CN101962524B - Waterborne polyurethane adhesive and preparation method thereof - Google Patents
Waterborne polyurethane adhesive and preparation method thereof Download PDFInfo
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- CN101962524B CN101962524B CN201010500510A CN201010500510A CN101962524B CN 101962524 B CN101962524 B CN 101962524B CN 201010500510 A CN201010500510 A CN 201010500510A CN 201010500510 A CN201010500510 A CN 201010500510A CN 101962524 B CN101962524 B CN 101962524B
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- polyurethane adhesive
- based polyurethane
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- organosilane
- viscotrol
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Abstract
The invention discloses a waterborne polyurethane adhesive and a preparation method thereof. The waterborne polyurethane adhesive is obtained by synthesizing raw materials such as polyester polyol, castor oil, isocyanate, a hydrophilic extended chain agent, organosilane, a salt forming agent, a solvent, a catalyst and deionized water. The polyester polyol and the castor oil with high water resistance are used, the castor oil is a polyether substance with lyophobic structure and the internal crosslinking structure of silane is adopted, so that the water resistance of the waterborne polyurethane adhesive is enhanced greatly; after an ammonia silane coupling agent is added, an amidogen reacts with residual isocyanate and a hydrolysable silica group undergoes hydrolytic polycondensation so as to perform crosslinking and chain extension on a system; and glue prepared by the process has high bonding strength and high water resistance and can meet the performance requirement of the waterborne polyurethane adhesive.
Description
Technical field
The present invention relates to a kind of polyurethane adhesive, relate in particular to a kind of preparation method of water-based polyurethane adhesive.
Background technology:
Along with the continuous variation with consumption structure of improving constantly of people's living standard, the flexible packing material that has good Practical Performance and superior barrier properties in recent years is rapidly developed, and has driven the quick growth of the multiple film glue demand of solvent borne polyurethane thus.Because solvent-based adhesive contains a large amount of solvents, glue is in production and use, the volatilization of a large amount of solvents, can pollute air, influence operator's health, have inflammable and explosive major safety risks simultaneously, residual solvent, cause the pollution of packing material easily, cause a serious accident.Water-based polyurethane adhesive is dispersion medium with water, have nontoxicly, do not burn, smell is little, safety, pollution-free, the same with solvent-borne type, have low temperature resistant, snappiness is good, the characteristics that bonding strength is big meet green industrial expansion requirement, have been widely used in fields such as tackiness agent, coating, hide finishes at present.
Soft packaging use polyurethane adhesive is with two layers of plastics film compound tackiness agent.The bonding strength height, heat seal strength that keeps urethane except need well, also to satisfy special functional demands such as water-fast, temperature tolerance.
Commercially available water-based polyurethane adhesive will keep the stability of its storage at present, must use wetting ability chainextender dimethylol propionic acid, and dimethylolpropionic acid like this, though solved the stability of its storage, has reduced the water tolerance of tackiness agent.PAUR ester group internal cohesive energy is big, and is good with the adhesive power of polar substrates, but ester group is than facile hydrolysis, and water tolerance is good not as polyether(poly)urethane, and polyether(poly)urethane ether internal cohesive energy is little, to the poor adhesion of polar substrates, but water-tolerant.
Summary of the invention:
One of purpose of the present invention provides a kind of water-based polyurethane adhesive, and another purpose provides the preparation method of this water-based polyurethane adhesive.
Described water-based polyurethane adhesive, it is the synthetic gained of raw material by polyester polyol, Viscotrol C, isocyanic ester, hydrophilic chain extender, organosilane, salt forming agent, solvent, catalyzer, deionized water, wherein, the mixture of the pure and mild Viscotrol C of polyester polyols: isocyanic ester: hydrophilic chain extender: organosilane: the weight ratio of salt forming agent is (110～120): (35～45): (6～8): (2～4): (6～10), the weight ratio between the pure and mild Viscotrol C of polyester polyols is 100: (10～20).
Described polyester polyol is poly-hexanodioic acid-1,6-hexylene glycol, poly-hexanodioic acid-1,4-butyleneglycol neopentyl glycol, polycaprolactone glycol, polycarbonate-1, any of 6-hexylene glycol esterdiol.
Described isocyanic ester be tolylene diisocyanate, ditan-4,4 '-in the vulcabond, hexamethylene diisocyanate, isophorone diisocyanate any.
Described solvent is acetone, butanone or N-Methyl pyrrolidone;
Described catalyzer is dibutyl tin laurate or stannous octoate.
Described wetting ability chainextender is any in dimethylol propionic acid, the dimethylolpropionic acid.
