CN107384242A - A kind of preparation method of the double curing conductive gluing agent of ultraviolet light - Google Patents
A kind of preparation method of the double curing conductive gluing agent of ultraviolet light Download PDFInfo
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- CN107384242A CN107384242A CN201710451340.XA CN201710451340A CN107384242A CN 107384242 A CN107384242 A CN 107384242A CN 201710451340 A CN201710451340 A CN 201710451340A CN 107384242 A CN107384242 A CN 107384242A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/67—Unsaturated compounds having active hydrogen
- C08G18/671—Unsaturated compounds having only one group containing active hydrogen
- C08G18/672—Esters of acrylic or alkyl acrylic acid having only one group containing active hydrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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Abstract
The present invention relates to a kind of preparation method of the double curing conductive gluing agent of ultraviolet light, the double curing conductive gluing agent of ultraviolet light by following raw material by weight：Make 15~30 parts of low surface tension polyurethane acrylate prepolymer by oneself, 12~20 parts of bifunctionality polyurethane acrylate prepolymer, 13~32 parts of acrylics reactive diluent, 0.5~5 part of levelling wetting agent, 2~4 parts of light trigger, 6~24 parts of 16~30 parts of epoxy resin, 5~13 parts of thermal curing agents, 1~3 part of silane coupler and crystalline flake graphite alkene.Surface tension of the present invention is low, and wettability is good, and surface drying is good, toughness is good, and has excellent heat resistance and resistant to elevated temperatures performance.
Description
Technical field
The invention belongs to UV curing field, and in particular to a kind of preparation method of the double curing conductive gluing agent of ultraviolet light.
Background technology
As electronic product is fast-developing, electronics industry proposes higher requirement to Electronic Packaging and gluing, wide at present
The general Pb/Sn solders applied in the fields such as electronics, household electrical appliances have cost is low, fusing point is low, intensity is high, working plasticity is good, leaching
The features such as lubricant nature is good.But the density of Pb/Sn solders is big, it is poor with the wellability of organic material, be connected the shortcomings of temperature is high
The requirement that electronic product develops to lightweight can not be adapted to.In recent years, Pb/Sn solders are substituted to connect with novel conductive adhesive
Connect material and achieve extensive research and increasing application in electronics industry.
In recent years, ultraviolet cured adhesive sticks agent due to fast, the suitable electronics industry production line operation of curing rate
The features such as, it is developed rapidly.Common ultraviolet cured adhesive sticks agent based on radical UV curing, and it, which has to trigger, polymerize
Speed is fast, the advantages that free radical type initiator type and all more resin types.But there is oxygen resistance in the solidification of free radical ultraviolet light
The shortcomings of cubical contraction is big after poly-, solidification, poor adhesive force, deep layer hardly possible solidify.Because stop of the conductive filler to ultraviolet light is made
With causing in general UV-Curing Electric Conductive Adhesives to be not easy the more difficult solidification of completion of cure, especially deep layer.
The shortcomings that in order to overcome single ultraviolet light to solidify, its advantage is played, in recent years, ultraviolet light solidification and other solidification sides
The dual UV curable paint that formula combines has obtained the attention of more and more researchers, and common ultraviolet light dual UV curable paint has
：Ultraviolet optical free radical-cation dual UV curable paint, ultraviolet-heat dual UV curable paint, ultraviolet light-air are dual solid
Change, ultraviolet light-moisture dual cure, ultraviolet-anaerobic dual curing etc..It is double with ultraviolet-heat in these curing systems
Weight curing system in actual applications solidification process be easily controlled, excellent performance, have a good application prospect, it is other dual
Curing system solidification process is influenceed greatly by extraneous factor, and application is not also strong.
The content of the invention
The technical problem to be solved by the invention is to provide a kind of preparation method of the double curing conductive gluing agent of ultraviolet light,
The present invention solves problem of the double curing conductive gluing agent of ultraviolet light of the prior art to low surface energy substrates adhesive effect difference.
In order to solve the above-mentioned technical problem, the present invention uses following technical scheme：
15~30 parts of low surface tension polyurethane acrylate prepolymer, bifunctionality polyurethane acrylate prepolymer will be made by oneself
5~20 parts, 13~32 parts of acrylics reactive diluent, 0.5~5 part of levelling wetting agent, 2~4 parts of light trigger, asphalt mixtures modified by epoxy resin
16~30 parts of fat, 6~24 parts of 5~13 parts of latent curing agent, 1~3 part of silane coupler and crystalline flake graphite alkene are added sequentially to
It is 8~15 DEG C in temperature in mixer, pressure is -0.08~-0.098MPa, under conditions of rotating speed is 500~1000r/min,
0.5~2h is stirred, lucifuge packs, and produces the double curing conductive gluing agent of ultraviolet light；
The self-control bifunctionality polyurethane acrylate prepolymer follows the steps below：
