CN109293250A - It is a kind of to be conducive to demould convenient and breakage-proof film plating process - Google Patents
It is a kind of to be conducive to demould convenient and breakage-proof film plating process Download PDFInfo
- Publication number
- CN109293250A CN109293250A CN201811113268.0A CN201811113268A CN109293250A CN 109293250 A CN109293250 A CN 109293250A CN 201811113268 A CN201811113268 A CN 201811113268A CN 109293250 A CN109293250 A CN 109293250A
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- CN
- China
- Prior art keywords
- convenient
- demould
- breakage
- conducive
- plating process
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
- C03C17/009—Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/007—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/114—Deposition methods from solutions or suspensions by brushing, pouring or doctorblading
Abstract
The invention belongs to substrate surfaces to plate attached masking technique field, in particular to a kind of to be conducive to demould convenient and breakage-proof film plating process, unsaturated monomer, crosslinking agent, foaming agent, initiator, silicon source, water are mixed into progress emulsion polymerization first and obtain the compound expended microsphere of silica, thus obtained microsphere is distributed in the coating liquid dissolved with polymer again, dry solidification forms a film together, after cooling, film layer often generates disengaging with substrate surface automatically, and demoulding is convenient.
Description
Technical field
The invention belongs to substrate surfaces to plate attached masking technique field, in particular to one kind is conducive to demould convenient and breakage-proof
Film plating process.
Background technique
The process flow of polymer dissolution film forming is substantially are as follows: first polymer and its auxiliary material are dissolved in organic solvent and mixed
Close, by gained mixed liquor in substrate surface film, be dried solidification after the completion of film, it is cooling after again by molding film product and
Substrate separation, that is, demould.
In heat drying process, membrane material can be firmly adhered to substrate surface in substrate surface forming and hardening, cooling
It is usually not easy to separate film layer with substrate afterwards, film is directly pulled open to the breakage or fracture for easilying lead to film layer from substrate surface,
Film layer and substrate are placed in water immersion together in some measures penetrates into hydrone gradually between substrate and film layer, to film layer with
Binding force between substrate is slowly disintegrated, then is demoulded, usually too long the time required to only impregnating, and also needs after impregnating demoulding
Film product and substrate are dried, which increases process procedures.
Summary of the invention
In order to solve the above technical problems, be conducive to demould convenient and breakage-proof film plating process the present invention provides a kind of,
It can be separated automatically with substrate after making film layer dry solidification, process flow when demoulding, concrete operations are greatly reduced are as follows:
(1) the compound expended microsphere of silica is prepared
Unsaturated monomer, crosslinking agent, foaming agent, initiator, silicon source are mixed sufficiently as oily phase, gained oil is added to
In water, and triethylamine is added into water simultaneously, obtains pre-emulsion after being sufficiently mixed, by resulting pre-emulsion in a heated state into
Row polymerization reaction filters after reaction, is dried filter cake to get the expended microsphere compound to silica,
Unsaturated monomer is acrylic ester monomer, acrylonitrile monomer or vinyl ester monomer etc.,
Crosslinking agent be trimethylol-propane trimethacrylate or trimethylolpropane trimethacrylate,
Foaming agent is butane type organic, pentane type organic, hexane type organic etc.,
Silicon source is ethyl orthosilicate；
(2) coating film forming
It will be including fully dispersed in the addition solvent of expended microsphere obtained in polymer and step (1), by resulting point
Dispersion liquid is cooled down in pretreated glass basic surface film, and by the substrate of glass heating, drying after film,
Polymer is polyimides, polypropylene, polyethylene, polymethyl methacrylate, Kynoar, polyvinyl pyrrole
Alkanone etc.,
The pretreatment operation of substrate of glass is, after sufficiently being cleaned with acetone and deionized water to glass basic surface, by glass
Glass substrate is dried under low temperature.
Using the method for this programme, film layer be heated together with substrate drying and after supercooling, film layer often automatically with
Substrate surface generates disengaging, directly removes film layer, such as meet it is cooling after film layer the case where can't directly being removed, can be with
Substrate connection film layer is immersed in together in normal-temperature water and realizes automatically disengaging for film layer and substrate, required soaking time is also remote
Considerably shorter than existing film plating process, thinks this applicant:
It is by joined the compound expended microsphere of silica, one side silica into coating liquid in this programme
Close with the material of glass, interface of the microballoon in film forming system between oriented film layer and substrate of glass after silica is compound is moved
The trend of shifting, on the other hand, in heat drying process after application, microballoon can be heated and expand, when microballoon film layer with
It when being thermally expanded between substrate of glass, is equivalent to film layer is apart from one another with substrate of glass, efficiently reduces between the two
Binding force is provided convenience for subsequent demoulding；The swelling theoretically covers the entire boundary between film layer and glass simultaneously
Face avoids film layer and integrally ruptures when being detached from substrate.
