CN103131254A - Zinc-oxide-containing dual-wavelength light-absorption aquosity anti-forgery ink easer preparation technology - Google Patents
Zinc-oxide-containing dual-wavelength light-absorption aquosity anti-forgery ink easer preparation technology Download PDFInfo
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- CN103131254A CN103131254A CN2013100458142A CN201310045814A CN103131254A CN 103131254 A CN103131254 A CN 103131254A CN 2013100458142 A CN2013100458142 A CN 2013100458142A CN 201310045814 A CN201310045814 A CN 201310045814A CN 103131254 A CN103131254 A CN 103131254A
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- Prior art keywords
- solution
- acid
- zinc oxide
- alkyl
- salt
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000005516 engineering process Methods 0.000 title claims abstract description 13
- 229960001296 zinc oxide Drugs 0.000 title abstract 6
- 230000031700 light absorption Effects 0.000 title abstract 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000002253 acid Substances 0.000 claims abstract description 31
- 239000008367 deionised water Substances 0.000 claims abstract description 23
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 23
- 239000007787 solid Substances 0.000 claims abstract description 18
- 239000004094 surface-active agent Substances 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 74
- -1 polyethylene Polymers 0.000 claims description 72
- 238000002156 mixing Methods 0.000 claims description 51
- 239000002245 particle Substances 0.000 claims description 49
- 230000009977 dual effect Effects 0.000 claims description 35
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 34
- 230000008033 biological extinction Effects 0.000 claims description 34
- 239000011701 zinc Substances 0.000 claims description 34
- 229910052725 zinc Inorganic materials 0.000 claims description 34
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 30
- 241000282326 Felis catus Species 0.000 claims description 26
- 125000000217 alkyl group Chemical group 0.000 claims description 26
- 239000000203 mixture Substances 0.000 claims description 26
- 229920002472 Starch Polymers 0.000 claims description 24
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 claims description 24
- 239000008107 starch Substances 0.000 claims description 24
- 235000019698 starch Nutrition 0.000 claims description 24
- 125000004432 carbon atom Chemical group C* 0.000 claims description 23
- YMMGRPLNZPTZBS-UHFFFAOYSA-N 2,3-dihydrothieno[2,3-b][1,4]dioxine Chemical compound O1CCOC2=C1C=CS2 YMMGRPLNZPTZBS-UHFFFAOYSA-N 0.000 claims description 21
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 13
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 13
- 229930195729 fatty acid Natural products 0.000 claims description 13
- 239000000194 fatty acid Substances 0.000 claims description 13
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 11
- 239000013543 active substance Substances 0.000 claims description 10
- 150000002190 fatty acyls Chemical group 0.000 claims description 10
- 229920000570 polyether Polymers 0.000 claims description 10
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 150000002148 esters Chemical class 0.000 claims description 7
- MTNDZQHUAFNZQY-UHFFFAOYSA-N imidazoline Chemical compound C1CN=CN1 MTNDZQHUAFNZQY-UHFFFAOYSA-N 0.000 claims description 7
- 230000001476 alcoholic effect Effects 0.000 claims description 6
- 239000003945 anionic surfactant Substances 0.000 claims description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 4
- 239000004698 Polyethylene Substances 0.000 claims description 4
- 229930006000 Sucrose Natural products 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 150000003862 amino acid derivatives Chemical class 0.000 claims description 4
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical class [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 4
- 239000003093 cationic surfactant Substances 0.000 claims description 4
- 229920000768 polyamine Polymers 0.000 claims description 4
- 229920000573 polyethylene Polymers 0.000 claims description 4
- 229920005862 polyol Polymers 0.000 claims description 4
- 150000003077 polyols Chemical class 0.000 claims description 4
- 229920000136 polysorbate Polymers 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 150000003335 secondary amines Chemical class 0.000 claims description 4
- 239000005720 sucrose Substances 0.000 claims description 4
- 239000004711 α-olefin Substances 0.000 claims description 4
- ZEMPKEQAKRGZGQ-AAKVHIHISA-N 2,3-bis[[(z)-12-hydroxyoctadec-9-enoyl]oxy]propyl (z)-12-hydroxyoctadec-9-enoate Chemical compound CCCCCCC(O)C\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CC(O)CCCCCC)COC(=O)CCCCCCC\C=C/CC(O)CCCCCC ZEMPKEQAKRGZGQ-AAKVHIHISA-N 0.000 claims description 3
