CN101955858A - Die cleaning agent composition and mould cleaning material and the mould cleaning method that uses it - Google Patents
Die cleaning agent composition and mould cleaning material and the mould cleaning method that uses it Download PDFInfo
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- CN101955858A CN101955858A CN201010233007XA CN201010233007A CN101955858A CN 101955858 A CN101955858 A CN 101955858A CN 201010233007X A CN201010233007X A CN 201010233007XA CN 201010233007 A CN201010233007 A CN 201010233007A CN 101955858 A CN101955858 A CN 101955858A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C33/00—Moulds or cores; Details thereof or accessories therefor
- B29C33/70—Maintenance
- B29C33/72—Cleaning
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/50—Solvents
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- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
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- Moulds For Moulding Plastics Or The Like (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Injection Moulding Of Plastics Or The Like (AREA)
Abstract
The present invention relates to the die cleaning agent composition, it carries out the cleansing composition of the hot briquetting of moulding repeatedly with mould for using formed material, wherein contain: as the synthetic rubber and/or the synthetic resins of mother metal, an alkali metal salt and/or alkali metal hydroxide and water and/or organic solvent.
Description
Technical field
The present invention relates to owing to carry out injection forming repeatedly or transmit forming operation such as shaping and contaminated mould, for example be used for the die cleaning agent composition and the mould cleaning material of uses such as cleaning and regeneration of semiconductor device molding die etc. of forming operation of compositions of thermosetting resin and the mould cleaning method that uses it.
Background technology
Generally speaking, because operations such as injection forming repeatedly or transmission shaping, the releasing agent of the volatile component that produces when on the die surface of mould, being attached with the heating shaped material, the exudate on molding surface, use when being shaped etc., and these dirt settlings are owing to oxidation is gone bad, and mould is contaminated thus.When mould is contaminated like this, finish size, outward appearance, the release property etc. of molding are had a negative impact, therefore not preferred.
Therefore, for the disadvantageous effect that prevents to be caused by contaminated like this mould, the mould that is used for injection forming or transmission shaping need regularly carry out clean-out operation, and above-mentioned pollutent is removed from die surface.As existing mould purging method, for example known: as from building mortion, to take apart a die and the method for cleaning with strong base solution or solvent etc.
But, from building mortion, take apart a die and need the operation such as cooling, intensification, desorption, cleaning of mould with the method that strong base solution or solvent clean, the problem that exists is need for a long time to clean, labor capacity is big, and exist since the use of strong base solution or solvent and liquid waste disposal after the operator had a negative impact, cleans etc. to the big such problem of load of people or environment.
Therefore, use thermoset melamine resin shaped material, unvulcanized rubber class mixture etc. have been proposed, use these materials in mould, to form, thus will be integrated at pollutent and shaping thing that die surface generates, and should the shaping thing from mould, take out the method on cleaning die surface, and part is implemented (for example, referring to Patent Document 1).
Patent documentation 1: Japanese kokai publication hei 10-226799 communique
Summary of the invention
For example, the semiconductor device molding die that uses in the forming operation of compositions of thermosetting resin cleans by aforesaid method, but, above-mentioned compositions of thermosetting resin is grouped into difference according to the one-tenth that its desired characteristic constitutes, multiple kind is arranged, therefore, the state of the mold fouling that produces repeatedly by forming operation and the composition of pollutent also are varied.Wherein, use and removed with lead or halogen the pollution substance carrying capacity of environment material, that the corresponding phenol resin molding material of without halide environment forms on mould when being shaped repeatedly as representative, sintering (the baked I is paid け) especially severe to die surface, existing purging method by aforesaid use thermoset melamine resin shaped material or unvulcanized rubber class mixture can not be removed pollution substance fully, also needs the cleaning material that also can clean such pollution substance.
The present invention carries out in view of such situation, and its purpose is to provide for by forming operation repeatedly and contaminated mould has the die cleaning agent composition and the mould cleaning material of good cleaning performance and the mould cleaning method that uses it.
To achieve these goals, of the present invention first will be intended to a kind of die cleaning agent composition, it carries out the cleansing composition of the hot briquetting of moulding repeatedly with mould for using formed material, wherein contain: as the synthetic rubber and/or the synthetic resins of mother metal, an alkali metal salt and/or alkali metal hydroxide and water and/or organic solvent.
In addition, of the present invention second will be intended to a kind of mould cleaning material, and it obtains by using the die cleaning agent composition to be configured as sheet.
And, the of the present invention the 3rd will be intended to a kind of cleaning method of mould, it comprises following operation: the mould cleaning material that will comprise described die cleaning agent composition is placed into the operation on the profile of mould of unlatching, described mould and clip described mould cleaning material and carry out heating and pressurizing closes, make the pollutent that forms at die surface and the incorporate operation of described mould cleaning material thus and by peel off cleaning mold surface from mould with the incorporate mould cleaning material of pollutent.
Promptly, even the pollution substance that the inventor forms on mould when obtaining using as previously mentioned the corresponding phenol resin molding material of Halogen environment to be shaped repeatedly also can clean the cleansing composition of removing effectively, carried out research extensively and profoundly, found that, when the synthetic rubber and/or the synthetic resins that contain as mother metal, an alkali metal salt and/or alkali metal hydroxide, during with water and/or organic solvent, produce the dissolving or the Decomposition of dirt by the effect of water or organic solvent, and by making above-mentioned an alkali metal salt and/or alkali metal hydroxide and depositing, can realize promoting the dissolving of dirt or the effect of Decomposition, therefore, by their synergy, can realize than existing better cleaning performance, thereby finish the present invention.