Polyether Glycols are vacuumized into 1.5~2h of dehydration at a temperature of 110 DEG C~120 DEG C；Diisocyanate is added, in temperature
Spend for 50 DEG C~70 DEG C, under the conditions of vacuum pressure is -0.07~-0.098MPa, stir 0.5~1h；Catalyst is added, in temperature
For 70 DEG C~80 DEG C, vacuum pressure reacts 2~3h under the conditions of being -0.07~-0.098MPa；Add polymerization inhibitor and dihydroxypropyl
Ester, it is 60 DEG C~80 DEG C in temperature, vacuum pressure stirs 2~3h under the conditions of being -0.07~-0.098MPa, uses infrared spectrometer
The content of NCO group is analyzed, when NCO peak is wholly absent, stops heating response, produces low surface tension polyurethane acroleic acid
Ester performed polymer；
Polyether Glycols in the low surface tension polyurethane acrylate prepolymer, diisocyanate and crylic acid hydroxy ester
Mol ratio is 1:1.8~2.0:2~2.2, catalyst and polymerization inhibitor are respectively accounted for from system low surface tension polyurethane acrylate prepolymer
The 0.1 ‰ of aggressiveness weight~1 ‰；
The crystalline flake graphite alkene follows the steps below：
a）Prepare ore pulp：Crystalline flake graphite ore deposit and water after will be broken is according to mass ratio 25~35:100 mix, and ore pulp is made；
b）Prepare flotation crystalline flake graphite：Roughing：Ore pulp is added in flotation device, addition 50~100g of butyl xanthate, stirring 3~
5min, scrape 8~15min of bubble；Once purging selection：20~40g butyl xanthates are added into ore pulp, stirs 1 minute, scrapes 3~5 points of bubble
Clock；It is secondary to scan：20~40g butyl xanthates are added into ore pulp, stirs 1 minute, scrapes bubble 3~5 minutes；Obtain flotation scale stone
Ink and mine tailing；
c）Prepare flotation essence crystalline flake graphite：Flotation crystalline flake graphite is filtered, obtains flotation essence crystalline flake graphite and filtrate；
d）Prepare crystalline flake graphite alkene liquid：By flotation essence crystalline flake graphite, 5040 dispersants and water according to mass ratio 20~50:0.1~
0.5:50~80 are added in homogenizer, at least homogeneous 1 time under the conditions of 50~75 DEG C, and homogeneous pressure is 4~40MPa, homogeneous
Time is 5~30min, obtains crystalline flake graphite alkene liquid；
e）Prepare crystalline flake graphite alkene：After crystalline flake graphite alkene liquid is spray-dried, crystalline flake graphite alkene is obtained；
Described bifunctionality polyurethane acrylate prepolymer, refer to RAHN companies 4217, the CN9001 of Sartomer,
The CN9021 of Sartomer, state, which refine and learn the GU2500K of limited company, state refines learns the 2600K of limited company
Refined with state the mixture of one or both of the 3030Z any of the above ratio for learning limited company；
The polyether Glycols include one or both of polyethylene glycol, polypropylene glycol and PTMG to take up an official post
The mixture of meaning ratio；
The diisocyanate includes toluene di-isocyanate(TDI)（TDI）, methyl diphenylene diisocyanate（MDI）, the methylene of benzene two
Group diisocyanate (XDI), hexamethylene diisocyanate (HDI) and one kind in IPDI (IPDI) or
The mixture of two or more any ratios；
The catalyst is dibutyl tin laurate；
The polymerization inhibitor include hydroquinones, one or both of MEHQ and 2,6 toluene di-tert-butyl phenols with
The mixture of upper any ratio；
The crylic acid hydroxy ester includes hydroxy-ethyl acrylate（HEA）, hydroxypropyl acrylate (HPA), hydroxyethyl methacrylate
（HEMA）, methacrylic acid hydroxypropyl fat（HPMA）And trimethylolpropane diacrylate（TMPDA）One or more
The mixture of any ratio；
The acrylics reactive diluent includes tetrahydrofuran methyl acrylate, tetrahydrofuran acrylate, 3,3,5-
It is trimethyl-cyclohexane acrylate, isobornyl methacrylate, hydroxyethyl methacrylate, hydroxy propyl methacrylate, different
The mixture of one or both of decyl acrylate and the third oxidation neopentylglycol diacrylate any of the above ratio；
The levelling wetting agent include one or both of TEGO-4000, TEGO-4100, TEGO-4200 and TEGO-270 with
The mixture of upper any ratio；
The light trigger is 1173（2- hydroxyls -2- methyl isophthalic acids-phenylacetone）、184（1- hydroxy cyclohexyl phenylketones）、
819（It is double（2,4,6- trimethylbenzoyls）Phenylphosphine oxide）, 651 (α, α '-dimethyl benzil ketals), ITX it is (different
Propyl group thioxanthone), one kind in BP (benzophenone) and TPO (2,4,6- trimethyl benzoyl diphenyl bases phosphorous oxide)
Or the mixture of two or more any ratios；
Described epoxy resin includes Japanese ADEKA EP-4100HF, EP-4000S, EP-4901HF, EP-4088L, Taiwan
One or both of NAN YA NPEL-127, NPEL-128, NPEL-128R, NPEF-170 any of the above than mixture；
Described latent curing agent includes Japanese ADEKA EH-5031S, EH-4360S, EH-3293S, Japanese aginomoto
One or both of PN-23, PN-31, AH-154, AH-162 any of the above than mixture；
Described silane coupler includes the mixed of one or both of KH551, KH172, KH560 and KH570 any of the above ratio
Compound.
Weigh 28 parts of self-control low surface tension polyurethane acrylate prepolymer, the CN9021 of Sartomer:6 parts；Four
13 parts of hydrogen furanacrylate；6 parts of isodecyl acrylate；Light trigger 184:2 parts；Light trigger TPO:1 part；ADEKA is public
Epoxy resin-the 4088L of department：20 parts；The latent curing agent EH-3293S of ADEKA companies：7 parts；Levelling wetting agent TEGO-
4100:2.5 part；Silane coupler KH570:1.5 parts and 12 parts of crystalline flake graphite alkene.
The molecular weight of the PTMEG is 1000~3000.
Step d）For homogeneous 3 times, first time homogeneous pressure is 35MPa, homogeneous 20min；Second of homogeneous pressure be
15MPa, homogeneous 20min；Third time homogeneous pressure is 6MPa, homogeneous 20min.
