CN103045014B - Naturally dried photosensitive acid-corrosion-resistant electroplating printing ink and preparation method thereof - Google Patents
Naturally dried photosensitive acid-corrosion-resistant electroplating printing ink and preparation method thereof Download PDFInfo
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- CN103045014B CN103045014B CN201310031967.1A CN201310031967A CN103045014B CN 103045014 B CN103045014 B CN 103045014B CN 201310031967 A CN201310031967 A CN 201310031967A CN 103045014 B CN103045014 B CN 103045014B
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Abstract
The invention discloses a naturally dried photosensitive acid-corrosion-resistant electroplating printing ink and a preparation method thereof. The naturally dried photosensitive acid-corrosion-resistant electroplating printing ink comprises the following components in parts by weight: 50-80 parts of alkali soluble photosensitive resin, 0-5 parts of cellulose used for coating, 2-10 parts of active diluents, 2-8 parts of photosensitizer, 10-40 parts of filler, 0.5-1 part of pigment, 5-15 parts of solvent and 0.5-3 parts of auxiliaries, wherein the alkali soluble photosensitive resin is prepared from the following components in parts by weight: 40-60 parts of mixture consisting of 20-30 parts of n-butyl acetate, 0-30 parts of methyl isobutyl ketone, 0-20 parts of methylbenzene and 0-20 parts of propylene glycol monomethyl ether acetate, 25-40 parts of styrene-maleic anhydride resin, 15-20 parts of acrylic acid monomer, 0.1-1.0 part of catalyst and 0.1-1.0 part of polymerization inhibitor. The naturally dried photosensitive acid-corrosion-resistant electroplating printing ink disclosed by the invention does not need baking, is dried naturally after being diluted and is energy-saving and is resistant to acid and electroplating, and a film formed after the electroplating printing ink sprayed and dried naturally is high in adhesive force, high in hardness, quick in development, capable of obtaining clear images and resistant to acid corrosion.
Description
Technical field
Ink of the present invention, particularly from dry photosensitive Sprouting resistance resist ink.
The invention still further relates to the above-mentioned preparation method from dry photosensitive Sprouting resistance resist ink.
Background technology
Sensitive technologies is widely used in label, panel and decorative product graphic making now, and sensitive technologies is also applied to the processing of accurate hardware products in addition, can obtain accurate graph image.Metallic surface obtains precision profile, the method for image has multiple, such as, be the gelatine masking method, dry film method, wet film method etc. of photosensitizers with dichromate.Gelatine mask is a kind of serious source of pollution and carcinogens, very big to harm, does not substantially adopt now; Dry film technique does not reach requirement to precision graphic, image; Wet film technology is completely pollution-free, can obtain precision graphic, image technique.
At present, photosensitive-ink is toasted based on silk-screen type.The Application comparison of silk-screen type baking-type photosensitive-ink is ripe, has that sticking power is good, hardness is high, image definition is high.But silk-screen type baking-type ink needs baking, limits its use range, can not process, can not use some temperature-sensitive materials the graph image of some large complicated accurate zero devices.In addition, baking-type photosensitive-ink is due to needs roasting plant, and output investment ratio is larger; Also need to consume a large amount of energy, be unfavorable for resources conservation.
Summary of the invention
The present invention completes to solve deficiency of the prior art, the object of this invention is to provide do not need to toast, seasoning after dilution, energy-conservation, can the film adhesive that formed after dry of antiacid, anti-plate and spraying good, hardness is high, development is fast, clear picture, resistance to acid attack certainly do photosensitive Sprouting resistance resist ink.
Of the present invention from dry photosensitive Sprouting resistance resist ink, following component is comprised: the alkaline soluble photosensitive resin of 50-80 part according to parts by weight, the coating Mierocrystalline cellulose of 0-5 part, the reactive thinner of 2-10 part, the photosensitizers of 2-8 part, the filler of 10-40 part, the pigment of 0.5-1 part, the solvent of 5-15 part and the auxiliary agent of 0.5-3 part, wherein, described alkaline photosensitive resin is made up of following component according to parts by weight: according to parts by weight 40-60 part by 20-30 part N-BUTYL ACETATE, 0-30 part methyl iso-butyl ketone (MIBK), the mixture of 0-20 part toluene and 0-20 part 1-Methoxy-2-propyl acetate composition, 25-40 part phenylethylene-maleic anhydride resin, 15-20 part acrylic monomer, the catalyzer of 0.1-1.0 part and the stopper of 0.1-1.0 part.
Certainly dry photosensitive Sprouting resistance resist ink of the present invention can also be:
Described coating Mierocrystalline cellulose is at least one in cellulose acetate butyrate, cellulose acetate propionate, cellulose acetate, at least one in described reactive thinner tripropylene glycol diacrylate, 1,6 hexanediol diacrylate, Viscoat 295, ethoxyquin Viscoat 295, tetramethylol methane tetraacrylate.