Described organosilane is 3-aminopropyl triethoxysilane or 3-glycidyl ether oxygen base propyl trimethoxy silicane.
Described salt forming agent is triethylamine or sodium hydroxide.
Though the alternative of the component raw material of preparation water-based polyurethane adhesive is very big, its preparation method is all identical.
The preparation method of described water-based polyurethane adhesive is as follows:
The pure and mild Viscotrol C of polyester polyols is placed in the encloses container, and the weight ratio of the two is 100: 10～20, and vacuum-drying is 1 hour under 100 ℃～120 ℃ conditions, be cooled to 70 ℃ then, drip catalyzer after adding isocyanic ester, be warming up to 75～90 ℃ of reactions 2 hours, added wetting ability chainextender and solvent reaction 1 hour, be cooled to 40 ℃, add organosilane reaction 0.5 hour, in salt forming agent and after, be scattered in the deionized water fast, intensification steams solvent, thereby obtains target compound; Wherein, the mixture of the pure and mild Viscotrol C of polyester polyols: isocyanic ester: hydrophilic chain extender: organosilane: the weight ratio of salt forming agent is (110～120): (35～45): (6～8): (2～4): (6～10).
Because the present invention has selected the pure and mild Viscotrol C of polyester polyols of water-tolerant for use, wherein, Viscotrol C is the polyethers material of hydrophobic structure, adopts the internal crosslinking structure of silane simultaneously, makes the water tolerance of water-based polyurethane adhesive be greatly improved; After adding the Ammonia silane coupling agent, amido and residual isocyanate react, hydrolyzable silica group generation hydrolytie polycondensation and make crosslinked, the chain extension of system; By above process, the existing good bonding strength of the glue that makes has good water tolerance again, can satisfy the performance of poach type polyurethane adhesive.
Embodiment:
Embodiment 1:
Agitator is being housed, in the glass reactor of thermometer reflux exchanger, add poly-hexanodioic acid-1,6-hexylene glycol 100g, Viscotrol C 10g, under 100 ℃～120 ℃ conditions, vacuum-drying 1 hour, add tolylene diisocyanate 35g, dibutyl tin laurate 0.02g, be warming up to 70～85 ℃ of reactions after 2 hours, add dimethylol propionic acid DMPA 5g reaction 1 hour, be cooled to then below 40 ℃, add 3-aminopropyl triethoxysilane 2g and stir 30min, adding triethylamine 6g makes and gives in the aggressiveness and salify, and adds acetone 50g reduction viscosity, adds the 237g deionized water then and carry out emulsification under high speed shear, heat up at last and steam acetone, obtain the milky water-based polyurethane adhesive of blueing light, its solid content: 40%, solid content is tested according to the GB/T2793-1995 standard; Viscosity is (being coated with-4 glasss, 25 ℃): 17s, and viscosity is tested according to the GB/T2794-1995 standard.
Embodiment 2:
Agitator is being housed, in the glass reactor of thermometer reflux exchanger, add poly-hexanodioic acid-1,4-butyleneglycol neopentyl glycol 100g, Viscotrol C 20g, isophorone diisocyanate 45g, add stannous octoate 0.02g, be warming up to 73～86 ℃ of reactions after 2 hours, add dimethylol propionic acid DMPA 8g reaction 1 hour, be cooled to then below 40 ℃, add 3-glycidyl ether oxygen base propyl trimethoxy silicane 4g and stir 30min, adding triethylamine 10g makes and gives in the aggressiveness and salify, and adding acetone 52g reduces viscosity, add the 305g deionized water then and carry out emulsification under high speed shear, heating up at last steams acetone, obtains the milky water-based polyurethane adhesive of blueing light, its solid content: 38%, solid content is tested according to the GB/T2793-1995 standard; Viscosity is (being coated with-4 glasss, 25 ℃): 15s, and viscosity is tested according to the GB/T2794-1995 standard.
Embodiment 3:
Agitator is being housed, in the glass reactor of thermometer reflux exchanger, add polycaprolactone glycol 100g, Viscotrol C 15g, vacuum-drying is 1 hour under 100 ℃～120 ℃ conditions, add ditan-4,4 ' vulcabond 40g, dibutyl tin laurate 0.03g, be warming up to 72～90 ℃ of reactions after 2 hours, add dimethylol propionic acid DMPA 7g reaction 1 hour, be cooled to then below 40 ℃, add 3-aminopropyl triethoxysilane 3g and stir 30min, adding triethylamine 8g makes and gives in the aggressiveness and salify, and adding acetone 47g reduces viscosity, add the 249g deionized water then and carry out emulsification under high speed shear, heating up at last steams acetone, obtains the milky water-based polyurethane adhesive of blueing light, its solid content: 41%, solid content is tested according to the GB/T2793-1995 standard; Viscosity is (being coated with-4 glasss, 25 ℃): 18s, and viscosity is tested according to the GB/T2794-1995 standard.
