CN109054711A - A kind of flexible screen frame envelope frame Wear Characteristics of Epoxy Adhesive mixture and preparation method thereof - Google Patents
A kind of flexible screen frame envelope frame Wear Characteristics of Epoxy Adhesive mixture and preparation method thereof Download PDFInfo
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- CN109054711A CN109054711A CN201810912139.1A CN201810912139A CN109054711A CN 109054711 A CN109054711 A CN 109054711A CN 201810912139 A CN201810912139 A CN 201810912139A CN 109054711 A CN109054711 A CN 109054711A
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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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- 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
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/66—Mercaptans
-
- 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
- C09J11/04—Non-macromolecular additives inorganic
-
- 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
-
- 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
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Abstract
A kind of flexible screen frame envelope frame Wear Characteristics of Epoxy Adhesive mixture, is made of: 50-70 parts of epoxy resin following component in parts by weight；5-10 parts of epoxide diluent；25-35 parts of curing agent；0.1-2 parts of catalyst；0.1-2 parts of stabilizer；5-10 parts of toughener；20-40 parts of filler；0.2-2 parts of auxiliary agent；The epoxy resin is one of bisphenol F epoxy resin or a variety of mixtures；The epoxide diluent is one of oxetanes, aliphatic glycidyl ether or a variety of mixtures；The curing agent is one or more mixtures of second level polythiol hardener；The catalyst is latency amine；The stabilizer is one or more mixtures of phosphoric acid ester stabilizer；The toughener is polyalcohol toughener；This flexible screen frame envelope frame Wear Characteristics of Epoxy Adhesive mixture is with strong to plastic rubber substrate bonding force, flexibility is good, solidification temperature is low and stability is good, water boiling resistance, hygroscopicity is small and reaches the standard of Halogen.
Description
Technical field
The invention belongs to field of adhesive technology, and in particular to a kind of flexible screen frame envelope frame Wear Characteristics of Epoxy Adhesive mixture.
Background technique
As the fast development of electronics and information industry, especially smart phone, Intelligent bracelet, TV, computer etc. are consumed
Electronic product shows that screen also experiencings " spherical surface screen-plane screen-towards the rapid development in the directions such as frivolous, portable, intelligent
The rapid evolution and iteration of flexible screen ", flexible screen is because of its application of characteristic with flexible bendable to wearable equipment
Far-reaching influence and development are brought, the following flexible screen will be widely applied with the continuous infiltration of intelligent terminal.
Current flexible screen technology mainly concentrates on flexible liquid crystal technology (Flexible LCD, abbreviation FLCD)
It with two aspects of flexible organic light emitting display technology (Flexible OLED, abbreviation FOLED), take height can
Band, the display technology folded become possible.So that flexible screen display technology develops rapidly, it has also become the point of electronics and information industry
End technology.
Flexible screen frame, which seals frame and sealed with the envelope frame that Wear Characteristics of Epoxy Adhesive mixture is mainly used for flexible screen display frame, to be glued
It connects, the envelope frame seal protection of frame envelope frame protection and flexibility FOLED including flexible FLCD, so its performance requirement is with respect to liquid crystal
Display (LCD) frame wants high with traditional single-component epoxy viscose binder, it is desirable that strong to plastic cement membrane material bonding force, flexible flexibility
Good, solidification temperature is low and stability is good, water boiling resistance, hygroscopicity are small and reach the standard of Halogen etc..
The traditional single-component epoxy viscose binder of LCD frame because it is inadequate to plastic rubber substrate bonding force, flexility is poor,
The problems such as solidification temperature is high, the envelope frame sealing performance that will lead to flexible screen is inadequate, bending property is poor and high temperature plastic cement base
The problems such as material, is not suitable for the frame envelope frame seal protection of flexible screen.
Summary of the invention
The technical problem to be solved in the present invention is that: overcome traditional single-component epoxy viscose binder to squeeze plastic cement and wipes bonding force
Not enough, the problems such as flexility is poor, solidification temperature is high proposes that a kind of flexible screen frame seals frame Wear Characteristics of Epoxy Adhesive mixture and its preparation
Method, binder performance feature are as follows: viscosity: 300 ± 100P (25 ± 1 DEG C)；Tg≥100℃；Solidification temperature≤85 DEG C, solidification
Time≤30min；Shear strength >=10MPa；Hygroscopicity≤5g/m2 (350 μm of film thickness, 50 DEG C/100%RH, for 24 hours)；Water boiling resistance
≥8h；Low-temperature storage time >=6 month (- 15 DEG C)；Cl≤900ppm, Br≤900ppm, Cl+Br≤1500ppm.
