CN105400472B - A kind of preparation method of the UV adhesives of space-time separation - Google Patents
A kind of preparation method of the UV adhesives of space-time separation Download PDFInfo
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- CN105400472B CN105400472B CN201510921307.XA CN201510921307A CN105400472B CN 105400472 B CN105400472 B CN 105400472B CN 201510921307 A CN201510921307 A CN 201510921307A CN 105400472 B CN105400472 B CN 105400472B
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Abstract
A kind of preparation method of the UV adhesives of space-time separation belongs to the technical field of ultraviolet light solidification quick molding method.It comprises the following steps：(1) oligomer and cation light initiator are well mixed by a certain percentage, stirred under ultraviolet light, make cation light initiator photodissociation, obtain uniform liquid A；(2) epoxy resin, reactive diluent are mixed with auxiliary agent, obtains uniform liquid B；(3) it is glued after liquid A is well mixed with liquid B；The mass fraction that liquid A accounts for mixing liquid is 0.1wt% 50wt%.During Illumination of the present invention realizes complete space-time with curing molding process and separated, and ultraviolet light is not needed during curing molding, can be in the unconfined extension solidification of light tight region；Also retains photocuring technology simultaneously can be under low temperature normal temperature condition the advantages of rapid curing；Simultaneously as During Illumination separates with the space-time of curing molding process, the applying glue of the extreme cases such as field and solidification are adapted to.
Description
Technical field
The present invention relates to field of polymer composite material, and in particular to prepares UV glue to a kind of method using space-time separation
Glutinous agent and its application field.
Background technology
Have that rapid curing, compatibility are good, intensity is high, some distinguishing features such as environmentally friendly because ultraviolet cured adhesive sticks agent,
Therefore it is widely used in the fields such as optical field, electronic apparatus, optical digital disk.Ultraviolet cured adhesive sticks the solidification limitation of agent at present
In the position of illumination, ultraviolet light less than position be difficult to carry out effectively solidification and curing depth has deficiency, and one
Have in the special applications of a little special dimensions ultraviolet light less than place be also required to effectively be solidified, be such as used for opaque glass
Glass plate is bonded, and wooden boards bond, and sheet metal bonds etc.；Particularly ultraviolet cured adhesive sticks agent and is bonded for composite
Technical field, can be in low-temperature setting because the activation energy required for UV-curing technology is low, therefore can avoid producing heat
Stress, and UV-curing technology equipment is simple, energy-conserving and environment-protective, is more suitable for outfield repairing, but due to ultraviolet light not
To position be difficult to carry out effectively solidification and curing depth has deficiency, while need reinforcing aids light transmission good, therefore only
The damage of composite layer can be repaired, limit ultraviolet cured adhesive and stick agent answering in composite repair field
With.
The present invention breaches the limitation of photocuring technology, space division when During Illumination realizes complete with curing molding process
From, ultraviolet light is not needed during curing molding, can be in the unconfined extension solidification of light tight region；Also protect simultaneously
Stay photocuring technology can be under low temperature normal temperature condition the advantages of rapid curing；Simultaneously as During Illumination and curing molding mistake
The space-time separation of journey, is adapted to the applying glue of the extreme cases such as field and solidification.
The content of the invention
The present invention is directed to the deficiency of above-mentioned prior art, there is provided a kind of UV adhesives of space-time separation.
It is a further object of the present invention to provide a kind of space-time partition method to prepare UV adhesives and its application field.
Present invention mainly solves existing UV-curing technology, exist the problem of, i.e., ultraviolet light less than
Position is difficult to carry out effectively solidification and curing depth has deficiency, while the defects of need auxiliary agent light transmission good.
To achieve the above object, the present invention adopts the following technical scheme that.
The preparation method of the composite repair glue of space-time separation, comprises the following steps：
(1) oligomer and cation light initiator are well mixed by a certain percentage, are stirred under ultraviolet light, make sun
Ionic photoinitiator photodissociation, obtain uniform liquid A；
(2) epoxy resin, reactive diluent are mixed by a certain percentage with auxiliary agent, obtains uniform liquid B；
(3) it is glued after liquid A is well mixed by a certain percentage with liquid B；
In the step of above-mentioned preparation method (1), (2), (3), preferred dry environment, the purple of extension solidification is thus prepared
The solidification effect of outer solidification glue is more preferable.
