CN101182406A - Method for preparing multiple modified self-crosslinking aqueous polyurethane adhesive agent - Google Patents
Method for preparing multiple modified self-crosslinking aqueous polyurethane adhesive agent Download PDFInfo
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Abstract
The invention discloses a preparation method of self cross-linking water-based polyurethane adhesive of multiple modifications. Polyisocyanate and oligomer polyol are added into a reaction device for reaction; then chain extender is added for reaction to prepare polyurethane prepolymer; then polyurethane prepolymer modified by rosin and epoxy resin is added to prepare modified polyurethane prepolymer; finally water is added into the modified polyurethane prepolymer and a high-speed disperser is used for dispersion; neutralizer and cross-linker are added to prepare the self cross-linking water-based polyurethane dispersoid of multiple modifications; thickening agent and defoamer are added into the dispersoid to prepare the modified polyurethane adhesive. The adhesive prepared in the invention has the rapid drying, good water resistance and high bond strength; the adhesive can meet the bonding requirements of vehicles and a plurality of other materials; the invention has the advantages of simple operation, simple process, short production cycle, low cost of operation and easiness of promotion and application.
Description
Technical field
The present invention relates to can be used for the preparation method of a kind of modified water-soluble tackiness agent in fields such as automobile, family property, timber, wrapping material, fiber, leather, be specifically related to a kind of preparation method of multiple modified self-crosslinking aqueous polyurethane adhesive agent.
Background technology
Solvent-based adhesive is owing to contain a large amount of volatile organic compoundss (VOC), and environmental pollution is serious.The cry of public opinion of preserving the ecological environment grows with each passing day, and some developed countries have formulated fire codes and solvent rules in succession, have limited the use of solvent-based adhesive.Enhancing along with sound day by day and people's environmental consciousness of Environmental Protection in China rules, the environmental-protection type adhesive that quality is good, pollution-free, integrate with international standard will replace solvent-borne type, become the main product of synthetic adhesive, therefore developing environmental-protection type adhesive is the trend of domestic and international adhesives industries development.
At present, in China's aqueous adhesive, still based on " three urea formaldehydes " glue, polyvinyl acetate glue and acrylate resin glue etc." three urea formaldehydes " glue in use can produce irritating smell and toxic formaldehyde, and environment is polluted; The water tolerance of vinyl acetate resin glue, thermotolerance and adhesiveproperties are all relatively poor; The lower temperature resistance of acrylic size and cementability are not good.Water-based polyurethane adhesive, be called for short water-based PU tackiness agent, it has that resistance to low temperature is good, bonding strength is higher, snappiness good, do not fire, nontoxic, free from environmental pollution, save advantage such as the energy, and its viscosity does not have notable difference with the change of polymericular weight, can be with molecular-weight adjusting to desirable higher level, improve its cohesive strength, have vast potential for future development.
Yet home-made water-based polyurethane adhesive performance can't satisfy the needs of multiple material, show that mainly cohesive strength is low, rate of drying is slow, high thermal resistance is relatively poor, theoretical still applied research all lags behind very much, and output is very little, kind is single, does not satisfy the domestic market far away to the growing demand of this high-quality environment protective type tackiness agent.Therefore how improving its bonding strength, improve rate of drying, make its variety series, so that be fit to multi-purpose needs, is the problem that current scholar's research polyurethane adhesive will solve.
For improving the Application Areas of aqueous polyurethane and glue film performance thereof, expansion aqueous polyurethane, need urethane is carried out modification.Resins, epoxy has advantages such as high-modulus, high strength and chemical resistance are good, can participate in the reaction of aqueous polyurethane directly, forms reticulated structure.Mechanical property, water tolerance and the solvent resistance etc. of aqueous polyurethane glued membrane have been improved.The adding of Gum Rosin has reduced the cost of tackiness agent, has improved the first sticking strong of tackiness agent.
This patent is introduced Resins, epoxy and rosin in the water-based polyurethane adhesive modification, obtain Resins, epoxy and Abietyl modified water-based polyurethane adhesive, improved the performance of aqueous polyurethane greatly, this tackiness agent with water as solvent, help environmental protection, its excellent performance has vast potential for future development in fields such as automobile, family property, timber, wrapping material, fiber, leathers.
Summary of the invention
The object of the invention is to work out a kind of preparation method of multiple modified self-crosslinking aqueous polyurethane adhesive agent, and this preparation method's cohesive strength height, rate of drying are fast, water-tolerant, the preparation method is simple, cost is low.
