CN105400281A - Water-based UV conductive ink and preparation method thereof - Google Patents
Water-based UV conductive ink and preparation method thereof Download PDFInfo
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- CN105400281A CN105400281A CN201510790311.7A CN201510790311A CN105400281A CN 105400281 A CN105400281 A CN 105400281A CN 201510790311 A CN201510790311 A CN 201510790311A CN 105400281 A CN105400281 A CN 105400281A
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- water
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- conductive ink
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 37
- 229920001940 conductive polymer Polymers 0.000 claims abstract description 27
- 238000007639 printing Methods 0.000 claims abstract description 25
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052802 copper Inorganic materials 0.000 claims abstract description 20
- 239000010949 copper Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 12
- 239000013530 defoamer Substances 0.000 claims description 34
- 239000007864 aqueous solution Substances 0.000 claims description 24
- 239000000049 pigment Substances 0.000 claims description 18
- 239000002105 nanoparticle Substances 0.000 claims description 17
- 239000000758 substrate Substances 0.000 claims description 17
- GKWLILHTTGWKLQ-UHFFFAOYSA-N 2,3-dihydrothieno[3,4-b][1,4]dioxine Chemical compound O1CCOC2=CSC=C21 GKWLILHTTGWKLQ-UHFFFAOYSA-N 0.000 claims description 16
- 238000010907 mechanical stirring Methods 0.000 claims description 14
- 239000007921 spray Substances 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000011152 fibreglass Substances 0.000 claims description 12
- 238000007254 oxidation reaction Methods 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 9
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 8
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 8
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 8
- 101000927799 Homo sapiens Rho guanine nucleotide exchange factor 6 Proteins 0.000 claims description 7
- 102100033202 Rho guanine nucleotide exchange factor 6 Human genes 0.000 claims description 7
- YZQBYALVHAANGI-UHFFFAOYSA-N magnesium;dihypochlorite Chemical compound [Mg+2].Cl[O-].Cl[O-] YZQBYALVHAANGI-UHFFFAOYSA-N 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 229920002401 polyacrylamide Polymers 0.000 claims description 7
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 7
- QUAMTGJKVDWJEQ-UHFFFAOYSA-N octabenzone Chemical compound OC1=CC(OCCCCCCCC)=CC=C1C(=O)C1=CC=CC=C1 QUAMTGJKVDWJEQ-UHFFFAOYSA-N 0.000 claims description 6
- SATVIFGJTRRDQU-UHFFFAOYSA-N potassium hypochlorite Chemical compound [K+].Cl[O-] SATVIFGJTRRDQU-UHFFFAOYSA-N 0.000 claims description 6
- CNHDIAIOKMXOLK-UHFFFAOYSA-N toluquinol Chemical compound CC1=CC(O)=CC=C1O CNHDIAIOKMXOLK-UHFFFAOYSA-N 0.000 claims description 6
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 5
- 239000011231 conductive filler Substances 0.000 claims description 5
- 239000000178 monomer Substances 0.000 claims description 5
- 239000002383 tung oil Substances 0.000 claims description 5
- BBCLXYJRPRRZQW-UHFFFAOYSA-N 2-phenylnaphthalen-1-amine Chemical class C1=CC2=CC=CC=C2C(N)=C1C1=CC=CC=C1 BBCLXYJRPRRZQW-UHFFFAOYSA-N 0.000 claims description 4
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims description 4
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 4
- XJWSAJYUBXQQDR-UHFFFAOYSA-M dodecyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)C XJWSAJYUBXQQDR-UHFFFAOYSA-M 0.000 claims description 4
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- 229950000688 phenothiazine Drugs 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- WJFKNYWRSNBZNX-UHFFFAOYSA-N 10H-phenothiazine Chemical compound C1=CC=C2NC3=CC=CC=C3SC2=C1 WJFKNYWRSNBZNX-UHFFFAOYSA-N 0.000 claims description 3
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229950002083 octabenzone Drugs 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 abstract 2
- 239000002518 antifoaming agent Substances 0.000 abstract 1
- 239000003112 inhibitor Substances 0.000 abstract 1
- 239000007800 oxidant agent Substances 0.000 abstract 1
- 239000003381 stabilizer Substances 0.000 abstract 1
- 229920000642 polymer Polymers 0.000 description 14
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 9
- 239000012752 auxiliary agent Substances 0.000 description 9
- UMHFSEWKWORSLP-UHFFFAOYSA-N thiophene 1,1-dioxide Chemical compound O=S1(=O)C=CC=C1 UMHFSEWKWORSLP-UHFFFAOYSA-N 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 6
- 230000007547 defect Effects 0.000 description 6
- 239000010408 film Substances 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- -1 thiophene-1-oxide compound Chemical class 0.000 description 6
- 244000309464 bull Species 0.000 description 5
- 239000000975 dye Substances 0.000 description 5
- 238000003760 magnetic stirring Methods 0.000 description 5
- 229910052709 silver Inorganic materials 0.000 description 5
- 239000004332 silver Substances 0.000 description 5
- 108010053823 Rho Guanine Nucleotide Exchange Factors Proteins 0.000 description 4
- 102000016941 Rho Guanine Nucleotide Exchange Factors Human genes 0.000 description 4
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000004020 conductor Substances 0.000 description 3
- 238000001723 curing Methods 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000007806 chemical reaction intermediate Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000007344 nucleophilic reaction Methods 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 229930192474 thiophene Natural products 0.000 description 2
