CN102105546A - Method for provisional fixing/release of member and adhesive for provisional fixing suitable therefor - Google Patents

Method for provisional fixing/release of member and adhesive for provisional fixing suitable therefor Download PDF

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Publication number
CN102105546A
CN102105546A CN2009801287063A CN200980128706A CN102105546A CN 102105546 A CN102105546 A CN 102105546A CN 2009801287063 A CN2009801287063 A CN 2009801287063A CN 200980128706 A CN200980128706 A CN 200980128706A CN 102105546 A CN102105546 A CN 102105546A
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CN
China
Prior art keywords
methyl
acrylate
working fastening
temporarily fixing
glue
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Granted
Application number
CN2009801287063A
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Chinese (zh)
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CN102105546B (en
Inventor
栗村启之
金井朋之
大岛和宏
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Denka Co Ltd
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Denki Kagaku Kogyo KK
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J5/00—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/67—Unsaturated compounds having active hydrogen
    • C08G18/671—Unsaturated compounds having only one group containing active hydrogen
    • C08G18/672—Esters of acrylic or alkyl acrylic acid having only one group containing active hydrogen
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D133/00—Coating compositions 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; Coating compositions based on derivatives of such polymers
    • C09D133/04—Homopolymers or copolymers of esters
    • C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C09D133/08—Homopolymers or copolymers of acrylic acid esters
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • C09J175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
    • C09J175/16—Polyurethanes having carbon-to-carbon unsaturated bonds having terminal carbon-to-carbon unsaturated bonds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J201/00—Adhesives based on unspecified macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
    • C09J2301/416—Additional features of adhesives in the form of films or foils characterized by the presence of essential components use of irradiation
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2433/00—Presence of (meth)acrylic polymer
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2475/00—Presence of polyurethane

Abstract

Provided is a method of provisional fixing which is remarkably effective in the dimensional accuracy of processed members. The method of provisional fixing comprises: a coating step in which a fixing member is coated with an adhesive for provisional fixing; a mounting step in which a member to be processed is mounted on the adhesive for provisional fixing; an irradiation step in which the adhesive for provisional fixing is irradiated with at least either visible rays or ultraviolet rays after the mounting step to heighten the adhesive force of the adhesive for provisional fixing; and a pressing step in which the fixing member and the member to be processed are pressed together from one side or both sides. The method of provisional fixing is characterized by simultaneously conducting the pressing step and the irradiation step for at least a certain time period. The adhesive for provisional fixing is a composition comprising a polyfunctional (meth)acrylate (A), a monofunctional (meth)acrylate (B), and a photopolymerization initiator (C).

Description

Working fastening/the stripping means of member and the working fastening that is suitable for it stick with glue agent
Technical field
Working fastening/stripping means when the present invention relates to process various member also relates to the working fastening that the working fastening that is suitable for this method uses and sticks with glue agent.For example, the light solidity working fastening that relates to the method for this member of working fastening when the processing optical member and stripping means and be suitable for this purposes sticks with glue agent.
Background technology
Working fastening as optical lens, prism, array, silicon wafer, semi-conductor installation component etc. sticks with glue agent, using double sticky tape or hot melt is tackiness agent, after will being the shape of regulation with these tackiness agent joints or stacked member machining, remove tackiness agent, make tool member.For example, in the semi-conductor installation component, be fixed on base material on double sticky tape these members after, machining becomes required member, and then by the double sticky tape irradiation ultraviolet radiation being carried out peeling off from the member.In addition, be under the situation of tackiness agent at hot melt, behind the engagement member, make tackiness agent be penetrated in the gap by heating after, machining becomes required member, carries out peeling off of tackiness agent in organic solvent.
But there are the following problems under the situation of double sticky tape: be difficult to obtain dimensional precision, or it is poor to cause member to add cutting in man-hour (チ Star ピ Application グ) owing to adhesive strength is low, or is not heated to more than 100 ℃ and just can not peels off.Utilizing uviolizing to make under its situation about peeling off, the problem that can not peel off when having the transmissivity deficiency when adherend.
Using hot melt is under the situation of tackiness agent, needs with an organic solvent when peeling off, and basic solution or halogen are that the clean operation of organic solvent is numerous and diverse, and in addition, operating environment also becomes problem.
In order to solve these defectives, solid type of light or heating type glue stick that the working fastening of water-soluble cpdss such as water-soluble vinyl monomer is used have been proposed to contain.Use in the method for temporarily fixing of these tackiness agent, solved the separability in water, but with respect to this, have that the solid periodic adhesive strength of member is low, an insufficient problem of dimensional precision of the member after the machining.
In addition, proposed a kind of working fastening and sticked with glue agent, it improves tackiness by using specific high (methyl) acrylate of wetting ability, utilizes swelling simultaneously or is partly dissolved and improve separability.This working fastening sticks with glue agent, when machining, produces the heat of friction of member and cutting tools such as blade or diamond cutter, therefore need it be cooled off.There are the following problems for the high composition of above-mentioned wetting ability: the cured article swelling limbers up during owing to cutting, therefore, can not reach higher dimensional precision.In addition, because the member top dissolved cured article adhesive paste peeled off is residual, so outward appearance aspect go wrong (with reference to patent documentation 1,2,3).
Patent documentation 1: Japanese kokai publication hei 6-116534 communique
Patent documentation 2: Japanese kokai publication hei 11-71553 communique
Patent documentation 3: TOHKEMY 2001-226641 communique
Summary of the invention
In order to improve the dimensional precision of the member after the machining, expectation hydrophobicity, high adhesive strength and the separability excellence in water, peel off no adhesive paste on the member of back residual, aspect environment operability also working fastening/the stripping means of excellence and the working fastening that is suitable for this method stick with glue agent.
The present invention has carried out various researchs for the problem that solves these prior aries, found that, by having the operation that side from stationary member and processed member or both sides exert pressure, and this operation of exerting pressure and this operation of shining are implemented certain hour at least simultaneously, thus, add and to obtain the excellent size precision man-hour, thereby can realize the present invention.
That is, the present invention has following formation.
(1) a kind of method of temporarily fixing, comprise: working fastening is sticked with glue agent be applied to operation (hereinafter referred to as painting process) on the stationary member, processed member carried in working fastening stick with glue operation (hereinafter referred to as carrying operation) in the agent, with this lift-launch back working fastening is sticked with glue at least a in agent irradiation visible light or the ultraviolet ray and improve the operation (hereinafter referred to as irradiation process) that working fastening sticks with glue the adhesive power of agent, also comprise the operation (hereinafter referred to as the pressurization operation) that side from stationary member and processed member or both sides exert pressure, wherein, the operation that this is exerted pressure and this operation of shining are implemented certain hour at least simultaneously.
(2) a kind of method of temporarily fixing, comprise: working fastening is sticked with glue agent be applied to operation (hereinafter referred to as painting process) on the processed member, stationary member carried in working fastening stick with glue operation (hereinafter referred to as carrying operation) in the agent, with this lift-launch back working fastening is sticked with glue at least a in agent irradiation visible light or the ultraviolet ray and improve the operation that working fastening sticks with glue the adhesive power of agent, also comprise the operation (hereinafter referred to as the pressurization operation) that side from stationary member and processed member or both sides exert pressure, wherein, the operation that this is exerted pressure and this operation of shining are implemented certain hour at least simultaneously.
(3) as above-mentioned (1) or (2) described method of temporarily fixing, wherein, a side or both sides' applied pressure from stationary member and processed member are controlled at 1g/cm 2More than and 1000kg/cm 2Below.
(4), wherein, stationary member, working fastening sticked with glue be controlled at more than 0 ℃ more than any in agent, the processed member and below 150 ℃ as above-mentioned (1) or (3) described method of temporarily fixing.
(5) as each described method of temporarily fixing in above-mentioned (1) to (4), wherein, working fastening sticks with glue agent for containing (A) multifunctional (methyl) acrylate, (B) simple function (methyl) acrylate and (C) composition of Photoepolymerizationinitiater initiater.
(6), wherein, (A) and (B) be hydrophobicity as the method for temporarily fixing of above-mentioned (5) described member.
(7) as each described method of temporarily fixing in above-mentioned (1) to (6), wherein, working fastening sticks with glue the second-order transition temperature of agent for more than-50 ℃ and below 50 ℃.
(8) as each described method of temporarily fixing in above-mentioned (5) to (7), wherein, working fastening sticks with glue agent, in (A) and total amount 100 mass parts (B), contain (A) 1～90 mass parts, (B) 10～99 mass parts, and contain (C) 0.1～30 mass parts with respect to (A) and total amount 100 mass parts (B).