Invention has following advantageous effects：
1st, the double curing conductive gluing agent of ultraviolet light prepared by the present invention, by controlling synthesis of polyurethane acrylate prepolymer body process
In NCO/OH ratio be 0.8~1.1, obtained a kind of polyurethane acrylate prepolymer of low surface tension, and add
The organic silicon wetting agent that can be good at reducing dynamic surface tension is added, has solved the double solidifications of ultraviolet light of the prior art and lead
Electric adhesive is poor to low surface tension material wetting effect, the low problem of adhesive strength, extends the application neck of ultraviolet cured adhesive
Domain, there is provided a kind of ultraviolet cured adhesive for low table energy substrate bonding, the adhesive wettability is good, and surface drying is good, toughness
It is good, the performance such as excellent heat resistance and high temperature resistant.
2nd, the present invention adds crystalline flake graphite alkene, can substantially increase the toughness of the double curing conductive gluing agent of ultraviolet light, Bu Huiyin
Conduction production
Raw temperature change, causes adhesive crackle.
3rd, because graphene has a floatability in itself, therefore the present invention is only with adding a small amount of butyl xanthate flotation, and roughing one
It is secondary, scan twice, without selected, you can obtain flotation essence crystalline flake graphite.
4th, graphene of the crystalline flake graphite alkene through homogeneous acquisition three times of the present invention, there is the characteristics of number of plies is low, good toughness.
Embodiment
The present invention is further illustrated with reference to instantiation.
Embodiment 1
Each raw material is accurately weighed by weight percentage, makes low surface tension polyurethane acrylate prepolymer 22g by oneself, and Sartomer is public
The CN9021 of department:12g；Tetrahydrofuran acrylate 18g；Isodecyl acrylate 5g；Light trigger 184:2g ；Light trigger
TPO:1g ；Epoxy resin-the 4100HF of ADEKA companies：21g；The latent curing agent EH-5031S of ADEKA companies：7g；
Levelling wetting agent TEGO-4100:2g；Silane coupler KH560:1g and crystalline flake graphite alkene 9g.Above-mentioned each component is sequentially added
In double-planet power mixing and blending machine, it is -0.08MPa to be evacuated to vacuum, is stirred 2 hours in 500 r/min, and stirring is equal
It is even, hang naturally to room temperature, obtain ultraviolet cured adhesive, pack.
Wherein self-control low surface tension polyurethane acrylate prepolymer follows the steps below：
By 200 grams of PTMGs（Mn=2000）Be added in reactor, in 115 DEG C of temperature, vacuum pressure for-
Be dehydrated 2 hours under conditions of 0.08MPa, be cooled to 60 DEG C, add 42.2 grams of IPDIs, vacuum pressure for-
Stirred under conditions of 0.08MPa 0.5 hour, then add 0.02 gram of dibutyl tin laurate, reacted 2.5 hours at 70 DEG C,
27 grams of hydroxyethyl methacrylates are sequentially added, 0.01g hydroquinones continues to react 2 hours at 75 DEG C, samples and uses every 30min
Infrared spectrometer analyzes the content of NCO group, when NCO peak is wholly absent, stops heating response, can obtain low surface tension
Polyurethane acrylate prepolymer, it is -33.1mN/m to measure surface tension；
The crystalline flake graphite alkene follows the steps below：
a）Prepare ore pulp：Roughing will it is broken after crystalline flake graphite alkene ore deposit and water according to mass ratio 30:100 mix, and ore pulp is made；
b）Prepare flotation crystalline flake graphite：Roughing：Ore pulp is added in flotation device, adds butyl xanthate 60g, 4min is stirred, scrapes
Steep 10min；Once purging selection：30g butyl xanthates are added into ore pulp, are stirred 1 minute, scrape bubble 4 minutes；It is secondary to scan：To ore pulp
Middle addition 20g butyl xanthates, stir 1 minute, scrape bubble 4 minutes；Obtain flotation crystalline flake graphite and mine tailing；
c）Prepare flotation essence crystalline flake graphite：Flotation crystalline flake graphite is filtered, obtains flotation essence crystalline flake graphite and filtrate；
d）Prepare crystalline flake graphite alkene liquid：By flotation essence crystalline flake graphite, 5040 dispersants and water according to mass ratio 30:0.2:69.8 add
Enter into homogenizer, homogeneous 3 times under the conditions of 60 DEG C, first time homogeneous pressure is 35MPa, homogeneous 20min；Second of homogeneous pressure
Power is 15MPa, homogeneous 20min；Third time homogeneous pressure is 6MPa, homogeneous 20min, obtains crystalline flake graphite alkene liquid；
e）Prepare crystalline flake graphite alkene：After crystalline flake graphite alkene liquid is spray-dried, crystalline flake graphite alkene is obtained.
Embodiment 2
Each raw material, self-control low surface tension polyurethane acrylate prepolymer 22g, Guo Jing companies are accurately weighed by weight percentage
3030Z:12g；Tetrahydrofuran acrylate 15g；Isodecyl acrylate 4g；Light trigger 184:2g ；Light trigger TPO,
1g ；The epoxy resin NAN YA of NAN YA companies NPEL-127：21g；The latent curing agent EH-3293S of ADEKA companies：
6g；Levelling wetting agent TEGO-4100:1.5g；Silane coupler KH560:1.5g and crystalline flake graphite alkene 14g.By above-mentioned each component
Sequentially add in double-planet power mixing and blending machine, it is -0.08MPa to be evacuated to vacuum, is stirred 2 hours in 500 revs/min,
Stir, hang naturally to room temperature, obtain ultraviolet cured adhesive, pack.