Described photosensitizers is benzophenone, benzoin dimethylether, 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone, 2-isopropyl thioxanthone, at least one in 2-hydroxy-methyl phenyl-propane-1-ketone, described filler is talcum powder, calcium carbonate, barium sulfate, kaolin, glass powder, at least one in mica powder, described monastral blue is blue, phthalein is dark green, at least one in Pigment Yellow 73, described solvent is toluene, dimethylbenzene, 1-Methoxy-2-propyl acetate, Virahol, N-BUTYL ACETATE, vinyl acetic monomer, methyl iso-butyl ketone (MIBK), at least one in ethylene glycol monobutyl ether, described auxiliary agent is BYK-306, BYK-141, BYK-502, BYK333, moral modest 410, at least one in moral modest 835, described acrylic monomer comprises vinylformic acid, methacrylic acid, ethyl propenoate, at least one in Hydroxyethyl acrylate and Propylene glycol monoacrylate, described stopper is to tertiary butyl pyrocatechol, Tempol (free radical) or 4,6-dinitrobenzene-2-sec-butyl phenol, described catalyzer is tetraethylammonium bromide, Tetrabutyl amonium bromide, triphenyl phosphorus, trolamine, at least one in tetrabutyl tin.
Of the present invention from dry photosensitive Sprouting resistance resist ink, because it comprises following component according to parts by weight: the alkaline soluble photosensitive resin of 50-80 part, the coating Mierocrystalline cellulose of 0-5 part, the reactive thinner of 2-10 part, the photosensitizers of 2-8 part, the filler of 10-40 part, the pigment of 0.5-1 part, the solvent of 5-15 part and the auxiliary agent of 0.5-3 part, wherein, described alkaline photosensitive resin is made up of following component according to parts by weight: according to parts by weight 40-60 part by 20-30 part N-BUTYL ACETATE, 0-30 part methyl iso-butyl ketone (MIBK), the mixture of 0-20 part toluene and 0-20 part 1-Methoxy-2-propyl acetate composition, 25-40 part phenylethylene-maleic anhydride resin, 15-20 part acrylic monomer, the catalyzer of 0.1-1.0 part and the stopper of 0.1-1.0 part.Being from dry photosensitive Sprouting resistance resist ink advantage like this: 1) can seasoning, do not need baking, energy-conservation; 2) simple, antiacid, the anti-plate of production technique; 3) owing to adopting homemade alkaline soluble acrylic resin to be main binder, have that clear picture transparency is high, development is fast, sticking power is good, acidproof.This ink in use, spray on the metallic substance such as stainless steel, iron, aluminium after being diluted, under state of nature, dry 15-45 minute, namely forms film, and the sticking power of contact exposure, the rear film of exposure is good, hardness rank is F-2H, development is fast, clear picture, resistance to acid attack, anti-plate.Therefore, present invention process is simple, formula is reasonable, excellent property.Technical feature of the present invention and experimental data as follows: color is green or blue, and viscosity is 40-100PS (25 DEG C): time of drying: room temperature places 15-45 minute; Exposure energy: 80-200mj/cm; Levels of exposure: 7-9 level; Development: 1%Na
2cO
3the aqueous solution, 40-60s; Hardness:>=F; Sticking power: one-level.Compared with prior art, tool of the present invention has the following advantages:
(1) can from dry.By the present invention from dry photosensitive Sprouting resistance resist ink ink thinner open rare after be sprayed on the base materials such as stainless steel, naturally place 15-45 minute, surface can be reached and do solid work effect, the completely sticky film.
(2) development is fast, image definition is high.By the present invention after dry photosensitive Sprouting resistance resist ink spraying, after placing drying, expose under ultraviolet lamp, use 1%Na
2cO
3aqueous development 40-60s, photo-cured portion image is stayed on base material, and image definition is high.
(3) anti-etching.Of the present invention after dry photosensitive Sprouting resistance resist ink exposure imaging, after etching solution etching, image etches, and without stain, does not expand without burr, image.
(4) of the present invention also have easy construction, the advantage of fast drying, sticking power excellent (one-level), anti-plate from dry photosensitive Sprouting resistance resist ink.
Another object of the present invention is to provide above-mentionedly not to be needed to toast, seasoning after dilution, energy-conservation, can the film adhesive that formed after dry of antiacid, anti-plate and spraying good, hardness is high, development is fast, the preparation method certainly doing photosensitive Sprouting resistance resist ink of clear picture, resistance to acid attack.