- FVIMRJIDRHUTQP-UHFFFAOYSA-N 2-[bis(2-hydroxyethyl)amino]ethyl octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCCN(CCO)CCO FVIMRJIDRHUTQP-UHFFFAOYSA-N 0.000 claims description 3
- IMBPNEGZDBFLBN-UHFFFAOYSA-N 3-n-ethylbutane-1,3-diamine Chemical compound CCNC(C)CCN IMBPNEGZDBFLBN-UHFFFAOYSA-N 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical class S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 claims description 3
- 150000001408 amides Chemical class 0.000 claims description 3
- 150000007942 carboxylates Chemical class 0.000 claims description 3
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- 150000002306 glutamic acid derivatives Chemical group 0.000 claims description 3
- 125000005908 glyceryl ester group Chemical group 0.000 claims description 3
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 claims description 3
- SMWDFEZZVXVKRB-UHFFFAOYSA-O hydron;quinoline Chemical compound [NH+]1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-O 0.000 claims description 3
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 claims description 3
- 150000004714 phosphonium salts Chemical class 0.000 claims description 3
- 229920000075 poly(4-vinylpyridine) Polymers 0.000 claims description 3
- 229920000223 polyglycerol Polymers 0.000 claims description 3
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 3
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 3
- 150000003141 primary amines Chemical class 0.000 claims description 3
- 150000003222 pyridines Chemical class 0.000 claims description 3
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 claims description 3
- 150000003512 tertiary amines Chemical class 0.000 claims description 3
- 239000000811 xylitol Substances 0.000 claims description 3
- 235000010447 xylitol Nutrition 0.000 claims description 3
- 229960002675 xylitol Drugs 0.000 claims description 3
- HDIFHQMREAYYJW-XFXZXTDPSA-N 2,3-dihydroxypropyl (z)-12-hydroxyoctadec-9-enoate Chemical compound CCCCCCC(O)C\C=C/CCCCCCCC(=O)OCC(O)CO HDIFHQMREAYYJW-XFXZXTDPSA-N 0.000 claims description 2
- HDIFHQMREAYYJW-UHFFFAOYSA-N Monoricinolein Natural products CCCCCCC(O)CC=CCCCCCCCC(=O)OCC(O)CO HDIFHQMREAYYJW-UHFFFAOYSA-N 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims description 2
- 229930182470 glycoside Natural products 0.000 claims description 2
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 claims description 2
- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 claims description 2
- 125000002811 oleoyl group Chemical group O=C([*])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])/C([H])=C([H])\C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 229940113162 oleylamide Drugs 0.000 claims description 2
- 229920001451 polypropylene glycol Polymers 0.000 claims description 2
- 239000000047 product Substances 0.000 claims description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 abstract description 11
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 abstract description 2
- 239000000243 solution Substances 0.000 abstract 5
- 239000011259 mixed solution Substances 0.000 abstract 3
- 239000005456 alcohol based solvent Substances 0.000 abstract 1
- 150000001450 anions Chemical class 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 235000011187 glycerol Nutrition 0.000 description 24
- 125000001424 substituent group Chemical group 0.000 description 18
- 239000000654 additive Substances 0.000 description 16
- 230000000996 additive effect Effects 0.000 description 16
- 238000002242 deionisation method Methods 0.000 description 15
- 238000009775 high-speed stirring Methods 0.000 description 15
- 239000006185 dispersion Substances 0.000 description 14
- 238000007639 printing Methods 0.000 description 6
- 150000001412 amines Chemical class 0.000 description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 4
- BDEXTGBSHOQSGO-UHFFFAOYSA-M 3-aminopropyl-benzyl-dimethylazanium;chloride Chemical group [Cl-].NCCC[N+](C)(C)CC1=CC=CC=C1 BDEXTGBSHOQSGO-UHFFFAOYSA-M 0.000 description 3
- 235000019270 ammonium chloride Nutrition 0.000 description 3
- 229940117927 ethylene oxide Drugs 0.000 description 3
- 125000003696 stearoyl group Chemical group O=C([*])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- 229940022860 xylitan Drugs 0.000 description 3
- 239000000263 2,3-dihydroxypropyl (Z)-octadec-9-enoate Substances 0.000 description 2
- GVNVAWHJIKLAGL-UHFFFAOYSA-N 2-(cyclohexen-1-yl)cyclohexan-1-one Chemical compound O=C1CCCCC1C1=CCCCC1 GVNVAWHJIKLAGL-UHFFFAOYSA-N 0.000 description 2
- VIWIWXKTPWZMEW-UHFFFAOYSA-N 2-hydroxypropanoic acid;propane-1,2,3-triol Chemical compound CC(O)C(O)=O.OCC(O)CO VIWIWXKTPWZMEW-UHFFFAOYSA-N 0.000 description 2
