CN101671354B - Method for preparing release agent - Google Patents

Method for preparing release agent Download PDF

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Publication number
CN101671354B
CN101671354B CN2009101903334A CN200910190333A CN101671354B CN 101671354 B CN101671354 B CN 101671354B CN 2009101903334 A CN2009101903334 A CN 2009101903334A CN 200910190333 A CN200910190333 A CN 200910190333A CN 101671354 B CN101671354 B CN 101671354B
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Prior art keywords
grating
parts
remover
preparation
release agent
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CN101671354A (en
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魏伟
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Shenzhen Super Technology Co Ltd
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深圳超多维光电子有限公司
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Abstract

The invention discloses a method for preparing release agent, and the release agent is prepared by silane coupling agent monomer through hydrolytic condensation reaction. The silane coupling agent monomer can be 4-methyl-(perfluoroalkyl hexyl ethyl) propyl trimethoxy silane or tetraethoxysilane. A Mould modified by the release agent prepared by the method can be used for manufacturing a micro-lens array grating, and the manufactured grating has good appearance, has no phenomenon of burr, orange peel, water wave, uneven photo-permeability and the like, and can meet the requirement of producing the high quality grating.

Description

A kind of preparation method of releasing agent
Technical field
The present invention relates to a kind of preparation method of releasing agent.
Background technology
In stereo display technique; Especially in the bore hole stereo display technique; The use of microlens array grating more and more widely; The production technique of microlens array grating also reaches its maturity with various, and the technology that especially adopts UV to solidify glue (UV-irradiation curing glue) production microlens array grating more and more receives publicity and develops.The UV cured adhesive is by prepolymer, reactive monomer, and principal constituents such as light trigger are equipped with auxiliary agents such as stablizer, flow agent and form.It is under the UV rayed of suitable wavelength, and light trigger generates radical or ion rapidly, causes prepolymer and reactive monomer polymerization crosslinking and reticulates structure, glues the bonding of material thereby accomplish with quilt.
On the slightly concave array mold, can prepare dimpling lens arra grating; On dimpling shape array mold, can prepare nick lens arra grating; The material of mould can be metal (copper, iron, tin etc.) in the preparation; Also can be that UV solidifies glue material (epoxy resin, polyester, urethane etc.), perhaps organic polymer (polymethylmethacrylate, Z 150PH, PS etc.).Be elaborated in the face of the method for making nick lens arra grating in the prior art down.
Making method comprises the steps:
Step 1: coating UV is solidified glue on mould.UV is solidified glue to be coated on the column dimpling shape array mold;, UV covers base materials such as one deck PET (polyethylene terephthalate) material or glass on solidifying glue; Roll squeezer or laminating machine roll extrusion through adjusting spacing are smooth, and unnecessary glue amount is extruded; Make UV solidify glue nature levelling through the suitable UV roller coating machine of spacing after also can UV being solidified the glue coating.
Step 2: ultraviolet light polymerization.The dimpling shape array mold that coating is accomplished is placed in the oxygen-free environment, like nitrogen environment etc., makes UV solidify adhesive curing with ultra violet lamp.
Step 3: the demoulding.Just peel off, can also can obtain column nick lens arra grating by mechanically peel by manual removal.
In order can intactly to peel off, before making grating, need carry out modification to the surface of mould and handle, change the performance of die surface, make grating break away from and be more prone to from mould.Present modification mode is surface coating and use remover, and the advantage of surface coating is that the grating surface pattern that makes is good.But coating temperature is high, is prone to make that mould deforms, and protruding grating and most concave(diffraction)grating narrow for arch span and that sagitta is big are inapplicable, and the demoulding number of times of making grating is limited, and the technology cost is more high.It is cheap using the advantage of remover, and all gratings all are suitable for, and the demoulding number of times is than adopting the many of plated film.But also can produce grating smoothly behind the at present commercially available remover modification mould, but that the sub-gratings that makes can occur is scared, orange peel, water wave, printing opacity are inhomogeneous etc., can not satisfy application.
Summary of the invention
The object of the present invention is to provide the preparation method of the better releasing agent of a kind of modified effect with low cost, the releasing agent that this method obtains can remedy the deficiency of existing releasing agent.
In order to realize the object of the invention, the spy provides a kind of preparation method of remover, adopts the silane coupling agent monomer to prepare through hydrolysis-condensation reaction.
Said silane coupling agent monomer can be 4-methyl-(perfluoro hexyl ethyl) propyl trimethoxy silicane, and concrete preparation process is following:
4-methyl-(perfluoro hexyl ethyl) propyl trimethoxy silicane and 15 parts of deionized waters of 1) measuring 1 part of purity 96% respectively with graduated cylinder are mixed in the round-bottomed flask;
