CN107987783A - A kind of preparation method of the heat-resisting ultraviolet cured adhesive of high-adhesive-strength - Google Patents
A kind of preparation method of the heat-resisting ultraviolet cured adhesive of high-adhesive-strength Download PDFInfo
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- CN107987783A CN107987783A CN201711246601.0A CN201711246601A CN107987783A CN 107987783 A CN107987783 A CN 107987783A CN 201711246601 A CN201711246601 A CN 201711246601A CN 107987783 A CN107987783 A CN 107987783A
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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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- 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
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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
- C09J11/08—Macromolecular additives
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention relates to a kind of technical field of adhesive preparation, and in particular to a kind of preparation method of the heat-resisting ultraviolet cured adhesive of high-adhesive-strength.The present invention is used as matrix using urethane acrylate, tetrahydrofuran acrylate and isobornyl acrylate mixing are used as diluting monomer, ultraviolet cured adhesive is prepared in self-control nano grade silica particles and self-control reactant etc., using snail mucus and silane coupling agent to tetrahydrofuran acrylate, isobornyl acrylate and 1 hydroxycyclohexyl phenyl ketone are modified jointly, ultraviolet cured adhesive is set to strengthen the adhesive strength of material, 1 hydroxycyclohexyl phenyl ketone has the high active and preferable heat endurance of initiation, the heat resistance for being conducive to ultraviolet cured adhesive is improved, it is continuously increased by making carboxyl-content in prepolymer by oneself, this network structure plays the role of when heated preventing high molecular polymer from degrading, so as to improve the heat endurance of ultraviolet cured adhesive, it is with a wide range of applications.
Description
Technical field
The present invention relates to a kind of technical field of adhesive preparation, and in particular to a kind of heat-resisting ultraviolet light of high-adhesive-strength cures
The preparation method of glue.
Background technology
Ultraviolet cured adhesive, also known as UV optic-solidified adhesives, are a kind of efficient, environmentally friendly, energy-saving adhesive, not only have and be free of
The advantages of solvent, storage time is long, it is fast, it can be achieved that instantaneous cured advantage also to show curing rate.
It is widely used in glassware and jewellery industry, glass furniture, medical apparatus, electronics, electric appliance, photoelectron, optics instrument
The fields such as the manufacture of device.
The usual of ultraviolet cured adhesive is made of prepolymer, monomer and photoinitiator, wherein, prepolymer is UV optic-solidified adhesives
Skeleton, there is provided the key performance of glue-line such as viscosity, tensile strength, shear strength, hardness and compliance etc..Monomer is called activity
Diluent, main function be adjust viscosity and participate in polymerisation, its such as hardness of performance to glue-line, toughness, viscosity and
Solidification process has a major impact.Photoinitiator plays a decisive role the solidification rate of UV solidification glues, has one to the performance of glue-line
It is fixing to ring.In addition, ultraviolet cured adhesive can also include other auxiliary agents, such as stabilizer, adhesive promoter, paint pigment, touch
Become agent etc..Ultraviolet cured adhesive is since its curing rate is fast, environmental-friendly, energy-output ratio is few, solvent-free volatilization etc. is numerous prominent
Go out advantage and be widely studied, and promoted rapidly in all trades and professions.
At present, the moisture-resistance of most of ultraviolet cured adhesives used is poor on the market, and Zhu wants Biao Xian Wei ︰ initially to glue
Intensity is connect to meet the requirements, but with the extension of bonding time, after placing a period of time especially under hygrothermal environment, adhesive strength
Decline to a great extent.The accelerating agent of usual ultra-violet curing adhesive is phosphoric acid ester, but their polarity is larger, initial bond strenght
It is higher, but since its water absorption rate strengthens with the increase of polar group, cause its adhesive effect to die down with the time.It is in addition, purple
Outer optic-solidified adhesive can decline with the lengthening of usage time, viscosity coefficient, while big there are cure shrinkage, and curing rate is slow,
The problem of product brittleness is big.
Therefore, developing a kind of ultraviolet cured adhesive that can solve above-mentioned performance issue is highly desirable.
The content of the invention
It is relatively low and hot there are adhesive strength that Ben Faming skill arts to be solved ask that topic ︰ is directed to current common ultraviolet cured adhesive
Stability is poor, the defects of can not meet market demands, there is provided a kind of preparation of the heat-resisting ultraviolet cured adhesive of high-adhesive-strength
Method.