- YMMGRPLNZPTZBS-UHFFFAOYSA-N 2,3-dihydrothieno[2,3-b][1,4]dioxine Chemical compound O1CCOC2=C1C=CS2 YMMGRPLNZPTZBS-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 241000675108 Citrus tangerina Species 0.000 description 1
- 238000003848 UV Light-Curing Methods 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000012764 mineral filler Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 125000001484 phenothiazinyl group Chemical group C1(=CC=CC=2SC3=CC=CC=C3NC12)* 0.000 description 1
- 229920000867 polyelectrolyte Polymers 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
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- 229920003169 water-soluble polymer Polymers 0.000 description 1
Abstract
The invention discloses water-based UV conductive ink and a preparation method thereof. By adopting the total weight of the conductive ink as a benchmark, the water-based UV conductive ink consists of the following components by weight percent: 40 to 60 percent of conductive polymer PEDOT, 10 to 30 percent of deionized water, 1 to 8 percent of oxidizing agent, 10 to 20 percent of nano copper powder, 0.2 to 1.2 percent of stabilizer, 2 to 5 percent of binding agent, 1 to 6 percent of flatting agent, 0.2 to 1.2 percent of defoaming agent, 0.2 to 2 percent of polymerization inhibitor and 10 to 30 percent of solvent. By adopting the technical scheme, the conductive ink is prepared by adopting the conductive polymer PEDOT and nano copper which are relatively low in price, so that the cost is greatly reduced, the operation is simple, and the industrialized production is liable to realize; meanwhile, by adopting the technical scheme, the ink is not required to be sintered at a high temperature during the printing process, so that not only is the process simplified, but also the stability and consistency of the conductive ink are improved.
Description
Technical field
The invention belongs to macromolecule conducting material field, particularly relate to a kind of water-based UV electrically conductive ink and preparation method thereof.
Background technology
Water-based UV (ultraviolet light polymerization) electrically conductive ink is a kind of novel ink of development in recent years, water-based UV ink setting speed is fast, environmental pollution is low, energy consumption is few, become the universally recognized novel ink kind of current ink industry, be mainly used in radio frequency identification (RFID), printed circuit board (PCB), electrical screen indicating meter, sensor, Electronic Paper, the field such as solar cell and thin film switch, water-based UV electrically conductive ink represents film printing electronic material, the developing direction of even whole printed electronic industry, be expected to become the following cutting edge technology changing human life style.Be applied to the electrically conductive ink mainly filled-type electrically conductive ink of printed electronics industry at present, conductive filler material used mostly is mineral filler, as gold and silver, copper, nickel, carbon black, graphite, carbon fiber etc., wherein, argent is with good electroconductibility, stability and being most widely used.Water-based UV electrically conductive ink take water borne UV curing resin as binder, and interpolation nano-silver powder is filler, and is aided with other compositions and is prepared from.Its print principle is with being printed on the base materials such as above-mentioned printed circuit board by silver system electrically conductive ink, to be first positioned in baking oven dry, with after through uv curing machine solidification, it is sintered at about 150 DEG C ~ 350 DEG C, to be cooled to normal temperature.After sintering, the specific conductivity of silver conductive layer can reach 2.4 × 10-5 Ω cm, surface resistivity can reach 0.1 Ω/, and (is square resistance typography, refer to the resistance between a foursquare thin film of conductive material limit to limit, the characteristic of square resistance be arbitrary size square to while resistance be all the same, only relevant with factors such as the thickness of conducting film) below, the application demand of the aspect such as RFID antenna and PCB can be met completely.
But following reason constrains the industrial applications of water-based UV electrically conductive ink: chemical reaction can occur in (1) printing process, and the temperature of sintering is high.ShlomoMagdassi etc. as American Chemical Society points out in paper " Triggeringthesinteringofsilvernanoparticlesatroomtempera ture ", after nano-Ag particles contacts with reverse charging polyelectrolyte, the spontaneous formation melts combine of meeting, thus realize the normal temperature sintering of electrically conductive ink, but experimental assembly is comparatively complicated.(2) silver is the metal that under normal temperature, electroconductibility is best, but nano-silver powder expensive be the major cause of restriction water-based UV electrically conductive ink industrialization widespread use.The novel aqueous UV electrically conductive ink that research can solve the problem, is the study hotspot of domestic and international printing-ink industry, therefore has very important realistic meaning to the research and development of water-based UV electrically conductive ink.
Therefore, for the above-mentioned defect existed in currently available technology, be necessary to study in fact, to provide a kind of scheme, solve the defect existed in prior art.
Summary of the invention
In view of this, necessaryly provide a kind of water-based UV electrically conductive ink and preparation method thereof.
