CN103555258A - Preparation method of polyester/polyether mixed system polyurethane adhesive for spinning - Google Patents
Preparation method of polyester/polyether mixed system polyurethane adhesive for spinning Download PDFInfo
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- CN103555258A CN103555258A CN201310513900.1A CN201310513900A CN103555258A CN 103555258 A CN103555258 A CN 103555258A CN 201310513900 A CN201310513900 A CN 201310513900A CN 103555258 A CN103555258 A CN 103555258A
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Abstract
The invention discloses a polyester/polyether mixed system polyurethane adhesive for spinning and a preparation method thereof. The preparation method comprises the following steps: (1) heating, stirring and mixing polyester polyol, polyether polyol, tackifying resin, an antioxidant and a fluorescent whitening agent at a certain temperature, decompressing and degassing for 2.0 hours simultaneously, and cooling to 90 DEG C; (2) adding isocyanate and catalysts into the reaction system under the protection of nitrogen, and reacting for 45 minutes at 85-95 DEG C; (3) adding a chain extender under the protection of nitrogen, and reacting for 1.0 hour at 85-95 DEG C, thus obtaining a prepolymer; (4) transferring the reaction mixture into an aluminum foil bag under the protection of nitrogen, sealing and curing at 85 DEG C for 6 hours, thus obtaining the product which is excellent in property.
Description
Technical field
The present invention relates to a kind of weaving by the preparation method of polyester and polyether mixed system adhesive for polyurethane, especially, improving product feel and the poor water resistance causing due to unitary system material reason, finally make product performance reach the preparation method of excellent effect
Background technology.
Polyester and polyether system sizing agent is owing to having 100% solid content, in environment, do not discharge solvent, environmentally safe, to human body toxicological harmless, meets " environmental protection, health, safety " three large environmental protection sizing agents that require, and no drying process, power consumption is few, easy to operate, can be used for high-speed and continuous production line, a series of incomparable advantages such as enhance productivity |, become a class sizing agent more and more important in sizing agent field.Urethane mixed system sizing agent not only possesses above-mentioned advantage, and the reason forming due to himself raw material makes it all show very big advantage in range of application or development space, so the speed that the adhesive for polyurethane of mixed system also can be very fast development.
Both at home and abroad the research of adhesive for polyurethane has been carried out a lot of years, has been obtained great achievement, in a lot of fields, obtained application, but domestic in weaving with aspect polyurethane hot melt, its product feel and wash durability have very big difference with external product.
Summary of the invention
The object of the invention is to invent a kind of inventive method of new polyester/polyethers system polyurethane hot melt adhesive, by adjusting, fill a prescription, improve feel and the wash durability of product, make sizing agent on bonding substrates, can not make because of the defect of itself quality product after bonding decline.
The solution of the present invention is: a kind of weaving by the preparation method of polyester and polyether mixed system adhesive for polyurethane, is characterized in that comprising following step:
(1) by a certain amount of polyester polyol, polyether glycol, the glutinous resin of increasing, antioxidant, white dyes, be heated to 120-140 ℃, be uniformly mixed, degassed 2.0 h that simultaneously reduce pressure, are cooled to 90 ℃ subsequently; Add tackifying resin, degassed 1 h reduces pressure;
(2) under nitrogen protection, in (1) described reaction system, add MDI, catalyzer, under 85～95 ℃ of conditions, react 45 min;
(3) under nitrogen protection, chainextender is joined in (2) described system, under 85～95 ℃ of conditions, react 1.0 h, obtain prepolymer.
(4) under nitrogen protection, step (3) reaction mixture is transferred in aluminium foil bag, after sealing, under 85 ℃ of conditions, slaking 6 h, obtain the product of excellent performance.
By mass fraction, be 100 parts, the mass fraction of above-mentioned each component is respectively:
1, polyether glycol is 100 parts, polyester polyol 10-40 part, MDI 10-40 part, tackifying resin 20-40 part, antioxidant 0.2-0.8 part, catalyzer 0.05-0.1 part, chainextender 1-5 part, white dyes 0.05-0.1 part.