Wherein self-control low surface tension polyurethane acrylate prepolymer follows the steps below：
By 200 grams of PTMGs（Mn=2000）Be added in reactor, in 115 DEG C of temperature, vacuum pressure for-
Be dehydrated 2 hours under conditions of 0.08MPa, be cooled to 60 DEG C, add 34.2 grams of toluene di-isocyanate(TDI)s, vacuum pressure for-
Stirred under conditions of 0.08MPa 0.5 hour, then add 0.02 gram of dibutyl tin laurate, reacted 2.5 hours at 70 DEG C,
27 grams of hydroxyethyl methacrylates are sequentially added, 0.01g hydroquinones continues to react 2 hours at 75 DEG C, samples and uses every 30min
Infrared spectrometer analyzes the content of NCO group, when NCO peak is wholly absent, stops heating response, can obtain low surface tension
Polyurethane acrylate prepolymer, it is -33.6mN/m to measure surface tension；
The crystalline flake graphite alkene follows the steps below：
a）Prepare ore pulp：Roughing will it is broken after crystalline flake graphite alkene ore deposit and water according to mass ratio 30:100 mix, and ore pulp is made；
b）Prepare flotation crystalline flake graphite：Roughing：Ore pulp is added in flotation device, adds butyl xanthate 60g, 4min is stirred, scrapes
Steep 10min；Once purging selection：30g butyl xanthates are added into ore pulp, are stirred 1 minute, scrape bubble 4 minutes；It is secondary to scan：To ore pulp
Middle addition 20g butyl xanthates, stir 1 minute, scrape bubble 4 minutes；Obtain flotation crystalline flake graphite and mine tailing；
c）Prepare flotation essence crystalline flake graphite：Flotation crystalline flake graphite is filtered, obtains flotation essence crystalline flake graphite and filtrate；
d）Prepare crystalline flake graphite alkene liquid：By flotation essence crystalline flake graphite, 5040 dispersants and water according to mass ratio 30:0.2:69.8 add
Enter into homogenizer, homogeneous 3 times under the conditions of 60 DEG C, first time homogeneous pressure is 35MPa, homogeneous 20min；Second of homogeneous pressure
Power is 15MPa, homogeneous 20min；Third time homogeneous pressure is 6MPa, homogeneous 20min, obtains crystalline flake graphite alkene liquid；
e）Prepare crystalline flake graphite alkene：After crystalline flake graphite alkene liquid is spray-dried, crystalline flake graphite alkene is obtained.
Embodiment 3
Each raw material is accurately weighed by weight percentage, makes low surface tension polyurethane acrylate prepolymer 28g by oneself, and Sartomer is public
The CN9021 of department:6g；Tetrahydrofuran acrylate 13g；Isodecyl acrylate 6g；Light trigger 184:2g；Light trigger
TPO:1g；Epoxy resin-the 4088L of ADEKA companies：20g；The latent curing agent EH-3293S of ADEKA companies：7g；Stream
Flat wetting agent TEGO-4100:2.5g；Silane coupler KH570:1.5g and crystalline flake graphite alkene 12g.Above-mentioned each component is added successively
Enter in double-planet power mixing and blending machine, it is -0.08MPa to be evacuated to vacuum, is stirred 2 hours in 500 r/ min, stirring
Uniformly, hang naturally to room temperature, obtain ultraviolet cured adhesive, pack.
Wherein self-control low surface tension polyurethane acrylate prepolymer follows the steps below：
By 200 grams of PTMGs（Mn=2000）Be added in reactor, in 115 DEG C of temperature, vacuum pressure for-
Be dehydrated 2 hours under conditions of 0.08MPa, be cooled to 60 DEG C, add 33.5 grams of hexamethylene diisocyanates, vacuum pressure for-
Stirred under conditions of 0.08MPa 0.5 hour, then add 0.02 gram of dibutyl tin laurate, reacted 2.5 hours at 70 DEG C,
27 grams of hydroxyethyl methacrylates are sequentially added, 0.01g hydroquinones continues to react 2 hours at 75 DEG C, sampled every 30min
With the content of infrared spectrometer analysis NCO group, when NCO peak is wholly absent, stop heating response, can obtain low surface
Power polyurethane acrylate prepolymer, it is -32.1mN/m to measure surface tension；
The crystalline flake graphite alkene follows the steps below：
a）Prepare ore pulp：Roughing will it is broken after crystalline flake graphite alkene ore deposit and water according to mass ratio 30:100 mix, and ore pulp is made；
b）Prepare flotation crystalline flake graphite：Roughing：Ore pulp is added in flotation device, adds butyl xanthate 60g, 4min is stirred, scrapes
Steep 10min；Once purging selection：30g butyl xanthates are added into ore pulp, are stirred 1 minute, scrape bubble 4 minutes；It is secondary to scan：To ore pulp
Middle addition 20g butyl xanthates, stir 1 minute, scrape bubble 4 minutes；Obtain flotation crystalline flake graphite and mine tailing；
c）Prepare flotation essence crystalline flake graphite：Flotation crystalline flake graphite is filtered, obtains flotation essence crystalline flake graphite and filtrate；
d）Prepare crystalline flake graphite alkene liquid：By flotation essence crystalline flake graphite, 5040 dispersants and water according to mass ratio 30:0.2:69.8 add
Enter into homogenizer, homogeneous 3 times under the conditions of 60 DEG C, first time homogeneous pressure is 35MPa, homogeneous 20min；Second of homogeneous pressure
Power is 15MPa, homogeneous 20min；Third time homogeneous pressure is 6MPa, homogeneous 20min, obtains crystalline flake graphite alkene liquid；
e）Prepare crystalline flake graphite alkene：After crystalline flake graphite alkene liquid is spray-dried, crystalline flake graphite alkene is obtained.
Embodiment 4
Each raw material is accurately weighed by weight percentage, makes low surface tension polyurethane acrylate prepolymer 25g by oneself, and Sartomer is public
The CN9001 of department:11g;Isobornyl methacrylate 17g；Isodecyl acrylate 5g；Light trigger 184:2g ；It is light-initiated
Agent TPO:1g ；The epoxy resin NPEL-127 of NAN YA companies：22g；The latent curing agent AH-154 of aginomoto company：6g；
Levelling wetting agent TEGO-4200:2g；Silane coupler KH560:1g and crystalline flake graphite alkene 8g.Above-mentioned each component is sequentially added
In double-planet power mixing and blending machine, it is -0.08MPa to be evacuated to vacuum, is stirred 2 hours in 500 revs/min, and stirring is equal
It is even, hang naturally to room temperature, obtain ultraviolet cured adhesive, pack.
