CN104673172A - Thermo-sensitive type waterborne polyurethane adhesive and preparation method of thermo-sensitive type waterborne polyurethane adhesive - Google Patents
Thermo-sensitive type waterborne polyurethane adhesive and preparation method of thermo-sensitive type waterborne polyurethane adhesive Download PDFInfo
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- CN104673172A CN104673172A CN201510041516.5A CN201510041516A CN104673172A CN 104673172 A CN104673172 A CN 104673172A CN 201510041516 A CN201510041516 A CN 201510041516A CN 104673172 A CN104673172 A CN 104673172A
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Abstract
The invention relates to a thermo-sensitive type waterborne polyurethane adhesive and a preparation method of the thermo-sensitive type waterborne polyurethane adhesive, and is mainly used in the field of electronic device splicing and assembling. Crystal type polyester dihydric alcohol is adopted by the thermo-sensitive type waterborne polyurethane adhesive to react with aliphatic isocyanate, and hydrophilic components and epoxy resin are introduced so as to obtain the thermo-sensitive type waterborne polyurethane adhesive. The adhesive has a switch temperature in an application temperature range, the bonding strength of the adhesive manifests a temperature response property before and after the switch temperature, and the adhesive has a good adhesive property to an electronic device when below the switch temperature; when the adhesive is heated above the switch temperature, the bonding strength is reduced obviously, so as to make the electronic device capable of being disassembled easily. The thermo-sensitive type waterborne polyurethane adhesive can bring great convenience to the disassembly, assembly, replacement and recycle of the electronic device (particularly for a precise and valuable electronic device). Therefore, the thermo-sensitive type waterborne polyurethane adhesive disclosed by the invention has a wide application prospect in the field of the electronic device splicing and assembling.
Description
Technical field
The present invention relates to a kind of temperature sensitive type water-based polyurethane adhesive for the bonding assembling of electron device and preparation method thereof particularly, belongs to adhesive area.
Background technology
Along with environmental regulation requires increasingly strict, traditional solvent-borne tackiness agent just gradually by aqueous adhesive substitute, the development and application research of aqueous, environmental protective tackiness agent gets more and more, and the market demand potential is huge.Aqueous polyurethane is dispersion medium with water, have nontoxic, do not fire, the advantage such as pollution-free, and have the constitutional features of polyurethane material and excellent performance concurrently, in field extensive application such as coating, synthetic leather, tackiness agent.Water-based polyurethane adhesive has the plurality of advantages such as adhesiveproperties excellence, the easy adjusted design of structure properties, Application Areas be wide, has become the study hotspot in aqueous adhesive field.
Along with the high speed development of information, communication industry, the sharp increase of electron device demand.Many devices need temporary bonding in the course of processing, in post-treatment process, need dismounting, re-assemble, need in use procedure to change, need when scrapping process to recycle, and traditional glue paste is firmly difficult to dismounting due to bonding, force the fragile electron device of dismounting.From the bonding assembling angle of electron device, particularly realized by stripping feature easy under good bonding under temperature sensitive tackiness agent low temperature and high temperature electron device dismounting, re-assemble, replacing or recycling research there is not been reported.The cementability that the present invention utilizes water-based polyurethane adhesive good and crystallinity, design a kind of temperature sensitive type water-based polyurethane adhesive, makes it for the bonding assembling of electron device.Can according to application demand, the molecular structure optimization of the Soft segment microcell formed by crystalline polyester and isocyanic ester, design has the temperature sensitive type water-based polyurethane adhesive of respective switch temperature.Its bonding strength shows temperature response characteristics before and after switch temperature, below switch temperature, to electron device, there is good cementability, when related electronic devices removed by needs, by being heated to more than switch temperature, bonding strength obviously reduces, and electron device can be removed easily.This can bring great convenience to the dismounting of electron device, assembling, replacing, recycling.
Because electron device mostly is metallic substance, thus tackiness agent used must have good cementability to metal base.The present invention utilizes epoxy resin to the superior adhesion of metal base, is incorporated into by epoxy resin in polyurethane molecular structure, improves the adhesiveproperties of temperature sensitive type water-based polyurethane adhesive to metal base, thus realizes the good bonding to electron device.Meanwhile, more than switch temperature, although temperature sensitive type water-based polyurethane adhesive has obvious decline to electron device bonding strength, due to the effect of epoxy resin, still there is certain bonding strength, automatic degumming phenomenon can not be caused.