Preparation method from dry photosensitive Sprouting resistance resist ink of the present invention, comprises the following steps:
A. starting material are prepared: the alkaline soluble photosensitive resin according to parts by weight being 50-80 part, the coating Mierocrystalline cellulose of 0-5 part, the reactive thinner of 2-10 part, the photosensitizers of 2-8 part, the filler of 10-40 part, the pigment of 0.5-1 part, the solvent of 5-15 part and the auxiliary agent of 0.5-3 part, wherein, described alkaline photosensitive resin is made up of following component according to weight ratio: according to parts by weight 40-60 part by 20-30 part N-BUTYL ACETATE, 0-30 part methyl iso-butyl ketone (MIBK), the mixture of 0-20 part toluene and 0-20 part 1-Methoxy-2-propyl acetate composition, 25-40 part phenylethylene-maleic anhydride resin, 15-20 part acrylic monomer, the catalyzer of 0.1-1.0 part and the stopper of 0.1-1.0 part,
B. alkaline soluble photosensitive resin is prepared: by the N-BUTYL ACETATE in steps A, methyl iso-butyl ketone (MIBK), toluene, 1-Methoxy-2-propyl acetate mixes, by parts by weight be 40-60 part by N-BUTYL ACETATE, methyl iso-butyl ketone (MIBK), the mixture of toluene and 1-Methoxy-2-propyl acetate mixing adds in reactor and is warming up to 85-95 DEG C, then 25-40 part phenylethylene-maleic anhydride resin agitating is added to phenylethylene-maleic anhydride resin dissolves, and then add by 15-20 part acrylic monomer in reactor, the mixture of the catalyzer of 0.1-1.0 part and the stopper composition of 0.1-1.0 part, reaction system is incubated 25-35 hour, then the temperature of mixture in reactor is reduced to less than 60 DEG C, obtains alkaline soluble photosensitive resin,
C. high speed dispersion stirs: add dispersion in high speed dispersor after the solvent of the alkaline soluble photosensitive resin obtained according to the step B of 50-80 part of weight ratio number, the coating Mierocrystalline cellulose of 0-5 part, the reactive thinner of 2-10 part, the photosensitizers of 2-8 part and 5-15 part and stir, and then add the filler of 10-40 part and the pigment of 0.5-1 part to telling that in dispersion machine, 20-30 minute is stirred in dispersion, then disperse to stir 3-7 minute in high speed dispersor at the auxiliary agent adding 0.5-3 part, obtain the work in-process disperseing to stir;
D. grind: the work in-process obtained in step C are ground in three-roller, be ground to the certainly dry photosensitive Sprouting resistance resist ink that namely fineness obtains lower than 15 μm.
Preparation method from dry photosensitive Sprouting resistance resist ink of the present invention, owing to adopting above-mentioned steps, advantage is compared to existing technology that synthetic operation technique is simple, the components such as caustic solubility bright resin, thinner, photosensitizers and color stuffing are only needed to weigh by weight percentage, on dispersion machine high speed dispersion evenly after, grind on three-roller, and solvent cut adjustment viscosity is namely obtained from dry photosensitive Sprouting resistance resist ink.And obtained do not need to toast from dry photosensitive Sprouting resistance resist ink, seasoning after dilution, energy-conservation, can the film adhesive that formed after dry of antiacid, anti-plate and spraying good, hardness is high, development is fast, clear picture, resistance to acid attack.
Embodiment
Be described in further detail from dry photosensitive Sprouting resistance resist ink and preparation method thereof of the present invention below.
Of the present invention from dry photosensitive Sprouting resistance resist ink, following component is comprised: the alkaline soluble photosensitive resin of 50-80 part according to parts by weight, the coating Mierocrystalline cellulose of 0-5 part, the reactive thinner of 2-10 part, the photosensitizers of 2-8 part, the filler of 10-40 part, the pigment of 0.5-1 part, the solvent of 5-15 part and the auxiliary agent of 0.5-3 part, wherein, described alkaline photosensitive resin is made up of following component according to parts by weight: according to parts by weight 40-60 part by 20-30 part N-BUTYL ACETATE, 0-30 part methyl iso-butyl ketone (MIBK), the mixture of 0-20 part toluene and 0-20 part 1-Methoxy-2-propyl acetate composition, 25-40 part phenylethylene-maleic anhydride resin, 15-20 part acrylic monomer, the catalyzer of 0.1-1.0 part and the stopper of 0.1-1.0 part.
Concrete analysis: photosensitizers plays curing inks, makes ink become hard solid-state coating from liquid state; Filler mainly works the physical and mechanical properties improving ink, as hardness, scratch resistance; Pigment gives ink certain color; Solvent plays dissolving resin, convenient construction, drying property; Auxiliary agent makes the easily disperse of ink, easy act, outward appearance good; The main synthetic resins use of acrylic monomer, makes that resin property is more outstanding, attachment is better, hardness is higher; Stopper prevents the gel of building-up process resin; Catalyzer accelerates resins synthesis speed, Reaction time shorten.
Being from dry photosensitive Sprouting resistance resist ink advantage like this: 1) can seasoning, do not need baking, energy-conservation; 2) simple, antiacid, the anti-plate of production technique; 3) owing to adopting homemade alkaline soluble acrylic resin to be main binder, have that clear picture transparency is high, development is fast, sticking power is good, acidproof.This ink in use, spray on the metallic substance such as stainless steel, iron, aluminium after being diluted, under state of nature, dry 15-45 minute, namely forms film, and the sticking power of contact exposure, the rear film of exposure is good, hardness rank is F-2H, development is fast, clear picture, resistance to acid attack, anti-plate.Therefore, present invention process is simple, formula is reasonable, excellent property.Technical feature of the present invention and experimental data as follows: color is green or blue, and viscosity is 40-100PS (25 DEG C): time of drying: room temperature places 15-45 minute; Exposure energy: 80-200mj/cm; Levels of exposure: 7-9 level; Development: 1%Na
2cO
3the aqueous solution, 40-60s; Hardness:>=F; Sticking power: one-level.Compared with prior art, tool of the present invention has the following advantages:
(1) can from dry.By the present invention from dry photosensitive Sprouting resistance resist ink ink thinner open rare after be sprayed on the base materials such as stainless steel, naturally place 15-45 minute, surface can be reached and do solid work effect, the completely sticky film.
