CN108059930A - A kind of preparation method of ultra-thin exhaust masking tape/glued membrane - Google Patents

A kind of preparation method of ultra-thin exhaust masking tape/glued membrane Download PDF

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Publication number
CN108059930A
CN108059930A CN201711392434.0A CN201711392434A CN108059930A CN 108059930 A CN108059930 A CN 108059930A CN 201711392434 A CN201711392434 A CN 201711392434A CN 108059930 A CN108059930 A CN 108059930A
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China
Prior art keywords
mass parts
ultra
glued membrane
masking tape
preparation
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CN201711392434.0A
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Inventor
马慰栖
朱东海
刘洪乐
彭晓伟
张晖
李杰霞
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Sichuan Dongcai Technology Group Co Ltd
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Sichuan Dongcai Technology Group Co Ltd
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Priority to CN201711392434.0A priority Critical patent/CN108059930A/en
Publication of CN108059930A publication Critical patent/CN108059930A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04Polyurethanes
    • C09J175/14Polyurethanes having carbon-to-carbon unsaturated bonds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/16Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J133/00Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
    • C09J133/04Homopolymers or copolymers of esters
    • C09J133/14Homopolymers or copolymers of esters of esters containing halogen, nitrogen, sulfur or oxygen atoms in addition to the carboxy oxygen
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/16Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • C08F220/1804C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00Additional features of adhesives in the form of films or foils
    • C09J2301/10Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
    • C09J2301/12Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
    • C09J2301/122Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2423/00Presence of polyolefin
    • C09J2423/04Presence of homo or copolymers of ethene
    • C09J2423/046Presence of homo or copolymers of ethene in the substrate
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2423/00Presence of polyolefin
    • C09J2423/10Presence of homo or copolymers of propene
    • C09J2423/106Presence of homo or copolymers of propene in the substrate
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2427/00Presence of halogenated polymer
    • C09J2427/006Presence of halogenated polymer in the substrate
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2467/00Presence of polyester
    • C09J2467/006Presence of polyester in the substrate

Abstract

The invention discloses a kind of preparation method of ultra-thin exhaust masking tape/glued membrane, it is characterized in that:The acrylic acid adhesive that 100~200 mass parts of urethane acrylate, 100~200 mass parts of acrylic polymer mill base material, 2~5 mass parts of crosslinking agent and 65~120 mass parts of solvent are mixed to composition is uniformly coated on grid release film, 4~8 μm of rubberization thickness, 60~115 DEG C of temperature, long 15~25m totally 5 sections of drying tunnels formed are passed through with 15~30m/min linear velocities, it again will be after grid release film and Film laminated, drying chamber curing is put into, that is, ultra-thin exhaust masking tape/glued membrane is made;It is 0~0.3mm that the adhesive tape/glued membrane tack, which is 3#~5#, holds viscosity, 180 ° of peel strengths are 4~6.5N, light transmittance is 0%~0.6%, the fixations of various precise electronic products, damping, sealing, the sound-absorbing such as can be widely applied to communicate, show.

Description

A kind of preparation method of ultra-thin exhaust masking tape/glued membrane
Technical field
The invention belongs to adhesive tape/glued membranes, are related to a kind of preparation method of ultra-thin exhaust masking tape/glued membrane.Present invention system Standby ultra-thin exhaust masking tape/laminate product such as can be widely applied to communicate after reprocessing, show at the various precise electronics productions The effects that product use particularly suitable for electronic products such as mobile phone, tablet, computers, bumper and absorbing shock, sealing, sound-absorbing are played for clung body.
Background technology
In the prior art, masking tape it is general there are two types of, it is 4~6 μm of base material that a kind of masking tape, which is utilized in thickness, The clear acrylic adhesive of 4~9 μm of surface coating thickness, then come in fact in the mode of 2~3 μm of ink of substrate backside coating thickness Existing shielding, coating layer overall thickness is up to 6~12 μm;Ink is coated with the thickness for also adding adhesive tape, easily has the appearances such as shrinkage cavity not It is good;And be coated with twice, increase production cost.Another masking tape is that mill base is added in adhesive to be directly coated with, still Active ingredient grain size is big in mill base, and in order to make coating appearance uniform smooth, coating thickness is bigger than normal, at 10 μm or more, and mill base Add in the basic performance for generally requiring to sacrifice adhesive tape, such as peel strength, initial bonding strength, retentivity etc.;In addition, because of existing masking tape Select base material generally very thin (4~6 μm), it is not easy to flatten, when fitting easily generates bubble, influences viscous between adhesive tape and affixed object Performance and product appearance.
The content of the invention
The purpose of the present invention is intended to overcome above-mentioned deficiency of the prior art, provides a kind of ultra-thin exhaust masking tape/glue The preparation method of film.The present invention passes through 4~8 μm of coloured adhesive of hard textured surface applied thickness in grid separated type material Afterwards, then with ultrathin film (2~6 μm of thickness) pressure it is bonded and ultra-thin exhaust masking tape/glued membrane is made, so as to provides a kind of thickness It is thin compared with Classical adhesive tape, and properties of product are unaffected, and exhaust passage is introduced on the ultra-thin adhesive band base of tradition, increase row for adhesive tape Gas performance solves the preparation method that fitting generates ultra-thin exhaust masking tape/glued membrane of air bubble problem.