Summary of the invention
The object of the invention is for prior art not enough, a kind of temperature sensitive type water-based polyurethane adhesive is provided.
Another object of the present invention is to provide a kind of preparation method of above-mentioned temperature sensitive type water-based polyurethane adhesive.
A kind of temperature sensitive type water-based polyurethane adhesive provided by the invention, is characterized in that, described temperature sensitive type waterborne polyester tackiness agent is reacted by crystalline polyester dibasic alcohol and aliphatic isocyanates, and introduces hydrophilic component, epoxy resin, through emulsification gained.By salvage method, crystalline texture reasonable in design, obtain required Soft segment microcell and soft or hard section micro phase separation structure, described temperature sensitive type water-based polyurethane adhesive is made to have obvious temperature-sensing property, a switch temperature (Switch Temperature, Ts) is had in application of temperature interval.
The preparation method of above-mentioned temperature sensitive type water-based polyurethane adhesive provided by the invention, is characterized in that having operation steps as follows:
(1) crystalline polyester dibasic alcohol 50-100 part, aliphatic diisocyanate 5-10 part are added reaction vessel, under Keep agitation and nitrogen atmosphere protection, be warming up to 80-90 DEG C of reaction 2-3 hour;
(2) above-mentioned reaction system is cooled to 50-60 DEG C, after the dilution of acetone solvent 40-60 part, add hydrophilic chain extender 3-6 part, epoxy resin 5-15 part, aliphatic diisocyanate 5-10 part, holding temperature 50-60 DEG C of reaction 4-6 hour, obtains with the base polyurethane prepolymer for use as of-NCO end-blocking;
(3) in the base polyurethane prepolymer for use as of above-mentioned-NCO end-blocking, triethylamine 2.5-5 part is added, stir 30 minutes, then under high speed shear condition, add deionized water and chainextender quadrol 0.5-1.5 part, stir removed under reduced pressure acetone after 30 minutes, obtain stable polyaminoester emulsion, be described temperature sensitive type water-based polyurethane adhesive;
Above-mentioned raw materials used number is parts by weight.
Described crystalline polyester dibasic alcohol is at least one in the polybutylene glyool adipate of number-average molecular weight 2000-10000, polyhexamethylene adipate glycol, polycaprolactone glycol, polycarbonate diol.
Described aliphatic diisocyanate be isophorone diisocyanate IPDI, hexamethylene diisocyanate HDI,
4,4'-dicyclohexyl methane diisocyanate H
12at least one in MDI.
Described hydrophilic chain extender is
2,2-dimethylol propionic acid DMPA,
2,2at least one in-dimethylolpropionic acid DMBA.
Described epoxy resin is at least one in epoxy resin E44, epoxy resin E51.
Described temperature sensitive type water-based polyurethane adhesive may be used for the bonding assembling of electron device, has a switch temperature Ts in application of temperature interval, and its bonding strength shows temperature response characteristics before and after switch temperature; When application of temperature is lower than switch temperature, this glue paste has good cementability to electron device, and more than switch temperature, the bonding strength of electron device is obviously declined, electron device can be removed easily, be conducive to the re-assemblying of electron device, recovery and reuse.
The present invention compared with prior art, has the following advantages:
(1) the present invention is by crystalline polyester raw material and the design of special micro phase separation structure, prepare temperature sensitive type water-based polyurethane adhesive, be applicable to the bonding of electron device, and take full advantage of the temperature response characteristics of temperature sensitive type urethane, there is good cementability lower than during switch temperature to electron device, and decline obviously in the above bonding strength of switch temperature, be conducive to the dismounting of electron device;
(2) the present invention has taken into full account the singularity of electron device, the epoxy resin with good bonding performance is utilized to carry out modification, improve temperature sensitive type water-based polyurethane adhesive to metal and nonmetal between bonding strength, meet the actual demand that electronic components is bonding, simultaneously in conjunction with temperature-sensing property, make the dismounting of electron device, re-assemble and recycling more convenient;
(3) the present invention utilizes the potential reaction of the epoxy group(ing) of epoxy resin and the hydrophilic radical carboxyl of temperature sensitive type water-based polyurethane adhesive, can the negatively charged ion of shielding material, reduce the wetting ability of material, improve the insulativity of material, this use for electron device provides safety control.