In order to overcome the defect that prior art exists, the invention provides following technical scheme:
A kind of water-based UV electrically conductive ink, with the gross weight of this electrically conductive ink for benchmark, is made up of the component of following mass percentage:
Conductive polymers PEDOT (poly-3,4-ethylene dioxythiophene): 40 ~ 60%; Described PEDOT is the polymkeric substance of EDOT (3,4-ethylene dioxythiophene monomer);
Deionized water: 10 ~ 30%;
Oxygenant: 1 ~ 8%; Described oxygenant is one or more in Losantin, magnesium hypochlorite, clorox or potassium hypochlorite;
Solvent, 10 ~ 30%; Described solvent be in butyl, tung oil or n-propyl alcohol one or more;
Copper nanoparticle conductive filler material, 10 ~ 20%;
Stablizer: 0.2 ~ 1.2%; Described stablizer be in cetyl trimethylammonium bromide, Octabenzone, Trimethyllaurylammonium bromide or polyvinylpyrrolidone one or more;
Tackiness agent: 2 ~ 5%; Described tackiness agent be in 2,2-dimethylol propionic acid, dimethylolpropionic acid or polyacrylamide one or more;
Flow agent: 1 ~ 6%; Described flow agent is one or more in TEGOGlide100, pure acrylic acid flow agent, oxyethane or propylene oxide;
Defoamer: 0.2 ~ 1.2%; Described defoamer is one or more in defoamer 6800, defoamer 810, defoamer D105, defoamer T-20GA or defoamer DF-100;
Stopper: 0.2 ~ 2%; Described stopper be in Resorcinol, phenothiazine, beta-phenyl naphthylamines, toluhydroquinone THQ or methylene blue one or more.
Preferably, there is oxidizing reaction in deionized water and form the conductive polymers aqueous solution in described conductive polymers PEDOT and described oxygenant.
Preferably, described oxygenant is Losantin (Ca (ClO)
2), the oxidation reaction process of described conductive polymers PEDOT and described Losantin is as follows:
Preferably, the particle diameter of described copper nanoparticle is less than 50nm, and purity is greater than 99.9%.
Preferably, the pigment that mass percentage is 5 ~ 10% is also comprised.
In order to overcome the defect of prior art, the invention also discloses a kind of preparation method of water-based UV electrically conductive ink, comprising the following steps:
Step S1: prepare the conductive polymers PEDOT aqueous solution;
Step S2: be the copper nanoparticle of 10 ~ 20% by mass ratio, the conductive polymers PEDOT aqueous solution Homogeneous phase mixing prepared of the stablizer of 0.2 ~ 1.2%, tackiness agent, the flow agent of 1 ~ 6%, defoamer, the stopper of 0.2 ~ 2%, the solvent of 10 ~ 30% and the step S1 of 0.2 ~ 1.2% of 2 ~ 5%, be heated to 65 ~ 80 DEG C of Keep agitation 1 hour, then cool 2 hours at normal temperatures, obtain ink mixture;
Step S3: the ink mixture obtained in step S2 is printed in the mode of spray ink Printing after the substrate being preheated to 60 ~ 95 DEG C forms ink pattern and this substrate is put into hot air drier 30 minutes drying and mouldings;
Step S4: ultraviolet light polymerization is carried out to the ink pattern on substrate.
Preferably, described step S1 is further comprising the steps:
The PEDOT of weight percent 40 ~ 60% is placed in the round-bottomed flask of 1000ml, add the deionized water of weight 10 ~ 30%, mechanical stirring is carried out 10 minutes with the speed of 400r/min, pour 1 ~ 8% oxygenant again into, described oxygenant is one or more in Losantin, magnesium hypochlorite, clorox or potassium hypochlorite;
Round-bottomed flask heated and keeps between 50 ~ 80 DEG C, carrying out mechanical stirring 50 minutes with the speed of 800r/min, and then cooling 1 hour under normal temperature, forming the conductive polymers PEDOT aqueous solution.
Preferably, described oxygenant is Losantin (Ca (ClO)
2) time, in described step S1, the oxidation reaction process of described PEDOT and described Losantin is as follows:
Preferably, also comprise the step adding pigment in described step S2, the mass percent of described pigment is 5 ~ 10%.
Preferably, in described step S3, the PET plate after fiberglass reinforced selected by described substrate.
Compared with prior art, due to technical scheme of the present invention, adopt the high conductive polymers PEDOT of relative low price, specific storage and Nanometer Copper to prepare electrically conductive ink, compared to existing technology, adopt nano-Ag particles, greatly reduce cost and simple to operate, be easy to realize suitability for industrialized production; Technical scheme of the present invention in printing process without the need to carrying out high temperature sintering to ink, only the substrate preparing printing need be preheated to 60 ~ 95 DEG C, the water-based UV electrically conductive ink adopting the mode of spray ink Printing the present invention to be prepared again adopts the mode of spray ink Printing to be printed in preheated substrate, preheated substrate can accelerate ink at substrate printing shaping, finally that substrate drying is shaping and ultraviolet light polymerization.Therefore invention not only simplifies stability and consistence that technique improves electrically conductive ink simultaneously.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of its preparation method of a kind of water-based UV electrically conductive ink of the present invention.