Specific embodiment
Embodiment 1
(1) the compound expended microsphere of silica is prepared
By the butyl acrylate of 4 parts by weight, the acrylonitrile of 8 parts by weight, 0.04 parts by weight trimethylol propane trimethyl
The ethyl orthosilicate mixing of acrylate, the hexane of 4.5 parts by weight, the azobisisoheptonitrile of 0.25 parts by weight, 5.2 parts by weight is filled
It is allocated as oily phase,
The sodium chloride of 0.5 parts by weight is dissolved in the deionized water of 90 parts by weight and obtains water phase,
Above-mentioned gained oil is added in above-mentioned resulting water phase, and is added the three of 0.6 parts by weight into water phase simultaneously
Ethamine obtains pre-emulsion after being sufficiently mixed, and resulting pre-emulsion is carried out polymerization reaction 12 hours at 0.25MPa, 55 DEG C, instead
Should after filter, to sufficiently being dried at 60 DEG C after Washing of Filter Cake to get to the compound expended microsphere of silica；
(2) it is film-made
85 parts by weight are added in expended microsphere obtained in the PMMA polymer of 10 parts by weight, 2.7 parts by weight steps (1)
Ethyl alcohol in it is fully dispersed, by resulting dispersion liquid in uniform coating in the plate face of glass plate (before film with acetone and go from
After sub- water sufficiently cleans glass pane surface, glass plate is sufficiently dried at 60 DEG C), and by the glass plate after film in 85 DEG C
Lower drying and processing 1 hour naturally cools to room temperature (25 DEG C, similarly hereinafter).
Directly film layer entirety can be removed from glass sheet substrate surface after cooling, handled without immersion.
Embodiment 2
(1) the compound expended microsphere of silica is prepared
By the vinyl acetate of 5 parts by weight, the isobutyl acrylate of 10 parts by weight, 0.08 parts by weight trimethylolpropane
Triacrylate, the hexamethylene of 5.8 parts by weight, the azobisisoheptonitrile of 0.25 parts by weight, the ethyl orthosilicate of 5.5 parts by weight are mixed
It closes sufficiently as oily phase,
The sodium chloride of 0.5 parts by weight is dissolved in the deionized water of 95 parts by weight and obtains water phase,
Above-mentioned gained oil is added in above-mentioned resulting water phase, and is added the three of 0.6 parts by weight into water phase simultaneously
Ethamine obtains pre-emulsion after being sufficiently mixed, and resulting pre-emulsion is carried out polymerization reaction 17 hours at 0.2MPa, 50 DEG C, instead
Should after filter, to sufficiently being dried at 60 DEG C after Washing of Filter Cake to get to the compound expended microsphere of silica；
(2) it is film-made
85 weight are added in expended microsphere obtained in the polyacrylic polymer of 10 parts by weight, 2.5 parts by weight steps (1)
Fully dispersed in the ethyl alcohol of part, by resulting dispersion liquid, in uniform coating in the plate face of glass plate, (film with acetone and is gone before
After ionized water sufficiently cleans glass pane surface, glass plate is sufficiently dried at 60 DEG C), and by the glass plate after film in 90
Drying and processing 1.2 hours, naturally cool to room temperature at DEG C.
Film layer can not be directly removed from glass sheet substrate surface after cooling.Glass sheet substrate is immersed in together together with film layer
In normal-temperature water, impregnating only can be whole in smoothly removing in substrate by film layer after 4 minutes.
Blank control example
Expended microsphere is not added in film-forming process, remaining film operation is with embodiment 1:
Will be fully dispersed in the ethyl alcohol of PMMA polymer 85 parts by weight of addition of 10 parts by weight, by resulting dispersion liquid in glass
Uniform coating is (after using acetone and deionized water sufficiently to clean glass pane surface before film, by glass plate in the plate face of glass plate
At 60 DEG C sufficiently dry), and by the glass plate after film at 85 DEG C drying and processing 1 hour, naturally cool to room temperature.
Film layer is firmly combined with glass sheet substrate after cooling, can not directly remove film layer.By glass sheet substrate together with film layer
It is immersed in normal-temperature water, was at most checked every 10 minutes once together, it can be whole in substrate by film layer when being dipped to 50 minutes
On smoothly remove.