As mentioned above, die cleaning agent composition of the present invention contains synthetic rubber and/or the synthetic resins as mother metal, an alkali metal salt and/or alkali metal hydroxide and water and/or organic solvent.Therefore, even the pollutent that forms for forming operation repeatedly, particularly be difficult to fully clean with existing composition for cleaning, use got rid of the thermosetting resin shaped material with lead or halogen, antimony is the pollution substance that the corresponding phenol resin molding material of the Halogen environment behind the carrying capacity of environment material of representative forms at die surface when forming operation repeatedly, owing to have synergy, promptly produce the dissolving or the Decomposition of dirt by the effect of water or organic solvent, and, remove effect and bring into play good cleaning by making above-mentioned an alkali metal salt and/or alkali metal hydroxide and depositing the dissolving that promotes dirt or the effect of Decomposition.Therefore, the die cleaning agent composition of the application of the invention carries out the cleaning of die surface, the pollutent that forms at die surface is attached on this die cleaning agent composition also integrated, thereby pollutent can be removed from mould effectively, for example, the semiconductor element encapsulation that uses composition epoxy resin to be shaped repeatedly is integrated with the molding that comprises this die cleaning agent composition with the pollutent of die surface, can remove pollutent from mould effectively, effectively cleaning die.As a result, the semiconductor device that uses the mould after die cleaning agent composition of the present invention cleans to form obtains the no problem good goods of outward appearance.And, after the mould cleaning material that will comprise die cleaning agent composition of the present invention is placed on the profile of mould of unlatching, described mould and clip described mould cleaning material and carry out heating and pressurizing closes, make the pollutent and the described mould cleaning material that form at die surface integrated thus, can the cleaning mold surface by peeling off from mould with the incorporate mould cleaning material of pollutent.
When particularly above-mentioned synthetic rubber was ethylene-propylene class rubber and/or divinyl rubber, the processing ease when mould cleans can be realized the raising of clean-out operation.
In addition, the content of above-mentioned an alkali metal salt and/or alkali metal hydroxide when being set at specified proportion as the synthetic rubber of mother metal and/or synthetic resins 100 weight parts, can be obtained better cleanup action.
In addition, contain organic solvent and water when simultaneously, and with the content of water when being set at specified proportion as the synthetic rubber of mother metal and/or synthetic resins 100 weight parts, can obtain better cleanup action.
Embodiment
Below, describe embodiments of the present invention in detail.
Die cleaning agent composition of the present invention uses as the synthetic rubber of mother metal and/or synthetic resins, an alkali metal salt and/or alkali metal hydroxide and water and/or organic solvent to obtain as neccessary composition.
Above-mentioned synthetic rubber, be so-called unvulcanized rubber, for example can enumerate: natural rubber (NR), divinyl rubber (BR), paracril (NBR), ethylene-propylene rubber(EPR) ethene-alpha-olefins such as (EPR) rubber, styrene butadiene rubbers (SBR), polyisoprene rubber (IR), isobutylene-isoprene copolymer (IIR), silicon rubber (Q), contain viton (FKM) etc.These rubber may be used singly or two or more in combination.In addition, among the present invention, above-mentioned ethene-alpha-olefin rubber also comprises ethylene-propylene-polyenoid rubber ethylene-alpha-olefin-polyene rubber such as (EPDM).In addition, these unvulcanized rubbers vulcanize in mould and become vulcanized rubber.
In the above-mentioned synthetic rubber, the few viewpoint of foul smell when using mould to form during the few and sulfuration of contaminative considers, preferably uses EPR (comprising EPDM), BR separately or uses their mixture.
Above-mentioned EPDM is elaborated.EPDM be by ethene, alpha-olefin (particularly propylene) and below the terpolymer that constitutes of the polyenoid monomer enumerated, as above-mentioned polyenoid monomer, can enumerate: dicyclopentadiene, 1,5-cyclooctadiene, 1,1-cyclooctadiene, 1,6-encircles 12 carbon diene, 1,7-encircles 12 carbon diene, 1,5,9-cyclododecatriene, 1,4-cycloheptadiene, 1,4-cyclohexadiene, norbornadiene, methene norbornylene, 2-methyl isophthalic acid, 4-pentadiene, 1,5-hexadiene, 1,6-heptadiene, methyltetrahydro indenes, 1,4-hexadiene etc.
Each monomeric copolymerization ratio optimal ethylene is that 30～80 moles of %, polyenoid monomer are 0.1～20 mole of %, all the other are the terpolymer of alpha-olefin among the above-mentioned EPDM.More preferably ethene is 30～60 moles of %.
In addition,, can distinguish and use 1 separately, 2-polyhutadiene, 1 or its combination used as mixture as above-mentioned BR.
As above-mentioned synthetic resins, for example can enumerate: polyamide resins such as nylon 6 or nylon 66, vibrin such as polyethylene terephthalate or polybutylene terephthalate, polycarbonate resin, polyarylester (polyarylate) resin, vinyl chloride resin, chlorinated vinyl chloride resin, polyvinyl resin, chlorinated polyethylene resin, chlorinated polypropylene, acrylic resin, polystyrene resin, the acrylonitrile-styrene resinoid, vinylidene resin, vinyl acetate resin, polyacrylate resin, polyimide resin, butadiene resin, polyacetal resin, ionomer resin, the ethylene-vinyl chloride copolymer resins, ethylene-vinyl acetate copolymer resin, ethane-acetic acid ethyenyl ester-vinylchlorid graft polymerization resin, polyphenylene resin, polysulfone resin, methacrylic resin, acrylic acid or the like-fluorine resin, acrylic acid or the like-siloxane oligomer, silicone resin, contain epoxy group(ing) silicone-acrylic resinoid, vinylester resin, furane resin, resol, melamine resin, guanamine resin, urea resin, urethane resin, the diallyphthalate acid ester resin, ketone resin, Resins, epoxy, xylene resin, maleic acid resin, phenoxy resin, coumarone resin, vinyl-formal resin, polyvinyl butyral resin etc.These resins may be used singly or two or more in combination.In these synthetic resins, the few viewpoint of pollution during from the use die forming is considered, preferably uses polyvinyl resin, Resins, epoxy, melamine resin.
And in the mother metal that comprises these synthetic rubber and/or synthetic resins, synthetic rubber or synthetic resins can use separately separately, also synthetic rubber and synthetic resins can be used in combination, also can be with multiple being used in combination separately.Wherein, from carry out mould when cleaning maneuverable viewpoint consider, preferably use synthetic rubber, polyvinyl resin, Resins, epoxy, melamine resin.The above-mentioned synthetic rubber of preferred especially use, in this synthetic rubber, as previously mentioned, the preferred mixture that uses EPR separately or use this EPR and BR.