Fig. 2 is the SEM photo of the water-based UV electrically conductive ink of the embodiment of the present invention 1.
Fig. 3 is the SEM photo of the water-based UV electrically conductive ink of the embodiment of the present invention 2.
Fig. 4 is the SEM photo of the water-based UV electrically conductive ink of the embodiment of the present invention 3.
Fig. 5 is the SEM photo of the water-based UV electrically conductive ink of the embodiment of the present invention 4.
Following specific embodiment will further illustrate the present invention in conjunction with above-mentioned accompanying drawing.
Embodiment
Below with reference to accompanying drawing, the invention will be further described.
In prior art, its print principle is with being printed on the base materials such as printed circuit board by silver system electrically conductive ink, to be first positioned in baking oven dry, with after through uv curing machine solidification, it is sintered at about 150 DEG C ~ 350 DEG C, to be cooled to normal temperature.The expensive industrial applications greatly constraining electrically conductive ink of nano-silver powder; High temperature sintering can introduce uncertain chemical reaction simultaneously, thus cannot ensure stability and the consistence of electrically conductive ink, makes it add uncertainty in actual applications.
In order to overcome the defect of prior art, the present invention proposes that a kind of cost is low, the simple and water-based UV electrically conductive ink of excellent property of technique, with the gross weight of this ink for benchmark, its component primarily of following percentage composition forms:
The conductive polymers of 40 ~ 60%, the deionized water of 10 ~ 30%, 1 ~ 8% oxygenant, 10 ~ 20% conductive filler material, 0.2 ~ 1.2% stablizer, 2 ~ 5% tackiness agent, 1 ~ 6% flow agent, the defoamer of 0.2 ~ 1.2%, the stopper of 0.2 ~ 2% and 10 ~ 30% solvent, wherein, conductive polymers is the PEDOT (poly-3 of 40 ~ 60%, 4-ethylenedioxy thiophene), the feature that relative low price, specific storage are high.Conductive polymers is the key determining water-based UV electrically conductive ink performance.Conductive polymers PEDOT is the polymkeric substance of EDOT (3,4-ethylene dioxythiophene monomer), has special electricity, optical property, the features such as its molecular structure is simple, energy gap is little, specific conductivity high (600S/cm).
Because PEDOT is originally as insoluble polymer, the conductivity that can not directly utilize it special.But find in test, add after oxygenant carries out oxidizing reaction and PEDOT can be made to form water-soluble polymers, and there is high conductivity.Oxygenant is one or more in Losantin, magnesium hypochlorite, clorox or potassium hypochlorite, generates the aqueous solutions of polymers with high conductivity for there is chemical reaction with PEDOT.
In test of many times, find Losantin (Ca (ClO)
2) with after oxidizing reaction occurs PEDOT, the conductivity of aqueous solutions of polymers is promoted greatly, and concrete reaction process is as follows:
PEDOT is the polymkeric substance of EDOT (3,4-ethylene dioxythiophene monomer), and PEDOT (3,4-ethylene dioxythiophene polymkeric substance) is at Losantin Ca (ClO)
2lower oxidation reaction mechanism: wherein OCl-(hypochlorous acid) is oxygenant, the thiophene (a) in PEDOT (3,4-ethylene dioxythiophene polymkeric substance) is oxidized to its corresponding thiophene-1-oxide compound (b) by it.In like manner, thiophene-1-oxide compound (b) is oxidized to its corresponding thiophene-1,1-dioxide (c).In this reaction, thiophene-1-oxide compound (b) is assumed that a reaction intermediate in thiophene-1,1-dioxide (c).Finally, thiophene-1,1-dioxide (c) SO further in oxidation removal compound
2, and by the nucleophilic reaction of water, allow hydroxyl be attached to thiophene-1,1-dioxide (c), thus form the aqueous solutions of polymers with high conductivity.
Although the conductive polymer polymkeric substance of above-mentioned formation is pretty good at water-soluble state conductivity, after its solidification, conductivity can reduce greatly.In order to promote the conductivity of water-based UV electrically conductive ink of the present invention, in above-mentioned conductive polymers, add copper nanoparticle conductive filler material, thus the conductivity of significant increase ink.
Preferably, the particle diameter of copper nanoparticle is less than 50nm, and purity is greater than 99.9%, thus copper nanoparticle is evenly mixed in ink.
Copper nanoparticle is easily oxidized at normal temperatures, and the conductivity of the copper nanoparticle after oxidation reduces greatly.Therefore the oxidation that stablizer prevents copper nanoparticle is added in the present invention's formula, further, stablizer is one or more in cetyl trimethylammonium bromide, Octabenzone, Trimethyllaurylammonium bromide or polyvinylpyrrolidone.