For achieving the above object, the present invention has taked following technical scheme:
The preparation method of multiple modified self-crosslinking aqueous polyurethane adhesive agent of the present invention comprises the steps:
(1) preparation of base polyurethane prepolymer for use as: in the conversion unit that agitator, thermometer, prolong are housed, add polyisocyanates and oligomer polyol, react 2～3h down at 60～80 ℃, add chainextender then, reaction 2～5h obtains base polyurethane prepolymer for use as; The ratio of polyisocyanates and oligomer polyol amount of substance is: 3.1～1.3: 1; The mass ratio of polyisocyanates and chainextender is 10: 1.5～2.7
(2) base polyurethane prepolymer for use as of modification is synthetic: under 60～80 ℃ Gum Rosin and Resins, epoxy are added to base polyurethane prepolymer for use as reaction 3～5h that step (1) obtains simultaneously, obtain the base polyurethane prepolymer for use as of modification, wherein, Gum Rosin: polyisocyanates: the mass ratio of Resins, epoxy is 2～4: 20: 1～2;
(3) modified aqueous polyurethane dispersoid is synthetic: add water in the modified polyurethane prepolymer that step (2) obtains, disperse with the speed of 2500～4000rpm/min with high speed dispersor, add neutralizing agent and linking agent at 35 ℃～40 ℃ emulsification 10～30min, obtain modified aqueous adhesion agent of polyurethane; Described degree of neutralization is 85～100%, add emulsifying water after, the solid content that makes modified aqueous polyurethane dispersoid is 32～40%, described linking agent quality account for modified polyurethane prepolymer, water and neutralizing agent total mass 0.1%～0.25%;
(4) modified aqueous adhesion agent of polyurethane is joined glue: add thickening material and defoamer in the modified aqueous polyurethane dispersoid that step (3) obtains, get the modified waterborne polyurethane tackiness agent; Described thickening material: modified aqueous polyurethane dispersoid: the mass ratio of defoamer is 0.1～0.5: 100: 0.05～0.3.
The polyisocyanates of described step (1) be tolylene diisocyanate (TDI), hexamethylene diisocyanate (HDI), isophorone diisocyanate (IPDI), ditan-4,4 '-vulcabond (MDI), poly methylene poly phenyl poly isocyanate (PAPI), xylylene diisocyanate (XDI).
The oligomer polyol polyester polyol of described step (1), as: polyethylene glycol adipate glycol, poly-hexanodioic acid glycol ether esterdiol, poly-hexanodioic acid-1,4-butanediol ester glycol, glycol ether esterdiol, polycarbonate diol, polycaprolactone glycol; Polyether glycol, as: polyoxypropyleneglycol, polyoxytrimethylene triol, polytetrahydrofuran diol, other oligomer polyol are as polybutadiene diol.
The wetting ability chainextender of described step (1) is dihydroxymethyl acetate, dimethylol propionic acid, dimethylolpropionic acid.
The Gum Rosin of described step (2) is ester gum, pentalyn or rosin MALEIC ANHYDRIDE ester.
The Resins, epoxy of described step (2) is Resins, epoxy E-16, Resins, epoxy E-20, epoxy resin E-44 or Resins, epoxy E-51.
The neutralizing agent of described step (3) is triethylamine or trolamine.
The linking agent of described step (3) is quadrol or butanediamine.
The thickening material of described step (4) is a polyacrylic bases thickening material, and model is WZA-120, and WZA-121 it be; Defoamer is the silicone oil defoamer, and model is ATF-1, ATF-2.
