CN105153986A - Polyurethane modified SBS (styrene-butadiene-styrene) adhesive and preparation method thereof - Google Patents
Polyurethane modified SBS (styrene-butadiene-styrene) adhesive and preparation method thereof Download PDFInfo
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Abstract
The invention provides a polyurethane modified SBS (styrene-butadiene-styrene) adhesive and a preparation method thereof, relating to the technical field of adhesives. The polyurethane modified SBS adhesive comprises the following components in parts by weight: 10-20 parts of thermoplastic styrene-butadiene rubber, 10-20 parts of polyurethane prepolymer, 10-17 parts of tackifying resin, 1-5 parts of white carbon black, 0.1-5 parts of silane coupling agent, 0.1-5 parts of anti-aging agent, 0-1 part of catalyst, 0-2 parts of water absorbent and 40-55 parts of solvent. The polyurethane modified SBS adhesive has high elongation at break and tensile shear strength, thereby improving the service performance of the existing SBS adhesive and widening the application range of the SBS adhesive.
Description
Technical field
The present invention relates to field of adhesive technology, particularly polyurethane-modified SBS tackiness agent of one and preparation method thereof.
Background technology
SBS thermoplastic elastomer is the segmented copolymer of vinylbenzene and divinyl, existing cinnamic solvability and thermoplasticity, has again snappiness and the rebound resilience of cis-1,4-polybutadiene rubber, is the material having thermoplastics and vulcanized rubber dual nature concurrently.SBS solvability is good, can with a lot of polymer-compatible, without the need to mixing with plasticate, without High Temperature High Pressure sulfuration, be applicable to very much preparing tackiness agent, and it is high to have intensity, good toughness, quick solidifying and the construction advantage such as simple.
Urethane full name is polyurethane(s), is the general designation of the macromolecular cpd containing repetition carbamate groups on main chain.It is formed by organic diisocyanate or polyisocyanates and dihydroxyl or polyol addition polymerization.Polyurethane sealant has many good characteristics, comprising: 1, physical strength is large.2, adhesiveproperties is good.3, good springiness, has excellent Restoration, can be used for dynamic juncture.
Between polyurethane adhesive, there is above-mentioned characteristic, if will be good selection by adding urethane resin to improve the performance of SBS tackiness agent in SBS tackiness agent.But the most elongation at break of SBS tackiness agent commercially available at present and tensile shear strength lower, now need in the industry a kind of SBS tackiness agent with high elongation at tear and tensile shear strength badly.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of polyurethane-modified SBS tackiness agent with high elongation at tear and tensile shear strength.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme: a kind of polyurethane-modified SBS tackiness agent, comprises following component:
Thermoplastic styrene butadiene rubber: 10-20 weight part;
Base polyurethane prepolymer for use as: 10-20 weight part;
Tackifying resin: 10-17 weight part;
White carbon black: 1-5 weight part;
Silane coupling agent: 0.1-5 weight part;
Anti-aging agent: 0.1-5 weight part;
Catalyzer: 0-1 weight part;
Water-retaining agent: 0-2 weight part;
Solvent: 40-55 weight part.
Described thermoplastic styrene butadiene rubber is a kind of or linear mixture formed with the thermoplastic styrene butadiene rubber of hub-and-spoke configuration in linear/hub-and-spoke configuration thermoplastic styrene butadiene rubber;
Described base polyurethane prepolymer for use as is end NCO based polyurethanes performed polymer;
Described tackifying resin is rosin, rosin polyol ester, petroleum resin, hydrogenated petroleum resin, terpine resin, resol, the mixture of one or more in coumarone indene resin;
Described silane coupling agent is the mixture of one or more in the silane coupling agent of monoamine and polyamines structure;
Described anti-aging agent is the mixture of one or more of amine and phenolic type antioxidant;
Described catalyzer is the mixture of one or more in organic tin or two morpholine class;
Described water-retaining agent is the mixture of one or more in isocyanate terminated compound, silane compound and oxazolidine compounds;
Described solvent is sherwood oil, 120# solvent oil, methylcarbonate, ethyl acetate, butylacetate, the mixture of one or more in ethyl formate.