Resin in the step of above-mentioned preparation method (1) is polyether polyols alcohols, polyglycols ethers, polyethylene glycol, or poly-
Oxygen glycerine.
Cation light initiator described in the step of above-mentioned preparation method (1) includes salt compounded of iodine, sulfosalt and iron arene
In one or more.
Resin in the step of above-mentioned preparation method (2) includes epoxy resin, in vinyl ethers and oxygen helerocyclics
It is one or more of；Epoxy resin is bisphenol A epoxide resin, or bisphenol F epoxy resin, or novolac epoxy resin, or diepoxide
Polyolefin compound, or naphthalene system epoxy resin, or aliphatic epoxy resin, or cycloaliphatic epoxy resin.
Reactive diluent in the step of above-mentioned preparation method (2) is epoxy monomer, vinyl ether monomers or oxa- ring list
Body.
Auxiliary agent described in the step of above-mentioned preparation method (2) can according to different its species of application field reasonable selection and
Its dosage.
The mass fraction that cation light initiator described in the step of above-mentioned preparation method (1) accounts for liquid A is 0.5%-
80%.
The mass fraction that liquid A accounts in the step of above-mentioned preparation method (3) is 0.1%-50%.
Light polymerization process of the present invention is cationic photopolymerization, there is solidify afterwards behavior, can be by curing molding
Repair sheets afterwards carry out solidify afterwards processing, to improve its performance.
The present invention technological principle be：Cationic polymerization is a kind of living polymerisation process, after cation light initiator photodissociation
The cation group of generation is a kind of active group, and its activity is stabilized and unattenuated always in theory, in actual life
In production, the work property retention of cation group more than 1 year；Therefore by after cation light initiator photodissociation, the cation base of generation
The activity of group can be kept for a long time；But cation photocuring resin will be added after cation light initiator photodissociation, with reality
Existing illumination separates with the space-time of curing molding, it will following three be present：(1), it is unfavorable for storing for a long time；Light trigger light
It is easy to make moist after solution, causes the activity reduction of cation light initiator, or even cation photocuring resin can not be triggered to carry out
Reaction.(2), system induction period is too short；The activity of active group is high after cation light initiator photodissociation, with resin reaction speed
It hurry up, moment generates a gel group, and the initiator after photodissociation is wrapped in gel group, it is impossible to carried out with light-cured resin anti-
Should；(3), cation light initiator is bad in the dissolubility of cation photocuring resin system, longer the time required to being well mixed.
The present invention successfully solves problem above, realizes illumination and is separated with the space-time of curing molding.
The present invention mixes cation light initiator with not volatile oligomer such as polyether polyols alcohols, to stir illumination
Form make its photodissociation (obtaining photoinitiator system PI)；The active group generated after photodissociation is uniformly dispersed in liquid, is gathered
The oligomer such as ethoxylated polyhydric alcohol class serve as chain-transferring agent in system, the activity of the cation group of generation is stabilized always；
Solve the problems, such as to be unfavorable for store for a long time.
It is overall to consolidate with cationic photopolymerization after cation light initiator mixes with not volatile oligomer such as polyether polyols alcohols
Changing the dissolubility of resin can improve, it is easier to and it is quick well mixed, solve its deliquescent problem.
Active group has been evenly spread in the oligomer such as polyether polyols alcohols, reduces the concentration of active group, so as to
Photoinitiator system PI will not occur gel group moment, simultaneously with light-cured resin mixed process, there is longer induction period
The reaction speed of whole system and induction period can be controlled by control system temperature, stage induction period complete liquid A with
The mixing of liquid B, bubble that may be present in exclusion system, and Process of Applying Glue；Can be by changing the temperature of system, with purple
The methods of outer light irradiation, terminates induction period；After induction period terminates, whole system will fast reaction, curing molding.Meanwhile polyethers
Contain hydroxyl in the oligomer such as polyalcohols, eventually combined with epoxide group, therefore do not have solvent volatilization in whole process；
After induction period terminates, its reaction speed is similar to the speed of Stereolithography, finally gives excellent adhesive property.