Wherein self-control low surface tension polyurethane acrylate prepolymer follows the steps below：
By 200 grams of polypropylene glycols（Mn=2000）It is added in reactor, in 115 DEG C of temperature, vacuum pressure is -0.08MPa's
Under the conditions of be dehydrated 2 hours, be cooled to 60 DEG C, add 33.5 grams of hexamethylene diisocyanates, vacuum pressure is -0.08MPa
Under conditions of stir 0.5 hour, then add 0.02 gram of dibutyl tin laurate, react 2.5 hours, sequentially add at 70 DEG C
27 grams of hydroxyethyl methacrylates, 0.01g hydroquinones continues to react 2 hours at 75 DEG C, every 30min sampling infrared spectrums
Instrument analyzes the content of NCO group, when NCO peak is wholly absent, stops heating response, can obtain low surface tension polyurethane third
Olefin(e) acid ester performed polymer, it is -32.6mN/m to measure surface tension；
The crystalline flake graphite alkene follows the steps below：
a）Prepare ore pulp：Roughing will it is broken after crystalline flake graphite alkene ore deposit and water according to mass ratio 30:100 mix, and ore pulp is made；
b）Prepare flotation crystalline flake graphite：Roughing：Ore pulp is added in flotation device, adds butyl xanthate 60g, 4min is stirred, scrapes
Steep 10min；Once purging selection：30g butyl xanthates are added into ore pulp, are stirred 1 minute, scrape bubble 4 minutes；It is secondary to scan：To ore pulp
Middle addition 20g butyl xanthates, stir 1 minute, scrape bubble 4 minutes；Obtain flotation crystalline flake graphite and mine tailing；
c）Prepare flotation essence crystalline flake graphite：Flotation crystalline flake graphite is filtered, obtains flotation essence crystalline flake graphite and filtrate；
d）Prepare crystalline flake graphite alkene liquid：By flotation essence crystalline flake graphite, 5040 dispersants and water according to mass ratio 30:0.2:69.8 add
Enter into homogenizer, homogeneous 3 times under the conditions of 60 DEG C, first time homogeneous pressure is 35MPa, homogeneous 20min；Second of homogeneous pressure
Power is 15MPa, homogeneous 20min；Third time homogeneous pressure is 6MPa, homogeneous 20min, obtains crystalline flake graphite alkene liquid；
e）Prepare crystalline flake graphite alkene：After crystalline flake graphite alkene liquid is spray-dried, crystalline flake graphite alkene is obtained.
Embodiment 5
Each raw material, self-control low surface tension polyurethane acrylate prepolymer 26g, RAHN companies are accurately weighed by weight percentage
4217:8g；Isobornyl methacrylate 23g；Light trigger 184:2g ；Light trigger TPO:1g ；ADEKA companies
Epoxy resin -4088L：21g；The latent curing agent EH-3293S of ADEKA companies：7g；Levelling wetting agent TEGO-4200:
2g；Silane coupler KH560:1g and crystalline flake graphite alkene 9g.Above-mentioned each component is sequentially added into double-planet power mixing and blending machine
Interior, it is -0.08MPa to be evacuated to vacuum, is stirred 2 hours in 500 revs/min, stirs, hang to room temperature, obtain naturally
Ultraviolet cured adhesive, pack.
Wherein self-control low surface tension polyurethane acrylate prepolymer follows the steps below：
By 200 grams of polyethylene glycol（Mn=2000）It is added in reactor, in 115 DEG C of temperature, vacuum pressure is -0.08MPa's
Under the conditions of be dehydrated 2 hours, be cooled to 60 DEG C, add 42.2 grams of IPDIs, vacuum pressure is -0.08MPa's
Under the conditions of stir 0.5 hour, then add 0.02 gram of dibutyl tin laurate, reacted 2.5 hours at 70 DEG C, sequentially add 27
Gram hydroxyethyl methacrylate, 0.01g hydroquinones continues to react 2 hours at 75 DEG C, every 30min sampling infrared spectrometers
The content of NCO group is analyzed, when NCO peak is wholly absent, stops heating response, can obtain low surface tension polyurethane propylene
Acid esters performed polymer, it is -33.6mN/m to measure surface tension；
The crystalline flake graphite alkene follows the steps below：
a）Prepare ore pulp：Roughing will it is broken after crystalline flake graphite alkene ore deposit and water according to mass ratio 30:100 mix, and ore pulp is made；
b）Prepare flotation crystalline flake graphite：Roughing：Ore pulp is added in flotation device, adds butyl xanthate 60g, 4min is stirred, scrapes
Steep 10min；Once purging selection：30g butyl xanthates are added into ore pulp, are stirred 1 minute, scrape bubble 4 minutes；It is secondary to scan：To ore pulp
Middle addition 20g butyl xanthates, stir 1 minute, scrape bubble 4 minutes；Obtain flotation crystalline flake graphite and mine tailing；
c）Prepare flotation essence crystalline flake graphite：Flotation crystalline flake graphite is filtered, obtains flotation essence crystalline flake graphite and filtrate；
d）Prepare crystalline flake graphite alkene liquid：By flotation essence crystalline flake graphite, 5040 dispersants and water according to mass ratio 30:0.2:69.8 add
Enter into homogenizer, homogeneous 3 times under the conditions of 60 DEG C, first time homogeneous pressure is 35MPa, homogeneous 20min；Second of homogeneous pressure
Power is 15MPa, homogeneous 20min；Third time homogeneous pressure is 6MPa, homogeneous 20min, obtains crystalline flake graphite alkene liquid；
e）Prepare crystalline flake graphite alkene：After crystalline flake graphite alkene liquid is spray-dried, crystalline flake graphite alkene is obtained.