Preferably, the weight proportion of described component is:
Thermoplastic styrene butadiene rubber: 15 parts;
Base polyurethane prepolymer for use as: 13 parts;
Tackifying resin: 15 parts;
White carbon black: 3 parts;
Silane coupling agent: 3 parts;
Anti-aging agent: 2.5 parts;
Catalyzer: 0.5 part;
Water-retaining agent: 1 part;
Solvent: 47 parts.
Preferred, described thermoplastic styrene butadiene rubber is the mixture that YH-792SBS rubber and YH-802SBS rubber form by the weight ratio of 2:1;
The mixture that described tackifying resin is C9 petroleum resin, hydrogenated rosin glyceride, terpine resin form by the weight ratio of 6.5:2.5:6;
The mixture that described solvent is ethyl acetate, methylcarbonate, butylacetate, sherwood oil, 120# solvent oil form by the weight ratio of 12:15:4:8:8.
As another aspect of the present invention, a kind of method preparing above-mentioned polyurethane-modified SBS tackiness agent, comprises the following steps:
1, the preparation of NCO based polyurethanes performed polymer is held;
Get polyol compound, softening agent and thinner add in vacuum reaction still, vacuum hydro-extraction 1-5 hour under the vacuum environment of 100 DEG C-130 DEG C, to mixture water-content lower than 0.01%, then the temperature of charge of vacuum reaction still is down to 40-60 DEG C, add the isocyanate compound of metering, stir under vacuum environment and be warming up to 75-85 DEG C, reaction 3-7h arrives theoretical value to the isocyano-content of system, obtain end NCO based polyurethanes performed polymer, be cooled to afterwards 10-25 DEG C for subsequent use, described polyol compound is polyether glycol, polyester polyol, other main chain contains in the terminal hydroxy group compound of C-C chooses any one kind of them or several mixtures, the molecular weight of described polyether glycol is between 2000-8000, described isocyanate compound is the mixture of one or more in tolylene diisocyanate, diphenylmethanediisocyanate, isoflurane chalcone diisocyanate, hexamethylene diisocyanate,
2, the stirring of each component, mixing;
The first step, to get a reactor and control temperature in reactor be 10-25 DEG C, first in reactor, adds solvent, stir again and slowly add thermoplastic styrene butadiene rubber after stirring in reactor;
Second step, reactor airtight and in still temperature constantly stir under being the condition of 10-25 DEG C, until thermoplastic styrene butadiene rubber dissolve after in reactor, add tackifying resin again;
3rd step, reactor airtight and in still temperature stir 1-3h under being the condition of 10-25 DEG C, then in reactor, add white carbon black and be cooled to the end NCO based polyurethanes performed polymer of 10-25 DEG C;
4th step, reactor airtight and in still temperature add silane coupling agent, anti-aging agent, catalyzer and water-retaining agent after stirring 0.5-2h under being the condition of 10-25 DEG C, keep reactor airtight and in still, temperature is 10-25 DEG C and continues to stir after 20min-1h and can stop stirring, finally tackiness agent is poured out from reactor and filter to obtain described polyurethane-modified SBS tackiness agent.
The beneficial effect that the present invention obtains is: polyurethane-modified SBS tackiness agent provided by the invention has high elongation at tear and tensile shear strength, improves the use properties of existing SBS tackiness agent, expands the use range of SBS tackiness agent.
Embodiment
As one embodiment of the present invention, prepare polyurethane-modified SBS tackiness agent of the present invention and comprise two portions:
The end NCO based polyurethanes performed polymer that first-selected preparation is required for the present invention, getting polyol compound, softening agent and thinner adds in vacuum reaction still, vacuum hydro-extraction 1-5 hour under the vacuum environment of 100 DEG C-130 DEG C, to mixture water-content lower than 0.01%, then the temperature of charge of vacuum reaction still is down to 40-60 DEG C, add the isocyanate compound of metering, stir under vacuum environment and be warming up to 75-85 DEG C, reaction 3-7h arrives theoretical value to the isocyano-content of system, obtain end NCO based polyurethanes performed polymer, be cooled to afterwards 10-25 DEG C for subsequent use.It is emphasized that, above-mentioned polyol compound is polyether glycol, polyester polyol, other main chain contain in the terminal hydroxy group compound of C-C and choose any one kind of them or several mixtures, if above-mentioned polyol compound selects polyether glycol, then the molecular weight of polyether glycol should between 2000-8000, above-mentioned isocyanate compound is the mixture of one or more in tolylene diisocyanate, diphenylmethanediisocyanate, isoflurane chalcone diisocyanate, hexamethylene diisocyanate.