(9) as each described method of temporarily fixing in above-mentioned (5) to (8), wherein, working fastening sticks with glue agent, contains particulate matter (D) 0.1～20 mass parts that is insoluble to (A)～(C) with respect to (A) and total amount 100 mass parts (B).
(10) as above-mentioned (9) described method of temporarily fixing, wherein, be insoluble to (A)～(C) particulate matter (D) be shaped as spherical.
(11) as above-mentioned (9) or (10) described method of temporarily fixing, wherein, the particulate matter (D) that is insoluble to (A)～(C) is the mixture of any or they in crosslinked polymethylmethacrylaparticles particle, crosslinked polystyrene particle and the crosslinked polymethylmethacrylaparticles polystyrene copolymer particle.
(12) as each described method of temporarily fixing in above-mentioned (9) to (11), the median size that wherein, is insoluble to the particulate matter (D) of (A)～(C) is 5 μ m～200 μ m.
(13) as each described method of temporarily fixing in above-mentioned (9) to (12), wherein, the particle volume of particle diameter (μ m) when representing with logarithm that utilizes laser diffractometry to measure that will be insoluble to the particulate matter (D) of (A)～(C) distributes with respect to the standard deviation of particle diameter in 0.0001～0.25 scope.
(14) a kind of working fastening/stripping means of member, wherein, comprise: after each described method of temporarily fixing carries out the member processing of working fastening in above-mentioned to using (1) to (13), the member after this processing is immersed in the warm water below 100 ℃, removes the cured article of described composition.
(15) a kind of working fastening/stripping means of member, wherein, comprise: after each described method of temporarily fixing carries out the member processing of working fastening in above-mentioned to using (1) to (13), working fastening is sticked with glue agent irradiation visible light or ultraviolet ray, member after this processing is immersed in the warm water below 100 ℃, removes the cured article of described composition.
(16) as each described method of temporarily fixing in above-mentioned (1) to (13), wherein, visible light or ultraviolet irradiation amount are 1mJ/cm at wavelength 365nm place 2～4000mJ/cm 2Scope.
As above-mentioned (15) described working fastening/stripping means, it is characterized in that (17) visible light or ultraviolet irradiation amount that the member processing back of this working fastening is shone are 1000mJ/cm at wavelength 365nm place 2～40000mJ/cm 2Scope.
(18) as each described method of temporarily fixing in above-mentioned (5) to (13), wherein, (A) multifunctional (methyl) acrylate contains multifunctional (methyl) origoester acrylate/polymkeric substance and/or two senses (methyl) acrylate monomer.
(19) as each described method of temporarily fixing in above-mentioned (5) to (13), wherein, (A) multifunctional (methyl) acrylate contains multifunctional (methyl) origoester acrylate/polymkeric substance and two senses (methyl) acrylate monomer.
(20) as above-mentioned (18) or (19) described method of temporarily fixing, wherein, multifunctional (methyl) origoester acrylate/polymkeric substance contains polyester urethane (methyl) acrylate and/or polyethers urethane (methyl) acrylate.
(21) as above-mentioned (18) or (19) described method of temporarily fixing, wherein, two senses (methyl) acrylate monomer contains 1,6-hexylene glycol two (methyl) acrylate and/or two (methyl) vinylformic acid dicyclo pentyl ester.
(22) as each described method of temporarily fixing in above-mentioned (5) to (13), wherein, (B) simple function (methyl) acrylate contains 2 moles of modification (methyl) acrylate of phenol ring oxidative ethane and/or 2-(1,2-encircles six carboxyl imides) ethyl (methyl) acrylate.
(23) as each described method of temporarily fixing in above-mentioned (5) to (13), wherein, (B) simple function (methyl) acrylate contains 2 moles of modification (methyl) acrylate of phenol ring oxidative ethane and 2-(1,2-encircles six carboxyl imides) ethyl (methyl) acrylate.
(24) as each described method of temporarily fixing in above-mentioned (5) to (13), wherein, (C) Photoepolymerizationinitiater initiater contain be selected from benzyl dimethyl ketal, oxygen base-phenyl-acetic acid 2-[2-oxo-2-phenyl-acetic acid base-oxyethyl group]-ethyl ester and oxygen base-phenyl-acetic acid 2-[2-hydroxyl-oxyethyl group]-in the ethyl ester more than a kind or 2 kinds.
In the method for temporarily fixing of the present invention, implement certain hour at least simultaneously, obtaining significant effect aspect the dimensional precision of processed member by will pressurize operation and irradiation process.
Embodiment
Painting process among the present invention sticks with glue agent with working fastening and is applied on the stationary member or working fastening is sticked with glue agent and be applied on the processed member.In this painting process,, but be preferably on the gluing surface of stationary member that carries out fixed one side or processed member the operation of an amount of coating binder so long as known painting process then can use any means all without limits.The glue spread of tackiness agent is preferably 0.00000001～0.1mg/mm 2, 0.000001～0.001mg/mm more preferably 2The method that is coated with in right amount for example, uses the method for coating machine easy and accurate so long as known method just is not particularly limited, and is preferred aspect productivity.
Lift-launch operation among the present invention is to be coated with working fastening and to stick with glue on the stationary member of agent or the working fastening on the processed member sticks with glue operation in the agent behind the painting process processed member or stationary member being carried.In this lift-launch operation, so long as known method just is not particularly limited, for example, the operation of loading devices is easy and accurate automatically to use industrial robot etc., improve aspect the productivity preferred.
In method of temporarily fixing of the present invention, by stationary member, working fastening are sticked with glue be controlled at more than any in agent, the processed member more than 0 ℃ and 150 ℃ with the enforcement of getting off, can control the flowability that working fastening sticks with glue agent.When stationary member, working fastening stick with glue agent, processed member is more than 0 ℃ the time, mobile excellent, when it is below 150 ℃ the time, interim solidify stick with glue agent can be because of the thermofixation polymerization, the dimensional precision excellence.From the viewpoint consideration of mobile and dimensional precision, be preferably more than 10 ℃ and below 100 ℃, more preferably more than 20 ℃ and below 80 ℃.And then, more preferably more than 20 ℃ and below 60 ℃.
Pressurization operation of the present invention, preferred side from stationary member and processed member or the both sides operation of exerting pressure is more preferably so that the operation that the uniform mode in the interval of stationary member and processed member is exerted pressure from a side or both sides.In this pressurization operation, so long as known method just is not particularly limited, for example, the method for preferably using vacuum press or press to pressurize.
What is called among the present invention evenly is meant that the maximum at the interval of stationary member and processed member deducts in the scope of difference below 40 μ m at minimum place.If in this scope, obtain good dimensional precision when then processing processed member.Consider that from the viewpoint of dimensional precision the maximum at the interval of preferred stationary member and processed member deducts in the scope of difference below 20 μ m at minimum place, more preferably in the scope below 10 μ m, in the further preferred scope below 5 μ m.
In addition, in the pressurization operation of the present invention, preferably a side or the both sides from stationary member and processed member apply 1g/cm 2More than and 1000kg/cm 2Following pressure is implemented.As long as the interval of stationary member and processed member is even, even it is also no problem then stationary member and processed component partial to be exerted pressure, but from the viewpoint consideration at the interval of stationary member and processed member, preferably integral body is exerted pressure.Applied pressure is 1g/cm 2Under the above situation, can make the interval of stationary member and processed member even, when it is 1000kg/cm 2When following, stationary member or processed member can not sustain damage.Consider from the homogeneity at the interval of stationary member and processed member and the viewpoint of damage, be preferably 3g/cm 2More than and 800kg/cm 2Below, 5g/cm more preferably 2More than and 500kg/cm 2Below, 10g/cm more preferably 2More than and 300kg/cm 2Below.
In addition, in the present invention, need stick with glue in agent irradiation visible light or the ultraviolet ray any to working fastening and improve the irradiation process that working fastening sticks with glue the adhesive power of agent.As the lamp that in irradiation process or irradiation process more described later, uses, just be not particularly limited ultraviolet black lamp that preferably can illumination wavelength 365nm, metal halide lamp, high pressure mercury vapour lamp, LED lamp etc. so long as improve the lamp that working fastening sticks with glue the adhesive power of agent.Ultraviolet wavelength be preferably 10～430nm, more preferably 200～420nm, most preferably be 330～405nm.
In irradiation process of the present invention, visible light or ultraviolet irradiation amount are preferably 1mJ/cm at wavelength 365nm place 2～4000mJ/cm 2Scope.As long as in this scope, in that being added, processed member just can obtain good dimensional precision man-hour.Consider from the viewpoint of dimensional precision, preferably at 10mJ/cm 2～3000mJ/cm 2Scope, more preferably at 100mJ/cm 2～2000mJ/cm 2Scope, further preferably at 300mJ/cm 2～1000mJ/cm 2Scope.