The printing viscosity of ink is the key factor ensureing print quality, and the tackiness agent in the present invention's formula can control the viscosity of ink.Further, tackiness agent be in 2,2-dimethylol propionic acid, dimethylolpropionic acid or polyacrylamide one or more; Particularly preferably adopt the polyacrylamide (PAM) with good flocculence.Tackiness agent has flocculence and thickening power, can avoid separation phenomenon occurring between ink and mixed solvent.
Solvent in the present invention's formula is the auxiliary agent for diluting ink, above-mentioned PEDOT generation chemical reaction is generated the aqueous solutions of polymers with high conductivity and dilutes with other auxiliary agents.Further, solvent is one or more in butyl, tung oil or n-propyl alcohol.
Flow agent in the present invention's formula is mainly used to the mobility improving UV curable ink, enables ink levelling on base material.If levelling property is bad, printed matter can be caused to occur not only not having the phenomenon that tangerine peel, sagging, shrinkage cavity etc. are bad good conductive effect, but also other performances can be reduced.Further, flow agent be in TEGOGlide100, pure acrylic acid flow agent, oxyethane or propylene oxide one or more;
Defoamer in the present invention's formula is a kind of auxiliary agent eliminating the bubble that ultraviolet light polymerization electrically conductive ink occurs in stirring.Because some auxiliary agents in ink are as table, promoting agent, flow agent etc. can produce bubble in the process of ink stirring, grinding.Further, defoamer is one or more in defoamer 6800, defoamer 810, defoamer D105, defoamer T-20GA or defoamer DF-100;
Stopper in the present invention's formula is a kind of auxiliary agent of a kind of obstruction or retardation of curing reaction, can suppress the thermopolymerization of unsaturates, can avoid equipment gum deposit and blocking in printing process simultaneously.Further, stopper be in Resorcinol, phenothiazine, beta-phenyl naphthylamines, toluhydroquinone THQ or methylene blue one or more.
In the preferred embodiment of the present invention, it is 5 ~ 10% pigment that ink also comprises mass percentage, and by adding different types of pigment thus making ink have multiple color, meeting can not the application demand of occasion.Whether pigment adds can according to the actual demand of water-based UV electrically conductive ink, and the water-based UV electrically conductive ink not adding pigment is gloss oil; Needs can be one or both in pigment dyestuff or mineral dye.
In order to overcome the defect of prior art, the invention allows for a kind of preparation method of water-based UV electrically conductive ink, shown in Figure 1, comprise the following steps:
Step S1: prepare the conductive polymers PEDOT aqueous solution; This is further comprising the steps:
The PEDOT of weight percent 40 ~ 60% is placed in the round-bottomed flask of 1000ml, add the deionized water of weight 10 ~ 30%, mechanical stirring is carried out 10 minutes with the speed of 400r/min, pour 1 ~ 8% oxygenant again into, described oxygenant is one or more in Losantin, magnesium hypochlorite, clorox or potassium hypochlorite;
Round-bottomed flask heated and keeps between 50 ~ 80 DEG C, carrying out mechanical stirring 50 minutes with the speed of 800r/min, and then cooling 1 hour under normal temperature, forming the conductive polymers PEDOT aqueous solution.
When oxygenant is Losantin (Ca (ClO) 2), in described step S1, the oxidation reaction process of described PEDOT and described Losantin is as follows:
PEDOT is EDOT (3,4-ethylenedioxy thiophene monomer) polymkeric substance, PEDOT (3,4-ethylenedioxy thiophene polymkeric substance) at Losantin Ca (ClO) 2 times oxidation reaction mechanisms: wherein OCl-(hypochlorous acid) is oxygenant, thiophene (a) in PEDOT (3,4-ethylene dioxythiophene polymkeric substance) is oxidized to its corresponding thiophene-1-oxide compound (b) by it.In like manner, thiophene-1-oxide compound (b) is oxidized to its corresponding thiophene-1,1-dioxide (c).In this reaction, thiophene-1-oxide compound (b) is assumed that a reaction intermediate in thiophene-1,1-dioxide (c).Finally, thiophene-1,1-dioxide (c) SO2 further in oxidation removal compound, and by the nucleophilic reaction of water, allow hydroxyl be attached to thiophene-1,1-dioxide (c), thus form the aqueous solutions of polymers with high conductivity.
Step S2: be the copper nanoparticle of 10 ~ 20% by mass ratio, the conductive polymers PEDOT aqueous solution Homogeneous phase mixing prepared of the stablizer of 0.2 ~ 1.2%, tackiness agent, 1 ~ 6% flow agent, 0.2 ~ 1.2% defoamer, 0.2 ~ 2% stopper, 10 ~ 30% solvents and the step S1 of 2 ~ 5%, load and be placed on HJ-6A type digital display constant temperature bull magnetic stirring apparatus in vessel, be heated to 65 ~ 80 DEG C of Keep agitation 1 hour, then cool 2 hours at normal temperatures, obtain ink mixture;
Preferably, can certainly according to the actual demand of water-based UV electrically conductive ink, the water-based UV electrically conductive ink not adding pigment is gloss oil; Need the kind of pigment of adding to be any color wanting to add, can be one or both in pigment dyestuff or mineral dye, the pigment weight per-cent needing interpolation be 5 ~ 10%.