Present disclosure is:A kind of preparation method of ultra-thin exhaust masking tape/glued membrane, it is characterized in that including following step Suddenly:
A, urethane acrylate is prepared:
At room temperature by 36~50 mass parts of diisocyanate, 100~250 mass parts of dihydric alcohol, the acetic acid second of first portion 150~200 mass parts of ester are added to condenser temperature control in condensation reflux unit reaction kettle I, is made at 15 DEG C, with revolution 100~300rpm is stirred, and reacts 3~4h under nitrogen protection;Be warming up to 80~85 DEG C, add methyl methacrylate 15~ 60 mass parts, 15~40 mass parts of ethyl acetate of second portion, 3~6 mass parts of dibutyl tin laurate and polymerization inhibitor 0.4~1.5 mass parts react 3~4h, are cooled to room temperature, that is, urethane acrylate is made, spare;
The diisocyanate is that dicyclohexyl methyl hydride diisocyanate, methyl diphenylene diisocyanate, toluene two are different Mixture more than one or both of cyanate and isophorone diisocyanate;
B, acrylic polymer mill base material is prepared:
At room temperature, by 100 mass parts of n-butyl acrylate, 10~15 mass parts of methacrylic acid, hydroxy-ethyl acrylate 7 1.~10 mass parts, methyl methacrylate 25~30 mass parts, (adding in for the first time) solvent 300~350 mass parts and draw 0.5~3.0 mass parts of agent to be sent out, are added in the reaction kettle II with condensation reflux unit, condenser temperature is controlled below 15 DEG C, Stirring is opened, is uniformly mixed under 100~300rpm of control rotating speed, under the protection of logical nitrogen, 75~80 DEG C is gradually heating to, carries out Solution copolymerization reacts 4~6h, opens II bottom valve of reaction kettle, the material after reaction is put into blending tank A and is cooled to room temperature, then will 5~20 mass parts of colorant, (second add in) solvent 1. 36~60 mass parts, 1~5 mass parts of acetylbutyrylcellulose, one It rises and adds in blending tank A, open stirring, 30~60min is mixed under 100~300rpm of rotating speed, makes to be uniformly mixed, discharge, that is, make Acrylic polymer mill base material is obtained, it is spare;
C, acrylic acid adhesive is prepared:
Acrylic polymer color prepared by step a 100~200 mass parts of urethane acrylate prepared and step b 100~200 mass parts of slurry add in blending tank B, open stirring, 200~500rpm of rotating speed, mixing time 0.5~1h, Ran Houjia Enter 2~5 mass parts of crosslinking agent, solvent 2. 65~120 mass parts, be stirred for 0.5h, discharge to get to acrylic acid adhesive, it is standby With;
The crosslinking agent is that (production provides enterprise name and the trade mark to novolac epoxy resin:Wuxi is resistance to long anti- The trade mark F-51 that rotten Materials Co., Ltd provides;The trade mark F-51 that Shandong De Yuan epoxies Science and Technology Ltd. provides;And Jinan The trade mark SQAN-201 that holy well Group Plc provides), methyl diphenylene diisocyanate and toluene diisocynate Mixture more than one or both of ester;
D, ultra-thin exhaust masking tape/glued membrane is prepared:
On coating machine, acrylic acid adhesive is uniformly coated to thickness as 50 μm, width with glue by applicator roll For on the grid release film of 500~2500mm, rubberization thickness is 4~8 μm, and grid release film is suitable with 15~30m/min linear velocities Secondary by the Ith section of temperature is 60~80 DEG C, the IIth section of temperature is 90~100 DEG C, the IIIth section of temperature is 105~115 DEG C, the IVth section The length that temperature is 95~105 DEG C, the Vth section of temperature is 60~80 DEG C is 15~25m drying tunnels, further prepolymerization, and removing third Solvent in olefin(e) acid adhesive;To scribble again 2~6 μm of the grid release film of acrylic acid adhesive and thickness, width 500~ The film of 2500mm carried out under conditions of platen pressure is 0.4MPa and room temperature it is compound after, it is coiled or cut into dribbling, most After be put into 40~50 DEG C of drying chambers cure again 48~72 it is small when, that is, be made it is ultra-thin exhaust masking tape/glued membrane;
The grid release film can be pet film, brown paper, polyethylene film, with pass One kind in the paper of Racine, net hole shape can be diamond shape, taper, rectangle, and net hole can have different depth, size.
In present disclosure:Dihydric alcohol described in step a can be that (production provides enterprise name to polyether Glycols And the trade mark can be:Guangzhou Ying Hong Chemical Co., Ltd.s N210;Jiangsu Hai'an Petrochemical Plant PPG4000;Shandong mole Chemical industry PPG600) one or both of more than mixture.
In present disclosure:Polymerization inhibitor described in step a can be hydroquinone, p-hydroxyanisole and uncle 2- Mixture more than one or both of butylhydroquinone.
In present disclosure:1. solvent described in step b is one or both of ethyl acetate, toluene, for the first time The solvent of addition is 1. and 1. second of solvent added in is duplicate, i.e. substance classes and proportioning are completely the same.
In present disclosure:Initiator described in step b is benzoyl peroxide or azodiisobutyronitrile.
In present disclosure:Colorant described in step b can be the carbon black, titanium dioxide, kaolinite of 0.1~1 μm of grain size Any one of soil and lead chrome red (inorganic pigment).