By reasonable selection formula, induction period length can be changed to most obvious temperature control at 5 DEG C -30 DEG C, according to
Different construction conditions can use different formulas either to select different glue applying methods.
Compared with the prior art UV adhesives prepared by space-time partition method of the present invention have the substance gone out in fact special
Point and marked improvement：
1. being separated due to realizing illumination with the space-time of curing molding, illumination need not be wanted in the curing process, therefore do not have
There is the limitation of curing depth.
2. Preparation equipment, technique are simple, environmental protection, rapid curing is applied widely.
Embodiment
Technical scheme is described further below by preferred embodiment, following examples contribute to ability
The technical staff in domain further understands the present invention, but should not be construed as limiting the scope of the invention.It should be understood that
, it will be apparent to those skilled in the art that without departing from the inventive concept of the premise, some deformations can also be made and changed
Enter.These are belonged within protection scope of the present invention.
Embodiment 1：
Mass fraction is added in the polyethylene glycol for being 200 to molecular weight to be 5% (mass fraction is the quality point for accounting for liquid A
Number) triaryl hexafluoro-antimonic acid sulfosalt and be well mixed, take the well mixed samples of 20g to add in 50ml beaker, on one side
Stirring is while with mercury lamp with 100mw/cm2Light intensity irradiation 20min.Uniform liquid A (being named as PI) is obtained, is poured into bottle
It is stand-by.It is 3 in mass ratio by oxetanes and E-52:7 mixing.It is 2% that mass fraction is added into well mixed liquid
The chopped carbon fiber of (mass fraction is the mass fraction for accounting for liquid B), it is stand-by to obtain uniform liquid B after mixing.To liquid during use
Mass fraction is added in body B to be well mixed for the liquid A of 5% (mass fraction is the mass fraction for accounting for mixing liquid).
Embodiment 2：
It is that 10% (mass fraction is the quality for accounting for liquid A that mass fraction ratio is added in the polyethylene glycol for being 400 to molecular weight
Fraction) triaryl hexafluorophosphoric acid sulfosalt and be well mixed, take the well mixed samples of 20g to add in 50ml beaker, one
Stir while with mercury lamp with 100mw/cm on side2Light intensity irradiation 20min.Uniform liquid (being named as PI) is obtained, is poured into bottle
In it is stand-by.Oxetanes and E51 are pressed 2:8 mass ratio mixing, it is that 1% (mass fraction is to account for liquid B to add mass fraction
Mass fraction) short glass fiber, it is stand-by that uniform liquid B is obtained after mixing.It is 20% to add mass fraction into liquid B during use
The liquid A of (mass fraction is the mass fraction for accounting for mixing liquid) is well mixed.Embodiment 3：
It is that 40% (mass fraction is the quality for accounting for liquid A that mass fraction ratio is added in the polyethylene glycol for being 400 to molecular weight
Fraction) diaryl hexafluorophosphoric acid salt compounded of iodine and be well mixed, take the well mixed samples of 20g to add in 50ml beaker, one
Stir while with mercury lamp with 100mw/cm on side2Light intensity irradiation 20min.Uniform liquid A (being named as PI) is obtained, is poured into bottle
In it is stand-by.Epoxy monomer and E51 are pressed 3:7 mass ratio mixing, it is stand-by to obtain uniform liquid B.Added during use into liquid B
Mass fraction is well mixed for the liquid A of 30% (mass fraction is the mass fraction for accounting for mixing liquid).
Embodiment 4：
It is that 40% (mass fraction is the matter for accounting for liquid A that mass fraction ratio is added in the polyoxy glycerine for being 400 to molecular weight
Amount fraction) diaryl hexafluorophosphoric acid salt compounded of iodine and be well mixed, take the well mixed samples of 20g to add in 50ml beaker,
Stir while using mercury lamp with 100mw/cm2Light intensity irradiation 20min.Uniform liquid A (being named as PI) is obtained, is poured into
It is stand-by in bottle.By oxetanes, epoxy monomer presses 1 with F-44:2:7 mass ratio is well mixed, and it is 5% to add mass fraction
The short carbon fiber of (mass fraction is the mass fraction for accounting for liquid B), it is stand-by to obtain uniform liquid B after mixing.To liquid B during use
The middle mass fraction that adds is well mixed for the liquid A of 10% (mass fraction is the mass fraction for accounting for mixing liquid).