As mother metal, EPR (x) preferably is set in the scope of x/y=100/0～20/80 in weight ratio with the blending ratio (x/y) of BR (y) when stating the mixture of EPR and BR in the use.The scope of preferred especially x/y=70/30～30/70.That is, this be because: about both blending ratios, when EPR is lower than 20 (BR is more than 80), when when forming operation, removing the rubber molding product, therefore the strength degradation of molding is easy to generate problem such as break, and has the tendency that the operation of removing from mould becomes difficulty.
Comprise these synthetic rubber and/mother metal of synthetic resins, when the removing of dirt, when mould takes out, be preferably solid state.As the curing of realizing above-mentioned solid state, can enumerate be heating and curing, the cooling curing of thermoplastic resin etc. etc., for example, when being cured, use solidifying agent by heating.
Above-mentioned solidifying agent is so long as can make the mother metal solidified material get final product, for example, can enumerate organo-peroxide etc. for synthetic rubber or polyvinyl resin, under the situation of Resins, epoxy, can enumerate phenolic compound, aminated compounds, imidazoles, acid anhydride type curing agent, organic phosphoric acid compound etc.
As above-mentioned organo-peroxide, for example can enumerate: 1,1-bis(t-butylperoxy)-3,3, the 5-trimethyl-cyclohexane, 1, the 1-bis(t-butylperoxy) cyclohexane, the peroxy maleic acid tert-butyl ester, the peroxide oleic acid tert-butyl ester, 3,3,5-trimethylammonium peroxide hecanoic acid t-butyl ester, the pimelinketone superoxide, the t-butyl peroxy aryl carbonate, t-butyl peroxy isobutyl carbonate propyl ester, 2,5-dimethyl-2,5-two (benzoyl peroxy) hexane, 2,2-bis(t-butylperoxy) octane, tert-butyl peroxy acetate, 2,2-bis(t-butylperoxy) butane, t-butyl per(oxy)benzoate, 4,4-bis(t-butylperoxy) n-butyl pentanoate, peroxide m-phthalic acid di tert butyl carbonate, methyl ethyl ketone peroxide, dicumyl peroxide, 2,5-dimethyl-2,5-two (t-butylperoxy) hexane, α, isopropyl benzene between α '-bis(t-butylperoxy), the tert-butyl peroxide cumyl, diisopropylbenzenehydroperoxide, di-t-butyl peroxide, 2,5-2-organo-peroxides such as 3-alkynes.
As above-mentioned phenolic compound, for example can enumerate: as Resorcinol, Resorcinol, the pyrocatechol of monocycle difunctionality phenol; As the dihydroxyphenyl propane of many rings difunctionality phenol, Bisphenol F, naphthalenediol class, biphenyl phenols etc.; And multifunctional phenols such as their halides, alkyl substituent.
As above-mentioned aminated compounds, for example can enumerate: N, the N-benzyldimethylamine, 2-(dimethylamino methyl) phenol, 2,4,6-three (dimethylamino methyl) phenol, tetramethyl guanidine, trolamine, N, N '-lupetazin, 1,4-diazabicyclo [2.2.2] octane, 1,8-diazabicyclo [5.4.0]-7-undecylene, 1,5-diazabicyclo [4.4.0]-5-nonene, vulkacit H, pyridine, picoline, piperidines, tetramethyleneimine, dimethylcyclohexylamine, dimethylhexylamine, hexahydroaniline, diisobutylamine, Di-n-Butyl Amine, pentanoic, methylphenylamine, Tri-n-Propylamine, tri-n-octyl amine, tri-n-butylamine, triphenylamine, tetramethyl ammonium chloride, 4 bromide, Tetramethylammonium iodide, Triethylenetetramine (TETA), diaminodiphenyl-methane, diaminodiphenyl oxide, Dyhard RU 100, OTBG o tolylbiguanide, the guanidine radicals urea, dimethyl urea etc.
As above-mentioned imidazoles, for example can enumerate: imidazoles, the 2-ethyl imidazol(e), 2-ethyl-4-methylimidazole, glyoxal ethyline, the 2-phenylimidazole, the 2-undecyl imidazole, 1 benzyl 2 methyl imidazole, 2-heptadecyl imidazoles, 4, the 5-diphenyl-imidazole, the glyoxal ethyline quinoline, the 2-benzylimidazoline, 2-undecyl imidazole quinoline, 2-heptadecyl tetrahydroglyoxaline, 2 isopropyl imidazole, 2, the 4-methylimidazole, 2-phenyl-4-methylimidazole, 2-ethyl imidazol(e) quinoline, 2-phenyl-4-methylimidazole quinoline, benzoglyoxaline, 1-cyano ethyl imidazoles, 2,4-diamino-6-[2 '-methylimidazolyl-(1 ')] the ethyl s-triazine etc.
As above-mentioned acid anhydride type curing agent, for example can enumerate: acid anhydrides such as Tetra hydro Phthalic anhydride, hexahydrophthalic anhydride, pyromellitic dianhydride, benzophenone tetracarboxylic acid dianhydride.
As above-mentioned organic phosphoric acid compound, for example can enumerate: organo phosphorous compounds such as HMPA, tricresyl phosphate (two chloropropyls) ester, tricresyl phosphate (chloropropyl) ester, triphenyl phosphite, trimethyl phosphite 99, phenyl-phosphonic acid, triphenylphosphine, tri-n-butyl phosphine, diphenylphosphine and their halogenide etc.
These solidifying agent can use separately, also can two or more arbitrary combination use.
The use level of these solidifying agent can suitably be set, for example, if synthetic rubber then preferably sets in 1～3 part scope with respect to synthetic rubber 100 weight parts (hereinafter to be referred as " part ").
In addition, these solidifying agent not only have the function of the thermofixation of synthetic rubber or synthetic resins, also have the function as the clean-out system of mould, as required except as also may be fitted to the purpose of solidifying agent in the die cleaning agent composition of the present invention.The use level of the solidifying agent under such situation is preferably set to 5～60 parts for 100 parts, preferred especially 5～25 parts with respect to synthetic rubber and/or synthetic resins.
An alkali metal salt that cooperates in the above-mentioned mother metal and/alkali metal hydroxide in, as above-mentioned an alkali metal salt, can enumerate the metal-salt of lithium, sodium, potassium, rubidium, caesium etc.