In present disclosure:2. solvent described in step c is one or both of toluene, ethyl acetate.
In present disclosure:Film described in step d can be pet film, polyvinyl chloride One kind in film, polyethylene film and polypropylene film.
In present disclosure:The tack that ultra-thin exhaust masking tape/glued membrane is made described in step d is 3#~5#, holds Viscosity is 0~0.3mm, 180 ° of peel strengths are 4~6.5N and light transmittance is 0%~0.6%.
It is described it is ultra-thin exhaust masking tape/glued membrane technical performance test, tack, hold viscosity, 180 ° of peel strengths and Light transmittance is marked respectively according to GB/T 4852-2002, GB/T 4851-1998, GB/T 2792-1998, GB/T2410-2008 Standard carries out.
Compared with prior art, the present invention has following features and advantageous effect:
(1) by urethane acrylate, acrylic polymer mill base material and crosslinking agent, (crosslinking agent is epoxy novolac to the present invention Mixture more than one or both of resin, methyl diphenylene diisocyanate and toluene di-isocyanate(TDI)) carry out group It closes;The grain size of colorant is reduced within 1 μm, and is evenly distributed in adhesive;While light-proofness is met, bondline thickness It can control at 3~8 μm, and not influence other performances of product;It is applied by the hard textured surface in grid separated type material After adhesive, then it is compound with ultrathin film (2~6 μm of thickness), its clean mark, uniform reticulate structure are introduced in glue surface, The introducing of reticulate structure introduces exhaust passage for glue-line, adds exhaust performance, adhesive tape is made to be not easy when fitting with affixed object Generate bubble;
(2) ultra-thin exhaust masking tape/glued membrane measuring technology performance indicator prepared by the present invention is:Tack for > 3#, Hold that viscosity is 0~0.3mm, light transmittance 0%~0.6% and 180 ° of peel strengths are 4~6.5N/25mm, properties of product are good;
(3) a kind of thickness of present invention offer is thin compared with Classical adhesive tape, and properties of product are unaffected, and exhaust is introduced on base material Passage increases exhaust performance for adhesive tape, effectively solves the preparation that fitting generates ultra-thin exhaust masking tape/glued membrane of air bubble problem Method;Product preparation process is simple, and process is easy, easy to operate, highly practical.
Specific embodiment
The invention will be further described for example given below plan, but is not to be construed as to the scope of the present invention Limitation, some nonessential improvement and tune that person skilled in art makes the present invention according to the content of the invention described above It is whole, still fall within protection scope of the present invention.
First portion prepares urethane acrylate
1st, basic technology:
At room temperature by 36~50 mass parts of diisocyanate, 100~250 mass parts of dihydric alcohol, the acetic acid second of first portion (1) 150~200 mass parts of ester be added to in condensation reflux unit reaction kettle I, make condenser temperature control at 15 DEG C, with 100~300rpm of revolution is stirred, and reacts 3~4h under nitrogen protection;80~85 DEG C are warming up to, adds methyl methacrylate (2) 15~40 mass parts of ethyl acetate and 3~6 mass of dibutyl tin laurate of 15~60 mass parts and second portion Part, 0.4~1.5 mass parts of polymerization inhibitor react 3~4h, are cooled to room temperature, that is, urethane acrylate is made, spare;
The diisocyanate is that dicyclohexyl methyl hydride diisocyanate, methyl diphenylene diisocyanate, toluene two are different Cyanate, isophorone diisocyanate;
The dihydric alcohol is polyether Glycols;
The polymerization inhibitor is hydroquinone, p-hydroxyanisole, 2- tert-butyl hydroquinone;
2nd, the urethane acrylate formula material of the preparation of -1~ester of embodiment ester -8, dosage see the table below 1.
Table 1:- 1~ester of embodiment ester -8 prepares the raw material of urethane acrylate, with scale (unit:㎏)
Second portion prepares acrylic polymer mill base material
1st, basic technology:
At room temperature, by 100 mass parts of n-butyl acrylate, 10~15 mass parts of methacrylic acid, hydroxy-ethyl acrylate 7 ~10 mass parts, 25~30 mass parts of methyl methacrylate, solvent 1. 300~350 mass parts and the initiation added in for the first time 0.5~3.0 mass parts of agent are added in the reaction kettle II with condensation reflux unit, and condenser temperature is controlled below 15 DEG C, is opened Stirring is opened, is uniformly mixed under 100~300rpm of control rotating speed, under the protection of logical nitrogen, 75~80 DEG C is gradually heating to, carries out molten Liquid 4~6h of copolyreaction opens II bottom valve of reaction kettle, the material after reaction is put into blending tank A and is cooled to room temperature, then by color Expect 5~20 mass parts, second of solvent added in 1. 36~60 mass parts, 1~5 mass parts of acetylbutyrylcellulose, add together Enter blending tank A, open stirring, 100~300rpm of rotating speed is uniformly mixed 30~60min, acrylic polymer is made in discharging Mill base material, it is spare.
1. the solvent is ethyl acetate, toluene.
The initiator is benzoyl peroxide, azodiisobutyronitrile.
The colorant is carbon black, titanium dioxide, kaolin, lead chrome red.
2nd, the acrylic polymer mill base material formula material of -8 preparation of -1~slurry of embodiment slurry, dosage see the table below 2.