Among the present invention, preferably in the pressurization operation, implement the irradiation process certain hour at least simultaneously.By in the pressurization operation, implementing the irradiation process certain hour at least simultaneously, can make the interval of stationary member and processed member even, obtaining significant effect aspect the dimensional precision that adds man-hour of processed member.For example be meant in this so-called processing implement cutting, grind cut, polishing, perforate etc. make processed member become required shape.At this so-called certain hour, just be not particularly limited as long as comprise the time that is cured.Set out aspect even at the interval that can make stationary member and processed member, preferably after implementing the pressurization operation in advance, implement pressurization operation and irradiation process simultaneously.
In the present invention, the material of processed member and stationary member is not particularly limited, but is preferably by can transmitting UV or the member that constitutes of the material of visible light.As this class material, can enumerate quartzy member, glass component, plastic member etc.
As (A) multifunctional (methyl) acrylate that uses in the present invention, can use oligomer/polymer end or side chain more than 2 by multifunctional (methyl) origoester acrylate/polymkeric substance after (methyl) acrylization or have the monomer of (methyl) acryl more than 2.
As multifunctional (methyl) origoester acrylate/polymkeric substance, can enumerate: 1, the end capped urethane of 2-polyhutadiene (methyl) acrylate (for example, " TE-2000 " that Japan Cao Da company makes, " TEA-1000 "), above-mentioned hydride (for example, " TEAI-1000 " that Japan Cao Da company makes), 1, the end capped urethane of 4-polyhutadiene (methyl) acrylate (for example, " BAC-45 " that Osaka organic chemistry company makes), polyisoprene end capped (methyl) acrylate, polyester urethane (methyl) acrylate (for example, " UV-2000B " that Japan Synesis Company makes, " UV-3000B ", " UV-7000B ", " KHP-11 " that industrial makes on the root, " KHP-17 "), polyethers urethane (methyl) acrylate (for example, " UV-3700B " of Japanese Synesis Company manufacturing, " UV-6100B "), two A type epoxies (methyl) acrylate etc.Wherein, aspect effective, preferred polyester class urethane (methyl) acrylate and/or polyethers urethane (methyl) acrylate, more preferably polyester urethane (methyl) acrylate.
The weight-average molecular weight of multifunctional (methyl) origoester acrylate/polymkeric substance is preferably 10000～60000, more preferably 13000～40000.Weight-average molecular weight is used GPC system (SC-8010 that eastern Cao company makes) etc., makes typical curve with commercially available polystyrene standard and obtains.
As two senses (methyl) acrylate monomer, can enumerate: 1,3-butyleneglycol two (methyl) acrylate, 1,4-butyleneglycol two (methyl) acrylate, 1,6-hexylene glycol two (methyl) acrylate, 1,9-nonanediol two (methyl) acrylate, neopentyl glycol two (methyl) acrylate, two (methyl) vinylformic acid dicyclo pentyl ester, 2-ethyl-2-butyl-propylene glycol (methyl) acrylate, neopentyl glycol modification TriMethylolPropane(TMP) two (methyl) acrylate, stearic acid modified pentaerythritol diacrylate, polypropylene glycol two (methyl) acrylate, 2, two (4-(methyl) the acryloxy diethoxy phenyl) propane of 2-, 2, two (4-(methyl) the acryloxy propoxy-phenyl) propane of 2-, 2, two (4-(methyl) the acryloxy tetraethoxy phenyl) propane of 2-, 2-(1,2-encircles six carboxyl imides) ethyl propylene acid esters, hexanediyl ester etc.Wherein, preferred 1 aspect effective, 6-hexylene glycol two (methyl) acrylate and/or two (methyl) vinylformic acid dicyclo pentyl ester, more preferably two (methyl) vinylformic acid dicyclo pentyl ester.
As trifunctional (methyl) acrylate monomer, can enumerate: trimethylolpropane tris (methyl) acrylate, three [(methyl) acryloxy ethyl] isocyanuric acid ester etc.
As (methyl) acrylate monomer more than four senses, can enumerate: dihydroxy methylpropane four (methyl) acrylate, tetramethylolmethane four (methyl) acrylate, tetramethylolmethane oxyethyl group four (methyl) acrylate, Dipentaerythritol five (methyl) acrylate, Dipentaerythritol six (methyl) acrylate etc.
(A) multifunctional (methyl) acrylate, more preferably hydrophobic multifunctional (methyl) acrylate.Be meant in this so-called hydrophobicity and be difficult to be dissolved in the character of water or be difficult to and water blended character.As hydrophobic multifunctional (methyl) acrylate, for example can enumerate: 1,3-butyleneglycol two (methyl) acrylate, 1,4-butyleneglycol two (methyl) acrylate, 1,6-hexylene glycol two (methyl) acrylate, 1,9-nonanediol two (methyl) acrylate, neopentyl glycol two (methyl) acrylate, two (methyl) vinylformic acid dicyclo pentyl ester, 2-ethyl-2-butyl-propylene glycol (methyl) acrylate, neopentyl glycol modification TriMethylolPropane(TMP) two (methyl) acrylate, stearic acid modified pentaerythritol diacrylate, polypropylene glycol two (methyl) acrylate, 2, two (4-(methyl) the acryloxy diethoxy phenyl) propane of 2-, 2, two (4-(methyl) the acryloxy propoxy-phenyl) propane of 2-, 2, two (4-(methyl) the acryloxy tetraethoxy phenyl) propane of 2-, 2-(1,2-encircles six carboxyl imides) ethyl propylene acid esters, hexanediyl ester etc.As hydrophobic trifunctional (methyl) acrylate monomer, can enumerate: trimethylolpropane tris (methyl) acrylate, three [(methyl) acryloxy ethyl] isocyanuric acid ester etc.As (methyl) acrylate monomer more than hydrophobic four senses, can enumerate: dihydroxy methylpropane four (methyl) acrylate, tetramethylolmethane four (methyl) acrylate, tetramethylolmethane oxyethyl group four (methyl) acrylate, Dipentaerythritol five (methyl) acrylate, Dipentaerythritol six (methyl) acrylate etc.Under water miscible situation, may occurrence positions depart from owing to the cured article swelling of resin combination when machining, add the dimensional precision variation in man-hour, therefore not preferred.Even be wetting ability, if the cured article of its composition can be owing to water swelling or be partly dissolved greatly, then also can use.
In multifunctional (methyl) acrylate, aspect effective, preferably contain multifunctional (methyl) origoester acrylate/polymkeric substance and/or two senses (methyl) acrylate monomer, more preferably also with multifunctional (methyl) origoester acrylate/polymkeric substance and two senses (methyl) acrylate monomer.
And it is proportional with containing under the situation of multifunctional (methyl) origoester acrylate/polymkeric substance and two senses (methyl) acrylate monomer, in total 100 mass parts of multifunctional (methyl) origoester acrylate/polymkeric substance and two senses (methyl) acrylate monomer, by quality ratio, preferably multifunctional (methyl) origoester acrylate/polymkeric substance: two senses (methyl) acrylate monomer=30～95: 5～70, more preferably 40～90: 60～10, most preferably be 60～80: 40～20.
(A) consumption of multifunctional (methyl) acrylate in (A) and (B) total amount 100 mass parts, is preferably 1～90 mass parts, 30～85 mass parts more preferably.If be more than 1 mass parts, peel off the character (being designated hereinafter simply as " separability ") of this cured article in the time of then can fully promoting cured article with composition to impregnated in the warm water from adherend, guarantee that the cured article of composition is peeled off with membranaceous.In addition, if be below 90 mass parts, the possibility that does not then also exist initial tackiness to descend.