Embodiment 6
Each raw material, self-control low surface tension polyurethane acrylate prepolymer 24g, Guo Jing companies are accurately weighed by weight percentage
3030Z:10g;Isobornyl methacrylate 14g；Third oxidation neopentylglycol diacrylate 6g；Light trigger 184:2g ；
Light trigger TPO:1g ；The epoxy resin NPEL-128R of NAN YA companies:23g；The latent curing agent AH- of aginomoto company
162:5g；Levelling wetting agent TEGO-4000:2.5g；Silane coupler KH570:1.5g and crystalline flake graphite alkene 11g.Will be above-mentioned each
Component is sequentially added in double-planet power mixing and blending machine, and it is -0.08MPa to be evacuated to vacuum, and 2 are stirred in 500 revs/min
Hour, stir, hang naturally to room temperature, obtain ultraviolet cured adhesive, pack.
Wherein self-control low surface tension polyurethane acrylate prepolymer follows the steps below：
By 200 grams of polyethylene glycol（Mn=2000）It is added in reactor, in 115 DEG C of temperature, vacuum pressure is -0.08MPa's
Under the conditions of be dehydrated 2 hours, be cooled to 60 DEG C, add 34.2 grams of toluene di-isocyanate(TDI)s, vacuum pressure is -0.08MPa condition
Lower stirring 0.5 hour, then adds 0.02 gram of dibutyl tin laurate, is reacted 2.5 hours at 70 DEG C, sequentially adds 27 grams of first
Base hydroxy-ethyl acrylate, 0.01g hydroquinones continue to react 2 hours at 75 DEG C, analyzed every 30min samplings with infrared spectrometer
The content of NCO group, when NCO peak is wholly absent, stops heating response, can obtain low surface tension urethane acrylate
Performed polymer, it is -34.5mN/m to measure surface tension；
The crystalline flake graphite alkene follows the steps below：
a）Prepare ore pulp：Roughing will it is broken after crystalline flake graphite alkene ore deposit and water according to mass ratio 38:100 mix, and ore pulp is made；
b）Prepare flotation crystalline flake graphite：Roughing：Ore pulp is added in flotation device, adds butyl xanthate 80g, 4min is stirred, scrapes
Steep 10min；Once purging selection：35g butyl xanthates are added into ore pulp, are stirred 1 minute, scrape bubble 4 minutes；It is secondary to scan：To ore pulp
Middle addition 20g butyl xanthates, stir 1 minute, scrape bubble 4 minutes；Obtain flotation crystalline flake graphite and mine tailing；
c）Prepare flotation essence crystalline flake graphite：Flotation crystalline flake graphite is filtered, obtains flotation essence crystalline flake graphite and filtrate；
d）Prepare crystalline flake graphite alkene liquid：By flotation essence crystalline flake graphite, 5040 dispersants and water according to mass ratio 30:0.2:69.8 add
Enter into homogenizer, homogeneous 2 times under the conditions of 60 DEG C, first time homogeneous pressure is 35MPa, homogeneous 20min；Second of homogeneous pressure
Power is 15MPa, homogeneous 20min；Obtain crystalline flake graphite alkene liquid；
e）Prepare crystalline flake graphite alkene：After crystalline flake graphite alkene liquid is spray-dried, crystalline flake graphite alkene is obtained.
Beneficial effects of the present invention are further illustrated with reference to experimental data：
1 materials and methods：
1.1 test site：Laboratory.
1.2 experiment detections：Various sample is tested using SY-ZY-01-17 testing standards to be bonded low surface energy substrates PET.
1.3 material to be tested：For embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5, embodiment 6, contrast 1
（Except polyurethane acrylate prepolymer purchased from Changxing company 6148J75 in addition to, other manufacture crafts with the embodiment of the present invention 3
Unanimously）With contrast 2（Except not plus in addition to graphene, other manufacture crafts are consistent with the embodiment of the present invention 3）Effect is done to compare.
1.4 experimental design：Experiment sets 7 processing, 2 repetitions, respectively embodiment 1, embodiment 2, embodiment 3, implementation
Example 4, embodiment 5, embodiment 6, contrast 1（It is other in addition to polyurethane acrylate prepolymer is purchased from the 6148J75 of Changxing company
Manufacture craft is consistent with the embodiment of the present invention 3）With contrast 2（Except not plus in addition to graphene, other manufacture crafts are real with the present invention
It is consistent to apply example 3）, low surface energy substrates PET is bonded respectively.
This experiment is consistent with other management in addition to processing difference except testing.
2 results and analysis
It can be seen from the results above that embodiment 3 has stronger bond effect and good electric conductivity；Although embodiment 2
Electric conductivity is better than embodiment 3, but its adhesive property substantially reduces, and does not meet design original intention, embodiment 1, embodiment 4, implements
Example 5 and the bond effect of embodiment 6 and electric conductivity are markedly less than embodiment 3；Contrast 2 is no plus graphene is substantially without electric conductivity；
Contrast 1 effect and also can not show a candle to embodiment 3, Integrated comparative, the best results of embodiment 3.