Again each component is stirred afterwards, mixing, particularly, controlling temperature in reactor is 10-25 DEG C, solvent 40-55 weight part is added in reactor, then stir while slowly add the thermoplastic styrene butadiene rubber of 10-20 weight part, continue to keep temperature in reactor to be 10-25 DEG C and ensure that reactor continues to stir when airtight, the tackifying resin of 10-17 weight part is added again after above-mentioned thermoplastic styrene butadiene rubber dissolves, after this, then keep stirring 1-3h with temperature identical is before airtight, the white carbon black of 1-5 weight part and the end NCO based polyurethanes performed polymer being cooled to 10-25 DEG C of 10-20 weight part is added again in reactor, reactor airtight and in still temperature stir 0.5-2h under being the condition of 10-25 DEG C, finally add the silane coupling agent of 0.1-5 weight part, the anti-aging agent of 0.1-5 weight part, the catalyzer of 0-1 weight part and the water-retaining agent of 0-2 weight part, same maintenance reactor airtight and in still temperature be 10-25 DEG C and continue to stir after 20min-1h and can stop stirring, finally tackiness agent is poured out from reactor and filter and can obtain polyurethane-modified SBS tackiness agent of the present invention.It is emphasized that above-mentioned thermoplastic styrene butadiene rubber is a kind of or linear mixture formed with the thermoplastic styrene butadiene rubber of hub-and-spoke configuration in linear/hub-and-spoke configuration thermoplastic styrene butadiene rubber; Above-mentioned tackifying resin is rosin, rosin polyol ester, petroleum resin, hydrogenated petroleum resin, terpine resin, resol, the mixture of one or more in coumarone indene resin; Above-mentioned silane coupling agent is the mixture of one or more of the silane coupling agent of monoamine and polyamines structure; Above-mentioned anti-aging agent is the mixture that amine/phenolic type antioxidant or amines antioxidants and phenolic type antioxidant form; Above-mentioned solvent is sherwood oil, 120# solvent oil, methylcarbonate, ethyl acetate, butylacetate, the mixture of one or more in ethyl formate.
In order to the improvements allowing those skilled in the art more clearly understand hinge structure of the present invention, below in conjunction with embodiment, the present invention is further illustrated, and the content that embodiment is mentioned not is limitation of the invention.
What need to illustrate in advance is, in polyurethane-modified SBS tackiness agent provided by the invention, thermoplastic styrene butadiene rubber can be the mixture that a kind of thermoplastic styrene butadiene rubber of or any one linear structure in linear/hub-and-spoke configuration thermoplastic styrene butadiene rubber and the thermoplastic styrene butadiene rubber of any one hub-and-spoke configuration form, it will be appreciated by those skilled in the art that, in the present invention, affect experimental result of the present invention be the molecular morphosis of thermoplastic styrene butadiene rubber and non-specific selects the thermoplastic styrene butadiene rubber of which kind of trade mark.Although there is difference slightly between the thermoplastic styrene butadiene rubber of the different trade mark, these differences almost can be ignored the impact of experimental result of the present invention.In addition, no matter select the thermoplastic styrene butadiene rubber of linear structure or select hub-and-spoke configuration thermoplastic styrene butadiene rubber or be said two devices composition mixture, its final experimental result is all very close.Same, tackifying resin, silane coupling agent, anti-aging agent and solvent also can be done to select arbitrarily and adjustment in aforementioned component scope, compare the improvement amplitude of the present invention to existing SBS Adhensive performance, it is very small that the component of tackifying resin, silane coupling agent, anti-aging agent, catalyzer, water-retaining agent and solvent changes the impact of experimental result, therefore, in order to simplify statement, only list with the experiment of following component as thermoplastic styrene butadiene rubber, tackifying resin and solvent in the embodiment part of this specification sheets, and eliminate the example selecting other components.