In order to solve the above technical problems, the present invention uses technical solution Shi ︰ as described below
A kind of preparation method of the heat-resisting ultraviolet cured adhesive of high-adhesive-strength, it is characterised in that specific preparation process Wei ︰
（1）Ethyl orthosilicate, absolute methanol and ammonium hydroxide are mixed to be placed in ultrasonic disperse instrument and are stirred by ultrasonic, is put into after stirring
Dry in baking oven, grinding discharging, obtains self-control nano grade silica particles；
（2）Silane coupling agent KH-560 and mixed in hydrochloric acid are placed in beaker and stirred, obtains mixed liquor, then nano-silica will be made by oneself
SiClx powder, mixed liquor and lauryl sodium sulfate are mixed, heat temperature raising, cooled to room temperature, and centrifuge, and obtain
To solid product, as modified self-control nano grade silica particles；
（3）By polypropylene glycol and polycaprolactone glycol by etc. mass ratio be mixed to join equipped with blender, thermometer and condenser pipe
Four-hole boiling flask in stir, then decompression dehydration, Temperature fall obtain mixed alcohol, and mixed alcohol matter is then added into four-hole boiling flask
The isophorone diisocyanate hybrid reaction of amount 5%, obtains reaction solution, continues by reaction solution, hydroxy-ethyl acrylate, to benzene two
Phenol and hydrogen peroxide mixing are placed in beaker and stir reaction, and heat temperature raising, discharging, obtains self-control prepolymer；
（4）Tetrahydrofuran acrylate, isobornyl acrylate and 1- hydroxycyclohexyl phenyl ketones are mixed and are placed in beaker
Stirring reaction, obtain self-control reactant, then into beaker add self-control reactant quality 3% Silane coupling reagent KH-570 and from
The snail mucus of reactant 8% processed, continues to be mixed, and obtains modified self-control reactant；
（5）Weigh 100~120g self-controls prepolymer, 30~40g is modified self-control reactant, 16~20g is modified self-control nano-silica
SiClx powder and the mixing of 10~12g rosin are put into mixer and stir, and discharge, you can the heat-resisting UV light of high-adhesive-strength is made
Change glue.
Step（1）The volume ratio for the ammonium hydroxide that ethyl orthosilicate, absolute methanol and the mass fraction is 20% is 3 ︰, 1 ︰
1, the ultrasonic agitation time is 10~12min, and drying temperature is 55~65 DEG C, and drying time is 1~2h.
Step（2）The volume ratio for the hydrochloric acid that the silane coupling agent KH-560 and concentration are 0.1mol/L is 2 ︰ 1, stirring
Temperature is 65~75 DEG C, and mixing time is 20~30min, self-control nano grade silica particles, mixed liquor and dodecyl sulphate
The mass ratio of sodium is 4 ︰, 2 ︰ 1, and the mixing time is 1~2h, and heat temperature raising, temperature is 80~90 DEG C, centrifuges the time and is
20~30min.
Step（3）The whipping temp is 100~120 DEG C, and mixing time be 20~30min, dewatering time is 1~
2h, cooling temperature are 55~65 DEG C, and reaction temperature is 65~85 DEG C, and the reaction time is 16~20min, reaction solution, acrylic acid hydroxyl
The mass ratio for the hydrogen peroxide that ethyl ester, hydroquinone and mass fraction are 15% is 3 ︰, 2 ︰, 1 ︰ 1, and the stirring reaction time is 1~2h, is added
Hot warming temperature is 55~65 DEG C.
Step（4）The tetrahydrofuran acrylate, isobornyl acrylate and 1- hydroxycyclohexyl phenyl ketones
Mass ratio is 1 ︰, 1 ︰ 2, and the stirring reaction time is 20~30min, and continuation mixing time is 1~2h.
Step（5）The whipping temp is 35~45 DEG C, and mixing time is 20~24min.