Accompanying drawing explanation
Figure 1 shows that the result of testing the switch temperature of glued membrane with differential scanning calorimeter (DSC).
NETZSCH 200PC type differential scanning calorimeter (DSC) is adopted to test the switch temperature of glued membrane, heat-up rate 5 DEG C/min.
Embodiment
Below by embodiment, the present invention is specifically described; what be necessary to herein means out is that following examples are just used to further illustrate the present invention; limiting the scope of the invention can not be interpreted as; the person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of the invention described above, still belongs to protection scope of the present invention.
Embodiment 1
(1) 100 parts of polycaprolactone diols (number-average molecular weight 10000), 5 parts of HDI are added reaction vessel, under Keep agitation and nitrogen atmosphere protection, be warming up to 80-90 DEG C of reaction 2 hours;
(2) be cooled to 50-60 DEG C, add 6 parts of hydrophilic chain extender DMPA, 5 parts of epoxy resin E51,10 parts of IPDI and 60 part acetone, holding temperature 50-60 DEG C is reacted 6 hours, obtains with the base polyurethane prepolymer for use as of-NCO end-blocking;
(3) in the base polyurethane prepolymer for use as of above-mentioned-NCO end-blocking, 5 parts of triethylamines are added, stir 30 minutes, then under high speed shear condition, add deionized water and 0.5 part of chainextender quadrol, stir removed under reduced pressure acetone after 30 minutes, obtain stable polyaminoester emulsion, moisturizing regulates solid content to be 30%, obtains temperature sensitive type water-based polyurethane adhesive.
Embodiment 2
(1) 50 parts of PCDL (number-average molecular weight 2000), 7 parts of HDI are added reaction vessel, under Keep agitation and nitrogen atmosphere protection, be warming up to 80-90 DEG C of reaction 3 hours;
(2) be cooled to 50-60 DEG C, add 3 parts of hydrophilic chain extender DMPA, 10 parts of epoxy resin E44,7 parts of IPDI and 40 part acetone, holding temperature 50-60 DEG C is reacted 5 hours, obtains with the base polyurethane prepolymer for use as of-NCO end-blocking;
(3) in the base polyurethane prepolymer for use as of above-mentioned-NCO end-blocking, 2.5 parts of triethylamines are added, stir 30 minutes, then under high speed shear condition, add deionized water and 0.5 part of chainextender quadrol, stir removed under reduced pressure acetone after 30 minutes, obtain stable polyaminoester emulsion, moisturizing regulates solid content to be 30%, obtains temperature sensitive type water-based polyurethane adhesive.
Embodiment 3
(1) 70 parts of poly adipate succinic acid ester dibasic alcohol (number-average molecular weight 4000), 10 parts of HDI are added reaction vessel, under Keep agitation and nitrogen atmosphere protection, be warming up to 80-90 DEG C of reaction 2 hours;
(2) be cooled to 50-60 DEG C, add 4 parts of hydrophilic chain extender DMBA, 15 parts of epoxy resin E51,5 parts of H
12mDI and 50 part acetone, holding temperature 50-60 DEG C is reacted 4 hours, obtains with the base polyurethane prepolymer for use as of-NCO end-blocking;
(3) in the base polyurethane prepolymer for use as of above-mentioned-NCO end-blocking, 3 parts of triethylamines are added, stir 30 minutes, then under high speed shear condition, add deionized water and 1.5 parts of chainextender quadrols, stir removed under reduced pressure acetone after 30 minutes, obtain stable polyaminoester emulsion, moisturizing regulates solid content to be 30%, obtains temperature sensitive type water-based polyurethane adhesive.
Embodiment 4
(1) 60 parts of poly-hexanodioic acid hexylene glycol ester dibasic alcohol (number-average molecular weight 3000), 10 parts of HDI are added reaction vessel, under Keep agitation and nitrogen atmosphere protection, be warming up to 80-90 DEG C of reaction 2 hours;
(2) be cooled to 50-60 DEG C, add 5 parts of hydrophilic chain extender DMBA, 10 parts of epoxy resin E51,7 parts of H
12mDI and 45 part acetone, holding temperature 50-60 DEG C is reacted 6 hours, obtains with the base polyurethane prepolymer for use as of-NCO end-blocking;
(3) in the base polyurethane prepolymer for use as of above-mentioned-NCO end-blocking, 3.8 parts of triethylamines are added, stir 30 minutes, then under high speed shear condition, add deionized water and 1.2 parts of chainextender quadrols, stir removed under reduced pressure acetone after 30 minutes, obtain stable polyaminoester emulsion, moisturizing regulates solid content to be 30%, obtains temperature sensitive type water-based polyurethane adhesive.