Table 2:Raw material that -1~slurry of embodiment slurry -8 prepares acrylic polymer mill base material, with scale (unit:㎏)
The preparation of Part III acrylic acid adhesive
1st, basic technology:
By 100~200 mass parts of urethane acrylate prepared in above-mentioned 1 and the acrylic acid pre-polymerization prepared in above-mentioned 2 100~200 mass parts of slurry is looked for add in blending tank B, opens and stirs, 200~500rpm of rotating speed, 0.5~1h of mixing time, so Crosslinking agent 2~5 mass parts, solvent 2. 65~120 mass parts are added in afterwards, are stirred for 0.5h, are discharged to get to acrylic acid gluing Agent, it is spare.
The crosslinking agent is novolac epoxy resin, methyl diphenylene diisocyanate, toluene di-isocyanate(TDI).
2. the solvent is toluene, ethyl acetate.
2nd, the acrylic acid gluing agent prescription raw material of the preparation of -1~glue of embodiment glue -8, dosage see the table below 3.
Table 3:- 1~glue of embodiment glue -8 prepares the raw material of acrylic acid adhesive, with scale (unit:㎏)
Part IV prepares ultra-thin exhaust masking tape/glued membrane
1st, basic technology:
On coating machine, acrylic acid adhesive is uniformly coated to thickness with glue coating twill roller or comma scraper is 50 μm, width be 500~2500mm grid release film on, rubberization thickness be 4~8 μm, grid release film is with 15~30m/min Linear velocity, sequentially passes through that the Ith section of temperature is 60~80 DEG C, the IIth section of temperature is 90~100 DEG C, the IIIth section of temperature is 105~115 DEG C, the length that the IVth section of temperature is 95~105 DEG C, the Vth section of temperature is 60~80 DEG C be 15~25m drying tunnels, further pre-polymerization It closes, and removes the solvent in acrylic acid adhesive;The grid release film of acrylic acid adhesive and 2~6 μm of thickness, width will be scribbled again The film of 500~2500mm of degree carried out in pressure roller 0.4MPa and at room temperature it is compound after, it is coiled or cut into dribbling, be finally putting into 40~50 DEG C of drying chambers cure again 48~72 it is small when, that is, be made ultra-thin masking tape/glued membrane.
The release film base material of grid described in the grid release film is polyethylene terephthalate (PET), brown paper, gathers Vinyl film (PE), Ge Laxin paper.
The film is pet film (PET), polyvinyl chloride film (PVC), polyethylene film (PE), polypropylene film (PP).
2nd, 1~band of embodiment band 8 prepares ultra-thin exhaust masking tape/glued membrane raw material, process conditions see the table below 4.
Table 4:1~band of embodiment band 8 prepares raw material, the process conditions table of ultra-thin exhaust masking tape/glued membrane
3rd, 1~band of embodiment band 8 prepares ultra-thin exhaust masking tape/glued membrane and removes the measuring technology after grid release film 5 can be see the table below.
Table 5:Ultra-thin exhaust masking tape/glued membrane institute measuring technology performance table prepared by 1~band of Application Example band 8
Embodiment 9:
A kind of preparation method of ultra-thin exhaust masking tape/glued membrane, comprises the following steps:
A, urethane acrylate is prepared:
At room temperature by 36 mass parts of diisocyanate, 100 mass parts of dihydric alcohol, 150 mass of ethyl acetate of first portion Part is added to condenser temperature in condensation reflux unit reaction kettle I, is made to control at 15 DEG C, is stirred with revolution 100rpm, The lower reaction 3h of nitrogen protection;80 DEG C are warming up to, adds 15 mass parts of methyl methacrylate, the ethyl acetate 15 of second portion 0.4 mass parts of mass parts, 3 mass parts of dibutyl tin laurate and polymerization inhibitor react 3h, are cooled to room temperature, that is, poly- ammonia is made Ester acrylate, it is spare;
B, acrylic polymer mill base material is prepared:
At room temperature, by 100 mass parts of n-butyl acrylate, 10 mass parts of methacrylic acid, 7 mass of hydroxy-ethyl acrylate Part, 25 mass parts of methyl methacrylate, (adding in for the first time) solvent 1. 0.5 mass parts of 300 mass parts and initiator, add in In reaction kettle II with condensation reflux unit, condenser temperature is controlled below 15 DEG C, opens stirring, control rotating speed 100rpm It is lower to be uniformly mixed, under the protection of logical nitrogen, 75 DEG C are gradually heating to, solution copolymerization reaction 4h is carried out, opens II bottom valve of reaction kettle Door, is put into blending tank A by the material after reaction and is cooled to room temperature, then by 5 mass parts of colorant, (second add in) solvent 1. 36 Mass parts, 1 mass parts of acetylbutyrylcellulose add in blending tank A together, open stirring, are mixed under rotating speed 100rpm 30min makes to be uniformly mixed, discharging, that is, acrylic polymer mill base material is made, spare;
C, acrylic acid adhesive is prepared:
Acrylic polymer mill base material prepared by step a 100 mass parts of urethane acrylate prepared and step b 100 mass parts add in blending tank B, open stirring, rotating speed 200rpm, mixing time 0.5h, then add in crosslinking agent 2 mass parts, Solvent 2. 65 mass parts, are stirred for 0.5h, discharge to get to acrylic acid adhesive, spare;
D, ultra-thin exhaust masking tape/glued membrane is prepared:
On coating machine, acrylic acid adhesive is uniformly coated to thickness as 50 μm, width with glue by applicator roll For on the grid release film of 500mm, rubberization thickness is 4 μm, and grid release film sequentially passes through the Ith section of temperature with 15m/min linear velocities It is 90 DEG C to spend for 60 DEG C, the IIth section of temperature, the IIIth section of temperature is 105 DEG C, the IVth section of temperature is 95 DEG C, the Vth section of temperature is 60 DEG C Length for 15m drying tunnels, further prepolymerization, and remove the solvent in acrylic acid adhesive;Acrylic acid adhesive will be scribbled again Grid release film and 2 μm of thickness, the film of width 500mm carried out under conditions of platen pressure is 0.4MPa and room temperature it is compound Afterwards, it is coiled or cut into dribbling, be finally putting into 40 DEG C of drying chambers cure again 72 it is small when, that is, ultra-thin exhaust masking tape/glue is made Film.