The present invention is compared with other methods, advantageous effects Shi ︰
（1）The present invention using urethane acrylate as matrix, make by tetrahydrofuran acrylate and isobornyl acrylate mixing
For diluting monomer, and it is aided with coupling agent, modified self-control nano grade silica particles and modified self-control reactant etc. and purple is prepared
Outer optic-solidified adhesive, first by polypropylene glycol and polycaprolactone glycol mixing decompression dehydration, adds isophorone two after dehydration
Isocyanates, hydroxy-ethyl acrylate and hydroquinone, occur polymerisation under catalytic action and generate line style self-control prepolymer,
Wherein make the not only characteristic group-NHCOOR containing polyurethane, but also there is polymerization instead containing esters of acrylic acid in prepolymer molecule by oneself
The double bond of activity is answered, may occur from being polymerize by base under action of ultraviolet light, make to hand between polyurethane acrylates macromolecular chain
Connection cures, therefore adhesive strength is also improved, since polypropylene glycols and polycaprolactone glycol molecule all have height
Symmetry, this characteristic make it have crystallinity, and intermolecular force increase, then passes through snail mucus and silane coupling agent pair
Tetrahydrofuran acrylate, isobornyl acrylate and 1- hydroxycyclohexyl phenyl ketones are modified jointly, are made it have high viscous
Property, since both diluting monomers belong to Monofunctional monomers, and both side base volumes are larger, cause the body of ultraviolet cured adhesive
Product shrinking percentage is relatively low, and in addition both diluting monomers are stronger to the Swelling Capacity of material, are conducive to make ultraviolet cured adhesive
The adhesive strength of material is strengthened, and since 1- hydroxycyclohexyl phenyl ketones have the high active and preferable thermostabilization of initiation
Property, in polymerization process, effectively it is filled in inside ultraviolet cured adhesive, the heat resistance for being conducive to ultraviolet cured adhesive obtains
Improve；
（2）The present invention is continuously increased by making carboxyl-content in prepolymer by oneself, is conducive to degree of neutralization and is improved, increases poly- ammonia
Ester chain intermediate ion concentration, but due to electrostatic interaction so that ion chain is close to each other, so that " ion cluster " is generated, the shape of ion cluster
The adhesive strength of paired ultraviolet cured adhesive plays strengthening action, and the present invention passes through dispersant, coupling agent and acid solution pair
Nano silicon dioxide is modified, and nano silicon dioxide is dispersed in matrix surface, forms crosslinked Si-O-Si networks
Structure, this network structure play the role of when heated preventing high molecular polymer from degrading, so as to improve ultraviolet light curing
The heat endurance of glue, is with a wide range of applications.
Embodiment
The ammonium hydroxide mixing that ethyl orthosilicate, absolute methanol and mass fraction are 20% is placed in for 3 ︰, 1 ︰ 1 by volume super
10~12min is stirred by ultrasonic in sound separating apparatus, is put into after stirring in baking oven, dry 1~2h at being 55~65 DEG C in temperature,
Grinding discharging, obtains self-control nano grade silica particles；Silane coupling agent KH-560 and concentration are pressed for the hydrochloric acid of 0.1mol/L
Volume ratio is placed in beaker for 2 ︰ 1 mixing, is stirred 20~30min at being 65~75 DEG C in temperature, is obtained mixed liquor, then by quality
Than self-control nano grade silica particles, mixed liquor and lauryl sodium sulfate are mixed 1~2h, heat temperature raising for 4 ︰, 2 ︰ 1
To 80~90 DEG C, cooled to room temperature, and 20~30min is centrifuged, solid product is obtained, as modified self-control nanometer two
Silicon oxide powder；By polypropylene glycol and polycaprolactone glycol by etc. mass ratio be mixed to join equipped with blender, thermometer and cold
In the four-hole boiling flask of solidifying pipe, 20~30min, then 1~2h of decompression dehydration are stirred at being 100~120 DEG C in temperature, is naturally cooling to
55~65 DEG C, mixed alcohol is obtained, the isophorone diisocyanate of mixed alcohol quality 5% is then added into four-hole boiling flask,
Temperature is 16~20min of hybrid reaction at 65~85 DEG C, obtains reaction solution, continues to be in mass ratio 3 ︰, 2 ︰, 1 ︰ 1 by reaction solution, third
The hydrogen peroxide mixing that olefin(e) acid hydroxyl ethyl ester, hydroquinone and mass fraction are 15% is placed in 1~2h of stirring reaction, heating in beaker and rises
Temperature is to 55~65 DEG C, discharging, obtains self-control prepolymer；It is in mass ratio 1 ︰, 1 ︰ 2 by tetrahydrofuran acrylate, the different ice of acrylic acid
Piece ester and the mixing of 1- hydroxycyclohexyl phenyl ketones are placed in beaker stirring 20~30min of reaction, obtain self-control reactant, then to
The Silane coupling reagent KH-570 of self-control reactant quality 3% and the snail mucus of self-control reactant 8% are added in beaker, continues to mix
1~2h of stirring is closed, obtains modified self-control reactant；Weigh 100~120g self-control prepolymer, 30~40g be modified self-control reactant,
16~20g is modified self-control nano grade silica particles and the mixing of 10~12g rosin is put into mixer, is 35~45 DEG C in temperature
20~24min of lower stirring, discharging, you can the heat-resisting ultraviolet cured adhesive of high-adhesive-strength is made.