With respect to prior art, the present invention has following advantage:
(1) Resins, epoxy and Gum Rosin are introduced in the modification of polyurethane adhesive, improved the degree of crosslinking of water-based polyurethane adhesive, cohesive strength and initial bonding strength, by the epoxy group(ing) of Resins, epoxy and the NCO radical reaction of hydroxyl and vulcabond, adopt chemical process Resins, epoxy to be incorporated in the molecular structure of urethane, formation has the aqueous polyurethane of crosslinking structure, high film amount with Resins, epoxy, the advantages of advantages such as high strength and chemical resistant properties are good and urethane resin is got up, add Gum Rosin, reduced the cost of synthetic tackiness agent, improved the initial bonding strength of tackiness agent, made the polyurethane adhesive of synthetic modification have Resins, epoxy, the performance of Gum Rosin and urethane.Make that prepared tackiness agent rate of drying is fast, water-tolerant, cohesive strength height, can satisfy the demand of automobile and other multiple material adhesives;
(2) by latex particle design, synthetic polymer emulsion.Whole process using self-emulsification carries out letex polymerization need not add emulsifying agent in emulsion polymerization process, eliminated the influence of low molecule emulsifying agent to glued membrane;
(3) the inventive method is easy to operate, technology is simple, with short production cycle, process cost is low, is easy to promotion and application;
(4) the multiple modified self-crosslinking aqueous polyurethane adhesive agent of the present invention's preparation, its performance is suitable with the performance of external similar water-based polyurethane adhesive, and cost is more much lower than external sample.
Embodiment
For better understanding the present invention, the present invention is done detailed description further below in conjunction with embodiment.But the scope of protection of present invention is not limited to the scope that embodiment represents.
Embodiment 1
With 100g HDI, 384g molecular weight be 2000 polyoxypropyleneglycol at 80 ℃ of reaction 3h, add the 15g dimethylol propionic acid then, reaction 2h gets base polyurethane prepolymer for use as; 10g ester gum and 5g E-20 Resins, epoxy are joined in this performed polymer, with prepolymer reaction 3h, get the base polyurethane prepolymer for use as of ester gum and epoxy resin modification, be cooled to 35 ℃ then, add in the 9.6g triethylamine at last and 10min, under the 2500r/min rotating speed, add 1115g water, disperse 10min, add the 1.7g ethylene diamine linker again, get modified aqueous polyurethane dispersoid.
Get the above-mentioned modified waterborne polyurethane dispersion of 100g, add 0.1g thickening material WZA-120 in this dispersion, 0.1g defoamer ATF-1 obtains the modified waterborne polyurethane tackiness agent.
These product performance relatively see Table 1 with external certain company's product performance.
As shown in table 1, the product of present embodiment preparation is rotary viscosity when thickening not, the glued membrane tensile strength, 180 ° of stripping strengths of tackiness agent and external product are basic identical, but because the present invention introduces rosin and Resins, epoxy in the water-based polyurethane adhesive modification simultaneously, high film amount with Resins, epoxy, the good advantage of high strength and chemical resistant properties, and the rosiny initial bonding strength is strong, low cost and other advantages combines, adopt domestic starting material simultaneously mostly, can satisfy the demand of the multiple interior material of automobile, and total cost is more much lower than external like product, preparation technology is simple, be easy to promotion and application.
Table 1
| Quality index | External certain company's product | The product of present embodiment |
| Solid content, % | 32 | 32 |
| Rotary viscosity (not thickening) mPa.s | 30 | 28 |
| The glued membrane tensile strength, MPa | 10 | 9.8 |
| 180 ° of stripping strengths (glued board-leatheroid): N.mm -1 | 3.0 | 3.1 |
Embodiment 2
With 100g TDI, the polyethylene glycol adipate glycol of 370g, join be equipped with thermometer, agitator and and the dry reaction equipment of condenser in, react 2.5h down at 70 ℃ and add 27g dihydroxymethyl acetate then, reaction 2h, reaction process apparent viscosity size is added acetone, obtains base polyurethane prepolymer for use as; 20g rosin MALEIC ANHYDRIDE ester and 10g E-44 Resins, epoxy are joined in this performed polymer, reaction 2.5h, get the base polyurethane prepolymer for use as of ester gum and epoxy resin modification, be cooled to 40 ℃ then, add the 32.7g trolamine, in and 15min, add 850g water at the 4000r/min rotating speed, disperse 30min, add 3.6g butanediamine linking agent again, get modified aqueous polyurethane dispersoid.
The above-mentioned modified waterborne polyurethane dispersion of 100g adds 0.5g thickening material WZA-120 in this dispersion, 0.3g defoamer ATF-2 obtains the modified waterborne polyurethane tackiness agent.
Get the polyurethane adhesive of modification.These product performance are as shown in table 2 with external certain company's product performance comparable situation.