Step S3: the ink mixture obtained in step S2 is printed in the mode of spray ink Printing after the substrate being preheated to 60 ~ 95 DEG C forms ink pattern and this substrate is put into hot air drier 30 minutes drying and mouldings, thus without the need to high temperature sintering, substantially increase stability and the consistence of electrically conductive ink.
Step S4: carry out ultraviolet light polymerization to the ink pattern on substrate, by ultraviolet light polymerization, enables electrically conductive ink have stable structure, keeps stable conductivity.
Preferably, the PET plate after fiberglass reinforced selected by substrate, because the resistance toheat of pure PET is not high, heat-drawn wire is only about 90 DEG C, but the PET mechanical property after fiberglass reinforced is similar to the engineering plastics such as PC, PA, and heat-drawn wire can reach 225 DEG C.
Below again by the embodiment in specific experiment process to further instruction of the present invention.
Embodiment 1
The first step, the synthesis of PEDOT: the round-bottomed flask PEDOT of weight percent 40% being placed in 1000ml, add the deionized water of weight 28%, mechanical stirring is carried out 10 minutes with the speed of 400r/min, pour oxygenant 1% Losantin again into, round-bottomed flask heated and keeps between 80 DEG C, carrying out mechanical stirring 50 minutes with the speed of 800r/min, and then cool 1 hour under normal temperature, generate the aqueous solutions of polymers with high conductivity thus.
Second step, be that aqueous solutions of polymers and other auxiliary agents of 40%PEDOT high conductivity mixes according to certain ratio by the weight percent of above-mentioned generation, load and be placed on HJ-6A type digital display constant temperature bull magnetic stirring apparatus in vessel, 65 DEG C of heated and stirred 1 hour, and then cool 2 hours under normal temperature, obtain ink to be prepared.Wherein by weight percentage, selection of auxiliary: (copper nanoparticle 10% of 50nm99.9%, stablizer: cetyl trimethylammonium bromide 1%; Tackiness agent 2,2-dimethylol propionic acid, 2%, flow agent is TEGOGlide100,1%; Defoamer is defoamer 6800,0.2%; Stopper be Resorcinol, 1%; Solvent is butyl 15.8%.), do not add any pigment and intend generating water-based UV electrically conductive ink gloss oil.
3rd step, the PET plate after fiberglass reinforced preparing printing is preheated to 60 DEG C, then the mode of spray ink Printing is adopted to adopt the mode of spray ink Printing to be printed on the PET batten after fiberglass reinforced the water-based UV electrically conductive ink of above-mentioned preparation, then printed batten is put into hot air drier 30 minutes drying and mouldings, finally carry out ultraviolet light polymerization.
Embodiment 2
The first step, the synthesis of PEDOT: the round-bottomed flask PEDOT of weight percent 45% being placed in 1000ml, add the deionized water of weight 10%, mechanical stirring is carried out 10 minutes with the speed of 400r/min, pour oxygenant 2% magnesium hypochlorite again into, round-bottomed flask heated and keeps between 60 DEG C, carrying out mechanical stirring 50 minutes with the speed of 800r/min, and then cool 1 hour under normal temperature, generate the aqueous solutions of polymers with high conductivity thus.
Second step, the aqueous solutions of polymers of the PEDOT high conductivity of above-mentioned generation and other auxiliary agents are mixed according to certain ratio, load and be placed on HJ-6A type digital display constant temperature bull magnetic stirring apparatus in vessel, 75 DEG C of heated and stirred 1 hour, and then cool 2 hours under normal temperature, obtain ink to be prepared.Wherein by weight percentage, selection of auxiliary: (copper nanoparticle 16% of 50nm99.9%, stablizer: Trimethyllaurylammonium bromide 0.2%; Tackiness agent is dimethylolpropionic acid, 1%, and flow agent is pure acrylic acid flow agent, 1.8%; Defoamer is defoamer defoamer 810,0.5%; Stopper is phenothiazine, 0.8%; Solvent is tung oil 16%.), add 6.7% pigment dyestuff red 146 simultaneously.
3rd step, the PET plate after fiberglass reinforced preparing printing is preheated to 85 DEG C, then the mode of spray ink Printing is adopted to adopt the mode of spray ink Printing to be printed on the PET batten after fiberglass reinforced the water-based UV electrically conductive ink of above-mentioned preparation, then printed batten is put into hot air drier 30 minutes drying and mouldings, finally carry out ultraviolet light polymerization.
Embodiment 3
The first step, the synthesis of PEDOT: the round-bottomed flask PEDOT of weight percent 45.2% being placed in 1000ml, add the deionized water of weight 10%, mechanical stirring is carried out 10 minutes with the speed of 400r/min, pour oxygenant 5% clorox again into, round-bottomed flask heated and keeps between 70 DEG C, carrying out mechanical stirring 50 minutes with the speed of 800r/min, and then cool 1 hour under normal temperature, generate the aqueous solutions of polymers with high conductivity thus.