Embodiment 10:
A kind of preparation method of ultra-thin exhaust masking tape/glued membrane, comprises the following steps:
A, urethane acrylate is prepared:
At room temperature by 50 mass parts of diisocyanate, 250 mass parts of dihydric alcohol, 200 mass of ethyl acetate of first portion Part is added to condenser temperature in condensation reflux unit reaction kettle I, is made to control at 15 DEG C, is stirred with revolution 300rpm, The lower reaction 4h of nitrogen protection;85 DEG C are warming up to, adds 60 mass parts of methyl methacrylate, the ethyl acetate 40 of second portion 1.5 mass parts of mass parts, 6 mass parts of dibutyl tin laurate and polymerization inhibitor react 4h, are cooled to room temperature, that is, poly- ammonia is made Ester acrylate, it is spare;
B, acrylic polymer mill base material is prepared:
At room temperature, by 100 mass parts of n-butyl acrylate, 15 mass parts of methacrylic acid, 10 matter of hydroxy-ethyl acrylate Part, 30 mass parts of methyl methacrylate, (adding in for the first time) solvent 1. 3.0 mass parts of 350 mass parts and initiator are measured, are added Enter in the reaction kettle II with condensation reflux unit, condenser temperature is controlled below 15 DEG C, opens stirring, controls rotating speed It is uniformly mixed under 300rpm, under the protection of logical nitrogen, is gradually heating to 80 DEG C, carried out solution copolymerization reaction 6h, open reaction kettle Material after reaction is put into blending tank A and is cooled to room temperature by II bottom valve, then by 20 mass parts of colorant, (second add in) Solvent 1. 60 mass parts, 5 mass parts of acetylbutyrylcellulose add in blending tank A together, stirring are opened, under rotating speed 300rpm 60min is mixed, makes to be uniformly mixed, is discharged, that is, acrylic polymer mill base material is made, it is spare;
C, acrylic acid adhesive is prepared:
Acrylic polymer mill base material prepared by step a 200 mass parts of urethane acrylate prepared and step b 200 mass parts add in blending tank B, open stirring, rotating speed 500rpm, mixing time 1h, then add in crosslinking agent 2~5 mass parts, Solvent 2. 120 mass parts, are stirred for 0.5h, discharge to get to acrylic acid adhesive, spare;
D, ultra-thin exhaust masking tape/glued membrane is prepared:
On coating machine, acrylic acid adhesive is uniformly coated to thickness as 50 μm, width with glue by applicator roll For on the grid release film of 2500mm, rubberization thickness is 8 μm, and grid release film sequentially passes through the Ith section with 30m/min linear velocities Temperature is 80 DEG C, the IIth section of temperature is 100 DEG C, the IIIth section of temperature is 115 DEG C, the IVth section of temperature is 105 DEG C, the Vth section of temperature is 80 DEG C of length is 25m drying tunnels, further prepolymerization, and remove the solvent in acrylic acid adhesive;Acrylate glue will be scribbled again 6 μm of the grid release film of glutinous agent and thickness, the film of width 2500mm under conditions of platen pressure is 0.4MPa and room temperature into It is coiled or cut into dribbling after row is compound, be finally putting into 50 DEG C of drying chambers cure again 48 it is small when, that is, ultra-thin exhaust masking glue is made Band/glued membrane.