- RZRNAYUHWVFMIP-GDCKJWNLSA-N 3-oleoyl-sn-glycerol Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@H](O)CO RZRNAYUHWVFMIP-GDCKJWNLSA-N 0.000 description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 2
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- 235000011076 sorbitan monostearate Nutrition 0.000 description 1
- 229940035048 sorbitan monostearate Drugs 0.000 description 1
- AKUNSPZHHSNFFX-UHFFFAOYSA-M tributyl(tetradecyl)phosphanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[P+](CCCC)(CCCC)CCCC AKUNSPZHHSNFFX-UHFFFAOYSA-M 0.000 description 1
- GAJQCIFYLSXSEZ-UHFFFAOYSA-N tridecyl dihydrogen phosphate Chemical compound CCCCCCCCCCCCCOP(O)(O)=O GAJQCIFYLSXSEZ-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention provides a zinc-oxide-containing dual-wavelength light-absorption aquosity anti-forgery ink easer preparation technology. Nanometer zinc oxide, deionized water and surfactants are dispersed to be even in an ultrasonic mode, and nanometer zinc oxide solution is obtained. PEDOT solution with solid content of 1.3-1.7% and mixed with polystyrolsulfon acid is mixed with the deionized water, then anion surfactants are added, evenness is achieved through ultrasonic dispersion, and solution A is obtained. The nanometer zinc oxide solution is mixed with the solution A to obtain mixed solution B. The mixed solution B is heated to 40-70 DEG C, alcohol solvents and powder with the diameter of 200-1000 nm are added in the mixed solution B after stirring, reaction is carried out for 40-60 minutes, and finally zinc-oxide-containing dual-wavelength light-absorption aquosity anti-forgery ink easer is obtained. The anti-forgery ink easer has an absorption function in an infrared band of 1000-1200 nm and an ultraviolet band of 300-340 nm, and can be used as aquosity anti-forgery ink easer.
Description
Technical field
The present invention relates to a kind of preparation technology of anti-forgery ink additive, be specifically related to a kind of preparation technology who contains the dual wavelength extinction aqueous anti-counterfeiting easer of zinc oxide.
Background technology
Anti-forgery ink is used very wide in printing industry, and optical anti-counterfeiting printing ink is integral part very important in anti-forgery ink.Optical anti-counterfeiting printing ink in Valued Securities printing at present is mainly ultraviolet anti-forgery, and is commonplace in the application in market, but the problem that exists is that its anti-counterfeit capability is on the low side, and be easy to imitated; For the false proof demand on satisfying the market, be badly in need of the anti-counterfeiting technology of development of new.
Summary of the invention
The present invention is directed to above deficiency, a kind of preparation technology who contains the dual wavelength extinction aqueous anti-counterfeiting easer of zinc oxide is provided.
In order to achieve the above object, the technical solution used in the present invention comprises the following steps:
1) nano zine oxide is placed in deionized water, then adds tensio-active agent, at room temperature utilize ultrasonic wave that the mixed system that obtains is uniformly dispersed, namely obtain nano oxidized zinc solution; Wherein, the mass ratio of zinc oxide, deionized water, tensio-active agent is (4-5): (100-200): (0.20-0.35), tensio-active agent is cats product and/or nonionogenic tenside;
2) the poly-ethylenedioxy thiophene solution that is the polystyrolsulfon acid doping of 1.3-1.7% according to the mass ratio of 1:1 with solid content mixes with deionized water, then adds anion surfactant, then utilizes ultrasonic wave to be uniformly dispersed under 20-70 ℃, obtains solution A; Wherein, the poly-ethylenedioxy thiophene solution of polystyrolsulfon acid doping and the mass ratio of anion surfactant are 10:0.02;
3) with nano oxidized zinc solution with solution A with 1:(1-1.5) mass ratio mix, obtain mixing solutions B; Then mixing solutions B is heated to 40-70 ℃, more under agitation to add alcoholic solvent and particle diameter in the mixing solutions B be the powder of 200-1000nm, reacted 40-60 minute, finally obtain containing the dual wavelength extinction aqueous anti-counterfeiting easer of zinc oxide; Wherein, the alcoholic solvent that adds accounts for the 25-40% of the nano zine oxide solution quality of step 3), and alcoholic solvent is ethylene glycol or glycerol; The powder that adds accounts for the 5-10% of the nano zine oxide solution quality of step 3), and powder is polynite or carboxymethyl starch.
In described step 1), the particle diameter of nano zine oxide is 80-200nm.