To solve the above-mentioned problems, the present invention proposes following technical proposal: a kind of flexible screen frame envelope frame Wear Characteristics of Epoxy Adhesive
Mixture is made of following component in parts by weight: 50-70 parts of epoxy resin；5-10 parts of epoxide diluent；Curing agent
25-35 parts；0.1-2 parts of catalyst；0.1-2 parts of stabilizer；5-10 parts of toughener；20-40 parts of filler；0.2-2 parts of auxiliary agent；
The epoxy resin is one of bisphenol F epoxy resin or a variety of mixtures；
The epoxide diluent is one of oxetanes, aliphatic glycidyl ether or a variety of mixtures；
The curing agent is one or more mixtures of following second level polythiol hardener: four (3- mercaptobutyric acid) seasons penta
Four alcohol esters, 3 (3- mercaptobutyric acid) cyanuric acid, three ethyl alcohol ester, two (3- mercaptobutyric acid) butanediol esters and three (3- mercaptobutyric acids) third
Alkane front three alcohol ester；
The catalyst is one or more mixtures of following latency amine: imidazole adducts, imidazoles, modified amine
Class；
The stabilizer is one or more mixtures of following phosphoric acid ester stabilizer: four (2,4-di-tert-butyls
4,4 ' xenyl of base -) biphosphinate, poly- 4,4, isopropylidene diphenol C12-15 alcohol phosphite ester, double octadecyl pentaerythrites
Diphosphites；
The toughener is polyalcohol toughener；
The filler are as follows: one of talcum powder, fumed silica, calcium carbonate, titanium dioxide or a variety of mixtures；
The auxiliary agent is one of following defoaming agent, dispersing agent or a variety of mixtures；
The defoaming agent is selected from: the non-aqueous lotion of brokenly bubble polysiloxanes, brokenly bubble polymer and polysiloxane solution contain gas phase
Organic modified polyorganosiloxane, organic modified polyorganosiloxane, the dimethyl polysiloxane containing fumed silica, phosphorus of silica
Sour lipid hydrophobicity defoams foam inhibitor, esters of acrylic acid defoaming agent, organic modified polyorganosiloxane；
The dispersing agent is selected from: the block copolymer, amine-containing of high molecular weight copolymer alkylammonium salt, the affinity groups containing pigment
The polymeric polycarboxylic acid solution of radical derivative, the modified polyether containing high pigment affinity groups.
The above technical solution is further limited in that flexible screen frame of the present invention seals frame epoxy glue binder performance
Are as follows: viscosity: 300 ± 100P (25 ± 1 DEG C)；Tg≥100℃；Solidification temperature≤85 DEG C, curing time≤30min；Shear strength
≥10MPa；Hygroscopicity≤5g/m2 (350 μm of film thickness, 50 DEG C/100%RH, for 24 hours)；Water boiling resistance >=8h；Low-temperature storage time >=6
A month (- 15 DEG C)；Cl≤900ppm, Br≤900ppm, Cl+Br≤1500ppm.
To solve the above-mentioned problems, the present invention also proposes following technical proposal: flexible screen frame envelope frame described in one kind is used
The preparation method of Wear Characteristics of Epoxy Adhesive mixture, comprising the following steps:
Step 1: weighing according to parts by weight: 50-70 parts of epoxy resin；5-10 parts of epoxide diluent；Curing agent 25-35
Part；0.1-2 parts of catalyst；0.1-2 parts of stabilizer；5-10 parts of toughener；20-40 parts of filler；0.2-2 parts of auxiliary agent；
Step 2: first epoxy resin, epoxide diluent, curing agent, catalyst, stabilizer, toughener, auxiliary agent being added and held
It in device, is dispersed with stirring uniformly using high speed disperser, filler is then added while stirring, then high speed dispersion stirs 2-3 hours,
Until stirring evenly；
Step 3: the glue stirred evenly being subjected to three roller grindings using three-roll grinder, is ground equal to filler fineness twice
One uniformly.
The present invention, as epoxy hardener, under the action of basic catalyst, generates sulphur anion and epoxy using mercaptan
The addition reaction of group progress equimolar ratio, and the addition of epoxy group and active hydrogen compounds (amino, acid, phenol, sulfydryl)
Reaction has lower solid relative to self-polymeric reaction of the epoxy under anhydride copolymers condensation reaction and basic group or acidic-group
Change shrinking percentage, bonding force is stronger, and flexible softness is more preferable, while solidification temperature is also lower, curing rate faster, and because of sulphur
Anion stronger nucleophilicity in active hydrogen compounds is also more able to achieve with the other groups comparison in epoxy addition reaction
The low temperature and rapid curing of epoxy resin.So can achieve low cure shrinkage rate using the program, bonding force is strong, flexible
Softness is more preferable, while realizing low temperature and quick-setting performance.
For the present invention using second level mercaptan as epoxy hardener, thiol bond more preferably, while using acid in secondary position, stability
Property stabilizer reinforce system stability, improve the storage stability of epoxy adhesive.
