipic acid-aromatic acid-1, 4-butanediol ester diol is 3: 1-10: 1;
the aromatic acid is one or more of terephthalic acid, phthalic acid, isophthalic acid and phthalic anhydride;
the antioxidant is one or more of antioxidant 1010, antioxidant 1035, antioxidant 1076, antioxidant 245 and antioxidant 1098;
the catalyst is one or more of N-methylmorpholine, dimorpholine diethyl ether, dimorpholine triethyl ether and N- (dimethylaminoethyl) morpholine;
the stabilizer is phosphoric acid.
The preparation method of the single-component moisture-curing reaction type polyurethane hot melt adhesive comprises the steps of adding grafted polyester polyol, poly adipic acid-aromatic acid-glycol ester diol, poly adipic acid-aromatic acid-1, 4-butanediol ester diol and castor oil into a reaction kettle, heating to (100-130) DEG C, carrying out vacuum dehydration (1-2) h, cooling to (70-90) DEG C, adding an antioxidant and isocyanate, heating to (100-130) DEG C, reacting (2-3) h, adding a catalyst and a stabilizer, stirring (0.5-1.0) h, carrying out vacuum deaeration (1.0-1.5) h, discharging, carrying out nitrogen protection, and carrying out sealed packaging.
Compared with the prior art, the invention has the following advantages:
(1) the grafted polyester polyol and the poly adipic acid-aromatic acid-glycol ester diol, the poly adipic acid-aromatic acid-1, 4-butanediol ester diol and the like are used for synergistic cooperation without using tackifying resin, so that the peel strength and the low-temperature hand feeling of a product viscose prepared by the product viscose are improved.
(2) The hydrolysis resistance of the hot melt adhesive is improved by using castor oil.
Detailed Description
The present invention is further illustrated by the following specific examples, but it should be understood that the specific materials, process conditions and results described in the examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and all equivalent changes and modifications made according to the spirit of the present invention should be covered by the scope of the present invention.
Example 1
5.0kg of styrene grafted polyester polyol (number average molecular weight 1500), 40.0kg of poly (ethylene adipate-terephthalate) glycol (number average molecular weight 1000, molar ratio of adipic acid to terephthalic acid 3: 1), 10.0kg of poly (1, 4-butylene adipate-isophthalate) glycol (number average molecular weight 2000, molar ratio of adipic acid to isophthalic acid 3: 1) and 1.0kg of castor oil are added into a reaction kettle, the temperature is increased to 100 ℃, vacuum dehydration is carried out for 2h, the temperature is reduced to 70 ℃, 0.05kg of antioxidant 245 and 17.5kg of diphenylmethane diisocyanate (MDI) are added, the temperature is increased to 100 ℃ for reaction for 3h, 0.10kg of dimorpholintriethyl ether and 0.01kg of phosphoric acid are added, stirring is carried out for 0.5h, vacuum defoaming is carried out for 1.5h, discharging and nitrogen protection sealing packaging is carried out.
Example 2
15.0kg of styrene grafted polyester polyol (number average molecular weight 3000), 35kg of poly (ethylene adipate-phthalate) glycol (number average molecular weight 3000, the molar ratio of adipic acid to phthalic acid is 10: 1), 30.0kg of poly (adipic acid-terephthalic acid-1, 4-butanediol glycol) (number average molecular weight 5000, the molar ratio of adipic acid to terephthalic acid is 10: 1) and 5.0kg of castor oil are added into a reaction kettle, the temperature is increased to 130 ℃, vacuum dehydration is carried out for 1h, the temperature is reduced to 90 ℃, 0.5kg of antioxidant 245 and 14.3kg of MDI are added, the temperature is increased to 130 ℃ for reaction for 2h, 0.20kg of dimorpholinyl triethyl ether and 0.10kg of phosphoric acid are added, stirring is carried out for 1.0h, vacuum defoaming is carried out for 1.0h, discharging, and sealed packaging is carried out under the protection of nitrogen.
Example 3
5.0kg of styrene grafted polyester polyol (number average molecular weight 2000), 70.0kg of poly (ethylene adipate-isophthalate) glycol (number average molecular weight 2000, molar ratio of adipic acid to isophthalic acid is 8: 1), 25.0kg of poly (adipic acid-phthalic acid-1, 4-butanediol glycol) (number average molecular weight 3000, molar ratio of adipic acid to phthalic acid is 6: 1) and 2.0kg of castor oil are added into a reaction kettle, the temperature is increased to 100 ℃, vacuum dehydration is carried out for 2h, the temperature is reduced to 70 ℃, 0.08kg of antioxidant 1010 and 20.5kg of MDI are added, the temperature is increased to 100 ℃ for reaction for 3h, 0.15kg of dimorpholinyl triethyl ether and 0.05kg of phosphoric acid are added, stirring is carried out for 1.0h, vacuum defoaming is carried out for 1.5h, discharging is carried out, and nitrogen protection, sealing and packaging are carried out.