Table 1：
| Embodiment is numbered | Curing rate | Curing depth | Tensile shear strength |
| 1 | 13min | 15cm is fully cured | 26MPa |
| 2 | 15min | 15cm is fully cured | 22MPa |
| 3 | 3min | 15cm is fully cured | 21MPa |
| 4 | 6min | 15cm is fully cured | 32MPa |
Note：Curing depth：Ready-made groove before ready-made ultraviolet cured adhesive is uniformly filled, is then applied
Glue.
Finally it should be noted that：The above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof；To the greatest extent
The present invention is described in detail with reference to embodiment for pipe, those of ordinary skills in the art should understand that：Still can be with
The embodiment of the present invention is modified or equivalent substitution is carried out to some technical characteristics；Without departing from skill of the present invention
The spirit of art scheme, it all should cover among the claimed technical scheme scope of the present invention.
Claims (6)
1. a kind of preparation method of the UV adhesives of space-time separation, comprises the following steps：
(1) oligomer and cation light initiator are well mixed by a certain percentage, are stirred under ultraviolet light, make cation
Light trigger photodissociation, obtain uniform liquid A；The mass fraction that the cation light initiator accounts for liquid A is 0.5wt%-
80wt%；Oligomer includes polyether polyols alcohols；
(2) epoxy resin, reactive diluent are mixed with auxiliary agent, obtains uniform liquid B；
(3) it is glued after liquid A is well mixed with liquid B；The mass fraction that liquid A accounts for mixing liquid is 0.1wt%-
50wt%.
2. preparation method according to claim 1, it is characterised in that the oligomer in step (1) includes polyglycols ethers
Or polyoxy glycerine.
3. preparation method according to claim 1, it is characterised in that the cation light initiator bag described in step (1)
Include salt compounded of iodine, the one or more in sulfosalt and iron arene.
4. preparation method according to claim 1, it is characterised in that epoxy resin is bisphenol A epoxide resin, or Bisphenol F
Epoxy resin, or novolac epoxy resin, or diepoxide polyolefin compound, or naphthalene system epoxy resin, or aliphatic epoxy tree
Fat, or cycloaliphatic epoxy resin.
5. preparation method according to claim 1, it is characterised in that the reactive diluent in step (2) is epoxy monomer,
Vinyl ether monomers or oxygen heterocyclic monomer.
6. the UV adhesives prepared by preparation method described in application claim 1-5 any one.
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| CN201510921307.XA CN105400472B (en) | 2015-12-12 | 2015-12-12 | A kind of preparation method of the UV adhesives of space-time separation |
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| CN201510921307.XA CN105400472B (en) | 2015-12-12 | 2015-12-12 | A kind of preparation method of the UV adhesives of space-time separation |
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| CN105400472A CN105400472A (en) | 2016-03-16 |
| CN105400472B true CN105400472B (en) | 2018-01-12 |
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| CN111909643B (en) * | 2020-07-08 | 2022-05-03 | 江苏矽时代材料科技有限公司 | Time-delay photocuring epoxy resin composition and application thereof |
| CN114507479B (en) * | 2020-11-16 | 2023-12-15 | 常州强力先端电子材料有限公司 | Photocurable composition, binder, preparation method of binder and bonding method of substrate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6376070B1 (en) * | 1996-07-15 | 2002-04-23 | Sekisui Kagaku Kogyo Kabushiki Kaisha | Sheet-form, curable pressure-sensitive adhesive |
| CN103360977A (en) * | 2006-04-26 | 2013-10-23 | 日立化成株式会社 | Adhesive tape and solar cell module using the same |
-
2015
- 2015-12-12 CN CN201510921307.XA patent/CN105400472B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6376070B1 (en) * | 1996-07-15 | 2002-04-23 | Sekisui Kagaku Kogyo Kabushiki Kaisha | Sheet-form, curable pressure-sensitive adhesive |
| CN103360977A (en) * | 2006-04-26 | 2013-10-23 | 日立化成株式会社 | Adhesive tape and solar cell module using the same |
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