Described white dyes is stilbene biphenyl sodium disulfonate, triazine amino-stilbene, a kind of in Phthalimide derivative; Described catalyzer is one or more in dibutyl tin laurate, two morpholine Anaesthetie Ether and stannous octoate, forms by a certain percentage;
The number-average molecular weight of described polyester polyol is 1000-4000, is selected from a kind of in polyethylene glycol adipate glycol, polyhexamethylene adipate glycol, polybutylene glyool adipate, poly terephthalic acid hexylene glycol esterdiol, polybutylene terephthalate glycol, Poly(Trimethylene Terephthalate) glycol; The molecular weight of polyether glycol is 1000-4000, is selected from polyoxypropyleneglycol, polyoxyethylene glycol, one or more combinations in PTMG, propylene oxide copolymerization glycol.
Described tackifying resin is a kind of in acrylic resin, Gum Rosin, resol.
Described MDI is diphenylmethanediisocyanate, is selected from more than one in 4,4 '-MDI, 2,4 '-MDI, 2,2 '-MDI;
Described chainextender is ethylene glycol, 1.4-butyleneglycol, glycol ether, a kind of in 1,6-hexylene glycol, glycerine, TriMethylolPropane(TMP).
In described decompression degasification process, absolute pressure is controlled at 100-300Pa.
Beneficial effect of the present invention: polyester and polyether mixed system adhesive for polyurethane for a kind of weaving of the present invention, has improved sizing agent feel and laundry-resistant over-all properties.The present invention has not only retained the excellent properties of polyurethane body hot melt adhesive by compound design, and by adding corresponding formula rate, has improved the performance of the water-fastness and good hand touch of product, has made up on market and has weaved by the deficiency of glue.
Embodiment
Below by embodiment, the invention will be further described, and its object is only to understand better content of the present invention, but not limits the scope of the invention.
Embodiment 1
Thermometer, mechanical stirring, condenser and nitrogen access tube are installed on the four-hole boiling flask of 2000mL, take polypropylene glycol 150g, polyneopentyl glycol adipate 44.25g, polyhexamethylene adipate glycol 44.25g, acrylic resin 75.84g, antioxidant 1010 1.76g, white dyes stilbene biphenyl sodium disulfonate 0.05g, is then heated to 120-140 ℃, is uniformly mixed, degassed 2.0 h(absolute pressure 100-300Pa reduce pressure simultaneously), be cooled to 85 ℃; Under nitrogen protection, add 4,4 '-MDI, 60.5 g, the sub-tin of octoate catalyst and two (2,2-morpholine ethyl) ether compound 0.72 g, under 85 ~ 95 ℃ of conditions, react 45 min.Under nitrogen protection, add BDO 2.0 g, high-speed stirring is reacted 1.0 h at 85 ~ 95 ℃.By above-mentioned performed polymer, in nitrogen protection bottom discharge and pack, in 85 ℃ of environment, slaking is 6 hours, obtains product 1.
Embodiment 2
Thermometer, mechanical stirring, condenser and nitrogen access tube are installed on the four-hole boiling flask of 2000mL, take polypropylene glycol 160g, polyneopentyl glycol adipate 44.25g, polyhexamethylene adipate glycol 44.25g, acrylic resin 75.84g, antioxidant 1010 1.76g, white dyes stilbene biphenyl sodium disulfonate 0.05g, is then heated to 120-140 ℃, is uniformly mixed, degassed 2.0 h(absolute pressure 100-300Pa reduce pressure simultaneously), be cooled to 85 ℃; Under nitrogen protection, add 2,2 '-MDI, 60.5 g, the sub-tin of octoate catalyst and two (2,2-morpholine ethyl) ether compound 0.72 g, under 85 ~ 95 ℃ of conditions, react 45 min.Under nitrogen protection, add ethylene glycol 2.0 g, high-speed stirring is reacted 1.0 h at 85 ~ 95 ℃.By above-mentioned performed polymer, in nitrogen protection bottom discharge and pack, in 85 ℃ of environment, slaking is 6 hours, obtains product 2.Embodiment 3
Thermometer, mechanical stirring, condenser and nitrogen access tube are installed on the four-hole boiling flask of 2000mL, take polypropylene glycol 165g, polyneopentyl glycol adipate 44.25g, polyhexamethylene adipate glycol 44.25g, acrylic resin 75.84g, antioxidant 1010 1.76g, white dyes stilbene biphenyl sodium disulfonate 0.05g, is then heated to 120-140 ℃, is uniformly mixed, degassed 2.0 h(absolute pressure 100-300Pa reduce pressure simultaneously), be cooled to 85 ℃; Under nitrogen protection, add 2,4 '-MDI, 60.5 g, the sub-tin of octoate catalyst and two (2,2-morpholine ethyl) ether compound 0.72 g, under 85 ~ 95 ℃ of conditions, react 45 min.Under nitrogen protection, add 1,6-hexylene glycol, 2.0 g, high-speed stirring is reacted 1.0 h at 85 ~ 95 ℃.By above-mentioned performed polymer, in nitrogen protection bottom discharge and pack, in 85 ℃ of environment, slaking is 6 hours, obtains product 3.