Example 1
The ammonium hydroxide that ethyl orthosilicate, absolute methanol and mass fraction are 20% is mixed for 3 ︰, 1 ︰ 1 by volume and is placed in ultrasound point
10min is stirred by ultrasonic in scattered instrument, is put into after stirring in baking oven, dry 1h at being 55 DEG C in temperature, grinding discharging, obtains certainly
Nano grade silica particles processed；It is that 2 ︰ 1 are mixed by volume by the hydrochloric acid that silane coupling agent KH-560 and concentration are 0.1mol/L
It is placed in beaker, stirs 20min at being 65 DEG C in temperature, obtain mixed liquor, then will make nano-silica by oneself in mass ratio for 4 ︰, 2 ︰ 1
1h is mixed in SiClx powder, mixed liquor and lauryl sodium sulfate, is heated to 80 DEG C, cooled to room temperature, and from
The heart separates 20min, obtains solid product, as modified self-control nano grade silica particles；By polypropylene glycol and polycaprolactone two
Alcohol is stirred by waiting mass ratio to be mixed to join in the four-hole boiling flask equipped with blender, thermometer and condenser pipe at being 100 DEG C in temperature
20min, then decompression dehydration 1h are mixed, is naturally cooling to 55 DEG C, obtains mixed alcohol, mixed alcohol quality is then added into four-hole boiling flask
5% isophorone diisocyanate, hybrid reaction 16min at being 65 DEG C in temperature, obtains reaction solution, and continuation is in mass ratio
The hydrogen peroxide that reaction solution, hydroxy-ethyl acrylate, hydroquinone and mass fraction are 15% is mixed to be placed in beaker and stirred by 3 ︰, 2 ︰, 1 ︰ 1
Reaction 1h is mixed, is heated to 55 DEG C, discharging, obtains self-control prepolymer；It is in mass ratio 1 ︰, 1 ︰ 2 by tetrahydrofuran acrylic acid
Ester, isobornyl acrylate and the mixing of 1- hydroxycyclohexyl phenyl ketones are placed in stirring reaction 20min in beaker, and it is anti-to obtain self-control
Thing is answered, then the snail for the Silane coupling reagent KH-570 and self-control reactant 8% for adding self-control reactant quality 3% into beaker is glued
Liquid, continues that 1h is mixed, and obtains modified self-control reactant；Weigh 100g self-controls prepolymer, 30g is modified self-control reactant, 16g
Modified self-control nano grade silica particles and 10g rosin mixing is put into mixer, is stirred 20min at being 35 DEG C in temperature, is gone out
Material, you can the heat-resisting ultraviolet cured adhesive of high-adhesive-strength is made.