As (B) simple function (methyl) acrylate, can use simple function (methyl) acrylate monomer.As simple function (methyl) acrylate monomer, can enumerate: (methyl) methyl acrylate, (methyl) ethyl propenoate, (methyl) propyl acrylate, (methyl) butyl acrylate, (methyl) 2-EHA, (methyl) Isooctyl acrylate monomer, (methyl) isodecyl acrylate, (methyl) lauryl acrylate, (methyl) vinylformic acid stearyl, (methyl) phenyl acrylate, (methyl) cyclohexyl acrylate, (methyl) vinylformic acid dicyclo pentyl ester, (methyl) vinylformic acid dicyclopentenyloxyethyl methacrylate, (methyl) vinylformic acid two cyclopentenes oxygen base ethyl esters, (methyl) isobornyl acrylate, methoxylation ring triolefin in the last of the ten Heavenly stems (methyl) acrylate, (methyl) vinylformic acid 2-hydroxy methacrylate, (methyl) vinylformic acid 2-hydroxy propyl ester, (methyl) vinylformic acid 3-hydroxy propyl ester, (methyl) vinylformic acid 4-hydroxyl butyl ester, (methyl) vinylformic acid tetrahydro furfuryl ester, (methyl) vinylformic acid 2-hydroxyl-3-phenoxy group propyl ester, (methyl) glycidyl acrylate, caprolactone modification tetrahydrofurfuryl (methyl) acrylate, (methyl) vinylformic acid 3-chloro-2-hydroxy propyl ester, (methyl) vinylformic acid N, the N-dimethylaminoethyl, (methyl) vinylformic acid N, the N-lignocaine ethyl ester, (methyl) vinylformic acid uncle fourth amino ethyl ester, ethoxycarbonylmethyl group (methyl) acrylate, phenol ring oxidative ethane modification acrylate, phenol (2 moles of modifications of oxyethane) acrylate, phenol (4 moles of modifications of oxyethane) acrylate, to cumyl phenol oxyethane modification acrylate, the nonyl phenol EO modification acrylate, nonyl phenol (4 moles of modifications of oxyethane) acrylate, nonyl phenol (8 moles of modifications of oxyethane) acrylate, nonyl phenol (2.5 moles of modifications of propylene oxide) acrylate, 2-ethylhexyl Trivalin SF acrylate, oxyethane modification phthalic acid (methyl) acrylate, oxyethane modification succsinic acid (methyl) acrylate, (methyl) vinylformic acid trifluoro ethyl ester, vinylformic acid, methacrylic acid, toxilic acid, fumaric acid, ω-carboxyl-polycaprolactone list (methyl) acrylate, phthalic acid list hydroxyethyl (methyl) acrylate, (methyl) acrylic acid dimer, mono succinate β-(methyl) acryloxy ethyl ester, N-(methyl) acryloxyalkyl hexahydrophthalic phthalimide, 2-(1,2-encircles six carboxyl imides) ethyl propylene acid esters etc.
(B) simple function (methyl) acrylate more preferably is similarly hydrophobic simple function (methyl) acrylate with (A).Be meant in this so-called hydrophobicity and be difficult to be dissolved in the character of water or be difficult to and water blended character.So-called hydrophobic simple function (methyl) acrylate, can enumerate: (methyl) methyl acrylate, (methyl) ethyl propenoate, (methyl) propyl acrylate, (methyl) butyl acrylate, (methyl) 2-EHA, (methyl) Isooctyl acrylate monomer, (methyl) isodecyl acrylate, (methyl) lauryl acrylate, (methyl) vinylformic acid stearyl, (methyl) phenyl acrylate, (methyl) cyclohexyl acrylate, (methyl) vinylformic acid dicyclo pentyl ester, (methyl) vinylformic acid dicyclopentenyloxyethyl methacrylate, (methyl) vinylformic acid dicyclo amylene oxygen base ethyl ester, (methyl) isobornyl acrylate, methoxylation ring triolefin in the last of the ten Heavenly stems (methyl) acrylate, (methyl) vinylformic acid tetrahydro furfuryl ester, (methyl) vinylformic acid 2-hydroxyl-3-phenoxy group propyl ester, (methyl) glycidyl acrylate, caprolactone modification tetrahydrofurfuryl (methyl) acrylate, (methyl) vinylformic acid 3-chloro-2-hydroxy propyl ester, (methyl) vinylformic acid N, the N-dimethylaminoethyl, (methyl) vinylformic acid N, the N-lignocaine ethyl ester, (methyl) vinylformic acid uncle fourth amino ethyl ester, ethoxycarbonylmethyl group (methyl) acrylate, phenol ring oxidative ethane modification acrylate, phenol (2 moles of modifications of oxyethane) acrylate, phenol (4 moles of modifications of oxyethane) acrylate, to cumyl phenol oxyethane modification acrylate, the nonyl phenol EO modification acrylate, nonyl phenol (4 moles of modifications of oxyethane) acrylate, nonyl phenol (8 moles of modifications of oxyethane) acrylate, nonyl phenol (2.5 moles of modifications of propylene oxide) acrylate, 2-ethylhexyl Trivalin SF acrylate, oxyethane modification phthalic acid (methyl) acrylate, oxyethane modification succsinic acid (methyl) acrylate, (methyl) vinylformic acid trifluoro ethyl ester, ω-carboxyl-polycaprolactone list (methyl) acrylate, phthalic acid list hydroxyethyl (methyl) acrylate, (methyl) acrylic acid dimer, mono succinate β-(methyl) acryloxy ethyl ester, N-(methyl) acryloxyalkyl hexahydrophthalic phthalimide, 2-(1,2-encircles six carboxyl imides) ethyl propylene acid esters etc.Under water miscible situation, may occurrence positions depart from owing to the cured article swelling of resin combination when machining, the working accuracy variation, therefore not preferred.In addition, even be wetting ability,, then also can use as long as the cured article of its resin combination can or not be partly dissolved because of the water swelling.
In simple function (methyl) acrylate, aspect effective, preferably contain 2 moles of modification (methyl) acrylate of phenol ring oxidative ethane and/or 2-(1,2-encircles six carboxyl imides) ethyl (methyl) acrylate, more preferably also with 2 moles of modification (methyl) acrylate of phenol ring oxidative ethane and 2-(1,2-encircles six carboxyl imides) ethyl (methyl) acrylate.And with 2 moles of modification (methyl) acrylate of phenol ring oxidative ethane and 2-(1,2-encircles six carboxyl imides) under the situation of ethyl (methyl) acrylate contain proportional, at 2 moles of modification (methyl) acrylate of phenol ring oxidative ethane and 2-(1,2-encircles six carboxyl imides) in total 100 mass parts of ethyl (methyl) acrylate, by quality ratio, preferred 2 moles of modifications of phenol ring oxidative ethane (methyl) acrylate: 2-(1,2-encircles six carboxyl imides) ethyl (methyl) acrylate=30～90: 10～70, more preferably 40～80: 20～60, most preferably be 50～70: 30～50.
(B) consumption of simple function (methyl) acrylate in (A) and (B) total amount 100 mass parts, is preferably 10～99 mass parts, 15～70 mass parts more preferably.So long as more than 10 mass parts, initial tackiness is descended, so long as below 99 mass parts, just can guarantee separability, the cured article of composition is peeled off with membranaceous.
In addition; by in aforementioned (A) and blend compositions (B) and with (methyl) acryloxy ethyl phosphate ester acid, dibutyl 2-(methyl) acryloxy ethyl phosphate ester acid, dioctyl 2-(methyl) acryloxy ethyl phosphonic acid ester, phenylbenzene 2-(methyl) acryloxy ethyl phosphonic acid ester, (methyl) acryloxy ethyl polyoxyethylene glycol phosphate ester acid etc., having the phosphoric acid ester of vinyl or (methyl) acryl, can further improve adaptation to metal covering.
(C) Photoepolymerizationinitiater initiater is the material that cooperates in order to utilize visible light or ultraviolet active ray to make its sensitization promote the photocuring of resin combination, can use known various Photoepolymerizationinitiater initiater.As Photoepolymerizationinitiater initiater, can enumerate: benzophenone and derivative thereof; Benzil and derivative thereof; Benzoin derivatives such as anthraquinone and derivative thereof, bitter almond oil camphor, benzoin methylether, ethoxybenzoin, bitter almond oil camphor propyl ether, bitter almond oil camphor ethyl isobutyl ether, benzyl dimethyl ketal; Acetophenone derivs such as diethoxy acetophenone, 4-tertiary butyl Trichloroacetophenon; 2-dimethyl aminoethyl benzoic ether, to dimethyl aminoethyl benzoic ether, phenylbenzene disulfide, thioxanthone and derivative thereof; Camphorquinone, 7,7-dimethyl-2,3-dioxo-bicyclo [2.2.1] heptane-1-carboxylic acid, 7,7-dimethyl-2,3-dioxo-bicyclo [2.2.1] heptane-1-carboxyl-2-bromine ethyl ester, 7,7-dimethyl-2,3-dioxo-bicyclo [2.2.1] heptane-1-carboxyl-2-methyl ester, 7,7-dimethyl-2,3-dioxo-bicyclo [2.2.1] heptane-1-carboxylic acid chloride waits the camphorquinone derivative; 2-methyl isophthalic acid-[4-(methylthio group) phenyl]-2-morpholinyl-1-acetone, 2-benzyl-2-dimethylamino-1-(4-morpholinyl phenyl)-alpha-aminoalkyl benzophenone derivatives such as 1-butanone; Benzoyl diphenyl phosphine oxide, 2,4,6-trimethylbenzoyl diphenyl phosphine oxide, benzoyl diethoxy phosphine oxide, 2,4,6-trimethylbenzoyl Dimethoxyphenyl phosphine oxide, 2,4, acylphosphine oxide derivatives such as 6-trimethylbenzoyl diethoxy phenyl phosphine oxide; Oxygen base-phenyl-acetic acid 2-[2-oxo-2-phenyl-acetic acid base-oxyethyl group]-ethyl ester and/or oxygen base-phenyl-acetic acid 2-[2-hydroxyl-oxyethyl group]-ethyl ester etc.Photoepolymerizationinitiater initiater can use a kind or be used in combination more than 2 kinds.In these Photoepolymerizationinitiater initiaters, aspect effective, be preferably selected from 1-benzyl dimethyl ketal, oxygen base-phenyl-acetic acid 2-[2-oxo-2-phenyl-acetic acid base-oxyethyl group]-ethyl ester and oxygen base-phenyl-acetic acid 2-[2-hydroxyl-oxyethyl group]-in the ethyl ester more than a kind or 2 kinds.