Table 2
| Quality index | External certain company's product | The product of present embodiment |
| Solid content, % | 32 | 33 |
| Rotary viscosity (not thickening) | 30 | 33 |
| The glued membrane tensile strength, MPa | 10 | 10.1 |
| 180 ° of stripping strengths (glued board-leatheroid): N.m -1 | 3.0 | 3.2 |
As shown in table 2, the product of present embodiment preparation is rotary viscosity when thickening not, the glued membrane tensile strength, 180 ° of stripping strengths of tackiness agent are a little more than external product, but because the present invention introduces rosin and Resins, epoxy in the water-based polyurethane adhesive modification, high film amount with Resins, epoxy, high strength and the chemically-resistant advantage of acting charitably, the rosin initial bonding strength is good, the advantages of low cost and other advantages and urethane resin is got up, simultaneously adopt domestic starting material to synthesize a kind of high-performance tackiness agent fully, can satisfy the demand of the multiple interior material of automobile, and present embodiment product preparation cost is more much lower than abroad, its technology is simple, be easy to promotion and application.
Embodiment 3
100g IPDI and 349g polycaprolactone glycol add the 20g dimethylolpropionic acid then at 70 ℃ of reaction 2.5h, and reaction 2h gets base polyurethane prepolymer for use as; 15g rosin MALEIC ANHYDRIDE ester and 8g E-51 Resins, epoxy are joined in this performed polymer, with prepolymer reaction 2.5h, get Resins, epoxy and Abietyl modified base polyurethane prepolymer for use as, be cooled to 38 ℃ again, add in the 12.5g triethylamine and 10min, add 938g water-dispersion 15min at the 2500r/min rotating speed, add 2.9g linking agent quadrol again, get modified aqueous polyurethane dispersoid.
Add 0.3g thickening material WZA-121 in the above-mentioned modified aqueous polyurethane of 100g, 0.2g defoamer ATF-2 obtains the modified waterborne polyurethane tackiness agent.These product performance are as shown in table 3 with external certain company's product performance comparable situation.
Table 3
| Quality index | External certain company's product | The product of present embodiment |
| Solid content, % | 32 | 34 |
| Rotary viscosity (not thickening) | 30 | 33 |
| The glued membrane tensile strength, MPa | 10 | 10.1 |
| 180 ° of stripping strengths (glued board-leatheroid): N.m -1 | 3.0 | 3.2 |
As shown in table 3, the product of present embodiment preparation is rotary viscosity when thickening not, the glued membrane tensile strength, 180 ° of stripping strengths of tackiness agent and external product are basic identical, but because the present invention introduces Gum Rosin and Resins, epoxy in the water-based polyurethane adhesive modification, high film amount with Resins, epoxy, the advantages of advantages such as high strength and chemical resistant properties are good and Gum Rosin and urethane resin is got up, simultaneously adopt domestic starting material to synthesize a kind of high-performance tackiness agent fully, can satisfy the demand of the multiple interior material of automobile, and present embodiment product preparation cost is more much lower than abroad, its technology is simple, be easy to promotion and application.
Embodiment 4
70 ℃ of reactions of the poly-polybutadiene diol of 100g XDI and 418g 2.1h adds the 18g dimethylol propionic acid then, and reaction 2.5h gets base polyurethane prepolymer for use as; 13g pentalyn and 6g E-16 Resins, epoxy are joined in this performed polymer, with prepolymer reaction 2.5h, get Resins, epoxy and Abietyl modified base polyurethane prepolymer for use as, be cooled to 38 ℃ again, add in the 18.9g trolamine and 10min, add 907g water-dispersion 17min at the 2500r/min rotating speed, add 2.2g butanediamine linking agent again, get modified aqueous polyurethane dispersoid.
Add 0.2g thickening material WZA-121 in the above-mentioned modified aqueous polyurethane dispersoid of 100g, 0.1g defoamer ATF-1 obtains the modified waterborne polyurethane tackiness agent.These product performance are as shown in table 4 with external certain company's product performance comparable situation.
Table 4
| Quality index | External certain company's product | The product of present embodiment |
| Solid content, % | 32 | 31 |
| Rotary viscosity (not thickening) | 30 | 35 |
| The glued membrane tensile strength, MPa | 10 | 9.5 |
| 180 ° of stripping strengths (glued board-leatheroid): N.m -1 | 3.0 | 2.8 |
As shown in table 4, the product of present embodiment preparation is rotary viscosity when thickening not, the glued membrane tensile strength, 180 ° of stripping strengths of tackiness agent and external product are basic identical, but because the present invention introduces Gum Rosin and Resins, epoxy in the water-based polyurethane adhesive modification, high film amount with Resins, epoxy, the advantages of advantages such as high strength and chemical resistant properties are good and Gum Rosin and urethane resin is got up, simultaneously adopt domestic starting material to synthesize a kind of high-performance tackiness agent fully, can satisfy the demand of the multiple interior material of automobile, and present embodiment product preparation cost is more much lower than abroad, its technology is simple, be easy to promotion and application.