(2) development is fast, image definition is high.By the present invention after dry photosensitive Sprouting resistance resist ink spraying, after placing drying, expose under ultraviolet lamp, use 1%Na
2cO
3aqueous development 40-60s, photo-cured portion image is stayed on base material, and image definition is high.
(3) anti-etching.Of the present invention after dry photosensitive Sprouting resistance resist ink exposure imaging, after etching solution etching, image etches, and without stain, does not expand without burr, image.
(4) of the present invention also have easy construction, the advantage of fast drying, sticking power excellent (one-level), anti-plate from dry photosensitive Sprouting resistance resist ink.
Of the present invention from dry photosensitive Sprouting resistance resist ink, can be specifically described coating Mierocrystalline cellulose be at least one in cellulose acetate butyrate, cellulose acetate propionate, cellulose acetate, at least one in described reactive thinner tripropylene glycol diacrylate, 1,6 hexanediol diacrylate, Viscoat 295, ethoxyquin Viscoat 295, tetramethylol methane tetraacrylate.
Described photosensitizers is benzophenone, benzoin dimethylether, 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone, 2-isopropyl thioxanthone, at least one in 2-hydroxy-methyl phenyl-propane-1-ketone, described filler is talcum powder, calcium carbonate, barium sulfate, kaolin, glass powder, at least one in mica powder, described monastral blue is blue, phthalein is dark green, at least one in Pigment Yellow 73, described solvent is toluene, dimethylbenzene, 1-Methoxy-2-propyl acetate, Virahol, N-BUTYL ACETATE, vinyl acetic monomer, methyl iso-butyl ketone (MIBK), at least one in ethylene glycol monobutyl ether, described auxiliary agent is BYK-306, BYK-141, BYK-502, BYK333, moral modest 410, at least one in moral modest 835, described acrylic monomer comprises vinylformic acid, methacrylic acid, ethyl propenoate, at least one in Hydroxyethyl acrylate and Propylene glycol monoacrylate, described stopper is to tertiary butyl pyrocatechol, Tempol (free radical) or 4,6-dinitrobenzene-2-sec-butyl phenol, described catalyzer is tetraethylammonium bromide, Tetrabutyl amonium bromide, triphenyl phosphorus, trolamine, at least one in tetrabutyl tin.Poly-agent prevents the gel of building-up process resin; Catalyzer accelerates resins synthesis speed, Reaction time shorten.
Preparation method from dry photosensitive Sprouting resistance resist ink of the present invention, comprises the following steps:
A. starting material are prepared: the alkaline soluble photosensitive resin according to parts by weight being 50-80 part, the coating Mierocrystalline cellulose of 0-5 part, the reactive thinner of 2-10 part, the photosensitizers of 2-8 part, the filler of 10-40 part, the pigment of 0.5-1 part, the solvent of 5-15 part and the auxiliary agent of 0.5-3 part, wherein, described alkaline photosensitive resin is made up of following component according to weight ratio: according to parts by weight 40-60 part by 20-30 part N-BUTYL ACETATE, 0-30 part methyl iso-butyl ketone (MIBK), the mixture of 0-20 part toluene and 0-20 part 1-Methoxy-2-propyl acetate composition, 25-40 part phenylethylene-maleic anhydride resin, 15-20 part acrylic monomer, the catalyzer of 0.1-1.0 part and the stopper of 0.1-1.0 part,
B. alkaline soluble photosensitive resin is prepared: by the N-BUTYL ACETATE in steps A, methyl iso-butyl ketone (MIBK), toluene, 1-Methoxy-2-propyl acetate mixes, by parts by weight be 40-60 part by N-BUTYL ACETATE, methyl iso-butyl ketone (MIBK), the mixture of toluene and 1-Methoxy-2-propyl acetate mixing adds in reactor and is warming up to 85-95 DEG C, then 25-40 part phenylethylene-maleic anhydride resin agitating is added to phenylethylene-maleic anhydride resin dissolves, and then add by 15-20 part acrylic monomer in reactor, the mixture of the catalyzer of 0.1-1.0 part and the stopper composition of 0.1-1.0 part, reaction system is incubated 25-35 hour, then the temperature of mixture in reactor is reduced to less than 60 DEG C, obtains alkaline soluble photosensitive resin,
C. high speed dispersion stirs: add dispersion in high speed dispersor after the solvent of the alkaline soluble photosensitive resin obtained according to the step B of 50-80 part of weight ratio number, the coating Mierocrystalline cellulose of 0-5 part, the reactive thinner of 2-10 part, the photosensitizers of 2-8 part and 5-15 part and stir, and then add the filler of 10-40 part and the pigment of 0.5-1 part to telling that in dispersion machine, 20-30 minute is stirred in dispersion, then disperse to stir 3-7 minute in high speed dispersor at the auxiliary agent adding 0.5-3 part, obtain the work in-process disperseing to stir;
D. grind: the work in-process obtained in step C are ground in three-roller, be ground to the certainly dry photosensitive Sprouting resistance resist ink that namely fineness obtains lower than 15 μm.