2) add magnetic agitation and start magnetic agitation and solution was mixed in 2 minutes, this moment, solution was muddy state;
3) in flask, drip acidic solution and make solution pH value to 3.0 between 4.0, add 16 parts of absolute ethyl alcohols then, reflux obtains water white remover after 24 hours.
Said silane coupling agent monomer can also be tetraethoxy, and concrete preparation process is following:
1) measures 7 parts of absolute ethyl alcohols respectively with graduated cylinder and 3 parts of deionized waters are mixed in the round-bottomed flask, add magnetic agitation and also start magnetic agitation;
2) in flask, drip 8 parts of tetraethoxys, in flask, drip acidic solution again and make pH value to 3.0 between 4.0, stirring reaction obtained colourless transparent solution after 5 hours under the room temperature;
3) with this colourless transparent solution uniform mixing in the solvent of forming by 200 parts of ethanol and 2000 parts of deionized waters, stirred 1 hour, promptly obtain remover.
Said acidic solution can be Glacial acetic acid min. 99.5 or hydrochloric acid.
The mould that will pass through the releasing agent modification of method for preparing is used on the microlens array preparing grating, and the grating surface pattern that makes is good, and it is inhomogeneous etc. scared, orange peel, water wave, printing opacity can not to occur, can satisfy the requirement of production high-quality grating.
Description of drawings
Do not have
Embodiment
The be hydrolyzed method of condensation reaction of silane coupling agent monomer is all adopted in the preparation of remover among the present invention.The embodiment of the invention has been enumerated and has been utilized two kinds of silane coupling agent monomers to prepare the method for releasing agent, and two kinds of silane coupling agent monomers are respectively 4-methyl-(perfluoro hexyl ethyl) propyl trimethoxy silicane and tetraethoxy, describe respectively below.
(1) utilize 4-methyl-(perfluoro hexyl ethyl) propyl trimethoxy silicane to prepare the method for remover
4-methyl-(perfluoro hexyl ethyl) propyl trimethoxy silicane and the 150ml deionized water of 1) measuring 10ml purity 96% respectively with graduated cylinder are mixed in the round-bottomed flask;
2) add magnetic agitation and start magnetic agitation and solution was mixed in 2 minutes, this moment, solution was muddy state;
3) in flask, drip Glacial acetic acid min. 99.5 or hydrochloric acid conditioning solution pH value to 3.0 between 4.0, add the 160ml absolute ethyl alcohol then and do solubilizing agent, heating reflux reaction obtained colourless transparent solution after 24 hours, was remover.
In the aforesaid method, the ratio of 4-methyl-(perfluoro hexyl ethyl) propyl trimethoxy silicane, deionized water and absolute ethyl alcohol is 1: 15: 16.
(2) utilize tetraethoxy to prepare the method for remover
1) measures the 7ml absolute ethyl alcohol respectively with graduated cylinder and the 3ml deionized water is mixed in the round-bottomed flask, add magnetic agitation and also start magnetic agitation;
2) in flask, drip the 8ml tetraethoxy, drip and in flask, drip Glacial acetic acid min. 99.5 or hydrochloric acid conditioning solution pH value to 3.0 between 4.0, stirring reaction obtained colourless transparent solution after 5 hours under the room temperature;
3) this solution is evenly splashed in the solvent of being made up of 200ml ethanol and 2000ml deionized water, stirred 1 hour, promptly obtain remover.
After making above-mentioned releasing agent; To treat that the modification mould is immersed in the remover of the above-mentioned 4-of utilization methyl-(perfluoro hexyl ethyl) propyl trimethoxy silicane preparation; Soak after 0.5 minute and take out; Direction is vertically put into 60 ℃ constant temperature electric heating air dry oven along the mould gully, places 0.5-1.5 hour post-modification process and accomplishes.Storage period, length was decided according to the pitch of mould, and pitch is more little, in requisition for modification time long more.
For the above-mentioned remover that utilizes the tetraethoxy preparation; To treat that equally the modification mould soaks wherein taking-up after 0.5 minute; Mould gully, room temperature lower edge direction is vertically placed, and the post-modification process was accomplished in time 1-3 days, and storage period, length was decided according to the pitch of mould; Pitch is more little, in requisition for modification time long more.
The mould that will pass through above-mentioned modification is used in the preparing grating process, and the grating surface pattern that makes is good.It is inhomogeneous etc. scared, orange peel, water wave, printing opacity can not to occur, can satisfy the requirement of production high-quality grating.Those skilled in the art will envision that the application that accordings to the releasing agent of the present invention's preparation is not limited to the preparation of grating, can also be used for the field that other adopts mould to produce.And being not limited to above-mentioned two kinds of silane coupling agent monomers, other silane coupling agent monomer can obtain identical effect equally.
The present invention prepares the remover that is fit to the die surface modification, and mould can unlimited preparation grating after surface-treated and the surface topography of grating is bright and clean, printing opacity is even, can satisfy application.
Above-mentioned embodiment only is schematic; Rather than restrictive, those skilled in the art is not breaking away under the scope situation that present method aim and claim protect under the enlightenment of present method; Can also make a lot of distortion, these all belong within protection scope of the present invention.