Claims (10)
1. the preparation method of a multiple modified self-crosslinking aqueous polyurethane adhesive agent comprises the steps:
(1) preparation of base polyurethane prepolymer for use as: add polyisocyanates and oligomer polyol in conversion unit, react 2～3h down at 60～80 ℃, add then, reaction 2～5h obtains base polyurethane prepolymer for use as; The ratio of polyisocyanates and oligomer polyol amount of substance is: 3.1～1.3: 1; The mass ratio of polyisocyanates and chainextender is 10: 1.5～2.7;
(2) base polyurethane prepolymer for use as of modification is synthetic: under 60～80 ℃ Gum Rosin and Resins, epoxy is added to simultaneously in the base polyurethane prepolymer for use as that step (1) obtains and reacts 3～5h, obtain the base polyurethane prepolymer for use as of modification, wherein, Gum Rosin: polyisocyanates: the mass ratio of Resins, epoxy is 2～4: 20: 1～2;
(3) modified aqueous polyurethane dispersoid is synthetic: add water in the modified polyurethane prepolymer that step (2) obtains, disperse with the speed of 2500～4000rpm/min with high speed dispersor, add neutralizing agent and linking agent at 35 ℃～40 ℃ emulsification 10～30min, obtain modified aqueous polyurethane dispersoid; The degree of neutralization of neutralizing agent is 85～100%, and the quality of described water is that to make the solid content of this modified aqueous polyurethane dispersoid be 32～40%, the quality of described linking agent account for modified polyurethane prepolymer, water, neutralizing agent total mass 0.1%～0.25%;
(4) modified aqueous adhesion agent of polyurethane is joined glue: add thickening material and defoamer in the modified aqueous polyurethane dispersoid that step (3) obtains, obtain the modified waterborne polyurethane tackiness agent; Described thickening material: modified aqueous polyurethane dispersoid: the mass ratio of defoamer is 0.1～0.5: 100: 0.05～0.3.
2. preparation method according to claim 1, the polyisocyanates that it is characterized in that described step (1) be tolylene diisocyanate, hexamethylene diisocyanate, isophorone diisocyanate, ditan-4,4 '-vulcabond, poly methylene poly phenyl poly isocyanate or xylylene diisocyanate.
3. preparation method according to claim 1 is characterized in that, the oligomer polyol of described step (1) comprises polyester polyol or polyether glycol.
4. preparation method according to claim 3, it is characterized in that, the oligomer polyol of described step (1) also comprises polybutadiene diol, described polyester polyol comprises polyethylene glycol adipate glycol, poly-hexanodioic acid glycol ether esterdiol, poly-hexanodioic acid-1,4-butanediol ester glycol, glycol ether esterdiol, polycarbonate diol or polycaprolactone glycol; Described polyether glycol comprises polyoxypropyleneglycol, polyoxytrimethylene triol, polytetrahydrofuran diol or tetrahydrofuran (THF)-propylene oxide copolymerization glycol.
5. preparation method according to claim 1, the wetting ability chainextender that it is characterized in that described step (1) is dihydroxymethyl acetate, dimethylol propionic acid or dimethylolpropionic acid.
6. preparation method according to claim 1, the Gum Rosin that it is characterized in that described step (2) is ester gum, pentalyn or rosin MALEIC ANHYDRIDE ester.
7. preparation method according to claim 1, the Resins, epoxy that it is characterized in that described step (2) is Resins, epoxy E-16, Resins, epoxy E-20, epoxy resin E-44 or Resins, epoxy E-51.
8. preparation method according to claim 1 is characterized in that the neutralizing agent triethylamine or the trolamine of described step (3).
9. preparation method according to claim 1, the linking agent that it is characterized in that described step (3) is quadrol or butanediamine.
10. preparation method according to claim 1, the thickening material that it is characterized in that described step (4) is a polyacrylic bases thickening material, comprises that model is the thickening material of WZA-120 or WZA-121; Defoamer is the silicone oil defoamer, comprises that model is the defoamer of ATF-1 or ATF-2.
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