(C) consumption of Photoepolymerizationinitiater initiater is preferably 0.1～30 mass parts with respect to (A) and total 100 mass parts (B).0.5～25 mass parts more preferably.As long as be more than 0.1 mass parts, just guarantee to obtain to solidify promoted effect, below 25 mass parts, can obtain sufficient curing speed.As preferred mode, by using more than (C) composition 1 mass parts, can under the situation that does not rely on the rayed amount, solidify, and then the cross-linking density of the cured article of composition increases, just can not depart from etc. by occurrence positions during machining, improving aspect the separability more preferably.
In the present invention, preferably stick with glue the second-order transition temperature of the cured article that agent obtains in-50 ℃～50 ℃ scope by working fastening.Stick with glue the second-order transition temperature of the cured article that agent obtains in this scope by making by above-mentioned working fastening, after member being carried out gluing working fastening and the member of this working fastening is processed, when being immersed in this member that processes in the warm water below 100 ℃, working fastening sticks with glue the cured article thermal expansion greatly of agent itself.Its result, because gluing area is realized minimizing, thereby adhesive strength descends, and therefore, can easily only reclaim member.When the second-order transition temperature that sticks with glue the cured article that agent obtains by working fastening for more than-50 ℃ the time, be not easy to depart from excellence aspect dimensional precision during the member of processing working fastening.When below 50 ℃, warm water separability excellence.Consider from the aspect of separability and dimensional precision, the second-order transition temperature that sticks with glue the cured article that agent obtains by above-mentioned working fastening more preferably-25 ℃～45 ℃, more preferably-20 ℃～42 ℃, further be preferably 0 ℃～40 ℃.
Need to prove that the measuring method that is sticked with glue the second-order transition temperature of the cured article that agent obtains by the working fastening of using among the present invention is not particularly limited, known method such as available DSC or dynamic viscoelastic spectrum are measured.Preferable methods is to utilize the method for dynamic viscoelastic spectrum.
In the present invention, preferably (D) is insoluble to the particulate matter of (A)～(C) with (A), (B) use simultaneously.Thus, make cured composition keep certain thickness easily, can improve the dimensional precision that adds man-hour more simply.And then, because it is different with the coefficient of linear expansion of the particulate matter that is insoluble to (A)～(C) that working fastening sticks with glue the cured article of agent, therefore, after stating in the use that adhesive compound carries out gluing working fastening to member and the member of this working fastening being processed, when being immersed in the member after this processing in the warm water below 100 ℃, wriggle fluctuating shape or 3 D deformation take place in the interface that sticks with glue the cured article of agent in member and working fastening, its result, gluing area reduces, and separability further improves.
Be insoluble to the material of the particulate matter of (A)～(C) as (D), normally used organic and inorganic particle is all passable.As organic filler, can enumerate: polyethylene particles, polypropylene particles, crosslinked polymethylmethacrylaparticles particle, crosslinked polystyrene particle etc., as inorganic particulate, can enumerate the ceramic particle of glass, silicon-dioxide, aluminum oxide, titanium etc.
(D) be insoluble to the particulate matter of (A)～(C), from improvement add the dimensional precision in man-hour, the aspect of promptly controlling the thickness of tackiness agent considers, is preferably spherical.As organic filler, preferred: crosslinked polymethylmethacrylaparticles particle, crosslinked polystyrene particle or crosslinked polymethylmethacrylaparticles polystyrene copolymer particle that the known emulsion polymerization method that utilizes methyl methacrylate monomer, styrene monomer and cross-linkable monomer obtains with the form of monodisperse particle.As inorganic particulate, because the spherical silicon dioxide particles Deformation is little, the deviation of the thickness of the cured composition that is caused by the particle diameter deviation reduces, and is therefore preferred.Wherein, consider from the package stability that causes by the precipitation of particle etc. and the reactive aspect of composition, more preferably any of crosslinked polymethylmethacrylaparticles particle, crosslinked polystyrene particle or crosslinked polymethylmethacrylaparticles polystyrene copolymer particle, crosslinked polymethylmethacrylaparticles particle, crosslinked polystyrene particle, crosslinked polymethylmethacrylaparticles polystyrene copolymer particle or their mixture.Any of further preferred crosslinked polymethylmethacrylaparticles particle, crosslinked polystyrene particle and crosslinked polymethylmethacrylaparticles polystyrene copolymer particle or their mixture.
(D) particulate matter that is insoluble to (A)～(C) utilizes median size that laser method measures preferably in the scope of 5 μ m～200 μ m.When the median size of above-mentioned particulate matter is 5 μ m when above, the separability excellence when it is 200 μ m when following, is not easy to depart from excellence aspect dimensional precision during the member of processing working fastening.Consider that from the viewpoint of separability and dimensional precision preferred median size is 8 μ m～150 μ m, 9 μ m～120 μ m more preferably.Need to prove, the particle diameter among the present invention and the standard deviation of size distribution, " the laser diffraction formula particle size distribution device SALD-2200 " that utilize Shimadzu Seisakusho Ltd. to make measures.Particle diameter is a volume reference.
In addition, (D) is insoluble to (A)～(C) particulate matter utilize particle diameter (μ m) that laser method measures when representing with logarithm, particle volume distributes with respect to the standard deviation of particle diameter preferably in 0.0001～0.25 scope.When the standard deviation of the particle diameter of particulate matter during in this scope, the deviation of the thickness of the cured composition that causes because of the deviation of particle diameter diminishes, be not easy to depart from during the member of processing working fastening, excellence aspect dimensional precision not only, separability is significantly improvement also.Consider that from the viewpoint of dimensional precision and separability the standard deviation of the particle diameter of particulate matter more preferably 0.0001～0.15, more preferably 0.0001～0.1, further is preferably 0.0001～0.08, is preferably 0.0001～0.072 especially.
(D) be insoluble to the consumption of the particulate matter of (A)～(C), consider from adhesive strength, working accuracy, separability aspect, with respect to (A) and (B) total amount 100 mass parts, be preferably 0.1～20 mass parts, more preferably 0.2～10 mass parts, 0.2～6 mass parts more preferably.
Stick with glue agent for working fastening of the present invention,, can use a spot of stopper in order to improve its package stability.As stopper, can enumerate: methyl hydroquinone, Resorcinol, 2,2-methylene radical-two (4-methyl-6-tert butyl phenol), pyrocatechol, hydroquinone monomethyl ether, single Tert. Butyl Hydroquinone, 2,5-di-tert-butyl hydroquinone, para benzoquinone, 2,5-phenylbenzene-para benzoquinone, 2,5-di-t-butyl-para benzoquinone, picric acid, citric acid, thiodiphenylamine, tert-butyl catechol, 2-butyl-4-BHA and 2,6-di-t-butyl-p-cresol etc.
For the consumption of these stoppers,, be preferably 0.001～3 mass parts, 0.01～2 mass parts more preferably with respect to (A) and (B) total amount 100 mass parts.When 0.001 mass parts is above, can guarantee package stability, when 3 mass parts are following, obtain good tackiness, also can not cause uncured.
Stick with glue in the agent in working fastening of the present invention, also can use polar organic solvent simultaneously.
Stick with glue agent for working fastening of the present invention, in the scope that does not influence purpose of the present invention, can also use additives such as various elastomericss such as common employed acrylic rubber, urethanes, acrylonitrile-butadiene-styrene (ABS) rubber, inorganic filler, solvent, increase-volume material, reinforcement material, softening agent, thickening material, dyestuff, pigment, fire retardant, silane coupling agent and tensio-active agent.