Second step, the aqueous solutions of polymers of the PEDOT high conductivity of above-mentioned generation and other auxiliary agents are mixed according to certain ratio, load and be placed on HJ-6A type digital display constant temperature bull magnetic stirring apparatus in vessel, 80 DEG C of heated and stirred 1 hour, and then cool 2 hours under normal temperature, obtain ink to be prepared.Wherein by weight percentage, selection of auxiliary: (copper nanoparticle 12% of 50nm99.9%, stablizer: cetyl trimethylammonium bromide 0.5%; Tackiness agent is polyacrylamide, 1.5%, and flow agent is oxyethane, 1%; Defoamer is defoamer D105,0.8%; Stopper is beta-phenyl naphthylamines, 1%; Solvent is tung oil 18%.; ), add 5% phthalocyanine blue simultaneously.
3rd step, the PET plate after fiberglass reinforced preparing printing is preheated to 90 DEG C, then the mode of spray ink Printing is adopted to adopt the mode of spray ink Printing to be printed on the PET batten after fiberglass reinforced the water-based UV electrically conductive ink of above-mentioned preparation, then printed batten is put into hot air drier 30 minutes drying and mouldings, finally carry out ultraviolet light polymerization.
Embodiment 4
The first step, the synthesis of PEDOT: the round-bottomed flask PEDOT of weight percent 50% being placed in 1000ml, add the deionized water of weight 10%, mechanical stirring is carried out 10 minutes with the speed of 400r/min, pour oxygenant 3% Losantin again into, round-bottomed flask heated and keeps between 65 DEG C, carrying out mechanical stirring 50 minutes with the speed of 800r/min, and then cool 1 hour under normal temperature, generate the aqueous solutions of polymers with high conductivity thus.
Second step, the aqueous solutions of polymers of the PEDOT high conductivity of above-mentioned generation and other auxiliary agents are mixed according to certain ratio, load and be placed on HJ-6A type digital display constant temperature bull magnetic stirring apparatus in vessel, 80 DEG C of heated and stirred 1 hour, and then cool 2 hours under normal temperature, obtain ink to be prepared.Wherein by weight percentage, selection of auxiliary: ((copper nanoparticle 18% of 50nm99.9%, stablizer: polyvinylpyrrolidone 1%; Tackiness agent is polyacrylamide, 1%, and flow agent is pure acrylic acid flow agent, 1%; Defoamer is defoamer DF-100,0.2%; Stopper is methylene blue, 0.2%; Solvent is n-propyl alcohol 10.6%.), add 5% pigment orange 36 (Clariant HL) simultaneously.
3rd step, the PET plate after fiberglass reinforced preparing printing is preheated to 95 DEG C, then the mode of spray ink Printing is adopted to adopt the mode of spray ink Printing to be printed on the PET batten after fiberglass reinforced the water-based UV electrically conductive ink of above-mentioned preparation, then printed batten is put into hot air drier 30 minutes drying and mouldings, finally carry out ultraviolet light polymerization.
Below again the performance of the water-based UV electrically conductive ink of above-described embodiment is detected.
In order to measure the conductivity of the water-based UV electrically conductive ink of technical solution of the present invention, the water-based UV electrically conductive ink prepared by above-described embodiment is distinguished ink jet printing on circuit card, put into hot air drier 30 minutes drying and mouldings, finally carry out ultraviolet light polymerization, be cooled to normal temperature.Adopt the SEM photo after above-described embodiment ink rete being scanned by JSM6460 type scanning electronic microscope, specifically as shown in Fig. 2, Fig. 3, Fig. 4 and Fig. 5, be respectively the SEM photo of embodiment 1, embodiment 2, embodiment 3, embodiment 4.Adopt the specific conductivity of U.S. sensION+EC5 portable electric conductance test ink rete simultaneously, above 4 embodiments to be exerted oneself tearing ink film 30 times with 4M adhesive tape respectively simultaneously, then survey the ink rete specific conductivity after tearing.
In embodiment 1, particle granules in ink more greatly and not tight, there is larger gap, therefore the resistance of film is larger, its specific conductivity is only 0.15 × 10-5 Ω cm, square resistance is 203.1 Ω/ (is square resistance typography, refers to the resistance between a foursquare thin film of conductive material limit to limit); In embodiment 3, in ink, conducting polymer particle is all closely even, the conductive path that can have been formed, and therefore, laminated film specific conductivity now reaches 5.62 × 10-5 Ω cm, and its resistance is lower, and square resistance is only 0.23 Ω/.Embodiment 2 and its specific conductivity of embodiment 4 are between embodiment 1 and embodiment 3, and its value please refer to table 1.Its experimental result is as shown in table 1, and before and after ink film tearing, square resistance, conductivity variations not quite, show that ink has good sticking power.