Normal temperature peel strength test:
Cutting 25mm × 100mm batten on thickness 0.2mm aluminium flake, brushing gained temperature sensitive type water-based polyurethane adhesive, guarantee that brushing evenly, not piles glue, after room temperature places 10 minutes, be placed in 80 DEG C of baking ovens 5 minutes, fit while hot, and apply 0.2MPa pressure and keep 10 seconds, room temperature tests T-shaped normal temperature stripping strength after regulating 24 hours.Concrete data are as follows.
Hot peel strength test:
Laminating batten after above-mentioned room temperature is regulated 24 hours is placed in 80 DEG C of baking ovens 10 minutes, tests T-shaped hot stripping strength while hot.
Switch temperature is tested:
Tested the switch temperature of glued membrane by NETZSCH 200PC type differential scanning calorimeter (DSC), heat-up rate 5 DEG C/min, result as shown in drawings.
Each embodiment relevant test data is as shown in the table.
According to data in table, the various embodiments described above stripping strength is at normal temperatures all higher, and adhesiveproperties is good; After pyroprocessing, peel off while hot, then stripping strength is obviously lower, due to the modifying function of epoxy resin, still has certain bonding strength, there will not be automatic degumming phenomenon.Visible, gained temperature sensitive type water-based polyurethane adhesive can realize the good bonding to electron device, and when being heated to more than switch temperature, stripping strength declines obviously, is conducive to the easy removal of electron device.
Claims (6)
1. temperature sensitive type water-based polyurethane adhesive and preparation method thereof, is characterized in that concrete operation step is as follows:
(1) crystalline polyester dibasic alcohol 50-100 part, aliphatic diisocyanate 5-10 part are added reaction vessel, under Keep agitation and nitrogen atmosphere protection, be warming up to 80-90 DEG C of reaction 2-3 hour;
(2) above-mentioned reaction system is cooled to 50-60 DEG C, after the dilution of acetone solvent 40-60 part, add hydrophilic chain extender 3-6 part, epoxy resin 5-15 part, aliphatic diisocyanate 5-10 part, holding temperature 50-60 DEG C of reaction 4-6 hour, obtains with the base polyurethane prepolymer for use as of-NCO end-blocking;
(3) in the base polyurethane prepolymer for use as of above-mentioned-NCO end-blocking, triethylamine 2.5-5 part is added, stir 30 minutes, then under high speed shear condition, add deionized water and chainextender quadrol 0.5-1.5 part, stir removed under reduced pressure acetone after 30 minutes, obtain stable polyaminoester emulsion, be described temperature sensitive type water-based polyurethane adhesive;
Above-mentioned raw materials used number is parts by weight.
2. a kind of temperature sensitive type water-based polyurethane adhesive according to claim 1 and preparation method thereof, it is characterized in that, described crystalline polyester dibasic alcohol is at least one in the polybutylene glyool adipate of number-average molecular weight 2000-10000, polyhexamethylene adipate glycol, polycaprolactone glycol, polycarbonate diol.
3. a kind of temperature sensitive type water-based polyurethane adhesive according to claim 1 and preparation method thereof, is characterized in that, described aliphatic diisocyanate be isophorone diisocyanate IPDI, hexamethylene diisocyanate HDI,
4,4'-dicyclohexyl methane diisocyanate H
12at least one in MDI.
4. a kind of temperature sensitive type water-based polyurethane adhesive according to claim 1 and preparation method thereof, it is characterized in that, described hydrophilic chain extender is
2,2-dimethylol propionic acid DMPA,
2,2at least one in-dimethylolpropionic acid DMBA.
5. a kind of temperature sensitive type water-based polyurethane adhesive according to claim 1 and preparation method thereof, is characterized in that, described epoxy resin is at least one in epoxy resin E-44, epoxy resin E-51.