Example 2
The ammonium hydroxide that ethyl orthosilicate, absolute methanol and mass fraction are 20% is mixed for 3 ︰, 1 ︰ 1 by volume and is placed in ultrasound point
Dissipate in instrument and 11min is stirred by ultrasonic, be put into after stirring in baking oven, dry 1.5h at being 60 DEG C in temperature, grinding discharging, obtains
Make nano grade silica particles by oneself；It is that 2 ︰ 1 are mixed by volume by the hydrochloric acid that silane coupling agent KH-560 and concentration are 0.1mol/L
Conjunction is placed in beaker, and 25min is stirred at being 70 DEG C in temperature, obtains mixed liquor, then will make nanometer two by oneself in mass ratio for 4 ︰, 2 ︰ 1
1.5h is mixed in silicon oxide powder, mixed liquor and lauryl sodium sulfate, is heated to 85 DEG C, cooled to room temperature,
And 25min is centrifuged, solid product is obtained, as modified self-control nano grade silica particles；By polypropylene glycol and gather in oneself
Esterdiol is 105 DEG C in temperature by waiting mass ratio to be mixed to join in the four-hole boiling flask equipped with blender, thermometer and condenser pipe
Lower stirring 25min, then decompression dehydration 1.5h, are naturally cooling to 60 DEG C, obtain mixed alcohol, and mixing is then added into four-hole boiling flask
The isophorone diisocyanate of alcohol quality 5%, hybrid reaction 18min at being 75 DEG C in temperature, obtains reaction solution, continues by matter
Amount is placed in burning than mixing the hydrogen peroxide that reaction solution, hydroxy-ethyl acrylate, hydroquinone and mass fraction are 15% for 3 ︰, 2 ︰, 1 ︰ 1
Stirring reaction 1.5h in cup, is heated to 60 DEG C, discharging, obtains self-control prepolymer；It is in mass ratio 1 ︰, 1 ︰ 2 by tetrahydrofuran
Acrylate, isobornyl acrylate and the mixing of 1- hydroxycyclohexyl phenyl ketones are placed in stirring reaction 25min in beaker, obtain
Make reactant by oneself, then the Silane coupling reagent KH-570 and self-control reactant 8% of self-control reactant quality 3% are added into beaker
Snail mucus, continues that 1.5h is mixed, and obtains modified self-control reactant；Weigh 110g self-controls prepolymer, 35g is modified self-control instead
Answer thing, 18g modifications self-control nano grade silica particles and the mixing of 11g rosin to be put into mixer, stirred at being 40 DEG C in temperature
22min, discharging, you can the heat-resisting ultraviolet cured adhesive of high-adhesive-strength is made.
Example 3
The ammonium hydroxide that ethyl orthosilicate, absolute methanol and mass fraction are 20% is mixed for 3 ︰, 1 ︰ 1 by volume and is placed in ultrasound point
12min is stirred by ultrasonic in scattered instrument, is put into after stirring in baking oven, dry 2h at being 65 DEG C in temperature, grinding discharging, obtains certainly
Nano grade silica particles processed；It is that 2 ︰ 1 are mixed by volume by the hydrochloric acid that silane coupling agent KH-560 and concentration are 0.1mol/L
It is placed in beaker, stirs 30min at being 75 DEG C in temperature, obtain mixed liquor, then will make nano-silica by oneself in mass ratio for 4 ︰, 2 ︰ 1
2h is mixed in SiClx powder, mixed liquor and lauryl sodium sulfate, is heated to 90 DEG C, cooled to room temperature, and from
The heart separates 30min, obtains solid product, as modified self-control nano grade silica particles；By polypropylene glycol and polycaprolactone two
Alcohol is stirred by waiting mass ratio to be mixed to join in the four-hole boiling flask equipped with blender, thermometer and condenser pipe at being 120 DEG C in temperature
30min, then decompression dehydration 2h are mixed, is naturally cooling to 65 DEG C, obtains mixed alcohol, mixed alcohol quality is then added into four-hole boiling flask
5% isophorone diisocyanate, hybrid reaction 20min at being 85 DEG C in temperature, obtains reaction solution, and continuation is in mass ratio
The hydrogen peroxide that reaction solution, hydroxy-ethyl acrylate, hydroquinone and mass fraction are 15% is mixed to be placed in beaker and stirred by 3 ︰, 2 ︰, 1 ︰ 1
Reaction 2h is mixed, is heated to 65 DEG C, discharging, obtains self-control prepolymer；It is in mass ratio 1 ︰, 1 ︰ 2 by tetrahydrofuran acrylic acid
Ester, isobornyl acrylate and the mixing of 1- hydroxycyclohexyl phenyl ketones are placed in stirring reaction 30min in beaker, and it is anti-to obtain self-control
Thing is answered, then the snail for the Silane coupling reagent KH-570 and self-control reactant 8% for adding self-control reactant quality 3% into beaker is glued
Liquid, continues that 2h is mixed, and obtains modified self-control reactant；Weigh 120g self-controls prepolymer, 40g is modified self-control reactant, 20g
Modified self-control nano grade silica particles and 12g rosin mixing is put into mixer, is stirred 24min at being 45 DEG C in temperature, is gone out
Material, you can the heat-resisting ultraviolet cured adhesive of high-adhesive-strength is made.