Preparation method from dry photosensitive Sprouting resistance resist ink of the present invention, owing to adopting above-mentioned steps, advantage is compared to existing technology that synthetic operation technique is simple, the components such as caustic solubility bright resin, thinner, photosensitizers and color stuffing are only needed to weigh by weight percentage, on dispersion machine high speed dispersion evenly after, grind on three-roller, and solvent cut adjustment viscosity is namely obtained from dry photosensitive Sprouting resistance resist ink.And obtained do not need to toast from dry photosensitive Sprouting resistance resist ink, seasoning after dilution, energy-conservation, can the film adhesive that formed after dry of antiacid, anti-plate and spraying good, hardness is high, development is fast, clear picture, resistance to acid attack.
Of the present invention from dry photosensitive Sprouting resistance resist ink, above all technical schemes basis on can also be that the auxiliary agent adding 0.5-3 part in described step C again disperses stirring 5 minutes in high speed dispersor.Such advantage is conducive to auxiliary agent to be better scattered in inside ink component, prevents dispersion inequality from causing product defects.
Can be specifically described coating Mierocrystalline cellulose be at least one in cellulose acetate butyrate, cellulose acetate propionate, cellulose acetate.Its advantage is that resistance to thick property is good, good leveling property, wettability that surface drying is good, good.At least one in described reactive thinner tripropylene glycol diacrylate, 1,6 hexanediol diacrylate, Viscoat 295, ethoxyquin Viscoat 295, tetramethylol methane tetraacrylate.Its advantage improves curing speed, hardness of paint film, chemical resistance.
Described photosensitizers is benzophenone, benzoin dimethylether, 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone, 2-isopropyl thioxanthone, at least one in 2-hydroxy-methyl phenyl-propane-1-ketone, described filler is talcum powder, calcium carbonate, barium sulfate, kaolin, glass powder, at least one in mica powder, described monastral blue is blue, phthalein is dark green, at least one in Pigment Yellow 73, described solvent is toluene, dimethylbenzene, 1-Methoxy-2-propyl acetate, Virahol, N-BUTYL ACETATE, vinyl acetic monomer, methyl iso-butyl ketone (MIBK), at least one in ethylene glycol monobutyl ether, described auxiliary agent is BYK-306, BYK-141, BYK-502, BYK333, moral modest 410, at least one in moral modest 835, described acrylic monomer comprises vinylformic acid, methacrylic acid, ethyl propenoate, at least one in Hydroxyethyl acrylate and Propylene glycol monoacrylate, described stopper is to tertiary butyl pyrocatechol, Tempol (free radical) or 4,6-dinitrobenzene-2-sec-butyl phenol, described catalyzer is tetraethylammonium bromide, Tetrabutyl amonium bromide, triphenyl phosphorus, trolamine, at least one in tetrabutyl tin.Reaction efficiency is high, speed is fast, coloured product is shallow.
Specific embodiment
Embodiment 1
20 parts by weight acetic acid butyl esters, 20 weight part methyl iso-butyl ketone (MIBK) are added in reactor and is warming up to 95 DEG C, add 40 parts by weight of styrene-maleic anhydride resin, add 15 parts by weight of acrylic acid hydroxyl ethyl esters, the p-ten.-butylcatechol constant temperature of the tetraethylammonium bromide of the Propylene glycol monoacrylate of 6 weight parts, 0.1 weight part, 1.0 weight parts 25 hours, subsequently the temperature of reaction system is dropped to less than 60 DEG C, obtain the alkaline soluble photosensitive resin of needs.According to weight fraction than the alkaline soluble photosensitive resin 50 parts taking aforementioned preparation, the cellulose acetate butyrate of 5 parts, the Viscoat 295 of 2 parts, the 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone, the talcum powder of 26 parts, the phthalocyanine blue of 0.5 part, the vinyl acetic monomer of 11.5 parts, the BYK306 of 3 parts of 2 parts.The aforementioned alkaline soluble photosensitive resin taken, Mierocrystalline cellulose, reactive thinner, filler, pigment are added dispersion in high speed dispersor and stirs, add again after stirring photosensitizers, auxiliary agent, solvent to high speed dispersor dispersion stirring within 20 minutes, obtain work in-process, work in-process three-roller grinds 2 times, until below fineness 15um, obtain of the present invention from dry photosensitive Sprouting resistance resist ink.Its performance test results is as follows:
Solid content (150 DEG C of constant temperature toast 30 minutes): 55%
Product viscosity (30 DEG C, rotational viscosimeter; ): 8500mps
Time of drying: room temperature places 30 minutes
Time shutter: 10s
Development time: 60s
The etch resistant time: 25 minutes
Sticking power: one-level
Hardness: F
Embodiment 2
Press weight proportion to take: in embodiment 1 preparation alkaline soluble photosensitive resin: 80 parts, the tetramethylol methane tetraacrylate of 2 parts, the benzophenone of 2 parts, 40 parts barium sulfate, 0.5 part phthalein viridescent, the toluene of 5 parts, the moral modest 410 of 1 part.The above-mentioned alkaline soluble photosensitive resin taken, reactive thinner, filler, pigment are added dispersion in high speed dispersor and stirs, add again after stirring photosensitizers, auxiliary agent, solvent to high speed dispersor dispersion stirring within 25 minutes, obtain work in-process, work in-process three-roller grinds 3 times, until below fineness 15um, obtain of the present invention from dry photosensitive Sprouting resistance resist ink.Its performance test results is as follows:
Solid content (150 DEG C of constant temperature toast 30 minutes): 50%
Product viscosity (30 DEG C, rotational viscosimeter; ): 7500mps
Time of drying: room temperature places 30 minutes