The invention has the following advantages: the present invention is that a kind of flexible screen frame seals frame Wear Characteristics of Epoxy Adhesive mixture, have
It is strong to plastic rubber substrate bonding force, flexibility is good, solidification temperature is low and stability is good, water boiling resistance, hygroscopicity is small and reaches Halogen
Standard the advantages that.Overcome traditional single-component epoxy viscose binder have weak to plastic rubber substrate bonding force, flexility is poor, solidification
The problems such as temperature is high and low-temperature setting cannot coexist with storage stability completes a kind of flexible screen frame envelope frame epoxy glue
The preparation of adhesive, and the adhesive feature are as follows: viscosity: 300 ± 100P (25 ± 1 DEG C)；Tg≥100℃；Solidification temperature≤85
DEG C, curing time≤30min；Shear strength >=10MPa；Hygroscopicity≤5g/m2 (350 μm of film thickness, 50 DEG C/100%RH, for 24 hours)；
Water boiling resistance >=8h；Low-temperature storage time >=6 month (- 15 DEG C)；Cl≤900ppm, Br≤900ppm, Cl+Br≤1500ppm.
Specific embodiment
The present invention proposes a kind of flexible screen frame envelope frame Wear Characteristics of Epoxy Adhesive mixture, by following group in parts by weight
It is grouped as: 50-70 parts of epoxy resin；5-10 parts of epoxide diluent；25-35 parts of curing agent；0.1-2 parts of catalyst；Stabilizer
0.1-2 parts；5-10 parts of toughener；20-40 parts of filler；0.2-2 parts of auxiliary agent.
The epoxy resin is one of following bisphenol F epoxy resin or a variety of mixtures: bisphenol f type epoxy resin
(NPEF-170 of Jia Dida new material), bisphenol f type epoxy resin (the EPALLOY 8220E of Jia Dida new material), bisphenol-f type
Epoxy resin (the EPALLOY 8230E of Jia Dida new material), (nippon lives aurification strain formula to bisphenol f type epoxy resin
The YD-8125 of commercial firm), bisphenol f type epoxy resin (ZX-1059 that nippon lives golden Chemical Co., Ltd.).
The epoxide diluent is one of oxetanes, aliphatic glycidyl ether or a variety of mixtures.
The oxetanes is selected from: oxetanes (the CURALITE OX that chemistry is won in Shanghai west).
The aliphatic glycidyl ether is one of following substance or a variety of mixtures: the dilution of bifunctionality epoxy
Agent (JD-350 of Jia Dida new material), bifunctionality epoxide diluent (JD-351 of Jia Dida new material), trihydroxy methyl third
Alkane triglycidyl ether (the ERISYS GE-30 of Jia Dida new material), trimethylolethane trimethacrylate glycidol ether (Jia Didaxin
The ERISYS GE-31 of material), propoxylated glycerol triglycidyl ether (the ERISYS GE-36 of Jia Dida new material).
The curing agent is one or more mixtures of following second level polythiol hardener: four (3- mercaptobutyric acid) seasons penta
Four alcohol esters (PE1 of Japanese Showa Denko K. K), (the Japanese Showa electrician strain of 3 (3- mercaptobutyric acid) cyanuric acid, three ethyl alcohol ester
The NR1 of formula commercial firm), two (3- mercaptobutyric acid) butanediol esters (BD1 of Japanese Showa Denko K. K) and three (3- sulfydryl fourths
Acid) propane front three alcohol ester (TPMB of Japanese Showa Denko K. K) etc..
The catalyst is one or more mixtures of following latency amine: imidazole adducts (Japanese aginomoto
The PN-23 of fine chemistry Co., Ltd.), imidazole adducts (PN-31 of Japanese aginomoto fine chemistry Co., Ltd.), imidazoles add
At object (PN-40 of Japanese aginomoto fine chemistry Co., Ltd.), imidazoles (EH-3293S of Japanese ADEKA), modified amine (day
The EH-5031S of this ADEKA) etc..
The stabilizer is one or more mixtures of following phosphoric acid ester stabilizer: four (2,4-di-tert-butyls
4,4 ' xenyl of base -) biphosphinate (the Hostanox P-EPQ of Switzerland's Clariant), poly- 4,4, isopropylidene diphenol C12-15 alcohol
Phosphite ester (DP-613 of U.S. ICC-DOVER), double octadecyl pentaerythritol diphosphites be (U.S. ICC-DOVER's
DP-682) etc..
