CN101037580A - Nano silicon micronization modified double components, solventless polyurethane adhesive and preparation method thereof - Google Patents
Nano silicon micronization modified double components, solventless polyurethane adhesive and preparation method thereof Download PDFInfo
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- CN101037580A CN101037580A CN 200710034865 CN200710034865A CN101037580A CN 101037580 A CN101037580 A CN 101037580A CN 200710034865 CN200710034865 CN 200710034865 CN 200710034865 A CN200710034865 A CN 200710034865A CN 101037580 A CN101037580 A CN 101037580A
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Abstract
The invention relates to a nano silicon micro-powder modified double-component and solvent-free polyurethane adhesive and preparing method thereof. The adhesive is constituted of component A and component B, wherein the component A is constituted of toluene diisocyanate, polyhydric polyether and trimethylolpropane, and the component B is constituted of liquid amino resin, dibutylphthalate, fire retardant and nano silicon micro-powder. The prepared adhesive possesses character of high strength, and moisture and heat proof; and is mainly used for bonding soft materials, or hard materials such as metal, plastic, and glass with the soft materials, and occasion of high demanding strength and moisture and heat proof.
Description
Technical field:
The present invention relates to a kind of nano silicon micronization modified double components, solvent-free polyurethane adhesive, relate in particular to a kind of intensity height, tackiness agent that humidity resistance is good.
Background technology:
Dual-component polyurethane adhesive is the product that consumption at most in the polyurethane adhesive, purposes is the widest, is mainly used in the bonding of mechanically resistant materials such as soft material or itself and metal, plastics, glass, is widely used in industries such as boats and ships, machinery, automobile, instrument.General dual-component polyurethane adhesive bonding strength is not high, water-fast and poor heat resistance, reduce bonding strength in hot and humid easy hydrolysis down, use back intensity under the high situation of humidity and temperature to descend rapidly, shortened greatly by the work-ing life of sticking material, limited the application of dual-component polyurethane adhesive to a great extent.
Summary of the invention:
The objective of the invention is to overcome the weak point of original technology, provide that a kind of preparation method is simple, environmental protection, bonding strength height, change little nano silicon micronization modified double components, solvent-free polyurethane adhesive in hot and humid bonding strength down.
For achieving the above object, nano silicon micronization modified double components of the present invention, solvent-free polyurethane adhesive A component are made up of tolylene diisocyanate, TriMethylolPropane(TMP), polytetrahydrofuran diol, tetrahydroxy polyether glycol, hydrolysis stabilizer etc., the B component is made up of liquid aminoresin, dibutyl phthalate, fire retardant, nano silicon micronization etc., is a kind of intensity height, tackiness agent that wet-hot aging performance is good.
For achieving the above object, the starting material and the weight proportion of nano silicon micronization modified double components of the present invention, solvent-free polyurethane adhesive selection are:
The A component:
Tolylene diisocyanate 40%～55%
Polytetrahydrofuran diol 35%～50%
TriMethylolPropane(TMP) 3%～5%
Tetrahydroxy polyether glycol 5%～8%
Hydrolysis stabilizer 2%～5%
The B component:
Liquid aminoresin 80～90%
O-phthalic dibutylester 5～10%
Fire retardant 3～8%
Nano silicon micronization 2～5%
Two components weight percentage sum separately is 100%.
A component and B component weight ratio are 4: 3～4, the preceding thorough mixing of use.
The molecular weight of polytetrahydrofuran diol used in the present invention is 800～2000, and the molecular weight of tetrahydroxy polyether glycol is 500～1000.Hydrolysis stabilizer is carbodiimide, epoxy compounds, organo-silicon coupling agent.
Preparation method of the present invention is:
Synthesizing of A component:
1, by weight ratio polytetrahydrofuran diol, tetrahydroxy polyether glycol are added reactor, start agitator, open the electrically heated switch and be warming up to 100～110 ℃, vacuumize, vacuum tightness is 0.08MPa～0.1MPa, and temperature in the kettle is controlled at 100～120 ℃, dewaters 2～3 hours, vacuum is eliminated in cooling;
2, add tolylene diisocyanate reaction 3～4 hours 50 ℃ the time, temperature is 70～80 ℃;
3, drip the TriMethylolPropane(TMP) of fusing in advance, temperature is 70～80 ℃, drips off in 1.5～2 hours, continues reaction 1～2 hour.
4, logical cooling water temperature when temperature is reduced to 45～50 ℃, adds hydrolysis stabilizer and stirred 0.5～1 hour, and discharging makes the A component and packs in the container of good seal.
Synthesizing of B component:
1, liquid aminoresin is added reactor, start agitator, be warming up to 50～60 ℃;
2, add dibutyl phthalate, fire retardant, nano silicon micronization, stirred 2～3 hours;
3, logical cooling water temperature when temperature is reduced to 40～50 ℃, filters with 60 order filtering nets, in the container of the good seal of packing into.
A component and B component by weight 4: 3～4 mix product of the present invention.
The nano silicon micronization that the present invention uses is that median size is the powdery silicon powder of 20～100nm.