embodiment 1:
Getting polyol compound, softening agent and thinner adds in vacuum reaction still, vacuum hydro-extraction 1-5 hour under the vacuum environment of 100 DEG C-130 DEG C, to mixture water-content lower than 0.01%, then the temperature of charge of vacuum reaction still is down to 40-60 DEG C, add the isocyanate compound of metering, stir and be warming up to 75-85 DEG C under vacuum environment, reaction 3-7h arrives theoretical value to the isocyano-content of system, obtain end NCO based polyurethanes performed polymer, be cooled to afterwards 10-25 DEG C for subsequent use.It is emphasized that, above-mentioned polyol compound is polyether glycol, polyester polyol, other main chain contain in the terminal hydroxy group compound of C-C and choose any one kind of them or several mixtures, if above-mentioned polyol compound selects polyether glycol, then the molecular weight of polyether glycol should between 2000-8000, above-mentioned isocyanate compound is the mixture of one or more in tolylene diisocyanate, diphenylmethanediisocyanate, isoflurane chalcone diisocyanate, hexamethylene diisocyanate.
Again each component is stirred afterwards, mixing, particularly, controlling temperature in reactor is 10-25 DEG C, in reactor, add solvent 40 weight part (comprise the ethyl acetate of 12 weight parts, the butylacetate of 4 weight parts, the sherwood oil of 14 weight parts, the 120# solvent oil of 10 weight parts), then stir while slowly add the thermoplastic styrene butadiene rubber (comprising the YH-792SBS rubber of 7 weight parts and the YH-802SBS rubber of 3 weight parts) of 10 weight parts, continue to keep temperature in reactor to be 10-25 DEG C and ensure that reactor continues to stir when airtight, the tackifying resin adding 10 weight parts after above-mentioned thermoplastic styrene butadiene rubber dissolves again (comprises the C9 petroleum resin of 6 weight parts, the terpine resin of 4 weight parts), after this, then keep stirring 1-3h with temperature identical is before airtight, the white carbon black of 1 weight part and the end NCO based polyurethanes performed polymer being cooled to 10-25 DEG C of 20 weight parts is added again in reactor, reactor airtight and in still temperature stir 0.5-2h under being the condition of 10-25 DEG C, finally add the silane coupling agent of 5 weight parts, the anti-aging agent of 5 weight parts, the catalyzer of 1 weight part and the water-retaining agent of 2 weight parts, same maintenance reactor airtight and in still temperature be 10-25 DEG C and continue to stir after 20min-1h and can stop stirring, finally tackiness agent is poured out from reactor and filter and can obtain polyurethane-modified SBS tackiness agent of the present invention.It is emphasized that above-mentioned silane coupling agent is the mixture of one or more of the silane coupling agent of monoamine and polyamines structure; Above-mentioned anti-aging agent is the mixture that amine/phenolic type antioxidant or amines antioxidants and phenolic type antioxidant form.
After this, the polyurethane-modified SBS tackiness agent this embodiment 1 obtained tests its performance index according to the examination criteria of the mensuration of GB/T27561-2011 styrene-butadiene-styrene block copolymer (SBS) tackiness agent and GB/T528-2009 vulcanized rubber and thermoplastic elastomer tensile stress-strain performance, and concrete test result is in table 1.
embodiment 2:
Embodiment 2 is identical with the preparation method of embodiment 1, for easy statement, identical content does not repeat them here, and the proportioning of each component of the polyurethane-modified SBS tackiness agent of embodiment 2 is as follows: thermoplastic styrene butadiene rubber: 20 weight parts (comprising the YH-792SBS rubber of 12 weight parts and the YH-802SBS rubber of 8 weight parts); Base polyurethane prepolymer for use as: 10 weight parts; Tackifying resin: 17 weight parts (comprising the terpine resin of the C9 petroleum resin of 8 weight parts, the hydrogenated rosin glyceride of 3 weight parts and 6 weight parts); White carbon black: 5 weight parts; Silane coupling agent: 0.1 weight part; Anti-aging agent: 0.1 weight part; Catalyzer: 0 weight part; Water-retaining agent: 0 weight part; Solvent: 55 weight parts (comprising the ethyl acetate of 15 weight parts, the methylcarbonate of 14 weight parts, the butylacetate of 6 weight parts, 20 weight part sherwood oils).