Claims (3)

1. the preparation method of a remover is characterized in that adopting tetraethoxy to prepare through hydrolysis-condensation reaction, and its concrete preparation process is following:
1) measures 7 parts of absolute ethyl alcohols respectively with graduated cylinder and 3 parts of deionized waters are mixed in the round-bottomed flask, add magnetic agitation and also start magnetic agitation;
2) in flask, drip 8 parts of tetraethoxys, in flask, drip acidic solution again and make pH value to 3.0 between 4.0, stirring reaction obtained colourless transparent solution after 5 hours under the room temperature;
3) with this colourless transparent solution uniform mixing in the solvent of forming by 200 parts of ethanol and 2000 parts of deionized waters, stirred 1 hour, promptly obtain remover.
2. the preparation method of remover according to claim 1 is characterized in that, said acidic solution is a Glacial acetic acid min. 99.5.
3. the preparation method of remover according to claim 1 is characterized in that, said acidic solution is a hydrochloric acid.
CN2009101903334A 2009-09-17 2009-09-17 Method for preparing release agent Active CN101671354B (en)

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Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPWO2018163936A1 (en) 2017-03-07 2020-01-09 日本板硝子株式会社 Optical component and method of manufacturing optical component
CN108312396B (en) * 2018-01-31 2021-10-26 漳州丰笙新材料有限公司 Silicon release agent and preparation method thereof
CN114106601B (en) * 2021-12-30 2022-12-13 上海中化科技有限公司 Stripping coating composition and method for preparing polyimide film by using same

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5384365A (en) * 1990-12-28 1995-01-24 Dainichiseika Color & Chemicals Mfg. Co., Ltd. Release agents
JP2003236819A (en) * 2001-12-11 2003-08-26 Asahi Kasei Corp Mold release agent for form, and form

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5384365A (en) * 1990-12-28 1995-01-24 Dainichiseika Color & Chemicals Mfg. Co., Ltd. Release agents
JP2003236819A (en) * 2001-12-11 2003-08-26 Asahi Kasei Corp Mold release agent for form, and form

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
威娒等.硅烷偶联剂在金属上的应用.《表面技术》.1999,第28卷(第4期),37-40. *
黄汉生.硅烷偶联剂及其应用技术动向.《化工新型材料》.1995,(第11期),23-27,12. *

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