Time shutter: 10s
Development time: 40s
The etch resistant time: 25 minutes
Sticking power: one-level
Hardness: HB
Embodiment 3
Press weight proportion to take: the alkaline soluble photosensitive resin 65 parts of preparation in embodiment 1, the tripropylene glycol diacrylate of 3 parts, the 2-isopropyl thioxanthone of 3.5 parts, the talcum powder of 14 parts, 3 parts of kaolin, the phthalocyanine blue of 0.5 part, the N-BUTYL ACETATE of 10 parts, 5 parts of Virahols, the moral modest 410 of 1 part.The alkaline soluble photosensitive resin taken aforementioned, reactive thinner, filler, pigment add dispersion in high speed dispersor and stir, add again after stirring photosensitizers, auxiliary agent, solvent to high speed dispersor dispersion stirring within 30 minutes, obtain work in-process, work in-process three-roller grinds 2 times, until below fineness 15um, obtain of the present invention from dry photosensitive Sprouting resistance resist ink.Its performance test results is as follows:
Solid content (150 DEG C of constant temperature toast 30 minutes): 60%
Product viscosity (30 DEG C, rotational viscosimeter; ): 8500mps
Time of drying: room temperature places 30 minutes
Time shutter: 10s
Development time: 40s
The etch resistant time: 25 minutes
Sticking power: one-level
Hardness: F
Embodiment 4
The toluene of 30 parts by weight acetic acid butyl esters, 5 weight part methyl iso-butyl ketone (MIBK), 5 parts by weight of propylene glycol methyl ether acetates, 20 weight parts is added in reactor and is warming up to 85 DEG C, add 25 parts by weight of styrene-maleic anhydride resin, add 15 parts by weight of acrylic acid hydroxypropyl acrylates, the triphenyl phosphorus of 1.0 weight parts, 4 of 0.1 weight part, 6-dinitrobenzene-2-sec-butyl phenol constant temperature 35 hours, subsequently the temperature of reaction system is dropped to less than 60 DEG C, obtain alkaline soluble photosensitive resin.
Press weight proportion to take: the alkaline soluble photosensitive resin of the aforementioned preparation of the present embodiment 65 parts, the tripropylene glycol diacrylate of 10 parts, the 2-methyl isophthalic acid of 8 parts-(4-methylthio group phenyl)-2-morpholinyl-1-acetone, 25 parts talcum powder, 0.5 part phthalein viridescent, the dimethylbenzene of 5.5 parts, the BYK306 of 1 part.The alkaline soluble photosensitive resin taken above by the present embodiment, reactive thinner, filler, pigment add dispersion in high speed dispersor and stir, add again after stirring photosensitizers, auxiliary agent, solvent to high speed dispersor dispersion stirring within 20 minutes, obtain work in-process, work in-process three-roller grinds 3 times, until below fineness 15um, obtain of the present invention from dry photosensitive Sprouting resistance resist ink.Its performance test results is as follows:
Solid content (150 DEG C of constant temperature toast 30 minutes): 50%
Product viscosity (30 DEG C, rotational viscosimeter; ): 8000mps
Time of drying: room temperature places 30 minutes
Time shutter: 10s
Development time: 40s
The etch resistant time: 25 minutes
Sticking power: one-level
Hardness: HB
Embodiment 5
Press weight proportion to take: the alkaline soluble photosensitive resin 50 parts of preparation in embodiment 4, the Viscoat 295 of 2 parts, the benzophenone of 2.0 parts, the talcum powder of 25 parts, 10 parts of barium sulfate, 30 parts of kaolin, 0.5 part phthalein viridescent, the toluene of 5 parts, the moral modest 410 of 0.5 part.The alkaline soluble photosensitive resin taken aforementioned, reactive thinner, filler, pigment add dispersion in high speed dispersor and stir, add again after stirring photosensitizers, auxiliary agent, solvent to high speed dispersor dispersion stirring within 20 minutes, obtain work in-process, work in-process three-roller grinds 3 times, until below fineness 15um, obtain of the present invention from dry photosensitive Sprouting resistance resist ink.Its performance test results is as follows:
Solid content (150 DEG C of constant temperature toast 30 minutes): 61%
Product viscosity (30 DEG C, rotational viscosimeter; ): 8500mps
Time of drying: room temperature places 30 minutes
Time shutter: 10s
Development time: 40s
The etch resistant time: 25 minutes
Sticking power: one-level
Hardness: F
Embodiment 6
Press weight proportion to take: in embodiment 4 preparation alkaline soluble photosensitive resin 65 parts, the tetramethylol methane tetraacrylate of 2 parts, the 2-methyl isophthalic acid of 2 parts-(4-methylthio group phenyl)-2-morpholinyl-1-acetone, 22 parts talcum powder, 1.0 parts phthalein viridescent, the 1-Methoxy-2-propyl acetate of 5 parts, the BYK306 of 3 parts.The alkaline soluble photosensitive resin taken, reactive thinner, filler, pigment add dispersion in high speed dispersor and stir, add again after stirring photosensitizers, auxiliary agent, solvent to high speed dispersor dispersion stirring within 20 minutes, obtain work in-process, work in-process three-roller grinds 3 times, until below fineness 15um, obtain of the present invention from dry photosensitive Sprouting resistance resist ink.Its performance test results is as follows:
Solid content (150 DEG C of constant temperature toast 30 minutes): 58%
Product viscosity (30 DEG C, rotational viscosimeter; ): 8300mps
Time of drying: room temperature places 30 minutes
Time shutter: 10s
Development time: 40s
The etch resistant time: 25 minutes
Sticking power: one-level
Hardness: F
Can draw from the result of above-described embodiment and performance test thereof, what said ratio and aforesaid method obtained not need to toast from dry photosensitive Sprouting resistance resist ink, seasoning after dilution, energy-conservation, can the film adhesive that formed after dry of antiacid, anti-plate and spraying good, hardness is high, development is fast, clear picture, resistance to acid attack.