Technical indicator of the present invention is: the A component is yellow thick liquid, the B component is white or oyster white thick liquid, viscosity (25 ± 2 ℃) A component is≤0.3mpa.s, the B component is≤1mpa.s that solid content is 〉=95%, (23 ± 2 ℃ of normal temperature tensile shear strengths, relative humidity 45～55%), steel to steel 〉=15MPa, tensile shear strength (80 ± 2 ℃, relative humidity 80～90%) 〉=14MPa.
The tackiness agent that positively effect of the present invention is to make is under hot and humid condition, and tensile shear strength changes little.Sample is 80 ± 2 ℃ in temperature, relative humidity is to park the tensile shear strength that recorded in month under 80～90% the condition, with sample be 23 ± 2 ℃ in temperature, relative humidity is to park the tensile shear strength that recorded in one month under 45～55% the condition relatively, rate of descent＜8%.
Embodiment:
Embodiment 1
Nano silicon micronization modified double components, solvent-free polyurethane adhesive are made up of A component, B component.
The A component is synthetic:
With 75g polytetrahydrofuran diol (molecular weight 1800), 9g tetrahydroxy polyether glycol (molecular weight 900) adds reactor, starts agitator, is warming up to 100 ℃, the unlatching vacuum pump vacuumizes, vacuum tightness is 0.096MPa, and temperature in the kettle is 110 ℃, dewaters 2 hours, logical cooling water temperature, when temperature is reduced to 50 ℃, add the 78g tolylene diisocyanate and begin reaction, temperature is 75 ℃, reacted 3 hours, drip the TriMethylolPropane(TMP) 5.6g of fusing in advance, temperature is 77 ℃, drips off in 1.5 hours, continue reaction 2 hours, logical cooling water temperature when temperature is reduced to 50 ℃, adds the 4.5g carbodiimide, stirred 1 hour, discharging promptly gets the A component.
Synthesizing of B component:
86g liquid aminoresin is added reactor, start agitator, be warming up to 60 ℃, add the 3g dibutyl phthalate, the 6g fire retardant, the 5g nano silicon micronization stirred 3 hours, logical cooling water temperature when temperature is reduced to 40 ℃, filters blowing with 60 order filtering nets and gets final product.
Get A component 4g, B component 4g prepares sample immediately after mixing on the cardboard, press GB7124～86 " tackiness agent tensile shear strength measuring method (metal to metal) " and measure tensile shear strength, sample is at 23 ± 2 ℃, test under relative humidity 45～55% conditions, tensile shear strength is 16.2MPa; At 80 ± 2 ℃, to test under relative humidity 80～90% conditions, tensile shear strength is 15.3MPa.
Embodiment 2
Nano silicon micronization modified double components, solvent-free polyurethane adhesive are made up of A component, B component.
The A component is synthetic:
With 60g polytetrahydrofuran diol (molecular weight 1000g), 7.5g tetrahydroxy polyether glycol (molecular weight 600g) adds reactor, start agitator, be warming up to 100 ℃, open vacuum pump and vacuumize, vacuum tightness is 0.092MPa, temperature in the kettle is 110 ℃, dewaters 3 hours, logical cooling water temperature, when temperature is reduced to 50 ℃, add the 60g tolylene diisocyanate and begin reaction, temperature is 72 ℃, reacts 4 hours, drip the TriMethylolPropane(TMP) 5.1g of fusing in advance, temperature is 75 ℃, drips off in 2 hours, continues reaction 1.5 hours, logical cooling water temperature, when temperature is reduced to 50 ℃, add the 4g organo-silicon coupling agent, stirred 1 hour.
Synthesizing of B component:
90g aminoresin is added reactor, start agitator, be warming up to 55 ℃, add the 2g dibutyl phthalate, the 4g fire retardant, the 4g nano silicon micronization stirred 2.5 hours, and logical cooling water temperature when temperature is reduced to 40 ℃, filters blowing with 60 order filtering nets and gets final product.
Get A component 4g, B component 3.5g prepares sample immediately after mixing on the cardboard, press GB7124～86 " tackiness agent tensile shear strength measuring method (metal to metal) " and measure tensile shear strength, at 23 ± 2 ℃, test under relative humidity 45～55% conditions, tensile shear strength is 15.8MPa; At 80 ± 2 ℃, to test under relative humidity 80～90% conditions, tensile shear strength is 14.5MPa.
Reference examples 1
Replace nano silicon micronization with 5g400 order silicon powder, all the other conditions are carried out controlled trial with embodiment 1, at 23 ± 2 ℃, test under relative humidity 45～55% conditions, and tensile shear strength is 12.4MPa; At 80 ± 2 ℃, to test under relative humidity 80～90% conditions, tensile shear strength is 8.2MPa.
Claims (7)
1, a kind of nano silicon micronization modified double components, solvent-free polyurethane adhesive is characterized in that the A component is that 40%～55% tolylene diisocyanate, 35%～50% polytetrahydrofuran diol, 3%～5% TriMethylolPropane(TMP), 5%～8% tetrahydroxy polyether glycol, 2%～5% hydrolysis stabilizer are formed by parts by weight; The B component is that 80～90% liquid aminoresin, 5～10% dibutyl phthalates, 3～8% fire retardants, 2～5% nano silicon micronizations are formed by parts by weight, and A, B two components weight percentage sum separately are 100%.