Working fastening/the stripping means of member of the present invention is as follows: stick with glue after agent processes by the member of aforesaid method working fastening using working fastening, this member that processes be impregnated in the warm water below 100 ℃, remove the working fastening of having solidified and stick with glue agent.Utilize the present invention, not with an organic solvent, can improve the working accuracy of optics with various members such as members.
According to preferred implementation of the present invention, when the cured article that sticks with glue agent from working fastening is removed processed member, working fastening is sticked with glue agent irradiation visible light or ultraviolet ray, can shorten the cured article that working fastening is sticked with glue agent thus and be immersed in the warm water below 100 ℃ and remove the time that working fastening after the curing sticks with glue agent.
In the present invention, when the cured article that sticks with glue agent from working fastening is removed processed member, working fastening is sticked with glue agent irradiation visible light or ultraviolet visible light or ultraviolet irradiation amount be 1000mJ/cm at wavelength 365nm place 2More than and 40000mJ/cm 2Under the following situation, can shorten the cured article that working fastening is sticked with glue agent and be immersed in the warm water below 100 ℃ and remove time effective that working fastening after the curing sticks with glue agent, therefore preferred (irradiation process again).Irradiation dose is 2000mJ/cm more preferably 2More than and 38000mJ/cm 2Below, 4000mJ/cm more preferably 2More than and 36000mJ/cm 2Below.
In the present invention, use warm water after the suitably heating, for example during the warm water below 100 ℃, can be implemented in the separability in the water at short notice, productivity improves, and is therefore preferred.Use preferred 30 ℃～100 ℃, more preferably under 40～99 ℃ the situation of warm water, the thermal expansion at short notice of the cured article of tackiness agent, but the residual set stress that produces when release composition is solidified simultaneously.And then, because it is different with the coefficient of linear expansion of particulate matter that working fastening sticks with glue the cured article of agent, therefore, after using above-mentioned adhesive compound that member is carried out gluing working fastening and the member of this working fastening being processed, when being immersed in this member that processes in the warm water below 100 ℃, wriggle fluctuating shape or 3 D deformation take place in the interface that sticks with glue the cured article of agent in member and working fastening.Its result, gluing area reduces, and adhesive strength descends, and can remove with the membranaceous cured article that working fastening is sticked with glue agent.Need to prove, stick with glue the method that the cured article of agent contacts with water for working fastening,, therefore recommend because the method that is immersed in the water together with conjugant is easy.
Below, enumerate embodiment and comparative example illustrates in greater detail the present invention.The present invention is not limited to these embodiment.
Embodiment
(embodiment 1)
(working fastening sticks with glue the making of agent)
Sequentially built working fastening according to the following stated sticks with glue agent.As (A) multifunctional (methyl) acrylate, " UV-3000B " (the polyester urethane acrylate that uses Japanese Synesis Company to make, be designated hereinafter simply as " UV-3000B ", be hydrophobic (methyl) acrylate, weight-average molecular weight 15000) 30 mass parts, diacrylate dicyclo pentyl ester (" the KAYARAD R-684 " that Japanese chemical drug corporate system is made, be designated hereinafter simply as " R-684 ", be hydrophobic (methyl) acrylate) 15 mass parts; As (B) simple function (methyl) acrylate, use 2-(1,2-encircles six carboxyl imides) ethyl propylene acid esters (" the ARONIX M-140 " that East Asia Synesis Company makes, be designated hereinafter simply as " M-140 ", be hydrophobic (methyl) acrylate) 20 mass parts, 2 moles of modification acrylates of phenol ring oxidative ethane (" the ARONIX M-101A " that East Asia Synesis Company makes is hydrophobic (methyl) acrylate) 35 mass parts; As (C) Photoepolymerizationinitiater initiater, use benzyl dimethyl ketal (" IRGACURE651 " that Ciba company makes is designated hereinafter simply as " BDK ") 10 mass parts; Be insoluble to the particulate matter of (A)～(C) as (D), use median size 100 μ m, be 0.063 spherical crosslinked polystyrene particle (GANZ changes into " GS-100S " that company makes) 1 mass parts distribute standard deviation with respect to particle diameter of the particle volume of particle diameter (μ m) when representing with logarithm; As stopper, use 2,2-methylene radical-two (4-methyl-6-tert butyl phenol) (" ス ミ ラ イ ザ one MDP-S " that Sumitomo Chemical Co. Ltd. makes is designated hereinafter simply as " MDP ") 0.1 mass parts is made resin combination.
Use resulting resin combination, carry out second-order transition temperature, tensile shear adhesive strength, stripping test with the evaluation method shown in following.These be the results are shown in table 1.In addition, the median size and the particle volume of particle diameter (μ m) when representing with logarithm distributed that (D) is insoluble to the particulate matter of (A)～(C) is also measured with respect to the standard deviation of particle diameter.
(evaluation method)
Second-order transition temperature: with the thick silicon chip of 1mm is mould plate, and resin combination is inserted the PET film.The solidification equipment that has the Off ユ one ジ ヨ Application company of electrodeless discharge lamp to make by use is 2000mJ/cm in the accumulation light quantity of 365nm wavelength 2Condition under, make resin combination after top curing, the accumulation light quantity at the 365nm wavelength is 2000mJ/cm again 2Condition under make it from following curing, make the cured article of the resin combination of thickness 1mm.Is the wide 5mm of long 50mm with the cured article made from the cutting unit severing, measures as second-order transition temperature and uses cured article.Resulting cured article is utilized the Measurement of Dynamic Viscoelasticity device " DMS210 " of Seiko electronic industry company manufacturing, in nitrogen atmosphere, described cured article is applied the stress and the distortion of the draw direction of 1Hz, measure tan δ with the ratio arm intensification limit of 2 ℃ of heat-up rate per minutes, with the temperature of the summit of this tan δ as second-order transition temperature.
Tensile shear adhesive strength (" adhesive strength " in the table): measure according to JIS K 6850.Particularly, use as the thermal glass (25mm * 25mm * thickness 2.0mm) that is glued material, gluing position is set at diameter 8mm, with the resin combination of making 2 thermal glasses are pasted, the solidification equipment that has the Off ユ one ジ ヨ Application company of electrodeless discharge lamp to make by use is 2000mJ/cm in the accumulation light quantity of 365nm wavelength 2Condition under make its curing, make tensile shear adhesive strength test film.To the test film of making, use universal testing machine, under the environment of 23 ℃ of temperature, humidity 50%, be that 10mm/min measures the tensile shear adhesive strength with the draw speed.
Stripping test (" 80 ℃ of warm water splitting times " " peeling off state " in the table): coating composition on above-mentioned thermal glass, it is sticked on the soda-lime glass (150mm * 150mm * thickness 1.7mm) as upholder, in addition, with above-mentioned same condition under the resin combination of making is solidified, make the stripping test thing.Resulting trier is immersed in the warm water (80 ℃), measures the time that thermal glass is peeled off, also observe peeling off state.
The median size of particulate matter and the particle volume of particle diameter (μ m) when representing with logarithm distributed with respect to the standard deviation of particle diameter (" being insoluble to the standard deviation of particle diameter of the particulate matter of (A), (B), (C) " in the table): utilize laser diffraction formula particle size distribution device (" SALD-2200 " that Shimadzu Seisakusho Ltd. makes) to measure.
(working fastening/stripping means)
To be heated to 80 ℃ on hot-plate as the soda-lime glass (150mm * 150mm * thickness 1.7mm) of stationary member, the working fastening that coating 1g makes sticks with glue agent (painting process).Thereafter, from the soda-lime glass (80mm * 80mm * thickness 1.1mm) (lift-launch operation) of top lift-launch as processed member.Then, the silica glass (80mm * 80mm * thickness 5mm) of thickness 50mm is carried from the top on the soda-lime glass as processed member, applying load from the above-mentioned silica glass, the wt part that applies with silica glass adds up to 12.5g/cm 2Pressure, place 5 minutes (pressurization operation).The interval of stationary member and processed member, the difference that is deducted minimum place by maximum is below the 5 μ m.