Embodiment 11:
A kind of preparation method of ultra-thin exhaust masking tape/glued membrane, comprises the following steps:
A, urethane acrylate is prepared:
At room temperature by 43 mass parts of diisocyanate, 175 mass parts of dihydric alcohol, 175 mass of ethyl acetate of first portion Part is added to condenser temperature in condensation reflux unit reaction kettle I, is made to control at 15 DEG C, is stirred with revolution 200rpm, The lower reaction 3.5h of nitrogen protection;83 DEG C are warming up to, adds 38 mass parts of methyl methacrylate, the ethyl acetate of second portion 1 mass parts of 28 mass parts, 4.5 mass parts of dibutyl tin laurate and polymerization inhibitor react 3.5h, are cooled to room temperature, that is, are made Urethane acrylate, it is spare;
B, acrylic polymer mill base material is prepared:
At room temperature, by 100 mass parts of n-butyl acrylate, 13 mass parts of methacrylic acid, 9 mass of hydroxy-ethyl acrylate Part, 28 mass parts of methyl methacrylate, (adding in for the first time) solvent 1. 1.8 mass parts of 325 mass parts and initiator, add in In reaction kettle II with condensation reflux unit, condenser temperature is controlled below 15 DEG C, opens stirring, control rotating speed 200rpm It is lower to be uniformly mixed, under the protection of logical nitrogen, 78 DEG C are gradually heating to, solution copolymerization reaction 5h is carried out, opens II bottom valve of reaction kettle Door, is put into blending tank A by the material after reaction and is cooled to room temperature, then solvent is 1. by 13 mass parts of colorant, (second add in) 48 mass parts, 3 mass parts of acetylbutyrylcellulose add in blending tank A together, open stirring, are mixed under rotating speed 200rpm 45min makes to be uniformly mixed, discharging, that is, acrylic polymer mill base material is made, spare;
C, acrylic acid adhesive is prepared:
Acrylic polymer mill base material prepared by step a 150 mass parts of urethane acrylate prepared and step b 150 mass parts add in blending tank B, open stirring, then rotating speed 350rpm, mixing time 1.8h add in 3.5 mass of crosslinking agent Part, solvent 2. 92 mass parts, be stirred for 0.5h, discharge to get to acrylic acid adhesive, it is spare;
D, ultra-thin exhaust masking tape/glued membrane is prepared:
On coating machine, acrylic acid adhesive is uniformly coated to thickness as 50 μm, width with glue by applicator roll For on the grid release film of 1500mm, rubberization thickness is 6 μm, and grid release film sequentially passes through the Ith section with 28m/min linear velocities Temperature is 70 DEG C, the IIth section of temperature is 95 DEG C, the IIIth section of temperature is 110 DEG C, the IVth section of temperature is 100 DEG C, the Vth section of temperature is 70 DEG C of length is 20m drying tunnels, further prepolymerization, and remove the solvent in acrylic acid adhesive;Acrylate glue will be scribbled again 4 μm of the grid release film of glutinous agent and thickness, the film of width 1500mm under conditions of platen pressure is 0.4MPa and room temperature into It is coiled or cut into dribbling after row is compound, be finally putting into 45 DEG C of drying chambers cure again 60 it is small when, that is, ultra-thin exhaust masking glue is made Band/glued membrane.
Embodiment 12~18:
A kind of preparation method of ultra-thin exhaust masking tape/glued membrane, comprises the following steps:
A, urethane acrylate is prepared:
At room temperature by 36~50 mass parts of diisocyanate, 100~250 mass parts of dihydric alcohol, the acetic acid second of first portion 150~200 mass parts of ester are added to condenser temperature control in condensation reflux unit reaction kettle I, is made at 15 DEG C, with revolution 100~300rpm is stirred, and reacts 3~4h under nitrogen protection;Be warming up to 80~85 DEG C, add methyl methacrylate 15~ 60 mass parts, 15~40 mass parts of ethyl acetate of second portion, 3~6 mass parts of dibutyl tin laurate and polymerization inhibitor 0.4~1.5 mass parts react 3~4h, are cooled to room temperature, that is, urethane acrylate is made, spare;
The specific mass parts dosage of each component raw material (by said sequence) see the table below in each embodiment:
B, acrylic polymer mill base material is prepared:
At room temperature, by 100 mass parts of n-butyl acrylate, 10~15 mass parts of methacrylic acid, hydroxy-ethyl acrylate 7 1.~10 mass parts, methyl methacrylate 25~30 mass parts, (adding in for the first time) solvent 300~350 mass parts and draw 0.5~3.0 mass parts of agent to be sent out, are added in the reaction kettle II with condensation reflux unit, condenser temperature is controlled below 15 DEG C, Stirring is opened, is uniformly mixed under 100~300rpm of control rotating speed, under the protection of logical nitrogen, 75~80 DEG C is gradually heating to, carries out Solution copolymerization reacts 4~6h, opens II bottom valve of reaction kettle, the material after reaction is put into blending tank A and is cooled to room temperature, then will 5~20 mass parts of colorant, (second add in) solvent 1. 36~60 mass parts, 1~5 mass parts of acetylbutyrylcellulose, one It rises and adds in blending tank A, open stirring, 30~60min is mixed under 100~300rpm of rotating speed, makes to be uniformly mixed, discharge, that is, make Acrylic polymer mill base material is obtained, it is spare;
The specific mass parts dosage of each component raw material (by said sequence) see the table below in each embodiment:
C, acrylic acid adhesive is prepared:
Acrylic polymer color prepared by step a 100~200 mass parts of urethane acrylate prepared and step b 100~200 mass parts of slurry add in blending tank B, open stirring, 200~500rpm of rotating speed, mixing time 0.5~1h, Ran Houjia Enter 2~5 mass parts of crosslinking agent, solvent 2. 65~120 mass parts, be stirred for 0.5h, discharge to get to acrylic acid adhesive, it is standby With;
The specific mass parts dosage of each component raw material see the table below in each embodiment:
D, ultra-thin exhaust masking tape/glued membrane is prepared:
On coating machine, acrylic acid adhesive is uniformly coated to thickness as 50 μm, width with glue by applicator roll For on the grid release film of 500~2500mm, rubberization thickness is 4~8 μm, and grid release film is suitable with 15~30m/min linear velocities Secondary by the Ith section of temperature is 60~80 DEG C, the IIth section of temperature is 90~100 DEG C, the IIIth section of temperature is 105~115 DEG C, the IVth section The length that temperature is 95~105 DEG C, the Vth section of temperature is 60~80 DEG C is 15~25m drying tunnels, further prepolymerization, and removing third Solvent in olefin(e) acid adhesive;To scribble again 2~6 μm of the grid release film of acrylic acid adhesive and thickness, width 500~ The film of 2500mm carried out under conditions of platen pressure is 0.4MPa and room temperature it is compound after, it is coiled or cut into dribbling, most After be put into 40~50 DEG C of drying chambers cure again 48~72 it is small when, that is, be made it is ultra-thin exhaust masking tape/glued membrane.