In addition, as such an alkali metal salt, for example can enumerate: boric acid, phosphoric acid, metaphosphoric acid, diphosphanetetroic acid, phosphorous acid (phosphonic acid), Hypophosporous Acid, 50 (phosphinic acid), tetra-sodium, the trimerization metaphosphoric acid, four poly-metaphosphoric acids, phosphoric acid salt such as pyrophosphorous acid, carbonate, vitriol, nitrate, hydrochloride, vinylformic acid, hexanodioic acid, xitix, aspartic acid, benzaminic acid, Lalgine, phenylformic acid, oleic acid, formic acid, citric acid, oxyacetic acid, glyconic acid, L-glutamic acid, styracin, succsinic acid, acetate, Whitfield's ointment, oxalic acid, tartrate, toluenesulphonic acids, nicotinic acid, lactic acid, uric acid, halogenated acetic acids, phthalic acid, Phenylsulfonic acid, propanedioic acid, butyric acid, organic acid salts such as oxysuccinic acid etc.
These an alkali metal salts are under the situation of polyprotonic acid, also can use part to form the material of an alkali metal salt, for example, under the phosphatic situation as triprotic acid, can be dihydrogen phosphate, hydrophosphate, in the phosphoric acid salt with three metals any one with two metals and a hydrogen with a metal and two hydrogen.In addition, also can be any one of acid-salt, basic salt, neutral salt.Wherein, consider preferred basic salt, neutral salt from corrosive viewpoint of mould.In addition, the viewpoint of solubleness is considered from water, and these an alkali metal salts preferably use hydrate.
As above-mentioned alkali metal hydroxide, for example can enumerate: sodium hydroxide, potassium hydroxide etc.
These an alkali metal salts, alkali metal hydroxide can use separately, also can be used in combination.
In addition, above-mentioned an alkali metal salt and/or alkali metal hydroxide, with respect to as the synthetic rubber of mother metal and/or 100 parts of preferred settings of synthetic resins in 0.1～10 part scope, preferred especially 0.1～5 part.This be because: when use level is very few, the removing property of the pollution substance that forms at die surface significantly descends, and has to be difficult to tendency that the mould dirt is removed fully, and is opposite too much the time, an alkali metal salt, alkali metal hydroxide are separated out at die surface easily, have the tendency of polluting mould on the contrary.
In addition, the water as cooperating in the present invention can preferably use tap water, remove the RO water (water after anti-seepage membrane is handled), ion exchanged water of impurity etc.
The use level of above-mentioned water is with respect to as the synthetic rubber of mother metal and/or 100 parts of preferred settings of synthetic resins scope at 3～30 parts, preferred especially 5～20 parts.This be because: when use level was very few, the removing property of the pollution substance that forms at die surface significantly descended, and had to be difficult to tendency that the mould dirt is removed fully, when too much on the contrary, cleaning performance does not improve, and also increase the man-hour of cooperation, therefore has the tendency of waste.
In addition, the organic solvent as using in the present invention can use various organic solvents, for example, state in the use under the situation of an alkali metal salt, consider, can use amide solvent, alcoholic solvent, ketones solvent, ether solvent etc. from its deliquescent viewpoint.These solvents can use separately, also can be used in combination.
As above-mentioned amide solvent, can for example preferably use: methane amide, N-methylformamide, N, dinethylformamide, N, N-diethylformamide, ethanamide, N-methylacetamide, N, N-N,N-DIMETHYLACETAMIDE, N, N, N ', N '-tetramethyl-urea, 2-Pyrrolidone, N-N-methyl-2-2-pyrrolidone N-, hexanolactam, carbamate etc.
As above-mentioned alcoholic solvent, for example can enumerate: methyl alcohol, ethanol, the 1-propyl alcohol, the 2-propyl alcohol, the 1-butanols, the 2-butanols, isopropylcarbinol, the trimethyl carbinol, the 1-amylalcohol, the 2-amylalcohol, the 3-amylalcohol, 2-methyl-1-butene alcohol, primary isoamyl alcohol, tertiary amyl alcohol, 3-methyl-2-butanols, neopentyl alcohol, the 1-hexanol, 2-methyl-1-pentene alcohol, 4-methyl-2-amylalcohol, 2-ethyl-1-butanols, the 1-enanthol, the 2-enanthol, the 3-enanthol, hexalin, 1 methyl cyclohexanol, 2 methyl cyclohexanol, 3 methyl cyclohexanol, 4 methyl cyclohexanol, ethylene glycol, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol ether, ethylene glycol monobutyl ether, Diethylene Glycol, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, Diethylene glycol monopropyl ether, diethylene glycol monobutyl ether, triethylene glycol, triethylene glycol monomethyl ether, Triethylene glycol ethyl ether, TEG, polyoxyethylene glycol (weight-average molecular weight 200～400), 1, the 2-propylene glycol, 1, ammediol, 1, the 2-butyleneglycol, 1, the 3-butyleneglycol, 1, the 4-butyleneglycol, 2, the 3-butyleneglycol, 1, the 5-pentanediol, glycerine, propylene glycol, dipropylene glycol etc.
As above-mentioned ketones solvent, for example can enumerate: acetone, methylethylketone, 2 pentanone, propione, methyl-n-butyl ketone, methyl iso-butyl ketone (MIBK), 2-heptanone, dipropyl ketone, diisobutyl ketone, pimelinketone, methylcyclohexanone, sym.-diisopropylideneacetone, isophorone etc.
As above-mentioned ether solvent, for example can enumerate: dipropyl ether, diisopropyl ether, dibutyl ether, two hexyl ethers, methyl-phenoxide, phenyl ethyl ether, dioxane, tetrahydrofuran (THF), 1,1-diethoxyethane, glycol dimethyl ether, ethylene glycol diethyl ether, diethylene glycol dimethyl ether, diethylene glycol diethyl ether etc.