In described step 1), cats product is that rope Luo Ming A, handkerchief Sa Ming A, oleoyl are for aminoethyl diethylamide, A Keweier A, polyethylene polyamines salt, imidazoline surfactant, high fatty amine salt, quaternary ammonium salt cationic surfactant, N
αThe mixture of one or more arbitrary proportions in-coconut acyl arginine ethyl ester, pyridine salt type cats product, quinolinium type cats product, double quaternary ammonium salt type cats product, sulfonium salt type cats product, phosphonium salt type cats product, Arsenic salt type cats product;
Nonionogenic tenside is the mixture of one or more arbitrary proportions in polyoxyethylene-type surfactant, polyoxyethylene polyoxypropylene block type polyethers, EPE polyol EPE, triethanolamine monostearate, phosphorous nonionogenic tenside, amino acid derivative nonionogenic tenside.
Described polyethylene polyamines salt is quaternized poly 4 vinyl pyridine, poly-sulfuric acid trimethylammonium polyethylene ammonium or polyvinyl lactam hydrochloride;
Described imidazoline surfactant is 1-hydroxyethyl-2-alkyl-tetrahydroglyoxaline, and wherein, in 1-hydroxyethyl-2-alkyl-tetrahydroglyoxaline, the carbonatoms of alkyl is 5-20;
Described high fatty amine salt is to utilize in hydrochloric acid, formic acid or acetic acid and product that senior primary amine, senior secondary amine or senior tertiary amine obtain;
Described quaternary ammonium salt cationic surfactant is that alkyl trimethyl quaternary ammonium salt, alkyl dimethyl benzyl quaternary ammonium salt, alkyl dimethyl ethoxyl quaternary ammonium salt, fatty acyl are for the mixture of one or more arbitrary proportions in amino tri alkyl quaternary ammonium salt, imidazoline type quaternary ammonium salt;
Described polyoxyethylene-type surfactant is the mixture of one or more arbitrary proportions in fatty acyl alkanolamine, Viscotrol C ethylene oxide adduct, long-chain fat polyoxyethylenated alcohol, alkylphenol polyoxyethylene, polyoxyethylene carboxylate, aliphatic amine polyoxyethylene ether, fatty acyl alkanolamine Soxylat A 25-7;
Described polyoxyethylene polyoxypropylene block type polyethers is the mixture of one or more arbitrary proportions in polyoxyethylene polyoxypropylene block type polyethers, polyoxyethylene polyoxypropylene polyoxyethylene blocks type polyethers, polyoxyethylene polyoxypropylene polyoxypropylene block type polyethers;
Described EPE polyol EPE is the mixture of one or more arbitrary proportions in glyceryl ester type tensio-active agent, polyglycerol fatty acid ester, pentaerythritol fatty ester, dehydration Xylitol fatty acid ester, Span, sorbitan fatty acid ester, tween, sucrose fatty ester, alkyl glycoside, Polyglycerine poly monoricinolein;
The acid amides of the nonionogenic tenside that described amino acid derivative nonionogenic tenside is glutamic acid derivatives, the ester class of N-acylamino acid, N-acylamino acid, the mixture of one or more arbitrary proportions in urea groups methylene oleylamide.
Anion surfactant in described step 3) is sodium laurylsulfonate, benzene sulfonic acid sodium salt, sulfonated α-olefin, alpha-sulfo monocarboxylic acid or Yi Jiebang A.
Preferably, described senior primary amine is ROCH
2NH
2, one or more arbitrary proportions in coconut amine, tallow amine, rosin Amine D mixture; Wherein, ROCH
2NH
2In substituent R be that carbonatoms is the alkyl of 11-17; Senior secondary amine is R
2The mixture of one or more arbitrary proportions in NH; Wherein, the substituent R in senior secondary amine is that carbonatoms is the alkyl of 6-9; Senior tertiary amine is RN (CH
3)
2, fatty acyl is for the mixture of one or more arbitrary proportions in aminoethyl diethylamide, fatty group tetrahydroglyoxaline, triethanolamine monostearate; Wherein, RN (CH
3)
2In substituent R be that carbonatoms is the alkyl of 10-16.
Preferably, described pyridine salt type cats product is
And
In substituent R be that carbonatoms is the alkyl of 12-18, X is Cl or Br.
Preferably, described quinolinium type cats product is
And
In substituent R be that carbonatoms is the alkyl of 12-18, X is Cl or Br.
Preferably, described sulfonium salt type cats product is dodecyl dimethyl methyl-sulfuric acid sulfonium.
Preferably, Suo Shu De phosphonium salt type cats product is dodecyl dimethyl phenyl phosphonium bromide, dodecyl three p-methylphenyl phosphonium bromides, tetrakis hydroxymethyl phosphonium chloride or tetradecyl tributyl phosphonium chloride.