Comparative example
With the ultraviolet cured adhesive of company of Beijing production as a comparison case to the heat-resisting purple of high-adhesive-strength produced by the present invention
Ultraviolet cured adhesive in outer optic-solidified adhesive and comparative example is detected, testing result such as 1 Shi ︰ of table
1st, the measure of elongation at break and tensile strength
According to GB/T1040 standards, glue sample is solidified into dumbbell shape, is tested using electronic universal puller system.
2nd, heat stability testing
Example 1~3 and comparative example prepared by the present invention, is placed on temperature as 85 DEG C, humidity is in 85% environment, is seen
Examine 1000 it is small when after optical property situation of change.
Table 1
| Test event | Example 1 | Example 2 | Example 3 | Comparative example |
| Viscosity（cps） | 2752 | 2768 | 2773 | 2010 |
| Elongation at break（%） | 389 | 405 | 422 | 300 |
| Tensile strength（MPa） | 15.6 | 15.9 | 16.1 | 7.5 |
| Optical energy rate（%） | ≦1% | ≦1% | ≦1% | ≦15% |
| Cubical contraction（%） | 1.3 | 1.0 | 0.7 | 5.6 |
According to data in table 1, the heat-resisting ultraviolet cured adhesive mechanical property of high-adhesive-strength produced by the present invention is good, it is strong to bond
Degree is high, heat endurance is good, hence it is evident that better than comparative example product.Therefore, there is wide prospect of the application.
Claims (6)
1. a kind of preparation method of the heat-resisting ultraviolet cured adhesive of high-adhesive-strength, it is characterised in that specifically preparation process is：
（1）Ethyl orthosilicate, absolute methanol and ammonium hydroxide are mixed to be placed in ultrasonic disperse instrument and are stirred by ultrasonic, is put into after stirring
Dry in baking oven, grinding discharging, obtains self-control nano grade silica particles；
（2）Silane coupling agent KH-560 and mixed in hydrochloric acid are placed in beaker and stirred, obtains mixed liquor, then nano-silica will be made by oneself
SiClx powder, mixed liquor and lauryl sodium sulfate are mixed, heat temperature raising, cooled to room temperature, and centrifuge, and obtain
To solid product, as modified self-control nano grade silica particles；
（3）By polypropylene glycol and polycaprolactone glycol by etc. mass ratio be mixed to join equipped with blender, thermometer and condenser pipe
Four-hole boiling flask in stir, then decompression dehydration, Temperature fall obtain mixed alcohol, and mixed alcohol matter is then added into four-hole boiling flask
The isophorone diisocyanate hybrid reaction of amount 5%, obtains reaction solution, continues by reaction solution, hydroxy-ethyl acrylate, to benzene two
Phenol and hydrogen peroxide mixing are placed in beaker and stir reaction, and heat temperature raising, discharging, obtains self-control prepolymer；
（4）Tetrahydrofuran acrylate, isobornyl acrylate and 1- hydroxycyclohexyl phenyl ketones are mixed and are placed in beaker
Stirring reaction, obtain self-control reactant, then into beaker add self-control reactant quality 3% Silane coupling reagent KH-570 and from
The snail mucus of reactant 8% processed, continues to be mixed, and obtains modified self-control reactant；
（5）Weigh 100~120g self-controls prepolymer, 30~40g is modified self-control reactant, 16~20g is modified self-control nano-silica
SiClx powder and the mixing of 10~12g rosin are put into mixer and stir, and discharge, you can the heat-resisting UV light of high-adhesive-strength is made
Change glue.
A kind of 2. preparation method of the heat-resisting ultraviolet cured adhesive of high-adhesive-strength according to claim 1, it is characterised in that：
Step（1）The volume ratio for the ammonium hydroxide that ethyl orthosilicate, absolute methanol and the mass fraction is 20% is 3：1：1, ultrasound is stirred
It is 10~12min to mix the time, and drying temperature is 55~65 DEG C, and drying time is 1~2h.