Embodiment 4
Thermometer, mechanical stirring, condenser and nitrogen access tube are installed on the four-hole boiling flask of 2000mL, take polypropylene glycol 170g, polyneopentyl glycol adipate 44.25g, polyhexamethylene adipate glycol 44.25g, acrylic resin 75.84g, antioxidant 1010 1.76g, white dyes stilbene biphenyl sodium disulfonate 0.05g, is then heated to 120-140 ℃, is uniformly mixed, degassed 2.0 h(absolute pressure 100-300Pa reduce pressure simultaneously), cooling to 85 ℃; Under nitrogen protection, add 4,4 '-MDI, 60.5 g, the sub-tin of octoate catalyst and two (2,2-morpholine ethyl) ether compound 0.72 g, under 85 ~ 95 ℃ of conditions, react 45 min.Under nitrogen protection, add BDO 2.0 g, high-speed stirring is reacted 1.0 h at 85 ~ 95 ℃.By above-mentioned performed polymer, in nitrogen protection bottom discharge and pack, in 85 ℃ of environment, slaking is 6 hours, obtains product 4.
Sample test
After style completes, carry out viscosity, color, and stripping tests by force, viscosity win power by the U.S. and is flown DV-II+ PRO Viscometer viscometer and test, and during test, first handle is warmed up to 120 ℃ by style, under 120 ℃ of conditions, surveys constant temperature viscosity.Color directly obtains by the colour contrast of style after slaking.The strong test of stripping is by style is coated on polyester-mixed cotton cloth, under identical grammes per square metre, temperature humidity condition, measures stripping strength.Water-fastness specimen is made with the strong test of stripping, under identical water temperature, rinsing time, laundry dosing condition, carries out.
Peel strength test is with reference to standard GB/T 11402-1989, melting viscosity reference standard JRS K6862-1984, and water washing process is with reference to textile industry standard FZ/T 80007.1.
Test result is as table 1:
The technical parameter test result of table 1 product
Claims (4)
1. weave by a preparation method for polyester and polyether mixed system adhesive for polyurethane, comprise the following steps:
(1) by a certain amount of polyester polyol, polyether glycol, the glutinous resin of increasing, antioxidant, white dyes, be heated to 120-140 ℃, be uniformly mixed, degassed 2.0 h that simultaneously reduce pressure, are cooled to 90 ℃ subsequently;
(2) under nitrogen protection, in (1) described reaction system, add MDI, catalyzer, under 85～95 ℃ of conditions, react 45 min;
(3) under nitrogen protection, chainextender is joined in the product of step (2), under 85～95 ℃ of conditions, react 1.0 h, obtain prepolymer;
(4) under nitrogen protection, the product of step (3) is transferred in aluminium foil bag, after sealing, under 85 ℃ of conditions, after slaking 6 h, obtains the product of excellent performance;
By mass fraction, be 100 parts, the mass fraction of above-mentioned each component is respectively:
100 parts of polyether glycols, polyester polyol 10-40 part, MDI 10-40 part, increases glutinous resin 10-30 part, antioxidant 0.2-0.8 part, catalyzer 0.05-0.1 part, chainextender 1-5 part, white dyes 0.05-0.1 part;
Described MDI is diphenylmethanediisocyanate, is selected from a kind of in 4,4 '-MDI, 2,4 '-MDI, 2,2 '-MDI;
describedchainextender is ethylene glycol, 1.4-butyleneglycol, glycol ether, a kind of in 1.6-hexylene glycol, glycerine, TriMethylolPropane(TMP);
In described decompression degasification process, absolute pressure is controlled at 100-300Pa.