Comparative example 1
Only non-composite silicon dioxide ingredient during preparing microballoon, remaining operation is with embodiment 1:
(1) expended microsphere is prepared
By the butyl acrylate of 4 parts by weight, the acrylonitrile of 8 parts by weight, 0.04 parts by weight trimethylol propane trimethyl
The azobisisoheptonitrile mixing of acrylate, the hexane of 4.5 parts by weight, 0.25 parts by weight sufficiently as oily phase,
The sodium chloride of 0.5 parts by weight is dissolved in the deionized water of 90 parts by weight and obtains water phase,
Above-mentioned gained oil is added in above-mentioned resulting water phase, obtains pre-emulsion after being sufficiently mixed, it will be resulting pre-
Lotion carries out polymerization reaction 12 hours at 0.25MPa, 55 DEG C, filters after reaction, to after Washing of Filter Cake at 60 DEG C it is sufficiently dry
It is dry to get arrive expended microsphere；
(2) it is film-made
85 parts by weight are added in expended microsphere obtained in the PMMA polymer of 10 parts by weight, 2.7 parts by weight steps (1)
Ethyl alcohol in it is fully dispersed, by resulting dispersion liquid in uniform coating in the plate face of glass plate (before film with acetone and go from
After sub- water sufficiently cleans glass pane surface, glass plate is sufficiently dried at 60 DEG C), and by the glass plate after film in 85 DEG C
Lower drying and processing 1 hour, naturally cools to room temperature.
Film layer is firmly combined with glass sheet substrate after cooling, can not directly remove film layer.By glass sheet substrate together with film layer
It is immersed in normal-temperature water, was at most checked every 10 minutes once together, it can be whole in substrate by film layer when being dipped to 50 minutes
On smoothly remove.
Comparative example 2
Blowing agent substances (hexane) is not only added during preparing microballoon, microballoon is caused not have dilatancy, remaining
Process operations are the same as embodiment 1.
Film layer is firmly combined with glass sheet substrate after cooling, can not directly remove film layer.By glass sheet substrate together with film layer
It is immersed in normal-temperature water, was at most checked every 10 minutes once together, it can be whole in substrate by film layer when being dipped to 46 minutes
On smoothly remove.
Comparative example 3
The method for preparing the compound expended microsphere of silica is different from embodiment 1 (being directly added into silica),
Remaining process operations is with embodiment 1:
(1) the compound expended microsphere of silica is prepared
By the butyl acrylate of 4 parts by weight, the acrylonitrile of 8 parts by weight, 0.04 parts by weight trimethylol propane trimethyl
Acrylate, the hexane of 4.5 parts by weight, the azobisisoheptonitrile of 0.25 parts by weight, 1.5 parts by weight nano SiO 2 particle
It mixes sufficiently as oily phase,
The sodium chloride of 0.5 parts by weight is dissolved in the deionized water of 90 parts by weight and obtains water phase,
Above-mentioned gained oil is added in above-mentioned resulting water phase, obtains pre-emulsion after being sufficiently mixed, it will be resulting pre-
Lotion carries out polymerization reaction 12 hours at 0.25MPa, 55 DEG C, filters after reaction, to after Washing of Filter Cake at 60 DEG C it is sufficiently dry
It is dry to get to the compound expended microsphere of silica；
(2) it is film-made
With embodiment 1.
Film layer is firmly combined with glass sheet substrate after cooling, can not directly remove film layer.By glass sheet substrate together with film layer
It is immersed in normal-temperature water, was at most checked every 10 minutes once together, it can be whole in substrate by film layer when being dipped to 43 minutes
On smoothly remove.This may be the difference of combination process between silica and microballoon, largely effect on moving for microballoon in film forming procedure
Shifting ability and cause.
As it can be seen that convenient many is wanted when being detached from substrate of glass using film layer prepared by this programme method, it is more above-mentioned each
Embodiment, reference examples, comparative example have also confirmed the summary that applicant partially provides in " summary of the invention " to a certain extent.When
So, due to migrating microballoon and expands, the flatness that will lead to that face of abutting substrate of glass in film layer is declined,
Therefore this programme is primarily adapted for use in the filming technology of less demanding to surface smoothness.
Claims (7)
1. a kind of be conducive to demould convenient and breakage-proof film plating process, it is characterised in that: the method is,
(1) the compound expended microsphere of silica is prepared
Unsaturated monomer, crosslinking agent, foaming agent, initiator, silicon source are mixed sufficiently as oily phase, gained oil is added to water
In, and triethylamine is added into water simultaneously, pre-emulsion is obtained after being sufficiently mixed, resulting pre-emulsion is carried out in a heated state
Polymerization reaction filters after reaction, is washed, is dried to get the expended microsphere compound to silica to filter cake；
(2) coating film forming
It will be including fully dispersed in the addition solvent of expended microsphere obtained in polymer and step (1), by resulting dispersion liquid
In pretreated glass basic surface film, and by the substrate of glass heating, drying after film, cool down.