A kind of 3. preparation method of the heat-resisting ultraviolet cured adhesive of high-adhesive-strength according to claim 1, it is characterised in that：
Step（2）The volume ratio for the hydrochloric acid that the silane coupling agent KH-560 and concentration are 0.1mol/L is 2：1, whipping temp 65
~75 DEG C, mixing time is 20~30min, the quality of self-control nano grade silica particles, mixed liquor and lauryl sodium sulfate
Than for 4：2：1, the mixing time is 1~2h, heat temperature raising, and temperature is 80~90 DEG C, centrifuge the time for 20~
30min。
A kind of 4. preparation method of the heat-resisting ultraviolet cured adhesive of high-adhesive-strength according to claim 1, it is characterised in that：
Step（3）The whipping temp is 100~120 DEG C, and mixing time is 20~30min, and dewatering time is 1~2h, cooling temperature
Spend for 55~65 DEG C, reaction temperature is 65~85 DEG C, and the reaction time is 16~20min, reaction solution, hydroxy-ethyl acrylate, to benzene
The mass ratio for the hydrogen peroxide that diphenol and mass fraction are 15% is 3：2：1：1, the stirring reaction time is 1~2h, heat temperature raising temperature
Spend for 55~65 DEG C.
A kind of 5. preparation method of the heat-resisting ultraviolet cured adhesive of high-adhesive-strength according to claim 1, it is characterised in that：
Step（4）The mass ratio of the tetrahydrofuran acrylate, isobornyl acrylate and 1- hydroxycyclohexyl phenyl ketones is
1：1：2, the stirring reaction time is 20~30min, and continuation mixing time is 1~2h.
A kind of 6. preparation method of the heat-resisting ultraviolet cured adhesive of high-adhesive-strength according to claim 1, it is characterised in that：
Step（5）The whipping temp is 35~45 DEG C, and mixing time is 20~24min.
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| CN201711246601.0A CN107987783A (en) | 2017-12-01 | 2017-12-01 | A kind of preparation method of the heat-resisting ultraviolet cured adhesive of high-adhesive-strength |
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| CN201711246601.0A CN107987783A (en) | 2017-12-01 | 2017-12-01 | A kind of preparation method of the heat-resisting ultraviolet cured adhesive of high-adhesive-strength |
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| CN (1) | CN107987783A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108948915A (en) * | 2018-06-25 | 2018-12-07 | 合肥易美特建材有限公司 | A kind of low reflecting rate color steel plate surface coating material |
| CN108948917A (en) * | 2018-06-25 | 2018-12-07 | 合肥易美特建材有限公司 | A kind of preparation method of color steel plate weather-resistant coating |
| CN109021742A (en) * | 2018-06-25 | 2018-12-18 | 合肥易美特建材有限公司 | A kind of color steel plate shock resistance resist bending coating |
| CN109796917A (en) * | 2019-02-26 | 2019-05-24 | 浙江久大纺织科技有限公司 | A kind of preparation method of UV cured polyurethane acrylate adhesive |
| CN112680124A (en) * | 2020-12-25 | 2021-04-20 | 安徽金龙浩光电科技有限公司 | Novel glass bonding method |
| CN113956432A (en) * | 2021-11-16 | 2022-01-21 | 广东十辰十新材料有限公司 | Degradable UV resin and degradable UV pressure-sensitive adhesive based on same |
| CN116445124A (en) * | 2023-03-13 | 2023-07-18 | 山东凯恩新材料科技有限公司 | High-thermal-stability UV adhesive and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108948915A (en) * | 2018-06-25 | 2018-12-07 | 合肥易美特建材有限公司 | A kind of low reflecting rate color steel plate surface coating material |
| CN108948917A (en) * | 2018-06-25 | 2018-12-07 | 合肥易美特建材有限公司 | A kind of preparation method of color steel plate weather-resistant coating |
| CN109021742A (en) * | 2018-06-25 | 2018-12-18 | 合肥易美特建材有限公司 | A kind of color steel plate shock resistance resist bending coating |
| CN109796917A (en) * | 2019-02-26 | 2019-05-24 | 浙江久大纺织科技有限公司 | A kind of preparation method of UV cured polyurethane acrylate adhesive |
| CN112680124A (en) * | 2020-12-25 | 2021-04-20 | 安徽金龙浩光电科技有限公司 | Novel glass bonding method |
| CN113956432A (en) * | 2021-11-16 | 2022-01-21 | 广东十辰十新材料有限公司 | Degradable UV resin and degradable UV pressure-sensitive adhesive based on same |
| CN116445124A (en) * | 2023-03-13 | 2023-07-18 | 山东凯恩新材料科技有限公司 | High-thermal-stability UV adhesive and preparation method thereof |
| CN116445124B (en) * | 2023-03-13 | 2023-11-28 | 浙江凯越新材料技术有限公司 | High-thermal-stability UV adhesive and preparation method thereof |
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