2. method according to claim 1, is characterized in that the glutinous resin of described increasing is acrylic resin, resol and C
5-C
9a kind of in petroleum resin.
3. method according to claim 1, is characterized in that described white dyes is stilbene biphenyl sodium disulfonate, triazine amino-stilbene, a kind of in Phthalimide derivative; Described catalyzer is stannous octoate and two morpholine Anaesthetie Ethers, in mass ratio for 1:1 mixes.
4. method according to claim 1, the number-average molecular weight that it is characterized in that described polyester polyol is 1250-2000, is selected from a kind of in polyethylene glycol adipate glycol, polyhexamethylene adipate glycol, polybutylene glyool adipate, poly terephthalic acid hexylene glycol esterdiol, polybutylene terephthalate glycol, Poly(Trimethylene Terephthalate) glycol; The molecular weight of polyether glycol is 1000-4000, is selected from polyoxypropyleneglycol, polyoxyethylene glycol, a kind of in PTMG, propylene oxide copolymerization glycol.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103965822A (en) * | 2014-05-09 | 2014-08-06 | 上海天洋热熔粘接材料股份有限公司 | Epoxy modified moisture curing polyurethane hot melt adhesive for compounding fabrics |
| CN104449535A (en) * | 2014-11-25 | 2015-03-25 | 上海天洋热熔粘接材料股份有限公司 | Preparation method for silane-modified moisture-curable polyurethane hot melt adhesive |
| CN104479618A (en) * | 2014-12-23 | 2015-04-01 | 上海汇得化工有限公司 | Reactive polyurethane hot melt glue used for cloth composition and preparation method of reactive polyurethane hot melt glue |
| CN105297487A (en) * | 2015-11-20 | 2016-02-03 | 嘉兴洛克化学工业有限公司 | Washing resistant adhesive and preparation method thereof |
| WO2017088765A1 (en) * | 2015-11-24 | 2017-06-01 | 上海天洋热熔粘接材料股份有限公司 | Method for preparing modified wet-cured polyurethane hot melt adhesive |
| CN106832174A (en) * | 2017-03-23 | 2017-06-13 | 江苏耐斯数码科技股份有限公司 | A kind of autofluorescence brightens acrylic acid modified polyurethane emulsion and preparation method thereof |
| CN107254028A (en) * | 2017-06-09 | 2017-10-17 | 重庆市恒安化工有限公司 | Novel alkyl phenol resin viscosified for polyurethane adhesive and preparation method thereof |
| CN108467705A (en) * | 2018-02-13 | 2018-08-31 | 嘉兴市建川新材料科技有限公司 | A kind of moisture-curable polyurethane hot melt adhesive and preparation method of high initial bonding strength |
| CN109810240A (en) * | 2019-01-15 | 2019-05-28 | 陕西科技大学 | A kind of preparation method and applications of the fluorescent brightening of polyurethane containing piperidinamine lotion |
| CN110003836A (en) * | 2018-01-04 | 2019-07-12 | 潘小聪 | A kind of environment-friendly type weaving glue and its synthetic method |
| CN111040712A (en) * | 2019-12-20 | 2020-04-21 | 烟台德邦科技有限公司 | Preparation method of high-strength sweat-resistant polyurethane hot melt adhesive |
| 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 |
| CN112521901A (en) * | 2020-12-25 | 2021-03-19 | 东莞宏石功能材料科技有限公司 | Thermoplastic polyurethane hot melt adhesive with low-temperature bonding and high bonding strength and preparation method thereof |
| CN113980218A (en) * | 2021-10-29 | 2022-01-28 | 河南省科学院化学研究所有限公司 | Moisture-curing polyurethane hot-melt adhesive and preparation method and application thereof |
| CN114989765A (en) * | 2021-03-01 | 2022-09-02 | 深圳科创新源新材料股份有限公司 | Thermoplastic underfill material and preparation method and application thereof |