Claims (8)
1. water-based polyurethane adhesive, it is characterized in that: it is the synthetic gained of raw material by polyester polyol, Viscotrol C, isocyanic ester, hydrophilic chain extender, organosilane, salt forming agent, solvent, catalyzer, deionized water, wherein, the mixture of the pure and mild Viscotrol C of polyester polyols: isocyanic ester: hydrophilic chain extender: organosilane: the weight ratio of salt forming agent is (110～120): (35～45): (6～8): (2～4): (6～10), and the weight ratio between the pure and mild Viscotrol C of polyester polyols is 100: (10～20); Described organosilane is 3-aminopropyl triethoxysilane or 3-glycidyl ether oxygen base propyl trimethoxy silicane.
2. according to the described water-based polyurethane adhesive of claim 1, it is characterized in that: described polyester polyol is poly-hexanodioic acid-1,6-hexylene glycol, poly-hexanodioic acid-1,4-butyleneglycol neopentyl glycol, polycaprolactone glycol, polycarbonate-1, any of 6-hexylene glycol esterdiol.
3. according to the described water-based polyurethane adhesive of claim 1, it is characterized in that: described isocyanic ester be tolylene diisocyanate, ditan-4,4 '-in the vulcabond, hexamethylene diisocyanate, isophorone diisocyanate any.
4. according to the described water-based polyurethane adhesive of claim 1, it is characterized in that: described solvent is acetone, butanone or N-Methyl pyrrolidone;
5. according to the described water-based polyurethane adhesive of claim 1, it is characterized in that: described catalyzer is dibutyl tin laurate or stannous octoate.
6. according to the described water-based polyurethane adhesive of claim 1, it is characterized in that: described wetting ability chainextender is any in dimethylol propionic acid, the dimethylolpropionic acid.
7. according to the described water-based polyurethane adhesive of claim 1, it is characterized in that: described salt forming agent is triethylamine or sodium hydroxide.
8. the preparation method of the described water-based polyurethane adhesive of claim 1 is as follows:
The pure and mild Viscotrol C of polyester polyols is placed in the encloses container, and the weight ratio of the two is 100: 10～20, and vacuum-drying is 1 hour under 100 ℃～120 ℃ conditions, be cooled to 70 ℃ then, drip catalyzer after adding isocyanic ester, be warming up to 75～90 ℃ of reactions 2 hours, added wetting ability chainextender and solvent reaction 1 hour, be cooled to 40 ℃, add organosilane reaction 0.5 hour, in salt forming agent and after, be scattered in the deionized water fast, intensification steams solvent, thereby obtains target compound; Wherein, the mixture of the pure and mild Viscotrol C of polyester polyols: isocyanic ester: hydrophilic chain extender: organosilane: the weight ratio of salt forming agent is (110～120): (35～45): (6～8): (2～4): (6～10).
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| CN201010500510A CN101962524B (en) | 2010-09-29 | 2010-09-29 | Waterborne polyurethane adhesive and preparation method thereof |
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| CN201010500510A CN101962524B (en) | 2010-09-29 | 2010-09-29 | Waterborne polyurethane adhesive and preparation method thereof |
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| CN101962524B true CN101962524B (en) | 2011-12-21 |
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| CN104946177A (en) * | 2015-06-27 | 2015-09-30 | 广东远东高分子科技有限公司 | Water-based laminated adhesive and preparation method thereof |
| CN105153985A (en) * | 2015-07-10 | 2015-12-16 | 常州市禾香塑业有限公司 | Two-component polyurethane adhesive for soft packaging, and preparation method thereof |
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Family Cites Families (4)
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| CN101302416B (en) * | 2008-07-04 | 2011-12-14 | 中国科学院山西煤炭化学研究所 | Synthetic method of aqueous polyurethane adhesive |
| CN101429417A (en) * | 2008-12-08 | 2009-05-13 | 广州市科霖水性材料有限公司 | High-adhesive property watersoluble polyurethane adhesion agent and method of producing the same |
| CN101481451B (en) * | 2009-01-23 | 2011-06-08 | 华南理工大学 | High solid content latent curing polyurethane acroleic acid hybrid emulsion |
| CN101696262B (en) * | 2009-10-23 | 2011-11-02 | 华南理工大学 | Preparation method and application of modified polyurethane aqueous dispersions of polyisocyanate curing agents |
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