The toughener is one of following polyalcohol toughener or a variety of mixtures: extraordinary polyalcohol (Shang Haixi
Win the CAPA 4101 of chemistry), extraordinary polyalcohol (JA-782 of Jia Dida new material), extraordinary polyalcohol (Jia Dida new material
JA-783)。
The filler are as follows: one of talcum powder, fumed silica, calcium carbonate, titanium dioxide are a variety of；
The talcum powder is selected from: Italian Yi meter Fa ratio HTP1, HTP2, HM4, HTPULTRA5, Dongguan receive rubber and plastic difficult to understand
Type1048,Type1055；The fumed silica is selected from: Germany watt gram H20, win wound Degussa AEROSIL R792,
AEROSIL R794,AEROSIL R805,AEROSIL R812；The calcium carbonate is selected from: the grand magnificent canonical chemical industry CCR701 in Wuhan,
Guangzhou, which is opened up, flies 11000 mesh precipitated calcium carbonate of chemical industry；The titanium dioxide is selected from: German Kang Nuosi KRONOS 2233, Dupont R-
960、R-103。
The auxiliary agent is one of following defoaming agent, dispersing agent or a variety of mixtures.
The defoaming agent is selected from: the non-aqueous lotion of brokenly bubble polysiloxanes (Bick chemistry BYK067A), brokenly bubble polymer and poly-
Siloxane solution (Bick chemistry BYK141), the organic modified polyorganosiloxane containing fumed silica (win wound Degussa TEGO
Airex 900), organic modified polyorganosiloxane (win wound Degussa TEGO Airex 962), the dimethyl containing fumed silica
Polysiloxanes (winning wound Degussa TEGO Foamex N), phosphoric acid lipid hydrophobicity defoaming foam inhibitor (first create chemistry MOUSSEX
561PL), esters of acrylic acid defoaming agent (first creating chemistry MOUSSEX SF254), organic modified polyorganosiloxane (first wound chemistry
MOUSSEX 338SL)。
The dispersing agent is selected from: high molecular weight copolymer alkylammonium salt (Bick chemistry BYK9076), affinity groups containing pigment
Block copolymer (Bick chemistry BYK2155), amine-containing radical derivative polymeric polycarboxylic acid solution (win wound Degussa TEGO
630) modified polyether (winning wound Degussa TEGO 650), containing high pigment affinity groups.
The present invention also proposes the preparation method of above-mentioned flexible screen frame envelope frame Wear Characteristics of Epoxy Adhesive mixture comprising following step
It is rapid:
Step 1: weighing according to parts by weight: 50-70 parts of epoxy resin；5-10 parts of epoxide diluent；Curing agent 25-35
Part；0.1-2 parts of catalyst；0.1-2 parts of stabilizer；5-10 parts of toughener；20-40 parts of filler；0.2-2 parts of auxiliary agent；
Step 2: first epoxy resin, epoxide diluent, curing agent, catalyst, stabilizer, toughener, auxiliary agent being added and held
It in device, is dispersed with stirring uniformly using high speed disperser, filler is then added while stirring, then high speed dispersion stirs 2-3 hours,
Until stirring evenly；
Step 3: the glue stirred evenly being subjected to three roller grindings using three-roll grinder, is ground equal to filler fineness twice
One uniformly.
Flexible screen frame produced by the present invention seals frame epoxy glue binder performance are as follows: viscosity: 300 ± 100P (25 ± 1
℃)；Tg≥100℃；Solidification temperature≤85 DEG C, curing time≤30min；Shear strength >=10MPa；Hygroscopicity≤5g/m2 (film
It is 350 μm thick, 50 DEG C/100%RH, for 24 hours)；Water boiling resistance >=8h；Low-temperature storage time >=6 month (- 15 DEG C)；Cl≤900ppm, Br
≤ 900ppm, Cl+Br≤1500ppm.
Prepare embodiment 1
Weigh following each component:
Epoxy resin: 50g (bisphenol F epoxy resin of trade mark NPEF-170),
Epoxide diluent: 5g (oxetanes of trade mark CURALITE OX),
Curing agent: 25g (mercaptan of trade mark PE1),
Catalyst: 0.1g (catalyst of trade mark PN23),
Stabilizer: 0.1g (stabilizer of trade mark Hostanox P-EPQ)
Toughener: 5g (polyalcohol of trade mark CAPA4101),
Filler: 20g (the talcum powder 19g of trade mark HTP1, the fumed silica 1g of trade mark H20)
Auxiliary agent: 0.2g (the defoaming agent 0.1g of trade mark BYK067A；The dispersing agent 0.1g of trade mark BYK9076).
It fed, mixed according to above-mentioned preparation method, is dispersed with stirring and three rollers are ground, until uniformly deaeration point again and again
Fill getting the product.
Prepare embodiment 2
Weigh following each component:
Epoxy resin: 60g (bisphenol F epoxy resin of trade mark YD-8125),
Epoxide diluent: 6g (the oxetanes 3g of trade mark CURALITE OX；The aliphatic of trade mark JD-350 3g is shunk
Glycerin ether),
Curing agent: 30g (mercaptan of the NR1 of the trade mark),
Catalyst: 0.5g (catalyst of trade mark PN-31),
Stabilizer: 0.5g (stabilizer of trade mark DP-613)
Toughener: 6g (trade mark JA-782 polyalcohol),
Filler: 30g (the fumed silica 2g of the talcum powder 28g of trade mark HTP2, the trade mark AEROSIL R792)
Auxiliary agent: 1g (the defoaming agent 0.5g of trade mark BYK141；The dispersing agent 0.5g of trade mark BYK2155).