And, except above-mentioned organic solvent, also can use hydrocarbon, halohydrocarbon, phenols, acetal, lipid acid, acid anhydrides, ester cpds, nitrogen compound, amine compound (Monoethanolamine MEA BASF etc.), sulphur compound (methyl-sulphoxide etc.) equal solvent or have the solvent (ester and ether, pure and mild ether etc.) of two above functional groups.These solvents can use separately, also can two or morely make up (for example, between the amide solvent, the solvent beyond amide solvent and the amide solvent) and use.In addition, also can be used in combination other solvent, for example, also can mix ammonia as inorganic solvent etc. with these solvents.
Among the present invention, use under the situation of an alkali metal salt, consider, preferably above-mentioned organic solvent is used with above-mentioned illustrative water from the deliquescent viewpoint of this an alkali metal salt.In addition, when above-mentioned an alkali metal salt uses with the hydrate forms that is combined with crystal water, contain micro-moisture so solvability improves, still, consider, preferably hydrous water and accelerate dissolution rate on one's own initiative from the viewpoint of operation by this crystal water.
Above-mentioned organic solvent is preferably liquid when cleaning die, in addition, do not have volatile organic solvent during particularly preferably in mold heated.For example, preferably use polyalcohols, polyol alkyl ether class.Particularly, for the semiconductor device molding die that uses compositions of thermosetting resin as sealing material, it generally uses down for about 180 ℃ in die temperature, and therefore the solvent that uses as this moment preferably uses the solvent of boiling point more than 180 ℃.As boiling point is solvent more than 180 ℃, for example can enumerate: ethylene glycol monobutyl ether (boiling point: 188 ℃), propylene glycol (boiling point: 187 ℃), dipropylene glycol monomethyl ether (boiling point: 190 ℃), diethylene glycol monomethyl ether (194 ℃ of boiling points) etc.
The use level of above-mentioned organic solvent (the total use level when each solvent is used in combination), with respect to as the synthetic rubber of mother metal and/or 100 parts of preferred settings of synthetic resins in 3～30 parts scope, preferred especially 5～20 parts.This be because: when use level was very few, the removing property of the pollution substance that forms at die surface significantly descended, and had to be difficult to tendency that the mould dirt is removed fully, when too much on the contrary, cleaning performance does not improve, and also increase the man-hour of cooperation, therefore has the tendency of waste.
In the die cleaning agent composition of the present invention, except above-mentioned each gradation composition, also can suitably cooperate releasing agent, toughener etc. as required as neccessary composition.
As above-mentioned releasing agent, for example can enumerate: longer chain fatty acids such as stearic acid, docosoic, with Zinic stearas, calcium stearate etc. is the long-chain fat acid metal salt of representative, with partly-hydrolysed ester of carnauba wax, montanic acid wax, montanic acid etc. is the ester type waxes of representative, with ethylene bis stearamide etc. is the long chain fatty acids amides of representative, is paraffin class of representative etc. with polyethylene wax etc.These materials can use separately, also can be used in combination.
The content of above-mentioned releasing agent, with respect to as the synthetic rubber of mother metal and/100 parts of preferred settings of synthetic resins are 5～20 parts scope, preferred especially 8～16 parts.This be because: when content is very few, be difficult to bring into play sufficient stripping result, opposite too much the time, have that cleansing power descends and the tendency of the degraded appearance of this molding when using mould after the regeneration to make molding.
As above-mentioned toughener, for example can enumerate: inorganic fillers such as SiO 2 powder, talcum powder, aluminum oxide, lime carbonate, aluminium hydroxide, titanium oxide.These materials can use separately, perhaps are used in combination.As above-mentioned toughener, preferably use the toughener of median size for about 0.01～about 100 μ m.
The content of above-mentioned toughener, with respect to as the synthetic rubber of mother metal and/100 parts of preferred settings of synthetic resins are 10～50 parts scope, preferred especially 15～40 parts.This be because: when content is very few, thereby the decline of enhancing property has the tendency that causes physical strength to descend, and is opposite too much the time, still has the tendency that physical strength descends thereby become fragile.
In addition, in die cleaning agent composition of the present invention,, can for example suitably cooperate as required: aromatic hydrocarbon oil, cycloalkanes wet goods tenderizer, vulcanizing agent or vulcanization accelerators such as sulphur, antiaging agent, the flowers of zinc etc. as the additive except that above-mentioned.
Die cleaning agent composition of the present invention for example can followingly be made.That is, can will comprise that each gradation composition of above-mentioned each neccessary composition carries out mechanically milling and makes by using banbury mixers, kneader, mill (roll mixer), forcing machine etc.
The die cleaning agent composition of the present invention of Zhi Zaoing like this, the form of the mould cleaning material of for example Powdered to form, drug sheet, sheet or short strip shape is used for mould and cleans.The thickness of sheet is set at 3～10mm usually when making the sheet use.
In addition, as die cleaning agent composition of the present invention, be preferably formed into white to the grey such light color approaching with it.By setting like this, has following effect: after mould cleans, can easily estimate to confirm and remove and be attached to dirt on the die cleaning agent composition, and can easily confirm the cleaning situation of mould from mould.
When using, after being under the elastomeric situation, generally being preferably shaped to sheet, uses mother metal from mould cleaning material that die cleaning agent composition of the present invention obtains.In addition, mother metal is under the situation of synthetic resins, for example, if be the thermoset melamine resin, uses after then being preferably shaped to Powdered or drug sheet.
Use the cleaning method that forms the mould of flaky die cleaning agent composition of the present invention, carry out after in being loaded into the semiconductor device molding die.For example, be under the elastomeric situation at mother metal, above-mentioned is in not sulfided state certainly, it is loaded into carries out baking in the molding die, pollutent is attached on the sheet and integrated with it.Then, the sheet after the sulfuration is taken out from mould, carry out the cleaning of mould thus.
Use the mould cleaning method of above-mentioned sheet die cleaning agent composition about mother metal during for synthetic rubber, below progressively be elaborated.