After this, the polyurethane-modified SBS tackiness agent this embodiment 2 obtained tests its performance index according to the examination criteria of the mensuration of GB/T27561-2011 styrene-butadiene-styrene block copolymer (SBS) tackiness agent and GB/T528-2009 vulcanized rubber and thermoplastic elastomer tensile stress-strain performance, and concrete test result is in table 1.
embodiment 3:
Embodiment 3 is identical with the preparation method of embodiment 1 and 2, for easy statement, identical content does not repeat them here, and the proportioning of each component of the polyurethane-modified SBS tackiness agent of embodiment 3 is as follows: thermoplastic styrene butadiene rubber: 15 weight parts (comprising the YH-792SBS rubber of 10 weight parts and the YH-802SBS rubber of 5 weight parts); Base polyurethane prepolymer for use as: 13 weight parts; Tackifying resin: 15 weight parts (comprising the terpine resin of the C9 petroleum resin of 6.5 weight parts, the hydrogenated rosin glyceride of 2.5 weight parts and 6 weight parts); White carbon black: 3 weight parts; Silane coupling agent: 3 weight parts; Anti-aging agent: 2.5 weight parts; Catalyzer: 0.5 weight part; Water-retaining agent: 1 weight part; Solvent: 47 weight parts (comprising the ethyl acetate of 12 weight parts, the methylcarbonate of 15 weight parts, the butylacetate of 4 weight parts, the sherwood oil of 8 weight parts, the 120# solvent oil of 8 weight parts).
After this, the polyurethane-modified SBS tackiness agent this embodiment 3 obtained tests its performance index according to the examination criteria of the mensuration of GB/T27561-2011 styrene-butadiene-styrene block copolymer (SBS) tackiness agent and GB/T528-2009 vulcanized rubber and thermoplastic elastomer tensile stress-strain performance, and concrete test result is in table 1.
| name of product | gB standard | embodiment 1 | embodiment 2 | embodiment 3 |
| outward appearance | even thick liquid no suspended substance, without visible mechanical impurity and phenomenon of phase separation. | even thick liquid no suspended substance, without visible mechanical impurity and phenomenon of phase separation. | even thick liquid no suspended substance, without visible mechanical impurity and phenomenon of phase separation. | even thick liquid no suspended substance, without visible mechanical impurity and phenomenon of phase separation. |
| non-volatile content | >=35% | 46% | 48% | 45% |
| viscosity | 80-3000 | 520 | 470 | 710 |
| tensile shear strength | 1.15 | 1.32 | 1.38 | 1.40 |
| just glutinous intensity | 0.7 | 0.82 | 0.89 | 0.88 |
| tensile strength | nothing | 2.35 | 2.79 | 2.75 |
| elongation at break | nothing | 93% | 117% | 123% |
Table 1;
As can be seen from the test data of table 1, polyurethane-modified SBS tackiness agent provided by the invention is compared with existing SBS tackiness agent, it has higher elongation at break and tensile shear strength, the adhesiveproperties of this polyurethane-modified SBS tackiness agent is compared existing SBS tackiness agent and is obtained and significantly improve, and can determine that this tackiness agent will have broader use range thus.
Above-described embodiment is the present invention's preferably implementation, and in addition, the present invention can also realize by alternate manner, and under the prerequisite not departing from the technical program design, any apparent replacement is all within protection scope of the present invention.
Finally, it should be emphasized that, the improvements of the present invention relative to prior art are understood more easily in order to allow those of ordinary skill in the art, descriptions more of the present invention are simplified, and for the sake of clarity, present specification is omitted some other elements, and those of ordinary skill in the art it is to be appreciated that these elliptical elements also can form content of the present invention.