It fed, mixed according to above-mentioned preparation method, is dispersed with stirring and three rollers are ground, until uniformly deaeration point again and again
Fill getting the product.
Prepare embodiment 3
Weigh following each component:
Epoxy resin: 70g (bisphenol F epoxy resin of trade mark EPALLOY 8220E),
Epoxide diluent: 8g (the oxetanes 4g of trade mark CURALITE OX；The aliphatic of trade mark ERISYS GE-30
Glycidol ether 4g),
Curing agent: 35g (mercaptan of the BD1 of the trade mark),
Catalyst: 2g (catalyst of trade mark PN-40),
Stabilizer: 2g (stabilizer of trade mark DP-682)
Toughener: 7g (polyalcohol of trade mark JA-783),
Filler: 40g (fumed silica 3g, the trade mark of the talcum powder 36g of trade mark HM4, the trade mark AEROSIL R794
The calcium carbonate 1g of CCR701)
Auxiliary agent: 2g (the defoaming agent 1g of trade mark TEGO Airex 900；The dispersing agent 1g of trade mark TEGO 630).
It fed, mixed according to above-mentioned preparation method, is dispersed with stirring and three rollers are ground, until uniformly deaeration point again and again
Fill getting the product.
Prepare embodiment 4
Weigh following each component:
Epoxy resin: 50g (the Bisphenol F ring of the bisphenol F epoxy resin 20g of trade mark ZX-1059, trade mark EPALLOY 8230E
Oxygen resin 30g),
Epoxide diluent: 10g (trade mark CURALITE OX oxetanes 5g；The aliphatic of trade mark ERISYS GE-36 contracts
Water glycerin ether 5g),
Curing agent: 25g (mercaptan of the TPMB of the trade mark),
Catalyst: 2g (catalyst of trade mark EH-3293S),
Stabilizer: 2g (stabilizer of trade mark Hostanox P-EPQ)
Toughener: 8g (polyalcohol of trade mark CAPA4101),
Filler: 20g (the talcum powder 17g of trade mark HTPULTRA5；The fumed silica 1g of trade mark AEROSIL R805；Board
Number Guangzhou, which is opened up, flies 11000 mesh precipitated calcium carbonate 2g)
Auxiliary agent: 0.4g (the defoaming agent 0.2g of trade mark TEGO Airex 962；The dispersing agent 0.2g of trade mark TEGO 650).
It fed, mixed according to above-mentioned preparation method, is dispersed with stirring and three rollers are ground, until uniformly deaeration point again and again
Fill getting the product.
Prepare embodiment 5
Weigh following each component:
Epoxy resin: the 60g (bisphenol F epoxy resin of the bisphenol F epoxy resin 30g of trade mark YD-8125, trade mark ZX-1059
30g),
Epoxide diluent: 8g (oxetanes of trade mark CURALITE OX),
Curing agent: 30g (mercaptan of the PE1 of the trade mark),
Catalyst: 1g (catalyst of trade mark EH-5031S),
Stabilizer: 1g (stabilizer of trade mark Hostanox P-EPQ)
Toughener: 9g (polyalcohol of trade mark JA-783),
Filler: 30g (the fumed silica 2g of the talcum powder 27g of trade mark Type1048, the trade mark AEROSIL R812；Board
Number 2233 titanium dioxide 1g of KRONOS)
Auxiliary agent: 1g (the defoaming agent 0.5g of trade mark TEGO Foamex N；The dispersing agent 0.5g of trade mark BYK9076).
It fed, mixed according to above-mentioned preparation method, is dispersed with stirring and three rollers are ground, until uniformly deaeration point again and again
Fill getting the product.
Prepare embodiment 6
Weigh following each component:
Epoxy resin: the 70g (Bisphenol F of the bisphenol F epoxy resin 35g of trade mark NPEF-170, trade mark EPALLOY 8220E
Epoxy resin 35g),
Epoxide diluent: 10g (oxetanes of trade mark CURALITE OX),
Curing agent: 35g (mercaptan of the NR1 of the trade mark),
Catalyst: 1g (catalyst of trade mark PN-31),
Stabilizer: 1g (stabilizer of trade mark Hostanox P-EPQ)
Toughener: 10g (nitrile rubber of trade mark CTBN1300X8),
Filler: 40g (the fumed silica 3g of the talcum powder 35g of trade mark Type1055, trade mark H20, trade mark R-960
Titanium dioxide 2g)
Auxiliary agent 1.6g (the defoaming agent 0.8g of trade mark MOUSSEX 561PL；The dispersing agent 0.8g of trade mark BYK2155).