In above-described embodiment 9~18:
Diisocyanate described in step a is dicyclohexyl methyl hydride diisocyanate, methyl diphenylene diisocyanate, first Mixture more than one or both of phenylene diisocyanate and isophorone diisocyanate;
Dihydric alcohol described in step a is that (production provides enterprise name and the trade mark to polyether Glycols:Guangzhou Answer the trade mark PPG4000 and Shandong that the trade mark N210 of deep Chemical Co., Ltd.'s offer, Jiangsu Hai'an Petrochemical Plant are provided The polyether Glycols for the trade mark PPG600 that mole chemical industry provides) one or both of more than mixture;
Polymerization inhibitor described in step a is one kind in hydroquinone, p-hydroxyanisole and 2- tert-butyl hydroquinone Or two or more mixture;
1. solvent described in step b is one or both of ethyl acetate, toluene, the solvent added in for the first time is 1. with the 1. the solvent of secondary addition is duplicate, i.e. substance classes and proportioning are completely the same;
Initiator described in step b is benzoyl peroxide or azodiisobutyronitrile;
Colorant described in step b is appointing in carbon black, titanium dioxide, kaolin and the lead chrome red of 0.1~1 μm of grain size A kind of (inorganic pigment);
2. solvent described in step c is toluene or/and ethyl acetate;
Crosslinking agent described in step c is that (production provides enterprise name and the trade mark to novolac epoxy resin:Wuxi The trade mark F-51 that anti-corrosion Materials Co., Ltd provides long;The trade mark F-51 that Shandong De Yuan epoxies Science and Technology Ltd. provides;With And Shengquan Group Co. Ltd., Jinan provide trade mark SQAN-201 novolac epoxy resin), two isocyanide of diphenyl methane Mixture more than one or both of acid esters and toluene di-isocyanate(TDI);
Grid release film described in step d be pet film, brown paper, polyethylene film, with One kind in the paper of qualifying Racine, net hole shape can be diamond shape, taper, rectangle, and net hole can have different depth, size;
Film described in step d be pet film, polyvinyl chloride film, polyethylene film, with And one kind in polypropylene film.
In above-described embodiment 9~18:Described in step d be made it is ultra-thin exhaust masking tape/glued membrane tack for 3#~5#, Hold viscosity for 0~0.3mm, 180 ° of peel strengths are 4~6.5N and light transmittance is 0%~0.6%.
Above-described embodiment 9~18 it is described it is ultra-thin exhaust masking tape/glued membrane technical performance test, tack, hold viscosity, 180 ° of peel strengths and light transmittance respectively according to GB/T 4852-2002, GB/T 4851-1998, GB/T 2792-1998, GB/T 2410-2008 standards carry out.
In above-described embodiment:It is especially not dated in used percentage, be quality (weight) percentage or Well known to a person skilled in the art percentages;In used ratio, especially not dated, it is quality (weight) ratio; The parts by weight can be gram or kilogram.
In above-described embodiment:Technological parameter (temperature, time, speed, rotating speed etc.) and each component dosage number in each step Value etc. is scope, and any point is applicable.
The technology contents being not specifically delineated in present invention and above-described embodiment are compared with technology, the raw material Commercial product.
Can it implement the invention is not restricted to above-described embodiment, described in present invention and with the good result.