Example 4
6.0kg of styrene grafted polyester polyol (number average molecular weight 3000), 70.0kg of poly (ethylene adipate terephthalate glycol) (number average molecular weight 2000, molar ratio of adipic acid to terephthalic acid is 4: 1), 12.0kg of poly (isophthalic adipate-1, 4-butanediol glycol) (number average molecular weight 3000, molar ratio of adipic acid to isophthalic acid is 6: 1) and 2.0kg of castor oil are added into a reaction kettle, the temperature is increased to 130 ℃, vacuum dehydration is carried out for 1h, the temperature is reduced to 90 ℃, 0.5kg of antioxidant 1035 and 18.3kg of MDI are added, the temperature is increased to 130 ℃ for reaction for 2h, 0.20kg of dimorpholintriethyl ether and 0.10kg of phosphoric acid are added, stirring is carried out for 1.0h, vacuum defoaming is carried out for 1.0h, discharging is carried out, and nitrogen protection, sealing and packaging are carried out.
Comparative example 1
Adding 5.0kg of styrene grafted polyester polyol (number average molecular weight 1500), 40.0kg of poly adipic acid-ethylene terephthalate glycol (number average molecular weight 1000, molar ratio of adipic acid to terephthalic acid is 3: 1), 10.0kg of poly adipic acid-isophthalic acid-1, 4-butanediol glycol (number average molecular weight 2000, molar ratio of adipic acid to isophthalic acid is 3: 1) into a reaction kettle, heating to 100 ℃, carrying out vacuum dehydration for 2h, cooling to 70 ℃, adding 0.05kg of antioxidant 245 and 17.0kg of diphenylmethane diisocyanate (MDI), heating to 100 ℃, reacting for 3h, adding 0.10kg of dimorpholintriethyl ether and 0.01kg of phosphoric acid, stirring for 0.5h, carrying out vacuum defoaming for 1.5h, discharging, carrying out nitrogen protection, sealing and packaging.
Comparative example 2
Adding 35.0kg of poly (ethylene adipate-co-phthalate) glycol (with the number average molecular weight of 3000 and the molar ratio of adipic acid to phthalic acid of 10: 1), 30.0kg of poly (adipic acid-co-terephthalate) 1, 4-butanediol glycol (with the number average molecular weight of 5000 and the molar ratio of adipic acid to terephthalic acid of 10: 1), 5.0kg of castor oil and 15.0kg of tackifying resin into a reaction kettle, heating to 130 ℃, carrying out vacuum dehydration for 1h, cooling to 90 ℃, adding 0.50kg of antioxidant 245 and 13.0kg of MDI, heating to 130 ℃, reacting for 2h, adding 0.20kg of ditrimethylmorpholine ether and 0.10kg of phosphoric acid, stirring for 1.0h, carrying out vacuum defoaming for 1.0h, discharging, carrying out nitrogen protection, sealing and packaging.
Comparative example 3
Adding 5.0kg of styrene grafted polyester polyol (number average molecular weight 2000), 70.0kg of poly adipic acid-ethylene glycol (number average molecular weight 2000), 25.0kg of poly adipic acid-1, 4-butanediol glycol (number average molecular weight 3000) and 2.0kg of castor oil into a reaction kettle, heating to 100 ℃, carrying out vacuum dehydration for 2h, cooling to 70 ℃, adding 0.08kg of antioxidant 1010 and 20.5kg of MDI, heating to 100 ℃, reacting for 3h, adding 0.15kg of dimorpholine triethyl ether and 0.05kg of phosphoric acid, stirring for 1.0h, carrying out vacuum deaeration for 1.5h, discharging, carrying out nitrogen protection, and carrying out sealed packaging.
Comparative example 4
6.0kg of styrene grafted polyester polyol (number average molecular weight 3000), 70.0kg of poly (ethylene adipate-terephthalate) glycol (number average molecular weight 2000, molar ratio of adipic acid to terephthalic acid is 1: 1), 12.0kg of poly (1, 4-butylene adipate-isophthalate) glycol (number average molecular weight 3000, molar ratio of adipic acid to isophthalic acid is 1: 1) and 2.0kg of castor oil are added into a reaction kettle, the temperature is increased to 130 ℃, vacuum dehydration is carried out for 1h, the temperature is reduced to 90 ℃, 1.00kg of antioxidant 1035 and 18.3kg of MDI are added, the temperature is increased to 130 ℃ for reaction for 2h, 0.20kg of dimorpholinyl triethyl ether and 0.10kg of phosphoric acid are added, stirring is carried out for 1.0h, vacuum defoaming is carried out for 1.0h, discharging, nitrogen protection, sealing and packaging are carried out.
The results of the physical property tests of the one-component moisture-curable polyurethane hot melt adhesives obtained in the application examples 1 to 4 and the comparative examples 1 to 4 are shown in table 1.