The tearing of table 1 water-based UV electrically conductive ink 30 front and back square resistance, conductivity test results
The explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection domain of the claims in the present invention.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (10)
1. a water-based UV electrically conductive ink, is characterized in that, with the gross weight of this electrically conductive ink for benchmark, is made up of the component of following mass percentage:
Conductive polymers PEDOT (poly-3,4-ethylene dioxythiophene): 40 ~ 60%; Described PEDOT is the polymkeric substance of EDOT (3,4-ethylene dioxythiophene monomer);
Deionized water: 10 ~ 30%;
Oxygenant: 1 ~ 8%; Described oxygenant is one or more in Losantin, magnesium hypochlorite, clorox or potassium hypochlorite;
Solvent, 10 ~ 30%; Described solvent be in butyl, tung oil or n-propyl alcohol one or more;
Copper nanoparticle conductive filler material, 10 ~ 20%;
Stablizer: 0.2 ~ 1.2%; Described stablizer be in cetyl trimethylammonium bromide, Octabenzone, Trimethyllaurylammonium bromide or polyvinylpyrrolidone one or more;
Tackiness agent: 2 ~ 5%; Described tackiness agent be in 2,2-dimethylol propionic acid, dimethylolpropionic acid or polyacrylamide one or more;
Flow agent: 1 ~ 6%; Described flow agent is one or more in TEGOGlide100, pure acrylic acid flow agent, oxyethane or propylene oxide;
Defoamer: 0.2 ~ 1.2%; Described defoamer is one or more in defoamer 6800, defoamer 810, defoamer D105, defoamer T-20GA or defoamer DF-100;
Stopper: 0.2 ~ 2%; Described stopper be in Resorcinol, phenothiazine, beta-phenyl naphthylamines, toluhydroquinone THQ or methylene blue one or more.
2. water-based UV electrically conductive ink according to claim 1, is characterized in that, described conductive polymers PEDOT and described oxygenant oxidizing reaction occur in deionized water and form the conductive polymers aqueous solution.
3. water-based UV electrically conductive ink according to claim 2, is characterized in that, described oxygenant is Losantin (Ca (ClO)
2), the oxidation reaction process of described conductive polymers PEDOT and described Losantin is as follows:
4. water-based UV electrically conductive ink according to claim 1 and 2, is characterized in that, the particle diameter of described copper nanoparticle is less than 50nm, and purity is greater than 99.9%.
5. water-based UV electrically conductive ink according to claim 1 and 2, is characterized in that, also comprises the pigment that mass percentage is 5 ~ 10%.
6. a preparation method for water-based UV electrically conductive ink, is characterized in that, comprises the following steps:
Step S1: prepare the conductive polymers PEDOT aqueous solution;
Step S2: be the copper nanoparticle of 10 ~ 20% by mass ratio, the conductive polymers PEDOT aqueous solution Homogeneous phase mixing prepared of the stablizer of 0.2 ~ 1.2%, tackiness agent, the flow agent of 1 ~ 6%, defoamer, the stopper of 0.2 ~ 2%, the solvent of 10 ~ 30% and the step S1 of 0.2 ~ 1.2% of 2 ~ 5%, be heated to 65 ~ 80 DEG C of Keep agitation 1 hour, then cool 2 hours at normal temperatures, obtain ink mixture;
Step S3: the ink mixture obtained in step S2 is printed in the mode of spray ink Printing after the substrate being preheated to 60 ~ 95 DEG C forms ink pattern and this substrate is put into hot air drier 30 minutes drying and mouldings;
Step S4: ultraviolet light polymerization is carried out to the ink pattern on substrate.
7. the preparation method of water-based UV electrically conductive ink according to claim 6, is characterized in that, described step S1 is further comprising the steps:
The PEDOT of weight percent 40 ~ 60% is placed in the round-bottomed flask of 1000ml, add the deionized water of weight 10 ~ 30%, mechanical stirring is carried out 10 minutes with the speed of 400r/min, pour 1 ~ 8% oxygenant again into, described oxygenant is one or more in Losantin, magnesium hypochlorite, clorox or potassium hypochlorite;
Round-bottomed flask heated and keeps between 50 ~ 80 DEG C, carrying out mechanical stirring 50 minutes with the speed of 800r/min, and then cooling 1 hour under normal temperature, forming the conductive polymers PEDOT aqueous solution.
8. the preparation method of water-based UV electrically conductive ink according to claim 7, is characterized in that, described oxygenant is Losantin (Ca (ClO)
2) time, in described step S1, the oxidation reaction process of described PEDOT and described Losantin is as follows:
9. the preparation method of the water-based UV electrically conductive ink according to claim 6 or 7, is characterized in that, also comprises the step adding pigment in described step S2, and the mass percent of described pigment is 5 ~ 10%.
10. the preparation method of the water-based UV electrically conductive ink according to claim 6 or 7, is characterized in that, in described step S3, the PET plate after fiberglass reinforced selected by described substrate.
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| CN109935469A (en) * | 2017-12-15 | 2019-06-25 | 钰邦科技股份有限公司 | Printed form conduction composite mortar, capacitor and its manufacturing method |
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| CN111469573A (en) * | 2020-05-28 | 2020-07-31 | 安庆盛华纸质包装有限公司 | Printing ink processing technology of high-performance coated paper sheet |
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