At first, prepare to comprise the sheet mould cleaning material of die cleaning agent composition of the present invention.Then, above-mentioned flaky mould cleaning material (cleaning foil) is configured between the upper die and lower die that are formed with recess respectively of mould, begins upper die and lower die are closed from this state and clamp sheet mould cleaning material and carry out compression molding.In addition, the pressure when being shaped, above-mentioned sheet mould cleaning material are filled in the chamber that is made of recess that forms in patrix and the recess that forms in counterdie, and are crimped onto on the die surface.Heat when under this state, being shaped, synthetic rubber (unvulcanized rubber) baking and become vulcanized rubber, oxidative degradation layers of the releasing agent that form this moment in chamber etc. and vulcanized rubber form one.At this moment, according to circumstances, the burr that forms around chamber is also integrated.Then, through after the scheduled time, upper die and lower die are opened,, will be peeled off from two die surfaces up and down with the incorporate oxidative degradation layer of above-mentioned sheet mould cleaning material etc. (pollutent) thus from two moulds sheet mould cleaning material of vulcanized rubberization being peeled off up and down.Like this, carry out the cleaning of mould.
As clamping that above-mentioned sheet mould cleaning material carries out compression molding and condition when heating, suitably set according to mother metal kind etc.For example, under the elastomeric situation, be preferably set to 160～190 ℃ * 1～5 minute scope,, be preferably set to 160～190 ℃ * 1～5 minute scope using under the situation of thermosetting resin as synthetic resins.
Use object as die cleaning agent composition of the present invention is an example of mould, for example can enumerate: the semiconductor device that uses compositions of thermosetting resin to be shaped repeatedly seals the molding die of usefulness.
In semiconductor device molding die as the example of use object of die cleaning agent composition of the present invention, as the compositions of thermosetting resin that the sealing resin material uses, for example can enumerate: be the composition epoxy resin of principal constituent with Resins, epoxy.
And, as compositions of thermosetting resin, usually suitably cooperate additives such as solidifying agent and inorganic filler as required, curing catalyst with Resins, epoxy as above-mentioned principal constituent.
Then, with the mould after the die cleaning agent composition cleaning of the present invention, be removed the die surface of getting back to original state owing to pollutent, therefore, usually when using compositions of thermosetting resin as shaped material to carry out the shaping of semiconductor packages, in advance releasing agent is applied to die surface.For example, when containing montanic acid wax as the shaping of the shaped material of releasing agent, same preferred coating carnauba wax.And as the method for coating releasing agent on die surface, the preferred unvulcanized rubber composition of preparing to contain releasing agent uses after it is configured as sheet.For example, can enumerate the sheet that releasing agent is cooperated with aforesaid unvulcanized rubber and obtain.In addition, will be loaded in the mould by the sheet that the unvulcanized rubber composition that contains this releasing agent is made equally with the matting of using above-mentioned sheet die cleaning agent composition and heat, contained thus releasing agent is applied to die surface.This can think: the releasing agent fusion during baking in the unvulcanized rubber composition and being exuded on the die face, thus form uniform releasing agent film from the teeth outwards.
In addition, the content of above-mentioned releasing agent is for example with respect to the ratio of 100 parts of preferred settings of the elastomeric material in the unvulcanized rubber composition at 15～35 parts, preferred especially 20～30 parts.This be because: if the content of releasing agent is lower than 15 parts, then can not bring into play sufficient stripping result, if opposite surpass 35 parts, then excessively coat die surface and use and cleaning, when mould after the regeneration forms molding, having the tendency of the degraded appearance of this molding.
Embodiment
Below, embodiment and comparative example are described in the lump.But, the invention is not restricted to these embodiment.
At first, prepare to constitute each composition of die cleaning agent composition.
1) BR:[divinyl rubber: the JSR corporate system, BR-01 (cis 1,4 combination: 95%)]
2) EPR[ethylene-propylene-elastoprene: the Mitsui Chemicals corporate system, EPT4045 (ethylene content: 54 moles of %, diene component content: 8.1 moles of %)]
3) talcum powder: median size 9 μ m
4) SiO 2 powder: median size 9 μ m
5) titanium oxide: median size 0.25 μ m
6) carnauba wax: No. 1, カ Le Na バ (day emerging リ カ corporate system)
7) imidazoles: 2,4-diamino-6-[2 '-methylimidazolyl-(1 ')] the ethyl s-triazine
8) organo-peroxide: 4, two (t-butyl peroxy) n-butyl pentanoates of 4-
9) water: ion exchanged water
10) PEG: polyoxyethylene glycol (day oily corporate system, #200; Weight-average molecular weight 200)
11) PG: propylene glycol (boiling point: 187 ℃)
12) DGMM: diethylene glycol monomethyl ether (boiling point: 194 ℃)
(embodiment 1～8, comparative example 1～2)
Each composition shown in table 1 described later～table 2 is cooperated with the ratio shown in this table, use mixing roller that it is mixing.Then, use stack to be configured as sheet (thickness 5mm), make the sheet die cleaning agent composition (mould cleaning material) of target.
(embodiment 9)
To 100 parts of sprayings of crushed material of the Clean-thermoset melamine resin of commercially available mould (Japanese カ one バ ィ ト industrial system, ニ カ レ ッ ト ECR-T) 1 part of K as the clean-out system composition
3PO
4With 4 parts of water, it is adhered to, obtain pulverous die cleaning agent composition (mould cleaning material) thus.
(comparative example 3)
Use the tablet of the Clean-thermoset melamine resin of commercially available mould (Japanese カ one バ ィ ト industrial system, ニ カ レ ッ ト ECR-T), as the die cleaning agent composition (mould cleaning material) of drug sheet.
The embodiment product that use obtains like this and each die cleaning agent composition (mould cleaning material) of comparative example product, the removing property of the pollutent that forms on the following evaluation mould.Promptly, use is as corresponding Resins, epoxy (day eastern electrician's corporate system of environment of sealing material, GE-7470) be shaped repeatedly, in carrying out 800 surperficial contaminated molding dies after (シ ョ ッ ト), use above-mentioned each die cleaning agent composition (mould cleaning material) to clean shaping.In addition, will from mould, take out the removing property of the pollutent of visual assessment die surface by the shaping thing that cleaning forms.In this was estimated, the forming operation number of times that can remove pollutent fully was that the average evaluation below 5 times is good, and it is bad that removing of pollutent needed the average evaluation of the forming operation more than 6 times.