TABLE 1
Figure BSA0000157162010000051
In conclusion, the single-component moisture curing reaction type polyurethane hot melt adhesive disclosed by the invention is not added with tackifying resin, does not influence the peel strength and hand feeling of adhesive products, and is high in bonding strength and excellent in hydrolysis resistance.
Although the embodiments of the present invention have been described in detail, the technical aspects of the present invention are not limited to the embodiments, and equivalent changes or modifications made to the contents of the claims of the present invention should fall within the technical scope of the present invention without departing from the spirit and the spirit of the present invention.

Claims (7)

1. The single-component moisture-curing reaction type polyurethane hot melt adhesive is characterized by being a reaction product of grafted polyester polyol, poly adipic acid-aromatic acid-glycol ester diol, poly adipic acid-aromatic acid-1, 4-butanediol ester diol, castor oil, an antioxidant, isocyanate, a catalyst and a stabilizer;
the weight percentage of each raw material is as follows:
Figure FSB0000193381640000011
the NCO content of the single-component moisture-curing reaction type polyurethane hot melt adhesive is 2.0-3.0%;
the grafted polyester polyol is styrene grafted poly adipic acid polyester polyol;
the molar ratio of adipic acid to aromatic acid in the poly adipic acid-aromatic acid-glycol ester is 3: 1-10: 1;
the molar ratio of adipic acid to aromatic acid in the poly adipic acid-aromatic acid-1, 4-butanediol ester diol is 3: 1-10: 1.
2. The single-component moisture-curing reactive polyurethane hot melt adhesive according to claim 1, which is characterized by comprising the following raw materials in percentage by weight:
Figure FSB0000193381640000012
the NCO content of the single-component moisture-curing reaction type polyurethane hot melt adhesive is 2.3% -2.7%.
3. The one-component moisture-curable polyurethane hot melt adhesive according to claim 2, wherein the isocyanate is one or more of diphenylmethane diisocyanate, carbodiimide-modified diisocyanate, toluene diisocyanate, and polymethylene polyphenyl isocyanate.
4. The one-component moisture-curing reactive polyurethane hot melt adhesive according to claim 1, wherein the styrene-grafted poly (adipic acid) polyester polyol is styrene-grafted poly (ethylene glycol adipate) -1, 4-butylene glycol ester glycol, the number average molecular weight is 1500-3000, and the solid content is 15-35%.
5. The one-component moisture-curing reactive polyurethane hot melt adhesive according to claim 4, wherein the number average molecular weight of the poly (adipic acid-aromatic acid-ethylene glycol ester) is 1000-3000;
the number average molecular weight of the poly adipic acid-aromatic acid-1, 4-butanediol ester diol is 2000-5000.
6. The one-component moisture-curing reactive polyurethane hot melt adhesive according to claim 5, wherein the aromatic acid is one or more of terephthalic acid, phthalic acid, isophthalic acid and phthalic anhydride;
the antioxidant is one or more of antioxidant 1010, antioxidant 1035, antioxidant 1076, antioxidant 245 and antioxidant 1098;
the catalyst is one or more of N-methylmorpholine, dimorpholine diethyl ether, dimorpholine triethyl ether and N- (dimethylaminoethyl) morpholine;
the stabilizer is phosphoric acid.
7. The preparation method of the one-component moisture-curing reactive polyurethane hot melt adhesive according to any one of claims 1 to 6, wherein the grafted polyester polyol, the poly adipic acid-aromatic acid-ethylene glycol ester glycol, the poly adipic acid-aromatic acid-1, 4-butylene glycol ester glycol and the castor oil are added into a reaction kettle, the temperature is increased to 100-130 ℃, vacuum dehydration is performed for 1-2 h, the temperature is reduced to 70-90 ℃, the antioxidant and the isocyanate are added, the temperature is increased to 100-130 ℃, the reaction is performed for 2-3 h, the catalyst and the stabilizer are added, the stirring is performed for 0.5-1.0 h, the vacuum defoaming is performed for 1.0-1.5 h, the discharging is performed, and nitrogen protection, sealing and packaging are performed.
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CN109321191B (en) * 2018-08-22 2021-03-05 上海天洋热熔粘接材料股份有限公司 Preparation method of moisture-curing polyurethane hot melt adhesive
CN111607352B (en) * 2020-06-11 2022-06-21 苏州金枪新材料股份有限公司 Light, heat and moisture cured PUR hot melt adhesive for textiles and preparation method thereof
CN111718468A (en) * 2020-07-15 2020-09-29 烟台云泷化学制品有限公司 Low-cost high-hardness polyurethane stiffening agent slurry and preparation method and application thereof
CN112795350B (en) * 2020-12-30 2023-02-03 烟台德邦科技股份有限公司 Oil-acid-resistant reactive polyurethane hot melt adhesive
CN112852378B (en) * 2021-01-13 2022-11-18 广东省京极盛新材料科技有限公司 Reactive polyurethane hot melt adhesive

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