It fed, mixed according to above-mentioned preparation method, is dispersed with stirring and three rollers are ground, until uniformly deaeration point again and again
Fill getting the product.
Prepare embodiment 7
Weigh following each component:
Epoxy resin: 50g (the Bisphenol F ring of the bisphenol F epoxy resin 30g of trade mark YD-8125, trade mark EPALLOY 8230E
Oxygen resin 20g),
Epoxide diluent: 5g (the oxetanes 2g of trade mark CURALITE OX；The aliphatic of trade mark JD-350 is shunk sweet
Oily ether 3g),
Curing agent: 25g (mercaptan of the BD1 of the trade mark),
Catalyst: 1g (catalyst of trade mark PN-40),
Stabilizer: 1g (stabilizer of trade mark Hostanox P-EPQ)
Toughener: 8g (polyalcohol of trade mark CAPA4101),
Filler: 20g (the fumed silica 1g of the talcum powder 19g of trade mark HTP1, the trade mark AEROSIL R792)
Auxiliary agent: 0.2g (the defoaming agent 0.1g of trade mark MOUSSEX SF254；The dispersing agent 0.1g of trade mark TEGO 630).
It fed, mixed according to above-mentioned preparation method, is dispersed with stirring and three rollers are ground, until uniformly deaeration point again and again
Fill getting the product.
Prepare embodiment 8
Weigh following each component:
Epoxy resin: the 60g (bisphenol F epoxy resin of the bisphenol F epoxy resin 30g of trade mark ZX-1059, trade mark YD-8125
30g),
Epoxide diluent: 9g (the oxetanes 4g of trade mark CURALITE OX；The aliphatic of trade mark ERISYS GE-30
Glycidol ether 5g),
Curing agent: 30g (mercaptan of the PE1 of the trade mark),
Catalyst: 1g (catalyst of trade mark PN23),
Stabilizer: 1g (stabilizer of trade mark Hostanox P-EPQ),
Toughener: 5g (polyalcohol of trade mark CAPA4101),
Filler: 30g (the fumed silica 1g of the talcum powder 19g of trade mark HM4, the trade mark AEROSIL R794)
Auxiliary agent: 1g (the defoaming agent 0.5g of trade mark BYK067A；The dispersing agent 0.5g of trade mark BYK9076).
It fed, mixed according to above-mentioned preparation method, is dispersed with stirring and three rollers are ground, until uniformly deaeration point again and again
Fill getting the product.
Prepare embodiment 9
Weigh following each component:
Epoxy resin: 70g (bisphenol F epoxy resin of trade mark ZX-1059),
Epoxide diluent: 10g (the oxetanes 6g of trade mark CURALITE OX；The aliphatic of trade mark ERISYS GE-36
Glycidol ether 4g),
Curing agent: 35g (mercaptan of the PE1 of the trade mark),
Catalyst: 1g (catalyst of trade mark PN23),
Stabilizer: 1g (stabilizer of trade mark Hostanox P-EPQ),
Toughener: 8g (polyalcohol of trade mark JA-782),
Filler: 40g (the fumed silica 3g of the talcum powder 33g of trade mark Type1048, the trade mark AEROSIL R812；Board
The calcium carbonate 2g of number CCR701；The titanium dioxide 2g of trade mark KRONOS 2233),
Auxiliary agent: 2g (the defoaming agent 1g of trade mark BYK141；The dispersing agent 1g of trade mark TEGO 630).
It fed, mixed according to above-mentioned preparation method, is dispersed with stirring and three rollers are ground, until uniformly deaeration point again and again
Fill getting the product.
Prepare embodiment 10
Weigh following each component:
Epoxy resin: 70g (the bisphenol F epoxy resin 20g of trade mark ZX-1059；The Bisphenol F epoxy tree of trade mark NPEF-170
Rouge 30g；The bisphenol F epoxy resin 20g of trade mark YD-8125),
Epoxide diluent: 7g (oxetanes of trade mark CURALITE OX),
Curing agent: 35g (mercaptan of the PE1 of the trade mark),
Catalyst: 1g (catalyst of trade mark PN23),
Stabilizer: 1g (stabilizer of trade mark Hostanox P-EPQ)
Toughener: 10g (polyalcohol of trade mark JA-783),
Filler: 30g (the fumed silica 2g of the talcum powder 24g of trade mark Type1055, trade mark H20；Trade mark CCR701's
Calcium carbonate 2g；The titanium dioxide 2g of trade mark R-960),
Auxiliary agent: 1.2g (the defoaming agent 0.6g of trade mark BYK067A；The dispersing agent 0.6g of trade mark BYK9076).