Then, the limit applies 12.5g/cm 2The pressure limit from using black lamp as soda-lime glass one side of stationary member, the UV light 300mJ/cm of irradiation 365nm wavelength 2(implementing irradiation process (30 seconds) simultaneously) with the pressurization operation.Use cutting unit, only the soda-lime glass severing as processed member with resulting adhesive test thing is the square of length of side 10mm.Soda-lime glass as processed member in the severing process does not come off, and demonstrates good processibility.To only using the UV light 16000mJ/cm of metal halide light irradiation 365nm wavelength as the adhesive test thing after the soda-lime glass severing of processed member 2Back (irradiation process (40 seconds) again) is immersed in 80 ℃ the warm water, and the result peeled off (warm water splitting time) fully in 1 minute.In addition, take out arbitrarily 10 these severing test films after peeling off, with opticmicroscope each limit at the back side (sticking with glue the face of agent working fastening with working fastening) of its severing test film is observed, measured the maximum width that indentation, there appears in glass, obtain its mean value and standard deviation.And then, the severing test film that sticks with glue agent for the working fastening after peel off obtains the cured article film that working fastening sticks with glue agent, severing test film after 10 of taking-ups are peeled off arbitrarily, utilize thickness gauge (MICRO GAUGE) to measure the thickness of the film of described cured article, obtain its mean value and standard deviation.The glass on each limit is occurred the mean value of maximum width of indentation, there and standard deviation and working fastening stick with glue the mean value of thickness of film of cured article of agent and the measurement result of standard deviation is shown in table 1.
Table 1
Figure BPA00001306644100221
*) membranaceous: the adhesive compound after the curing is peeled off with membranaceous under the residual state of no adhesive paste from glass surface.
*) adhesive paste is residual: glass is peeled off, but the adhesive compound after solidifying remains in glass surface.
Table 2
Figure BPA00001306644100231
*) membranaceous: the adhesive compound after the curing is peeled off with membranaceous under the residual state of no adhesive paste from glass surface.
*) adhesive paste is residual: glass is peeled off, but the adhesive compound after solidifying remains in glass surface.
Table 3
Figure BPA00001306644100241
*) membranaceous: the adhesive compound after the curing is peeled off with membranaceous under the residual state of no adhesive paste from glass surface.
*) adhesive paste is residual: glass is peeled off, but the adhesive compound after solidifying remains in glass surface.
Table 4
Figure BPA00001306644100251
*) membranaceous: the adhesive compound after the curing is peeled off with membranaceous under the residual state of no adhesive paste from glass surface.
*) adhesive paste is residual: glass is peeled off, but the adhesive compound after solidifying remains in glass surface.
(embodiment 2～7, comparative example 1,2)
Under the condition shown in table 1～2,4, implement working fastening/stripping means, in addition, operation similarly to Example 1, the mean value and the standard deviation of thickness that the mean value of maximum width of indentation, there and standard deviation and working fastening stick with glue the cured article film of agent appears in the glass of measuring each limit, and its measurement result is shown in table 1～2,4.
(embodiment 8～11)
Press the raw material that the composition shown in the table 2,3 uses the kind shown in the table 2,3, in addition, operation similarly to Example 1, the mean value and the standard deviation of thickness that the mean value of maximum width of indentation, there and standard deviation and working fastening stick with glue the cured article film of agent appears in the glass of measuring each limit, and its measurement result is shown in table 2,3.
(embodiment 12)
Be insoluble to the particulate matter of (A)～(C) as (D), use median size be 140 μ m, with the particle volume of particle diameter (μ m) when representing with logarithm distribute standard deviation with respect to particle diameter be 0.086 spherical crosslinked polymethylmethacrylaparticles particle (" GM-5003 " that the GANZ company that changes into is made with size of mesh be the sieve of the sieve of 150 μ m and 125 μ m sieve make), press the raw material that the composition shown in the table 3 uses the kind shown in the table 3, in addition, operation is similarly to Example 1 made working fastening and is sticked with glue agent.Stick with glue agent for resulting working fastening, implement second-order transition temperature, tensile shear adhesive strength, stripping test similarly to Example 1.In addition, the median size and the particle volume of particle diameter (μ m) when representing with logarithm distributed that (D) is insoluble to the particulate matter of (A)～(C) is also measured with respect to the standard deviation of particle diameter.These be the results are shown in table 3.
Use this working fastening to stick with glue agent, implement working fastening/stripping means under the conditions shown in Table 3, in addition, the mean value and the standard deviation of thickness that the mean value of maximum width of indentation, there and standard deviation and working fastening stick with glue the cured article film of agent appears in operation similarly to Example 1, the glass of measuring each limit.Its measurement result is shown in table 3.
(embodiment 13)
Be insoluble to the particulate matter of (A)～(C) as (D), to use median size be 40 μ m, be 0.062 spherical crosslinked polystyrene particle (" GS-240 " that ponding chemical company makes) with the standard deviation of the particle volume distribution relative grain size of particle diameter (μ m) when representing with logarithm, press the raw material that the composition shown in the table 3 uses the kind shown in the table 3, in addition, operation is similarly to Example 1 made working fastening and is sticked with glue agent.Stick with glue agent for resulting working fastening, implement second-order transition temperature, tensile shear adhesive strength, stripping test similarly to Example 1.In addition, the median size and the particle volume of particle diameter (μ m) when representing with logarithm distributed that (D) is insoluble to the particulate matter of (A)～(C) is also measured with respect to the standard deviation of particle diameter.These be the results are shown in table 3.
Use this working fastening to stick with glue agent, implement working fastening/stripping means under the conditions shown in Table 3, in addition, the mean value and the standard deviation of thickness that the mean value of maximum width of indentation, there and standard deviation and working fastening stick with glue the cured article film of agent appears in operation similarly to Example 1, the glass of measuring each limit.Its measurement result is shown in table 3.
(embodiment 14)
Be insoluble to the particulate matter of (A)～(C) as (D), to use median size be 20 μ m, be 0.061 spherical crosslinked polystyrene particle (" GS-220 " that ponding chemical company makes) with the standard deviation of the particle volume distribution relative grain size of particle diameter (μ m) when representing with logarithm, press the raw material that the composition shown in the table 3 uses the kind shown in the table 3, in addition, operation is similarly to Example 1 made working fastening and is sticked with glue agent.Stick with glue agent for resulting working fastening, implement second-order transition temperature, tensile shear adhesive strength, stripping test similarly to Example 1.In addition, the median size and the particle volume of particle diameter (μ m) when representing with logarithm distributed that (D) is insoluble to the particulate matter of (A)～(C) is also measured with respect to the standard deviation of particle diameter.These be the results are shown in table 3.
Use this working fastening to stick with glue agent, implement working fastening/stripping means under the conditions shown in Table 3, in addition, the mean value and the standard deviation of thickness that the mean value of maximum width of indentation, there and standard deviation and working fastening stick with glue the cured article film of agent appears in operation similarly to Example 1, the glass of measuring each limit.Its measurement result is shown in table 3.
(embodiment 15)
Be insoluble to the particulate matter of (A)～(C) as (D), to use median size be 10 μ m, be 0.058 spherical crosslinked polystyrene particle (" SP-210 " that ponding chemical company makes) with distribute standard deviation with respect to particle diameter of the particle volume of particle diameter (μ m) when representing with logarithm, press the raw material that the composition shown in the table 3 uses the kind shown in the table 3, in addition, operation is similarly to Example 1 made working fastening and is sticked with glue agent.Stick with glue agent for resulting working fastening, implement second-order transition temperature, tensile shear adhesive strength, stripping test similarly to Example 1.In addition, the median size and the particle volume of particle diameter (μ m) when representing with logarithm distributed that (D) is insoluble to the particulate matter of (A)～(C) is also measured with respect to the standard deviation of particle diameter.These be the results are shown in table 3.
Use this working fastening to stick with glue agent, implement working fastening/stripping means under the conditions shown in Table 3, in addition, the mean value and the standard deviation of thickness that the mean value of maximum width of indentation, there and standard deviation and working fastening stick with glue the cured article film of agent appears in operation similarly to Example 1, the glass of measuring each limit.Its measurement result is shown in table 3.
(materials used)
UV-3700B: polyethers urethane acrylate (" UV-3700B " that Japanese synthetic chemistry company makes), hydrophobic (methyl) acrylate, weight-average molecular weight 38000
1.6-X-A: hexanediyl ester (" ラ イ ト ア Network リ レ one ト 1.6-HX-A " that chemical company of common prosperity society makes), hydrophobic (methyl) acrylate
I-754: oxygen base-phenyl-acetic acid 2-[2-oxo-2-phenyl-acetic acid base-oxyethyl group]-ethyl ester and oxygen base-phenyl-acetic acid 2-[2-hydroxyl-oxyethyl group]-mixture of ethyl ester (" IRGACURE754 " that vapour crust Japanese firm makes)
The interval that the present invention has in order to make stationary member and processed member evenly applies 1g/cm by a side or both sides 2More than and 1000kg/cm 2The pressurization operation of following pressure, and implement pressurization operation and irradiation process simultaneously can obtain the excellent size precision adding thus man-hour.