2. being conducive to demould convenient and breakage-proof film plating process as described in claim 1, it is characterised in that: in step (1)
The unsaturated monomer is acrylic ester monomer, acrylonitrile monomer or vinyl ester monomer.
3. being conducive to demould convenient and breakage-proof film plating process as described in claim 1, it is characterised in that: in step (1)
The crosslinking agent is trimethylol-propane trimethacrylate or trimethylolpropane trimethacrylate.
4. being conducive to demould convenient and breakage-proof film plating process as described in claim 1, it is characterised in that: in step (1)
The foaming agent is butane type organic, pentane type organic or hexane type organic.
5. being conducive to demould convenient and breakage-proof film plating process as described in claim 1, it is characterised in that: in step (1)
The silicon source is ethyl orthosilicate.
6. being conducive to demould convenient and breakage-proof film plating process as described in claim 1, it is characterised in that: in step (2)
The polymer is polyimides, polypropylene, polyethylene, polymethyl methacrylate, Kynoar or polyvinyl pyrrole
Alkanone.
7. being conducive to demould convenient and breakage-proof film plating process as described in claim 1, it is characterised in that: in step (2)
The pretreated operation is, after sufficiently being cleaned with acetone and deionized water to the glass basic surface, by the glass
Glass substrate is dried under low temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811113268.0A CN109293250A (en) | 2018-09-25 | 2018-09-25 | It is a kind of to be conducive to demould convenient and breakage-proof film plating process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811113268.0A CN109293250A (en) | 2018-09-25 | 2018-09-25 | It is a kind of to be conducive to demould convenient and breakage-proof film plating process |
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| Publication Number | Publication Date |
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| CN109293250A true CN109293250A (en) | 2019-02-01 |
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| CN201811113268.0A Pending CN109293250A (en) | 2018-09-25 | 2018-09-25 | It is a kind of to be conducive to demould convenient and breakage-proof film plating process |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103665419A (en) * | 2013-12-06 | 2014-03-26 | 四川达威科技股份有限公司 | Synthesis method and application method of low-medium temperature thermal expansion microspheres |
| US20140364521A1 (en) * | 2012-01-25 | 2014-12-11 | Matsumoto Yushi-Seiyaku Co., Ltd. | Heat-expandable microspheres, process for producing the same, and application thereof |
| CN105400443A (en) * | 2015-12-30 | 2016-03-16 | 深圳市森荣地科技有限公司 | Thermal-expansion strippable pressure-sensitive adhesive sheet and coater |
| CN105555851A (en) * | 2013-08-28 | 2016-05-04 | 松本油脂制药株式会社 | Method for producing thermally expandable microspheres |
| CN108219182A (en) * | 2016-12-15 | 2018-06-29 | 上海略发化工科技有限公司 | A kind of preparation method of heat-expandable microsphere |
| CN108314756A (en) * | 2018-03-09 | 2018-07-24 | 安徽大学 | A kind of microspheres and preparation method thereof prepared based on the original positions Pickering miniemulsion |
-
2018
- 2018-09-25 CN CN201811113268.0A patent/CN109293250A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140364521A1 (en) * | 2012-01-25 | 2014-12-11 | Matsumoto Yushi-Seiyaku Co., Ltd. | Heat-expandable microspheres, process for producing the same, and application thereof |
| CN105555851A (en) * | 2013-08-28 | 2016-05-04 | 松本油脂制药株式会社 | Method for producing thermally expandable microspheres |
| CN103665419A (en) * | 2013-12-06 | 2014-03-26 | 四川达威科技股份有限公司 | Synthesis method and application method of low-medium temperature thermal expansion microspheres |
| CN105400443A (en) * | 2015-12-30 | 2016-03-16 | 深圳市森荣地科技有限公司 | Thermal-expansion strippable pressure-sensitive adhesive sheet and coater |
| CN108219182A (en) * | 2016-12-15 | 2018-06-29 | 上海略发化工科技有限公司 | A kind of preparation method of heat-expandable microsphere |
| CN108314756A (en) * | 2018-03-09 | 2018-07-24 | 安徽大学 | A kind of microspheres and preparation method thereof prepared based on the original positions Pickering miniemulsion |
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Application publication date: 20190201 |
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