Above-mentionedly only several specific embodiments in the present invention to be illustrated; but can not as protection scope of the present invention; every according to the change of the equivalence done by design spirit in the present invention or to modify or equal proportion zooms in or out, all should think and fall into protection scope of the present invention.
Claims (7)
1. from dry photosensitive Sprouting resistance resist ink, it is characterized in that: comprise following component according to parts by weight: the alkaline soluble photosensitive resin of 50-80 part, the coating Mierocrystalline cellulose of 0-5 part, the reactive thinner of 2-10 part, the photosensitizers of 2-8 part, the filler of 10-40 part, the pigment of 0.5-1 part, the solvent of 5-15 part and the auxiliary agent of 0.5-3 part, wherein, described alkaline soluble photosensitive resin is made up of following component according to parts by weight: according to parts by weight 40-60 part by 20-30 part N-BUTYL ACETATE, 0-30 part methyl iso-butyl ketone (MIBK), the mixture of 0-20 part toluene and 0-20 part 1-Methoxy-2-propyl acetate composition, 25-40 part phenylethylene-maleic anhydride resin, 15-20 part acrylic monomer, the catalyzer of 0.1-1.0 part and the stopper of 0.1-1.0 part, described reactive thinner is at least one in tripropylene glycol diacrylate, 1,6 hexanediol diacrylate, Viscoat 295, ethoxyquin Viscoat 295, tetramethylol methane tetraacrylate.
2. according to claim 1 from dry photosensitive Sprouting resistance resist ink, it is characterized in that: described coating Mierocrystalline cellulose is at least one in cellulose acetate butyrate, cellulose acetate propionate, cellulose acetate.
3. according to claim 1 from dry photosensitive Sprouting resistance resist ink, it is characterized in that: described photosensitizers is benzophenone, benzoin dimethylether, 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone, 2-isopropyl thioxanthone, at least one in 2-hydroxy-methyl phenyl-propane-1-ketone, described filler is talcum powder, calcium carbonate, barium sulfate, kaolin, glass powder, at least one in mica powder, described monastral blue is blue, phthalein is dark green, at least one in Pigment Yellow 73, described solvent is toluene, dimethylbenzene, 1-Methoxy-2-propyl acetate, Virahol, N-BUTYL ACETATE, vinyl acetic monomer, methyl iso-butyl ketone (MIBK), at least one in ethylene glycol monobutyl ether, described auxiliary agent is BYK-306, BYK-141, BYK-502, BYK333, moral modest 410, at least one in moral modest 835, described acrylic monomer comprises vinylformic acid, methacrylic acid, ethyl propenoate, at least one in Hydroxyethyl acrylate and Propylene glycol monoacrylate, described stopper is to tertiary butyl pyrocatechol, Tempol (free radical) or 4,6-dinitrobenzene-2-sec-butyl phenol, described catalyzer is tetraethylammonium bromide, Tetrabutyl amonium bromide, triphenyl phosphorus, trolamine, at least one in tetrabutyl tin.