In addition, in the evaluation of embodiment 1～8 product and comparative example 1～2 product, flaky die cleaning agent composition (mould cleaning material) is clipped in the molding die, carries out heating in 5 minutes at 175 ℃ and be shaped.On the other hand, in the evaluation of embodiment 9 product, use pulverous die cleaning agent composition (mould cleaning material), in the evaluation of comparative example 3 product, use the die cleaning agent composition (mould cleaning material) of drug sheet, transmit shaping, carry out heating in 3 minutes at 175 ℃ and be shaped.
Above-mentioned evaluation result is shown in following table 1～table 2.
Table 1
(part)
Table 2
(part)
From The above results as can be seen, do not contain as the two comparative example product of an alkali metal salt of clean-out system composition and/or alkali metal hydroxide and water, the cleaning of its mould is evaluated as bad, and is relative therewith, and all the mould cleaning of embodiment product is evaluated as very.
The change of＜sealing material (1) 〉
In addition, will be as above-mentioned environment correspondence Resins, epoxy (day eastern electrician's corporate system of sealing material, GE-7470) change to the corresponding Resins, epoxy GE-1030 of environment that is all the manufacturing of eastern electrician of day company, for with above-mentioned molding die (after 800 times) after similarly being shaped repeatedly, by using the contaminant removal of each die cleaning agent composition (mould cleaning material) of embodiment 1～9 product and comparative example 1～3 product with above-mentioned same method visual assessment.As a result, with above-mentioned same, the mould cleaning of comparative example product is evaluated as bad, and is relative therewith, and all the mould cleaning of embodiment product is evaluated as very.
The change of＜sealing material (2) 〉
In addition, will be as above-mentioned environment correspondence Resins, epoxy (day eastern electrician's corporate system of sealing material, GE-7470) change to the corresponding Resins, epoxy GE-100 of environment that is all the manufacturing of eastern electrician of day company, for with above-mentioned molding die (after 800 times) after similarly being shaped repeatedly, by using the contaminant removal of each die cleaning agent composition (mould cleaning material) of embodiment 1～9 product and comparative example 1～3 product with above-mentioned same method visual assessment.As a result, with above-mentioned same, the mould cleaning of comparative example product is evaluated as bad, and is relative therewith, and all the mould cleaning of embodiment product is evaluated as very.
(embodiment 10～18, comparative example 4 and 5)
Each composition shown in table 3 described later～table 4 is cooperated with the ratio shown in this table, use mixing roller that it is mixing.Then, use stack to be configured as sheet (thickness 5mm), make the sheet die cleaning agent composition (mould cleaning material) of target.
(embodiment 19)
To 100 parts of sprayings of crushed material of the Clean-thermoset melamine resin of commercially available mould (Japanese カ one バ ィ ト industrial system, ニ カ レ ッ ト ECR-T) 1 part of K as the clean-out system composition
3PO
44 parts of PEG and 1 part of water with as organic solvent adhere to it, obtain pulverous die cleaning agent composition (mould cleaning material) thus.
(comparative example 6) (※ is identical with aforementioned comparative example 3)
Use the tablet of the Clean-thermoset melamine resin of commercially available mould (Japanese カ one バ ィ ト industrial system, ニ カ レ ッ ト ECR-T), as the die cleaning agent composition (mould cleaning material) of drug sheet.
The embodiment product that use obtains like this and each die cleaning agent composition (mould cleaning material) of comparative example product, the removing property of the pollutent that forms on the following evaluation mould.Promptly, use is as corresponding Resins, epoxy (day eastern electrician's corporate system of environment of sealing material, GE-7470) be shaped repeatedly, in the surperficial contaminated molding die that carries out after 800 times, use above-mentioned each die cleaning agent composition (mould cleaning material) to clean shaping.In addition, will from mould, take out the removing property of the pollutent of visual assessment die surface by the shaping thing that cleaning forms.In this was estimated, the forming operation number of times that can remove pollutent fully was that the average evaluation below 3 times is good, and it is bad that removing of pollutent needed the average evaluation of the forming operation more than 4 times.
In addition, in the evaluation of embodiment 10～18 product and comparative example 4 and 5 product, flaky die cleaning agent composition (mould cleaning material) is clipped in the molding die, carries out heating in 5 minutes at 175 ℃ and be shaped.On the other hand, in the evaluation of embodiment 19 product, use pulverous die cleaning agent composition (mould cleaning material), in the evaluation of comparative example 6 product, use the die cleaning agent composition (mould cleaning material) of drug sheet, transmit shaping, carry out heating in 3 minutes at 175 ℃ and be shaped.
Above-mentioned evaluation result is shown in following table 3～table 4.
Table 3
(part)
The ※ cleaning is good, but because hydrous water not, therefore for composition evenly need be taken time slightly
Table 4
(part)
From The above results as can be seen, do not contain as an alkali metal salt of clean-out system composition and/or the comparative example product of alkali metal hydroxide, the cleaning of its mould is evaluated as bad, relative therewith, the mould cleaning that contains whole embodiment product of mother metal, an alkali metal salt and/or alkali metal hydroxide and organic solvent or organic solvent and water is evaluated as very.
The change of＜sealing material (1) 〉
In addition, will be as above-mentioned environment correspondence Resins, epoxy (day eastern electrician's corporate system of sealing material, GE-7470) change to the corresponding Resins, epoxy GE-1030 of environment that is all the manufacturing of eastern electrician of day company, for with above-mentioned molding die (after 800 times) after similarly being shaped repeatedly, by using the contaminant removal of each die cleaning agent composition (mould cleaning material) of embodiment 10～19 product and comparative example 4～6 product with above-mentioned same method visual assessment.As a result, with above-mentioned same, the mould cleaning of comparative example product is evaluated as bad, and is relative therewith, and all the mould cleaning of embodiment product is evaluated as very.
The change of＜sealing material (2) 〉
In addition, will be as above-mentioned environment correspondence Resins, epoxy (day eastern electrician's corporate system of sealing material, GE-7470) change to the corresponding Resins, epoxy GE-100 of environment that is all the manufacturing of eastern electrician of day company, for with above-mentioned molding die (after 800 times) after similarly being shaped repeatedly, by using the contaminant removal of each die cleaning agent composition (mould cleaning material) of embodiment 10～19 product and comparative example 4～6 product with above-mentioned same method visual assessment.As a result, with above-mentioned same, the mould cleaning of comparative example product is evaluated as bad, and is relative therewith, and all the mould cleaning of embodiment product is evaluated as very.