Claims (4)
1. the preparation method of the double curing conductive gluing agent of a kind of ultraviolet light, it is characterised in that follow the steps below：
15~30 parts of low surface tension polyurethane acrylate prepolymer, bifunctionality polyurethane acrylate prepolymer will be made by oneself
5~20 parts, 13~32 parts of acrylics reactive diluent, 0.5~5 part of levelling wetting agent, 2~4 parts of light trigger, asphalt mixtures modified by epoxy resin
16~30 parts of fat, 6~24 parts of 5~13 parts of latent curing agent, 1~3 part of silane coupler and crystalline flake graphite alkene are added sequentially to
It is 8~15 DEG C in temperature in mixer, pressure is -0.08~-0.098MPa, under conditions of rotating speed is 500~1000r/min,
0.5~2h is stirred, lucifuge packs, and produces the double curing conductive gluing agent of ultraviolet light；
The self-control bifunctionality polyurethane acrylate prepolymer follows the steps below：
Polyether Glycols are vacuumized into 1.5~2h of dehydration at a temperature of 110 DEG C~120 DEG C；Diisocyanate is added, in temperature
Spend for 50 DEG C~70 DEG C, under the conditions of vacuum pressure is -0.07~-0.098MPa, stir 0.5~1h；Catalyst is added, in temperature
For 70 DEG C~80 DEG C, vacuum pressure reacts 2~3h under the conditions of being -0.07~-0.098MPa；Add polymerization inhibitor and dihydroxypropyl
Ester, it is 60 DEG C~80 DEG C in temperature, vacuum pressure stirs 2~3h under the conditions of being -0.07~-0.098MPa, uses infrared spectrometer
The content of NCO group is analyzed, when NCO peak is wholly absent, stops heating response, produces low surface tension polyurethane acroleic acid
Ester performed polymer；
Polyether Glycols in the low surface tension polyurethane acrylate prepolymer, diisocyanate and crylic acid hydroxy ester
Mol ratio is 1:1.8~2.0:2~2.2, catalyst and polymerization inhibitor are respectively accounted for from system low surface tension polyurethane acrylate prepolymer
The 0.1 ‰ of aggressiveness weight~1 ‰；
The crystalline flake graphite alkene follows the steps below：
a）Prepare ore pulp：Crystalline flake graphite ore deposit and water after will be broken is according to mass ratio 25~35:100 mix, and ore pulp is made；
b）Prepare flotation crystalline flake graphite：Roughing：Ore pulp is added in flotation device, addition 50~100g of butyl xanthate, stirring 3~
5min, scrape 8~15min of bubble；Once purging selection：20~40g butyl xanthates are added into ore pulp, stirs 1 minute, scrapes 3~5 points of bubble
Clock；It is secondary to scan：20~40g butyl xanthates are added into ore pulp, stirs 1 minute, scrapes bubble 3~5 minutes；Obtain flotation scale stone
Ink and mine tailing；
c）Prepare flotation essence crystalline flake graphite：Flotation crystalline flake graphite is filtered, obtains flotation essence crystalline flake graphite and filtrate；
d）Prepare crystalline flake graphite alkene liquid：By flotation essence crystalline flake graphite, 5040 dispersants and water according to mass ratio 20~50:0.1~
0.5:50~80 are added in homogenizer, at least homogeneous 1 time under the conditions of 50~75 DEG C, and homogeneous pressure is 4~40MPa, homogeneous
Time is 5~30min, obtains crystalline flake graphite alkene liquid；
e）Prepare crystalline flake graphite alkene：After crystalline flake graphite alkene liquid is spray-dried, crystalline flake graphite alkene is obtained；
Described bifunctionality polyurethane acrylate prepolymer, refer to RAHN companies 4217, the CN9001 of Sartomer,
The CN9021 of Sartomer, state, which refine and learn the GU2500K of limited company, state refines learns the 2600K of limited company
Refined with state the mixture of one or both of the 3030Z any of the above ratio for learning limited company；
The polyether Glycols include one or both of polyethylene glycol, polypropylene glycol and PTMG to take up an official post
The mixture of meaning ratio；
The diisocyanate includes toluene di-isocyanate(TDI)（TDI）, methyl diphenylene diisocyanate（MDI）, the methylene of benzene two
Group diisocyanate (XDI), hexamethylene diisocyanate (HDI) and one kind in IPDI (IPDI) or
The mixture of two or more any ratios；
The catalyst is dibutyl tin laurate；
The polymerization inhibitor include hydroquinones, one or both of MEHQ and 2,6 toluene di-tert-butyl phenols with
The mixture of upper any ratio；
The crylic acid hydroxy ester includes hydroxy-ethyl acrylate（HEA）, hydroxypropyl acrylate (HPA), hydroxyethyl methacrylate
（HEMA）, methacrylic acid hydroxypropyl fat（HPMA）And trimethylolpropane diacrylate（TMPDA）One or more
The mixture of any ratio；
The acrylics reactive diluent includes tetrahydrofuran methyl acrylate, tetrahydrofuran acrylate, 3,3,5-
It is trimethyl-cyclohexane acrylate, isobornyl methacrylate, hydroxyethyl methacrylate, hydroxy propyl methacrylate, different
The mixture of one or both of decyl acrylate and the third oxidation neopentylglycol diacrylate any of the above ratio；
The levelling wetting agent include one or both of TEGO-4000, TEGO-4100, TEGO-4200 and TEGO-270 with
The mixture of upper any ratio；
The light trigger is 1173（2- hydroxyls -2- methyl isophthalic acids-phenylacetone）、184（1- hydroxy cyclohexyl phenylketones）、
819（It is double（2,4,6- trimethylbenzoyls）Phenylphosphine oxide）, 651 (α, α '-dimethyl benzil ketals), ITX it is (different
Propyl group thioxanthone), one kind in BP (benzophenone) and TPO (2,4,6- trimethyl benzoyl diphenyl bases phosphorous oxide)
Or the mixture of two or more any ratios；
Described epoxy resin includes Japanese ADEKA EP-4100HF, EP-4000S, EP-4901HF, EP-4088L, Taiwan
One or both of NAN YA NPEL-127, NPEL-128, NPEL-128R, NPEF-170 any of the above than mixture；
Described latent curing agent includes Japanese ADEKA EH-5031S, EH-4360S, EH-3293S, Japanese aginomoto
One or both of PN-23, PN-31, AH-154, AH-162 any of the above than mixture；
Described silane coupler includes the mixed of one or both of KH551, KH172, KH560 and KH570 any of the above ratio
Compound.