The present invention is by using specific hydrophobic (methyl) Acrylic Acid Monomer, use sticks with glue agent with the working fastening of the specific composition that it combines, can make its cured article do not cut water etc. influences, manifest high adhesive strength, therefore, member adds and is not easy man-hour to depart from, and obtains processed member more excellent aspect dimensional precision easily.The present invention is immersed in after processing in the warm water by making stationary member and processed member, and adhesive strength is descended, and the adhesive power of stationary member and processed member descends, and can easily reclaim processed member.
The present invention has the light solidity according to the composition that its working fastening sticks with glue agent, utilizes visible light or ultraviolet ray to be cured.Therefore, be that tackiness agent is compared with existing hot melt, laborsaving, energy-conservation, shorten and to obtain significant effect aspect the operation.
The present invention is obtaining significant effect by implement irradiation process in the pressurization operation aspect the dimensional precision of processed member.That is,, can easily control the thickness that working fastening sticks with glue agent by in the pressurization operation, implementing irradiation process.
The present invention sticks with glue agent by the working fastening that use contains the little particulate matter of standard deviation that particle volume distributes, obtains preferred dimensional precision.
According to the present invention, the cured article of working fastening descends adhesive strength by the contact warm water below 100 ℃ particularly, makes between member or the adhesive power decline of member and anchor clamps, and therefore, the such effect of member can be easily reclaimed in acquisition.Therefore, the situation that sticks with glue agent with working fastening that existing working fastening is used is compared, and can obtain to use costliness, ignition quality is strong or produces the so significant effect of organic solvent of harmful gas.
With regard to the working fastening of specific preferred compositing range of the present invention sticks with glue agent,, can reclaim from member with membranaceous, so obtain the effect of operability excellence because cured article contacts with warm water below 100 ℃.
The present invention is illustrated in detail and with reference to specific embodiment, but can under the situation that does not break away from aim of the present invention and scope, carries out various changes or revision will be apparent to those skilled in the art.
The application is based on the Japanese patent application (Japanese Patent Application 2008-188295) of application on July 22nd, 2008, and its content is incorporated in this as a reference.
Applicability on the industry
For method of temporarily fixing of the present invention, stick with glue agent as optical lens, prism, array, silicon wafer, semiconductor installation component etc. temporary fixed, industrially useful.

Claims (24)

1. method of temporarily fixing, comprise: working fastening is sticked with glue agent be applied to operation on the stationary member, processed member is carried stick with glue operation in the agent and this lift-launchs in working fastening and afterwards working fastening is sticked with glue agent and shine at least a in visible light or the ultraviolet ray and improve the operation that working fastening sticks with glue the adhesive power of agent, also comprise the operation that side from stationary member and processed member or both sides exert pressure, wherein, the operation that this is exerted pressure and this operation of shining are implemented certain hour at least simultaneously.
2. method of temporarily fixing, comprise: working fastening is sticked with glue agent be applied to operation on the processed member, stationary member is carried stick with glue operation in the agent and this lift-launchs in working fastening and afterwards working fastening is sticked with glue agent and shine at least a in visible light or the ultraviolet ray and improve the operation that working fastening sticks with glue the adhesive power of agent, also comprise the operation that side from stationary member and processed member or both sides exert pressure, wherein, the operation that this is exerted pressure and this operation of shining are implemented certain hour at least simultaneously.
3. method of temporarily fixing as claimed in claim 1 or 2, wherein, a side or both sides' applied pressure from stationary member and processed member are controlled at 1g/cm 2More than and 1000kg/cm 2Below.
4. as each described method of temporarily fixing in the claim 1 to 3, wherein, stationary member, working fastening sticked with glue be controlled at more than 0 ℃ more than any in agent, the processed member and below 150 ℃.
5. as each described method of temporarily fixing in the claim 1 to 4, wherein, working fastening sticks with glue agent for containing (A) multifunctional (methyl) acrylate, (B) simple function (methyl) acrylate and (C) composition of Photoepolymerizationinitiater initiater.
6. the method for temporarily fixing of member as claimed in claim 5 wherein, (A) and (B) is hydrophobicity.
7. as each described method of temporarily fixing in the claim 1 to 6, wherein, working fastening sticks with glue the second-order transition temperature of agent for more than-50 ℃ and below 50 ℃.
8. as each described method of temporarily fixing in the claim 5 to 7, wherein, working fastening sticks with glue agent, in (A) and total amount 100 mass parts (B), contain (A) 1～90 mass parts, (B) 10～99 mass parts, and contain (C) 0.1～30 mass parts with respect to (A) and total amount 100 mass parts (B).
9. as each described method of temporarily fixing in the claim 5 to 8, wherein, working fastening sticks with glue agent and contains particulate matter (D) 0.1～20 mass parts that is insoluble to (A)～(C) with respect to (A) and total amount 100 mass parts (B).
10. method of temporarily fixing as claimed in claim 9, wherein, be insoluble to (A)～(C) particulate matter (D) be shaped as spherical.
11. as claim 9 or 10 described method of temporarily fixing, wherein, the particulate matter (D) that is insoluble to (A)～(C) is the mixture of any or they in crosslinked polymethylmethacrylaparticles particle, crosslinked polystyrene particle and the crosslinked polymethylmethacrylaparticles polystyrene copolymer particle.
12. as each described method of temporarily fixing in the claim 9 to 11, the median size that wherein, is insoluble to the particulate matter (D) of (A)～(C) is 5 μ m～200 μ m.
13. as each described method of temporarily fixing in the claim 9 to 12, particle volume when wherein, the unit that utilizes laser diffractometry to measure that will be insoluble to the particulate matter (D) of (A)～(C) represents with logarithm for the particle diameter of μ m distributes with respect to the standard deviation of particle diameter in 0.0001～0.25 scope.
14. the working fastening/stripping means of a member, wherein, comprise: to using after each described method of temporarily fixing carries out the member processing of working fastening in the claim 1 to 13, the member after this processing is immersed in the warm water below 100 ℃, removes the cured article of described composition.
15. the working fastening/stripping means of a member, wherein, comprise: after each described method of temporarily fixing in the use claim 1 to 13 being carried out the member processing of working fastening, working fastening is sticked with glue agent irradiation visible light or ultraviolet ray, member after this processing is immersed in the warm water below 100 ℃, removes the cured article of described composition.
16. as each described method of temporarily fixing in the claim 1 to 13, wherein, visible light or ultraviolet irradiation amount are 1mJ/cm at wavelength 365nm place 2～4000mJ/cm 2Scope.
17. working fastening/stripping means as claimed in claim 15 is characterized in that, visible light or ultraviolet irradiation amount that the member processing back of this working fastening is shone are 1000mJ/cm at wavelength 365nm place 2～40000mJ/cm 2Scope.
18. as each described method of temporarily fixing in the claim 5 to 13, wherein, (A) multifunctional (methyl) acrylate contains multifunctional (methyl) origoester acrylate/polymkeric substance and/or two senses (methyl) acrylate monomer.
19. as each described method of temporarily fixing in the claim 5 to 13, wherein, (A) multifunctional (methyl) acrylate contains multifunctional (methyl) origoester acrylate/polymkeric substance and two senses (methyl) acrylate monomer.
20. as claim 18 or 19 described method of temporarily fixing, wherein, multifunctional (methyl) origoester acrylate/polymkeric substance contains polyester urethane (methyl) acrylate and/or polyethers urethane (methyl) acrylate.
21. as claim 18 or 19 described method of temporarily fixing, wherein, two senses (methyl) acrylate monomer contains 1,6-hexylene glycol two (methyl) acrylate and/or two (methyl) vinylformic acid dicyclo pentyl ester.
22. as each described method of temporarily fixing in the claim 5 to 13, wherein, (B) simple function (methyl) acrylate contains 2 moles of modification (methyl) acrylate of phenol ring oxidative ethane and/or 2-(1,2-encircles six carboxyl imides) ethyl (methyl) acrylate.
23. as each described method of temporarily fixing in the claim 5 to 13, wherein, (B) simple function (methyl) acrylate contains 2 moles of modification (methyl) acrylate of phenol ring oxidative ethane and 2-(1,2-encircles six carboxyl imides) ethyl (methyl) acrylate.
24. as each described method of temporarily fixing in the claim 5 to 13, wherein, (C) Photoepolymerizationinitiater initiater contain be selected from benzyl dimethyl ketal, oxygen base-phenyl-acetic acid 2-[2-oxo-2-phenyl-acetic acid base-oxyethyl group]-ethyl ester and oxygen base-phenyl-acetic acid 2-[2-hydroxyl-oxyethyl group]-in the ethyl ester more than a kind or 2 kinds.
CN200980128706.3A 2008-07-22 2009-07-22 Interim fixing/stripping means of component and be suitable to the interim fixing of its and stick with glue agent Active CN102105546B (en)

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