6. a kind of temperature sensitive type water-based polyurethane adhesive according to claim 1 and preparation method thereof, it is characterized in that, described temperature sensitive type water-based polyurethane adhesive may be used for the bonding assembling of electron device, in application of temperature interval, have a switch temperature Ts, its bonding strength shows temperature response characteristics before and after switch temperature; When application of temperature is lower than switch temperature, this glue paste has good cementability to electron device, and more than switch temperature, the bonding strength of electron device is obviously declined, electron device can be removed easily, be conducive to the re-assemblying of electron device, recovery and reuse.
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| CN105441009A (en) * | 2015-12-30 | 2016-03-30 | 太仓卡斯特姆新材料有限公司 | Dual-responsiveness compound adhesive |
| CN106147686A (en) * | 2016-07-05 | 2016-11-23 | 上海英诺威新材料科技有限公司 | Environment-friendly water-based polyurethane plastics-absorbing oil |
| CN106753163A (en) * | 2016-12-27 | 2017-05-31 | 丽水学院 | A kind of footwear kind of flocked leather can be molded aqueous polyurethane flock glue and preparation method thereof |
| CN108068176A (en) * | 2017-12-26 | 2018-05-25 | 芜湖市长江起重设备制造有限公司 | A kind of preparation method of high temperature resistant polycarbonate waterborne polyurethane base rubber plywood |
| CN109535384A (en) * | 2018-11-19 | 2019-03-29 | 山东天庆科技发展有限公司 | A kind of aqueous polyurethane emulsion and preparation method thereof and vacuum plastic-absorption |
| CN110511349A (en) * | 2019-07-30 | 2019-11-29 | 湖北大学 | A kind of preparation method of new hyperbranched type temperature sensitive type aqueous polyurethane |
| CN112592689A (en) * | 2021-02-26 | 2021-04-02 | 山东万圣博化工有限公司 | Electronic adhesive and preparation method thereof |
| CN116265556A (en) * | 2021-12-16 | 2023-06-20 | 万华化学（北京）有限公司 | Moisture-curing polyurethane hot melt adhesive and preparation method and application thereof |
| WO2024028308A1 (en) | 2022-08-03 | 2024-02-08 | Covestro Deutschland Ag | Adhesive composition, the preparation method and use thereof |
| EP4339216A1 (en) | 2022-09-13 | 2024-03-20 | Covestro Deutschland AG | Adhesive composition, the preparation method and use thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105441009A (en) * | 2015-12-30 | 2016-03-30 | 太仓卡斯特姆新材料有限公司 | Dual-responsiveness compound adhesive |
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| CN106753163A (en) * | 2016-12-27 | 2017-05-31 | 丽水学院 | A kind of footwear kind of flocked leather can be molded aqueous polyurethane flock glue and preparation method thereof |
| CN108068176A (en) * | 2017-12-26 | 2018-05-25 | 芜湖市长江起重设备制造有限公司 | A kind of preparation method of high temperature resistant polycarbonate waterborne polyurethane base rubber plywood |
| CN109535384A (en) * | 2018-11-19 | 2019-03-29 | 山东天庆科技发展有限公司 | A kind of aqueous polyurethane emulsion and preparation method thereof and vacuum plastic-absorption |
| CN110511349A (en) * | 2019-07-30 | 2019-11-29 | 湖北大学 | A kind of preparation method of new hyperbranched type temperature sensitive type aqueous polyurethane |
| CN110511349B (en) * | 2019-07-30 | 2021-08-06 | 湖北大学 | Preparation method of hyperbranched temperature-sensitive waterborne polyurethane |
| CN112592689A (en) * | 2021-02-26 | 2021-04-02 | 山东万圣博化工有限公司 | Electronic adhesive and preparation method thereof |
| CN116265556A (en) * | 2021-12-16 | 2023-06-20 | 万华化学（北京）有限公司 | Moisture-curing polyurethane hot melt adhesive and preparation method and application thereof |
| WO2024028308A1 (en) | 2022-08-03 | 2024-02-08 | Covestro Deutschland Ag | Adhesive composition, the preparation method and use thereof |
| EP4339216A1 (en) | 2022-09-13 | 2024-03-20 | Covestro Deutschland AG | Adhesive composition, the preparation method and use thereof |
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