It fed, mixed according to above-mentioned preparation method, is dispersed with stirring and three rollers are ground, until uniformly deaeration point again and again
Fill getting the product.
Adhesive samples made from above 10 embodiments are tested for the property, mainly test its viscosity, vitrifying turns
The performances such as temperature (Tg), curing rate, shear strength, hygroscopicity, water boiling resistance, low-temperature storage, content of halogen.
The specific test method is as follows:
Viscosity: NDJ-1 rotary viscosimeter is used, tests gelatin viscosity at 25 DEG C.
Glass transition temperature (Tg): its Tg is tested using TMA thermomechanical analyzer；
Curing rate: its cured temperature and time is tested using baking oven and stopwatch.
Shear strength: the shear strength that its PET glues PET is tested using universal tensile test machine；
Hygroscopicity: balance, film thickness gauge and climatic chamber test 350 μm of its film thickness, and 50 DEG C/100%RH, suction for 24 hours
It is moist；
Water boiling resistance: its water boiling resistance performance is tested using water cooker；
Low-temperature storage performance: storage stability when testing its -15 DEG C using household freezer；
Content of halogen: the content of its chlorine element and bromo element is tested using Ux-220 energy color dispersing X fluorescent spectrometer；
Test performance data such as table 1.
Viscosity: 300 ± 100P (25 ± 1 DEG C)；Tg≥100℃；Solidification temperature≤85 DEG C, curing time≤30min；Shearing
Intensity >=10MPa；Hygroscopicity≤5g/m2 (350 μm of film thickness, 50 DEG C/100%RH, for 24 hours)；Water boiling resistance >=8h；The low-temperature storage time
>=6 months (- 15 DEG C)；Cl≤900ppm, Br≤900ppm, Cl+Br≤1500ppm.
1 various embodiments of the present invention of table prepare the properties test table of product
By the performance test results and the comparison of table 1 it is found that this product has the strong, flexibility to plastic rubber substrate bonding force
The advantages that good, solidification temperature is low and stability is good, water boiling resistance, hygroscopicity are small and reaches the standard of Halogen.It overcomes traditional single
Component epoxy viscose binder has that weak to plastic rubber substrate bonding force, flexility is poor, solidification temperature is high and low-temperature setting and storage
The problems such as stability cannot coexist is a flexible screen frame envelope frame Wear Characteristics of Epoxy Adhesive mixture haveing excellent performance.
Claims (3)
1. a kind of flexible screen frame seals frame Wear Characteristics of Epoxy Adhesive mixture, it is made of following component in parts by weight: epoxy
50-70 parts of resin；5-10 parts of epoxide diluent；25-35 parts of curing agent；0.1-2 parts of catalyst；0.1-2 parts of stabilizer；Toughener
5-10 parts；20-40 parts of filler；0.2-2 parts of auxiliary agent；
The epoxy resin is one of bisphenol F epoxy resin or a variety of mixtures；
The epoxide diluent is one of oxetanes, aliphatic glycidyl ether or a variety of mixtures；
The curing agent is one or more mixtures of following second level polythiol hardener: four (3- mercaptobutyric acid) pentaerythrites
Ester, 3(3- mercaptobutyric acid) three ethyl alcohol ester of cyanuric acid, two (3- mercaptobutyric acid) butanediol esters and three (3- mercaptobutyric acid) propane three
Methanol ester；
The catalyst is one or more mixtures of following latency amine: imidazole adducts, imidazoles, modified amine；
The stabilizer is one or more mixtures of following phosphoric acid ester stabilizer: four (2,4-di-tert-butyl-phenyls-
4,4 ' xenyls) biphosphinate, poly- 4,4, isopropylidene diphenol C12-15 alcohol phosphite ester, double octadecyl pentaerythrites two are sub-
Phosphate；
The toughener is polyalcohol toughener；
The filler are as follows: one of talcum powder, fumed silica, calcium carbonate, titanium dioxide or a variety of mixtures；
The auxiliary agent is one of following defoaming agent, dispersing agent or a variety of mixtures；
The defoaming agent is selected from: the non-aqueous lotion of brokenly bubble polysiloxanes, brokenly bubble polymer and polysiloxane solution, dioxy containing gas phase
Organic modified polyorganosiloxane, organic modified polyorganosiloxane, the dimethyl polysiloxane containing fumed silica, phosphate ester of SiClx
Class hydrophobicity defoams foam inhibitor, esters of acrylic acid defoaming agent, organic modified polyorganosiloxane；
The dispersing agent is selected from: high molecular weight copolymer alkylammonium salt, the affinity groups containing pigment block copolymer, amino-contained spread out
Polymeric polycarboxylic acid solution, the modified polyether containing high pigment affinity groups of biology.