4. the preparation method from dry photosensitive Sprouting resistance resist ink according to claim 1, is characterized in that: comprise the following steps:
A. prepare starting material: according to parts by weight be the alkaline soluble photosensitive resin of 50-80 part, 0-5 part coating Mierocrystalline cellulose,
The auxiliary agent of the filler of the reactive thinner of 2-10 part, the photosensitizers of 2-8 part, 10-40 part, the pigment of 0.5-1 part, the solvent of 5-15 part and 0.5-3 part, wherein, described alkaline soluble photosensitive resin is made up of following component according to weight ratio: the mixture be made up of 20-30 part N-BUTYL ACETATE, 0-30 part methyl iso-butyl ketone (MIBK), 0-20 part toluene and 0-20 part 1-Methoxy-2-propyl acetate according to parts by weight 40-60 part, 25-40 part phenylethylene-maleic anhydride resin, 15-20 part acrylic monomer, the catalyzer of 0.1-1.0 part and the stopper of 0.1-1.0 part;
B. alkaline soluble photosensitive resin is prepared: by the N-BUTYL ACETATE in steps A, methyl iso-butyl ketone (MIBK), toluene, 1-Methoxy-2-propyl acetate mixes, by parts by weight be 40-60 part by N-BUTYL ACETATE, methyl iso-butyl ketone (MIBK), the mixture of toluene and 1-Methoxy-2-propyl acetate mixing adds in reactor and is warming up to 85-95 DEG C, then 25-40 part phenylethylene-maleic anhydride resin agitating is added to phenylethylene-maleic anhydride resin dissolves, and then add by 15-20 part acrylic monomer in reactor, the mixture of the catalyzer of 0.1-1.0 part and the stopper composition of 0.1-1.0 part, reaction system is incubated 25-35 hour, then the temperature of mixture in reactor is reduced to less than 60 DEG C, obtains alkaline soluble photosensitive resin,
C. high speed dispersion stirs: add dispersion in high speed dispersor after the solvent of the alkaline soluble photosensitive resin obtained according to the step B of 50-80 part of weight ratio number, the coating Mierocrystalline cellulose of 0-5 part, the reactive thinner of 2-10 part, the photosensitizers of 2-8 part and 5-15 part and stir, and then 10-40 adds the filler of 10-40 part and the pigment of 0.5-1 part disperses to stir 20-30 minute to telling in dispersion machine, then disperse to stir 3-7 minute in high speed dispersor at the auxiliary agent adding 0.5-3 part, obtain the work in-process disperseing to stir;
D. grind: the work in-process obtained in step C are ground in three-roller, be ground to the certainly dry photosensitive Sprouting resistance resist ink that namely fineness obtains lower than 15 μm.
5. the preparation method from dry photosensitive Sprouting resistance resist ink according to claim 4, is characterized in that: the auxiliary agent adding 0.5-3 part in described step C again disperses stirring 5 minutes in high speed dispersor.
6. the preparation method from dry photosensitive Sprouting resistance resist ink according to claim 4, it is characterized in that: described coating Mierocrystalline cellulose is at least one in cellulose acetate butyrate, cellulose acetate propionate, cellulose acetate, at least one in described reactive thinner tripropylene glycol diacrylate, 1,6 hexanediol diacrylate, Viscoat 295, ethoxyquin Viscoat 295, tetramethylol methane tetraacrylate.
7. the preparation method from dry photosensitive Sprouting resistance resist ink according to claim 4, is characterized in that: described photosensitizers is benzophenone, benzoin dimethylether, 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone, 2-isopropyl thioxanthone, at least one in 2-hydroxy-methyl phenyl-propane-1-ketone, described filler is talcum powder, calcium carbonate, barium sulfate, kaolin, glass powder, at least one in mica powder, described monastral blue is blue, phthalein is dark green, at least one in Pigment Yellow 73, described solvent is toluene, dimethylbenzene, 1-Methoxy-2-propyl acetate, Virahol, N-BUTYL ACETATE, vinyl acetic monomer, methyl iso-butyl ketone (MIBK), at least one in ethylene glycol monobutyl ether, described auxiliary agent is BYK-306, BYK-141, BYK-502, BYK333, moral modest 410, at least one in moral modest 835, described acrylic monomer comprises vinylformic acid, methacrylic acid, ethyl propenoate, at least one in Hydroxyethyl acrylate and Propylene glycol monoacrylate, described stopper is to tertiary butyl pyrocatechol, Tempol (free radical) or 4,6-dinitrobenzene-2-sec-butyl phenol, described catalyzer is tetraethylammonium bromide, Tetrabutyl amonium bromide, triphenyl phosphorus, trolamine, at least one in tetrabutyl tin.
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| CN106031306B (en) * | 2014-02-18 | 2018-05-22 | 旭硝子株式会社 | Negative light-sensitive resin combination, resin cured film, partition wall and optical element |
| CN105884949A (en) * | 2014-12-02 | 2016-08-24 | 苏州瑞红电子化学品有限公司 | Photoresist composition with branched photosensitive polystyrene-maleic anhydride as matrix resin |
| CN104877448A (en) * | 2015-06-03 | 2015-09-02 | 王金海 | Light sensitive solder resist ink and preparation method thereof |
| CN105330807B (en) * | 2015-11-25 | 2017-11-07 | 山东一诺威新材料有限公司 | The synthetic method of liquid photoresist maleic anhydride of styrene modified resin |
| CN106280688B (en) * | 2016-08-08 | 2020-11-03 | 惠州市至上新材料有限公司 | Alkali-soluble UV coating for cutting 3C product glass screen and preparation method thereof |
| CN108003704B (en) * | 2017-12-25 | 2020-11-10 | 广东三求光固材料股份有限公司 | Photo-induced electroplating-resistant ink and preparation method thereof |
| CN111863308A (en) * | 2019-04-30 | 2020-10-30 | 北京梦之墨科技有限公司 | Colored conductive paste, preparation method thereof and electronic device |
| CN115185160B (en) * | 2022-09-09 | 2023-06-27 | 之江实验室 | Laser direct-writing photoresist composition based on cellulose derivative and patterning method |
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| CN1249826A (en) * | 1997-06-02 | 2000-04-05 | 西巴特殊化学品控股有限公司 | Liquid photosensitive composition |
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