2, nano silicon micronization modified double components according to claim 1, solvent-free polyurethane adhesive is characterized in that A component and B component are mixed and made into by weight 4: 3～4.
3, nano silicon micronization modified double components according to claim 1, solvent-free polyurethane adhesive, the molecular weight that it is characterized in that polytetrahydrofuran diol is 800～2000.
4, nano silicon micronization modified double components according to claim 1, solvent-free polyurethane adhesive, the molecular weight that it is characterized in that the tetrahydroxy polyether glycol is 500～1000.
5, nano silicon micronization modified double components according to claim 1, solvent-free polyurethane adhesive is characterized in that hydrolysis stabilizer is carbodiimide, epoxy compounds, organo-silicon coupling agent.
6, nano silicon micronization modified double components according to claim 1, solvent-free polyurethane adhesive is characterized in that used silicon powder is that median size is the powdery silicon powder of 20～100nm.
7, nano silicon micronization modified double components according to claim 1, the preparation method of solvent-free polyurethane adhesive, it is characterized in that the synthetic of A component: by weight ratio with polytetrahydrofuran diol, the tetrahydroxy polyether glycol adds reactor, start agitator, open the electrically heated switch, heat up, when temperature in the kettle rises to 100～110 ℃, open vacuum pump vacuum hydro-extraction, vacuum tightness is 0.08MPa～0.1MPa, and temperature in the kettle is 100～120 ℃, dewatering time 2～3 hours, close the electrically heated switch, logical cooling water temperature is when temperature is reduced to 50 ℃, eliminate vacuum, add tolylene diisocyanate by weight ratio and begin reaction, temperature is 70～80 ℃, 3～4 hours reaction times, drip the TriMethylolPropane(TMP) of fusing in advance by weight ratio, temperature is 70～80 ℃, drips off in 1.5～2 hours, continues reaction 1～2 hour, logical cooling water temperature, when temperature is reduced to 45～50 ℃, add hydrolysis stabilizer and stirred 0.5～1 hour, can get the A component by blowing; Synthesizing of B component: by weight ratio liquid aminoresin is added reactor, start agitator, open electrically heated switch, intensification, when temperature in the kettle rises to 50～60 ℃, add dibutyl phthalate, fire retardant, nano silicon micronization by weight ratio, stirred 2～3 hours, logical cooling water temperature, when temperature is reduced to 40～50 ℃, filter discharging with 60 order filtering nets and get the B component.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710034865 CN101037580A (en) | 2007-04-30 | 2007-04-30 | Nano silicon micronization modified double components, solventless polyurethane adhesive and preparation method thereof |
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| CN 200710034865 CN101037580A (en) | 2007-04-30 | 2007-04-30 | Nano silicon micronization modified double components, solventless polyurethane adhesive and preparation method thereof |
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| CN101037580A true CN101037580A (en) | 2007-09-19 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101323772B (en) * | 2008-08-05 | 2012-10-03 | 湖南神力实业有限公司 | Ultra-thin stone and aluminum honeycomb composite modified epoxy adhesive and preparation thereof |
| CN103045153A (en) * | 2012-11-20 | 2013-04-17 | 陈晴 | Acid liquor corrosion resistant dual-component polyurethane adhesive as well as preparation method and application thereof |
| CN107936287A (en) * | 2017-11-09 | 2018-04-20 | 湖南优冠体育材料有限公司 | A kind of method of preparation and use of Solvent-free Modification TPU plastic cement race track materials |
| CN114455885A (en) * | 2022-02-24 | 2022-05-10 | 江苏博嘉节能科技有限公司 | Inorganic expanded vermiculite composite material insulation board and preparation method thereof |
-
2007
- 2007-04-30 CN CN 200710034865 patent/CN101037580A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101323772B (en) * | 2008-08-05 | 2012-10-03 | 湖南神力实业有限公司 | Ultra-thin stone and aluminum honeycomb composite modified epoxy adhesive and preparation thereof |
| CN103045153A (en) * | 2012-11-20 | 2013-04-17 | 陈晴 | Acid liquor corrosion resistant dual-component polyurethane adhesive as well as preparation method and application thereof |
| CN103045153B (en) * | 2012-11-20 | 2015-11-25 | 陈晴 | Bi-component polyurethane adhesive of a kind of resistance to acid liquid corrosion and its preparation method and application |
| CN107936287A (en) * | 2017-11-09 | 2018-04-20 | 湖南优冠体育材料有限公司 | A kind of method of preparation and use of Solvent-free Modification TPU plastic cement race track materials |
| CN114455885A (en) * | 2022-02-24 | 2022-05-10 | 江苏博嘉节能科技有限公司 | Inorganic expanded vermiculite composite material insulation board and preparation method thereof |
| CN114455885B (en) * | 2022-02-24 | 2022-08-23 | 江苏博嘉节能科技有限公司 | Inorganic expanded vermiculite composite material insulation board and preparation method thereof |
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