2. a kind of flexible screen frame according to claim 1 seals frame Wear Characteristics of Epoxy Adhesive mixture, which is characterized in that the present invention is soft
Property screen frame seal frame epoxy glue binder performance are as follows: viscosity: 300 ± 100P(25 ± 1 DEG C)；Tg≥100℃；Solidification temperature≤
85 DEG C, curing time≤30min；Shear strength >=10MPa；Hygroscopicity≤350 μm of 5g/m2(film thickness, 50 DEG C/100%RH,
For 24 hours)；Water boiling resistance >=8h；Low-temperature storage time >=6 month (- 15 DEG C)；Cl≤900ppm, Br≤900ppm, Cl+Br≤
1500ppm。
3. a kind of preparation method of flexible screen frame envelope frame Wear Characteristics of Epoxy Adhesive mixture as described in claim 1, which is characterized in that
Itself the following steps are included:
Step 1: weighing according to parts by weight: 50-70 parts of epoxy resin；5-10 parts of epoxide diluent；25-35 parts of curing agent；It urges
0.1-2 parts of agent；0.1-2 parts of stabilizer；5-10 parts of toughener；20-40 parts of filler；0.2-2 parts of auxiliary agent；
Step 2: first epoxy resin, epoxide diluent, curing agent, catalyst, stabilizer, toughener, auxiliary agent are added in container,
It is dispersed with stirring uniformly using high speed disperser, filler is then added while stirring, then high speed dispersion stirs 2-3 hours, until
It stirs evenly；
Step 3: the glue stirred evenly being subjected to three roller grindings using three-roll grinder, grinding is uniform to filler fineness twice
It is even.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810912139.1A CN109054711A (en) | 2018-08-10 | 2018-08-10 | A kind of flexible screen frame envelope frame Wear Characteristics of Epoxy Adhesive mixture and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810912139.1A CN109054711A (en) | 2018-08-10 | 2018-08-10 | A kind of flexible screen frame envelope frame Wear Characteristics of Epoxy Adhesive mixture and preparation method thereof |
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|---|---|---|---|
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110184011A (en) * | 2019-06-21 | 2019-08-30 | 上海本诺电子材料有限公司 | A kind of low-temperature fast-curing epoxy glue |
| CN110194942A (en) * | 2019-06-20 | 2019-09-03 | 广州机械科学研究院有限公司 | A kind of low-temperature rapid thermal cured one-component epoxy adhesive and preparation method thereof |
| CN110684493A (en) * | 2019-10-12 | 2020-01-14 | 深圳飞世尔新材料股份有限公司 | Epoxy adhesive for flexible screen packaging |
| CN111440579A (en) * | 2019-12-24 | 2020-07-24 | 武汉市三选科技有限公司 | High-flexibility epoxy resin adhesive, and preparation method and application thereof |
| CN111849403A (en) * | 2020-08-10 | 2020-10-30 | 东莞初创应用材料有限公司 | Flexible epoxy adhesive for packaging and protecting components on FPC (Flexible printed Circuit) and preparation method thereof |
| CN112877013A (en) * | 2019-11-29 | 2021-06-01 | 深圳市优宝新材料科技有限公司 | Adhesive for screen and method of using the same |
| CN113583603A (en) * | 2021-08-19 | 2021-11-02 | 江苏矽时代材料科技有限公司 | Low-temperature fast-curing epoxy structural adhesive and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110194942A (en) * | 2019-06-20 | 2019-09-03 | 广州机械科学研究院有限公司 | A kind of low-temperature rapid thermal cured one-component epoxy adhesive and preparation method thereof |
| CN110194942B (en) * | 2019-06-20 | 2022-05-24 | 广州机械科学研究院有限公司 | Low-temperature fast thermosetting one-component epoxy adhesive and preparation method thereof |
| CN110184011A (en) * | 2019-06-21 | 2019-08-30 | 上海本诺电子材料有限公司 | A kind of low-temperature fast-curing epoxy glue |
| CN110684493A (en) * | 2019-10-12 | 2020-01-14 | 深圳飞世尔新材料股份有限公司 | Epoxy adhesive for flexible screen packaging |
| CN112877013A (en) * | 2019-11-29 | 2021-06-01 | 深圳市优宝新材料科技有限公司 | Adhesive for screen and method of using the same |
| CN111440579A (en) * | 2019-12-24 | 2020-07-24 | 武汉市三选科技有限公司 | High-flexibility epoxy resin adhesive, and preparation method and application thereof |
| CN111849403A (en) * | 2020-08-10 | 2020-10-30 | 东莞初创应用材料有限公司 | Flexible epoxy adhesive for packaging and protecting components on FPC (Flexible printed Circuit) and preparation method thereof |
| CN113583603A (en) * | 2021-08-19 | 2021-11-02 | 江苏矽时代材料科技有限公司 | Low-temperature fast-curing epoxy structural adhesive and preparation method thereof |
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Application publication date: 20181221 |