Claims (9)

1. a kind of preparation method of ultra-thin exhaust masking tape/glued membrane, it is characterized in that comprising the following steps:
A, urethane acrylate is prepared:
At room temperature by 36~50 mass parts of diisocyanate, 100~250 mass parts of dihydric alcohol, first portion ethyl acetate 150 ~200 mass parts be added to in condensation reflux unit reaction kettle I, make condenser temperature control at 15 DEG C, with revolution 100~ 300rpm is stirred, and reacts 3~4h under nitrogen protection;80~85 DEG C are warming up to, adds 15~60 matter of methyl methacrylate Measure part, 15~40 mass parts of ethyl acetate of second portion, 3~6 mass parts of dibutyl tin laurate and polymerization inhibitor 0.4 ~1.5 mass parts react 3~4h, are cooled to room temperature, that is, urethane acrylate is made, spare;
The diisocyanate is dicyclohexyl methyl hydride diisocyanate, methyl diphenylene diisocyanate, toluene diisocynate Mixture more than one or both of ester and isophorone diisocyanate;
B, acrylic polymer mill base material is prepared:
At room temperature, by 100 mass parts of n-butyl acrylate, 10~15 mass parts of methacrylic acid, hydroxy-ethyl acrylate 7~10 Mass parts, 25~30 mass parts of methyl methacrylate, solvent 1. 0.5~3.0 mass parts of 300~350 mass parts and initiator, It adds in the reaction kettle II with condensation reflux unit, condenser temperature is controlled below 15 DEG C, opens stirring, controls rotating speed Be uniformly mixed under 100~300rpm, under the protection of logical nitrogen, be gradually heating to 75~80 DEG C, carry out solution copolymerization react 4~ Material after reaction is put into blending tank A and is cooled to room temperature by 6h, then by 5~20 mass parts of colorant, solvent 1. 36~60 mass Part, 1~5 mass parts of acetylbutyrylcellulose, add in blending tank A, open stirring, under 100~300rpm of rotating speed mix 30~ Acrylic polymer mill base material is made in 60min, spare;
C, acrylic acid adhesive is prepared:
Acrylic polymer mill base material prepared by step a 100~200 mass parts of urethane acrylate prepared and step b 100~200 mass parts add in blending tank B, open stirring, then 200~500rpm of rotating speed, 0.5~1h of mixing time are added in and handed over Join agent 2~5 mass parts, solvent 2. 65~120 mass parts, be stirred for 0.5h to get to acrylic acid adhesive, it is spare;
The crosslinking agent is one kind in novolac epoxy resin, methyl diphenylene diisocyanate and toluene di-isocyanate(TDI) Or two or more mixture;
D, ultra-thin exhaust masking tape/glued membrane is prepared:
On coating machine, by acrylic acid adhesive with glue by applicator roll be uniformly coated to thickness be 50 μm, width 500 On the grid release film of~2500mm, rubberization thickness is 4~8 μm, and grid release film is sequentially led to 15~30m/min linear velocities Cross that the Ith section of temperature is 60~80 DEG C, the IIth section of temperature is 90~100 DEG C, the IIIth section of temperature is 105~115 DEG C, the IVth section of temperature For 95~105 DEG C, the Vth section of temperature be 60~80 DEG C length be 15~25m drying tunnels;The net of acrylic acid adhesive will be scribbled again 2~6 μm of lattice release film and thickness, the film of 500~2500mm of width under conditions of platen pressure is 0.4MPa and room temperature into It is coiled or cut into dribbling after row is compound, be finally putting into 40~50 DEG C of drying chambers cure again 48~72 it is small when, that is, ultra-thin row is made Gas masking tape/glued membrane;
The grid release film be pet film, brown paper, polyethylene film, in the paper of qualifying Racine One kind.
2. the preparation method of ultra-thin exhaust masking tape/glued membrane as described in claim 1, it is characterized in that:Binary described in step a Alcohol is mixtures more than one or both of polyether Glycols.
3. the preparation method of ultra-thin exhaust masking tape/glued membrane as described in claim 1, it is characterized in that:It is inhibited described in step a Agent is mixture more than one or both of hydroquinone, p-hydroxyanisole and 2- tert-butyl hydroquinone.
4. the preparation method of ultra-thin exhaust masking tape/glued membrane as described in claim 1, it is characterized in that:Solvent described in step b 1. it is one or both of ethyl acetate, toluene.
5. the preparation method of ultra-thin exhaust masking tape/glued membrane as described in claim 1, it is characterized in that:Trigger described in step b Agent is benzoyl peroxide or azodiisobutyronitrile.
6. the preparation method of ultra-thin exhaust masking tape/glued membrane as described in claim 1, it is characterized in that:Colorant described in step b It is any one of carbon black, titanium dioxide, kaolin and lead chrome red of 0.1~1 μm of grain size.
7. the preparation method of ultra-thin exhaust masking tape/glued membrane as described in claim 1, it is characterized in that:Solvent described in step c 2. it is one or both of toluene, ethyl acetate.
8. the preparation method of ultra-thin exhaust masking tape/glued membrane as described in claim 1, it is characterized in that:Film described in step d It is one kind in pet film, polyvinyl chloride film, polyethylene film and polypropylene film.
9. the preparation method of ultra-thin exhaust masking tape/glued membrane as described in claim 1, it is characterized in that:It is made described in step d super The tack of thin exhaust masking tape/glued membrane is 3#~5#, to hold viscosity be 0~0.3mm, 180 ° of peel strengths be 4~6.5N and Light transmittance is 0%~0.6%.
CN201711392434.0A 2017-12-21 2017-12-21 A kind of preparation method of ultra-thin exhaust masking tape/glued membrane Pending CN108059930A (en)

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CN112760046A (en) * 2020-12-28 2021-05-07 苏州德佑新材料科技股份有限公司 Ultrathin single-side grid adhesive tape and preparation method thereof
CN114621700A (en) * 2021-04-12 2022-06-14 常州威斯双联科技有限公司 Heat-conducting ultrathin grid adhesive tape and preparation method thereof
CN114836148A (en) * 2022-05-19 2022-08-02 浙江福莱新材料股份有限公司 Preparation method of grid release film, grid release film and anti-falling exhaust adhesive tape

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CN108676513A (en) * 2018-06-06 2018-10-19 芜湖夏鑫新型材料科技有限公司 A kind of mobile phone glass protective film and preparation method thereof
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CN114621700A (en) * 2021-04-12 2022-06-14 常州威斯双联科技有限公司 Heat-conducting ultrathin grid adhesive tape and preparation method thereof
CN114836148A (en) * 2022-05-19 2022-08-02 浙江福莱新材料股份有限公司 Preparation method of grid release film, grid release film and anti-falling exhaust adhesive tape

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Application publication date: 20180522