Claims (4)
1. a polyurethane-modified SBS tackiness agent, comprises following component and the ratio of each component is:
Thermoplastic styrene butadiene rubber: 10-20 weight part;
Base polyurethane prepolymer for use as: 10-20 weight part;
Tackifying resin: 10-17 weight part;
White carbon black: 1-5 weight part;
Silane coupling agent: 0.1-5 weight part;
Anti-aging agent: 0.1-5 weight part;
Catalyzer: 0-1 weight part;
Water-retaining agent: 0-2 weight part;
Solvent: 40-55 weight part;
Described thermoplastic styrene butadiene rubber is a kind of or linear mixture formed with the thermoplastic styrene butadiene rubber of hub-and-spoke configuration in linear/hub-and-spoke configuration thermoplastic styrene butadiene rubber;
Described base polyurethane prepolymer for use as is end NCO based polyurethanes performed polymer;
Described tackifying resin is rosin, rosin polyol ester, petroleum resin, hydrogenated petroleum resin, terpine resin, resol, the mixture of one or more in coumarone indene resin;
Described silane coupling agent is the mixture of one or more in the silane coupling agent of monoamine and polyamines structure;
Described anti-aging agent is the mixture of one or more of amine and phenolic type antioxidant;
Described catalyzer is the mixture of one or more in organic tin or two morpholine class;
Described water-retaining agent is the mixture of one or more in isocyanate terminated compound, silane compound and oxazolidine compounds;
Described solvent is sherwood oil, 120# solvent oil, methylcarbonate, ethyl acetate, butylacetate, the mixture of one or more in ethyl formate.
2. polyurethane-modified SBS tackiness agent according to claim 1, is characterized in that: the weight proportion of each component is:
Thermoplastic styrene butadiene rubber: 15 parts;
Base polyurethane prepolymer for use as: 13 parts;
Tackifying resin: 15 parts;
White carbon black: 3 parts;
Silane coupling agent: 3 parts;
Anti-aging agent: 2.5 parts;
Catalyzer: 0.5 part;
Water-retaining agent: 1 part;
Solvent: 47 parts.
3. polyurethane-modified SBS tackiness agent according to claim 2, is characterized in that: described thermoplastic styrene butadiene rubber is the mixture that YH-792SBS rubber and YH-802SBS rubber form by the weight ratio of 2:1;
The mixture that described tackifying resin is C9 petroleum resin, hydrogenated rosin glyceride, terpine resin form by the weight ratio of 6.5:2.5:6;
The mixture that described solvent is ethyl acetate, methylcarbonate, butylacetate, sherwood oil, 120# solvent oil form by the weight ratio of 12:15:4:8:8.
4. prepare a method for the polyurethane-modified SBS tackiness agent in claim 1-3 described in any one, comprise the following steps:
1, the preparation of NCO based polyurethanes performed polymer is held;
Get polyol compound, softening agent and thinner add in vacuum reaction still, vacuum hydro-extraction 1-5 hour under the vacuum environment of 100 DEG C-130 DEG C, to mixture water-content lower than 0.01%, then the temperature of charge of vacuum reaction still is down to 40-60 DEG C, add the isocyanate compound of metering, stir under vacuum environment and be warming up to 75-85 DEG C, reaction 3-7h arrives theoretical value to the isocyano-content of system, obtain end NCO based polyurethanes performed polymer, be cooled to afterwards 10-25 DEG C for subsequent use, described polyol compound is polyether glycol, polyester polyol, other main chain contains in the terminal hydroxy group compound of C-C chooses any one kind of them or several mixtures, the molecular weight of described polyether glycol is between 2000-8000, described isocyanate compound is the mixture of one or more in tolylene diisocyanate, diphenylmethanediisocyanate, isoflurane chalcone diisocyanate, hexamethylene diisocyanate,
2, the stirring of each component, mixing;
The first step, to get a reactor and control temperature in reactor be 10-25 DEG C, first in reactor, adds solvent, stir again and slowly add thermoplastic styrene butadiene rubber after stirring in reactor;
Second step, reactor airtight and in still temperature constantly stir under being the condition of 10-25 DEG C, until thermoplastic styrene butadiene rubber dissolve after in reactor, add tackifying resin again;
3rd step, reactor airtight and in still temperature stir 1-3h under being the condition of 10-25 DEG C, then in reactor, add white carbon black and be cooled to the end NCO based polyurethanes performed polymer of 10-25 DEG C;
4th step, reactor airtight and in still temperature add silane coupling agent, anti-aging agent, catalyzer and water-retaining agent after stirring 0.5-2h under being the condition of 10-25 DEG C, keep reactor airtight and in still, temperature is 10-25 DEG C and continues to stir after 20min-1h and can stop stirring, finally tackiness agent is poured out from reactor and filter to obtain described polyurethane-modified SBS tackiness agent.
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| CN106753045A (en) * | 2016-12-02 | 2017-05-31 | 陈佩珊 | A kind of polyurethane-modified high temperature resistant pressure sensitive adhesive and preparation method thereof |
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