2. the preparation method of the double curing conductive gluing agent of ultraviolet light as claimed in claim 1, it is characterised in that：It is low to weigh self-control
28 parts of surface tension polyurethane acrylate prepolymer, the CN9021 of Sartomer:6 parts；13 parts of tetrahydrofuran acrylate；
6 parts of isodecyl acrylate；Light trigger 184:2 parts；Light trigger TPO:1 part；The epoxy resin of ADEKA companies-
4088L：20 parts；The latent curing agent EH-3293S of ADEKA companies：7 parts；Levelling wetting agent TEGO-4100:2.5 part；Silane
Coupling agent KH570:1.5 parts and 12 parts of crystalline flake graphite alkene.
3. the preparation method of the double curing conductive gluing agent of ultraviolet light as claimed in claim 1, it is characterised in that：The polyethers two
The molecular weight of alcohol is 1000~3000.
4. the preparation method of the double curing conductive gluing agent of ultraviolet light as claimed in claim 1, it is characterised in that：Step d）To be even
Matter 3 times, first time homogeneous pressure are 35MPa, homogeneous 20min；Second of homogeneous pressure is 15MPa, homogeneous 20min；For the third time
Homogeneous pressure is 6MPa, homogeneous 20min.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005502183A (en) * | 2001-09-06 | 2005-01-20 | フラウンホーファー−ゲゼルシャフト・ツア・フォルデルング・デア・アンゲヴァンテン・フォルシュング・エー・ファウ | Particularly conductive particles dispersed in a liquid medium, and a method for producing the same |
| CN101465409A (en) * | 2008-12-31 | 2009-06-24 | 电子科技大学 | Substrate for flexible organic optoelectronic device and preparation method thereof |
| US20100148130A1 (en) * | 2008-12-11 | 2010-06-17 | Hyun Hee Namkung | Composition for circuit connection film and circuit connection film using the same |
| CN103436213A (en) * | 2013-09-09 | 2013-12-11 | 烟台德邦科技有限公司 | Ultraviolet-curing type optical resin adhesive and preparation method thereof |
| CN103525355A (en) * | 2013-10-16 | 2014-01-22 | 烟台德邦科技有限公司 | Ultraviolet curing adhesive for liquid crystal display television side frame and preparation method of ultraviolet curing adhesive |
| CN105255435A (en) * | 2015-10-19 | 2016-01-20 | 烟台德邦科技有限公司 | Preparation method of photo-moisture dual cured hot melt polyurethane sealant |
-
2017
- 2017-06-15 CN CN201710451340.XA patent/CN107384242B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005502183A (en) * | 2001-09-06 | 2005-01-20 | フラウンホーファー−ゲゼルシャフト・ツア・フォルデルング・デア・アンゲヴァンテン・フォルシュング・エー・ファウ | Particularly conductive particles dispersed in a liquid medium, and a method for producing the same |
| US20100148130A1 (en) * | 2008-12-11 | 2010-06-17 | Hyun Hee Namkung | Composition for circuit connection film and circuit connection film using the same |
| CN101465409A (en) * | 2008-12-31 | 2009-06-24 | 电子科技大学 | Substrate for flexible organic optoelectronic device and preparation method thereof |
| CN103436213A (en) * | 2013-09-09 | 2013-12-11 | 烟台德邦科技有限公司 | Ultraviolet-curing type optical resin adhesive and preparation method thereof |
| CN103525355A (en) * | 2013-10-16 | 2014-01-22 | 烟台德邦科技有限公司 | Ultraviolet curing adhesive for liquid crystal display television side frame and preparation method of ultraviolet curing adhesive |
| CN105255435A (en) * | 2015-10-19 | 2016-01-20 | 烟台德邦科技有限公司 | Preparation method of photo-moisture dual cured hot melt polyurethane sealant |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109370507A (en) * | 2018-11-01 | 2019-02-22 | 烟台信友新材料有限公司 | A kind of three proofings adhesive and preparation method thereof of low viscosity environmental protection UV/ moisture dual cure |
| CN109370507B (en) * | 2018-11-01 | 2021-08-06 | 烟台信友新材料有限公司 | Low-viscosity environment-friendly UV/moisture dual-curing three-proofing adhesive and preparation method thereof |
| CN109651999A (en) * | 2018-12-19 | 2019-04-19 | 同光（江苏）新材料科技有限公司 | A kind of color inhibition weatherability high-strength polyurethane glue and preparation method thereof |
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| CN110256995B (en) * | 2019-06-19 | 2021-08-13 | 烟台泰盛精化科技有限公司 | Flame-retardant two-component polyether adhesive and preparation method thereof |
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| WO2021135377A1 (en) * | 2019-12-31 | 2021-07-08 | 苏州桐力光电股份有限公司 | Graphene uv pressure-sensitive adhesive and preparation method therefor |
| CN111139024A (en) * | 2019-12-31 | 2020-05-12 | 苏州桐力光电股份有限公司 | Graphene UV pressure-sensitive adhesive and preparation method thereof |
| CN112080185A (en) * | 2020-09-29 | 2020-12-15 | 湖北奥斯鸣环保科技有限公司 | Waterborne polyurethane industrial paint and preparation method thereof |
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Denomination of invention: A preparation method of UV double curing conductive adhesive Effective date of registration: 20220225 Granted publication date: 20190412 Pledgee: Shanghai Pudong Development Bank Limited by Share Ltd. Yantai branch Pledgor: YANTAI XINYOU NEW MATERIAL Co.,Ltd. Registration number: Y2022980001866 |