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| JPH02296884A (en) * | 1989-05-10 | 1990-12-07 | Chisso Corp | Polyurethane adhesive |
| CN102634422A (en) * | 2012-03-31 | 2012-08-15 | 湖南洁宇日化新技术股份有限公司 | Preparation method of oxygen-containing washing agent and oxygen-containing washing agent prepared by same |
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Cited By (19)
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|---|---|---|---|---|
| CN103965822A (en) * | 2014-05-09 | 2014-08-06 | 上海天洋热熔粘接材料股份有限公司 | Epoxy modified moisture curing polyurethane hot melt adhesive for compounding fabrics |
| CN104449535A (en) * | 2014-11-25 | 2015-03-25 | 上海天洋热熔粘接材料股份有限公司 | Preparation method for silane-modified moisture-curable polyurethane hot melt adhesive |
| CN104479618A (en) * | 2014-12-23 | 2015-04-01 | 上海汇得化工有限公司 | Reactive polyurethane hot melt glue used for cloth composition and preparation method of reactive polyurethane hot melt glue |
| CN105297487A (en) * | 2015-11-20 | 2016-02-03 | 嘉兴洛克化学工业有限公司 | Washing resistant adhesive and preparation method thereof |
| WO2017088765A1 (en) * | 2015-11-24 | 2017-06-01 | 上海天洋热熔粘接材料股份有限公司 | Method for preparing modified wet-cured polyurethane hot melt adhesive |
| CN106832174A (en) * | 2017-03-23 | 2017-06-13 | 江苏耐斯数码科技股份有限公司 | A kind of autofluorescence brightens acrylic acid modified polyurethane emulsion and preparation method thereof |
| CN107254028B (en) * | 2017-06-09 | 2019-05-21 | 重庆市恒安化工有限公司 | Alkyl phenol resin and preparation method thereof for polyurethane adhesive thickening |
| CN107254028A (en) * | 2017-06-09 | 2017-10-17 | 重庆市恒安化工有限公司 | Novel alkyl phenol resin viscosified for polyurethane adhesive and preparation method thereof |
| CN110003836A (en) * | 2018-01-04 | 2019-07-12 | 潘小聪 | A kind of environment-friendly type weaving glue and its synthetic method |
| CN108467705A (en) * | 2018-02-13 | 2018-08-31 | 嘉兴市建川新材料科技有限公司 | A kind of moisture-curable polyurethane hot melt adhesive and preparation method of high initial bonding strength |
| CN109810240A (en) * | 2019-01-15 | 2019-05-28 | 陕西科技大学 | A kind of preparation method and applications of the fluorescent brightening of polyurethane containing piperidinamine lotion |
| CN109810240B (en) * | 2019-01-15 | 2021-06-15 | 陕西科技大学 | Preparation method and application of polyurethane fluorescent whitening emulsion containing piperidine amine |
| CN111040712A (en) * | 2019-12-20 | 2020-04-21 | 烟台德邦科技有限公司 | Preparation method of high-strength sweat-resistant polyurethane hot melt adhesive |
| 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 |
| CN112521901A (en) * | 2020-12-25 | 2021-03-19 | 东莞宏石功能材料科技有限公司 | Thermoplastic polyurethane hot melt adhesive with low-temperature bonding and high bonding strength and preparation method thereof |
| CN114989765A (en) * | 2021-03-01 | 2022-09-02 | 深圳科创新源新材料股份有限公司 | Thermoplastic underfill material and preparation method and application thereof |
| CN114989765B (en) * | 2021-03-01 | 2024-02-20 | 深圳科创新源新材料股份有限公司 | Thermoplastic underfill material, and preparation method and application thereof |
| CN113980218A (en) * | 2021-10-29 | 2022-01-28 | 河南省科学院化学研究所有限公司 | Moisture-curing polyurethane hot-melt adhesive and preparation method and application thereof |
| CN113980218B (en) * | 2021-10-29 | 2022-07-19 | 河南省科学院化学研究所有限公司 | Moisture-curing polyurethane hot-melt adhesive and preparation method and application thereof |
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Application publication date: 20140205 |