With reference to specific embodiment the present invention is had been described in detail, still, it is obvious to the skilled person that under the situation that does not break away from the spirit and scope of the present invention and can carry out various changes or correction.
The application is based on the Japanese patent application 2009-169331 of Japanese patent application 2009-169330 that proposed on July 17th, 2009 and proposition on July 17th, 2009, and the content of these two applications is incorporated this specification sheets as a reference into.
Die cleaning agent composition of the present invention, can be used for various shaping dies that the thermosetting resin shaped material uses etc., for example use epoxy resin molding material with semiconductor element by injection forming or transmit the cleaning and regeneration etc. of the molding die of use when carrying out resin-sealed the shaping repeatedly of being shaped.
Claims (10)
1. die cleaning agent composition, it carries out the cleansing composition of the hot briquetting of moulding repeatedly with mould for using formed material, wherein contains:
As the synthetic rubber and/or the synthetic resins of mother metal,
An alkali metal salt and/or alkali metal hydroxide and
Water and/or organic solvent.
2. die cleaning agent composition as claimed in claim 1, wherein,
Synthetic rubber is ethylene-propylene class rubber and/or divinyl rubber.
3. die cleaning agent composition as claimed in claim 1, wherein,
The content of an alkali metal salt and/or alkali metal hydroxide is 0.1～10 weight part with respect to synthetic rubber and/or synthetic resins 100 weight parts as mother metal.
4. die cleaning agent composition as claimed in claim 1, wherein,
The content of water is 3～30 weight parts with respect to synthetic rubber and/or synthetic resins 100 weight parts as mother metal.
5. die cleaning agent composition as claimed in claim 1, wherein,
Organic solvent is to be selected from least a in the group of being made up of polyalcohols and polyol alkyl ether class.
6. die cleaning agent composition as claimed in claim 1, wherein,
The content of organic solvent is 3～30 weight parts with respect to synthetic rubber and/or synthetic resins 100 weight parts as mother metal.
7. die cleaning agent composition as claimed in claim 5, wherein,
The content of organic solvent is 3～30 weight parts with respect to synthetic rubber and/or synthetic resins 100 weight parts as mother metal.
8. a mould cleaning material is configured as sheet by each described die cleaning agent composition in the use claim 1～7 and obtains.
9. mould cleaning method comprises following operation:
The mould cleaning material that will comprise each described die cleaning agent composition in the claim 1～7 is placed into the operation on the profile of mould of unlatching,
Close described mould and clip described mould cleaning material and carry out heating and pressurizing, make thus the pollutent that forms at die surface and the incorporate operation of described mould cleaning material and
By peel off cleaning mold surface from mould with the incorporate mould cleaning material of pollutent.
10. mould cleaning method as claimed in claim 9, wherein,
The mould cleaning material is the die cleaning agent composition to be formed sheet and the material that obtains.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2009169330A JP6116789B2 (en) | 2009-07-17 | 2009-07-17 | Semiconductor device molding die cleaning sheet and semiconductor device molding die cleaning method using the same |
| JP2009169331A JP5604822B2 (en) | 2009-07-17 | 2009-07-17 | Semiconductor device molding die cleaning composition, semiconductor device molding die cleaning material, and semiconductor device molding die cleaning method using the same |
| JP2009-169331 | 2009-07-17 | ||
| JP2009-169330 | 2009-07-17 |
Publications (2)
| Publication Number | Publication Date |
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| CN101955858A true CN101955858A (en) | 2011-01-26 |
| CN101955858B CN101955858B (en) | 2013-01-30 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010233007XA Active CN101955858B (en) | 2009-07-17 | 2010-07-16 | Mold cleaner composition and mold cleaning material, and method of cleaning using the same |
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| Country | Link |
|---|---|
| KR (2) | KR101788859B1 (en) |
| CN (1) | CN101955858B (en) |
| MY (1) | MY177272A (en) |
| SG (1) | SG168489A1 (en) |
| TW (1) | TWI499668B (en) |
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| CN103526214A (en) * | 2013-09-05 | 2014-01-22 | 汉中锌业有限责任公司 | Cleaning method of zinc ingot moulds in wet-process zinc smelting |
| CN104450302A (en) * | 2014-11-17 | 2015-03-25 | 厦门市钰林丰橡塑科技有限公司 | Flame-retardant high-temperature resistant environment-friendly cleaning product |
| KR20150115739A (en) * | 2013-01-31 | 2015-10-14 | 닛뽕 카바이도 고교 가부시키가이샤 | Resin composition for mold cleaning, and mold cleaning method |
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| TWI618611B (en) * | 2013-01-31 | 2018-03-21 | 日本電石工業股份有限公司 | Resin composition for mold cleaning and method of cleaning mold |
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| CN103526214A (en) * | 2013-09-05 | 2014-01-22 | 汉中锌业有限责任公司 | Cleaning method of zinc ingot moulds in wet-process zinc smelting |
| CN103526214B (en) * | 2013-09-05 | 2015-12-09 | 汉中锌业有限责任公司 | The method for cleaning of zinc ingot metal mould in a kind of zinc hydrometallurgy |
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| CN108431197A (en) * | 2016-08-25 | 2018-08-21 | 化研科技株式会社 | Cleansing composition and cleaning method |
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| CN112847973A (en) * | 2021-01-06 | 2021-05-28 | 珠海格力新元电子有限公司 | Mold cleaning method |
| CN114456884A (en) * | 2021-12-30 | 2022-05-10 | 安莱博医药(苏州)有限公司 | ICP component cleaning agent |
Also Published As
| Publication number | Publication date |
|---|---|
| MY177272A (en) | 2020-09-10 |
| CN101955858B (en) | 2013-01-30 |
| TW201107462A (en) | 2011-03-01 |
| KR101788859B1 (en) | 2017-10-20 |
| SG168489A1 (en) | 2011-02-28 |
| KR20110007983A (en) | 2011-01-25 |
| TWI499668B (en) | 2015-09-11 |
| KR20170091558A (en) | 2017-08-09 |
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