Preferably, Suo Shu De Arsenic salt type cats product is octyl dimethyl benzyl Xiuization Arsenic.
Preferably, described phosphorous nonionogenic tenside is polyoxyethylene two (dodecyl) phosphoric acid ester or two polyoxy ethene list tridecyl phosphoric acid ester.
Preferably, described alkyl trimethyl quaternary ammonium salt is alkyl trimethyl ammonium chloride or alkyl trimethyl ammonium bromide, and the carbonatoms of the alkyl in alkyl trimethyl ammonium chloride and alkyl trimethyl ammonium bromide is 5-18.
Preferably, described alkyl dimethyl benzyl quaternary ammonium salt is
And
In substituent R be that carbonatoms is the alkyl of 5-18.
Preferably, described alkyl dimethyl ethoxyl quaternary ammonium salt is
And
In substituent R be that carbonatoms is the alkyl of 5-18.
Preferably, described fatty acyl is that stearoyl replaces aminoethyl diethyl benzyl ammonium chloride, stearoyl to replace the aminopropyl dimethyl benzyl ammonium chloride for aminoethyl trimethylammonium ammonium sulfate or mnyristoyl for amino tri alkyl quaternary ammonium salt.
Preferably, described imidazoline type ammonium salt is 1-hydroxyethyl-1 benzyl-2-alkyl imidazoline ammonium chloride; And the carbonatoms of the alkyl in 1-hydroxyethyl-1 benzyl-2-alkyl imidazoline ammonium chloride is 5-18.
Preferably, described fatty acyl alkanolamine is
Wherein,
In substituent R be that carbonatoms is the alkyl of 5-20.
Preferably, to add up to be 40 to the ethyleneoxide addition in described Viscotrol C ethylene oxide adduct.
Preferably, the general formula of described long-chain fat polyoxyethylenated alcohol is:
And
Middle substituent R is that carbonatoms is the alkyl of 8-20.
Preferably, described alkylphenol polyoxyethylene is
And
In substituent R be that H or carbonatoms are the alkyl of 1-10.
Preferably, the general formula of described polyoxyethylene carboxylate is:
Wherein,
Middle substituent R is that carbonatoms is the alkyl of 8-20.
Preferably, described aliphatic amine polyoxyethylene ether is
In the mixture of one or both arbitrary proportions, wherein,
In substituent R be that carbonatoms is the alkyl of 8-20.
Preferably, described fatty acyl alkanolamine Soxylat A 25-7 is:
Or
In the mixture of one or more arbitrary proportions, wherein,
In substituent R be that carbonatoms is the alkyl of 8-20.
preferably, described glyceryl ester type tensio-active agent is Zerol, Stearic diglyceride, glyceryl monooleate, glycerol dioleate, the glycerine monopalmitate, dipalmitin, Tetradecanoic acid, monoester with 1,2,3-propanetriol, glycerine two myristinates, glyceryl monolaurate, Lauric acid, diester with glycerol, the acetic acid glycerol mono fatty acid ester, acetic acid dialycerides fat acid esters, the lactic acid glycerol mono fatty acid ester, lactic acid dialycerides fat acid esters, the polyoxyethylene glycerol mono fatty acid ester, the mixture of one or more arbitrary proportions in polyoxyethylene dialycerides fat acid esters.
Preferably, the general formula of described polyglycerol fatty acid ester is:
And
Middle substituent R is that carbonatoms is the alkyl of 5-20, substituent R
1And R
2That H or carbonatoms are the alkyl of 5-20.
Preferably, the general formula of described pentaerythritol fatty ester is:
And
Middle substituent R is that carbonatoms is the alkyl of 5-20.
Preferably, the described dehydration Xylitol fatty acid ester mixture that is one or more arbitrary proportions in xylitan monostearate or polyoxyethylene xylitan monostearate.
Preferably, the general formula of described Span is:
And
Middle substituent R is that carbonatoms is the alkyl of 5-20.
Preferably, described sorbitan fatty acid ester is the mixture of one or more arbitrary proportions in sorbitan mono-laurate, anhydrous sorbitol monopalmitate, sorbitan monooleate, sorbitan monostearate, Witconol AL 69-66 and anhydrous sorbitol tristearate.
Preferably, described tween is polysorbas20, tween 4, polysorbate40, polysorbate60, Tween61, polysorbate65, tween 80, sorbimacrogol oleate100 or polysorbate85.
Preferably, the nonionogenic tenside of described glutamic acid derivatives be pyrrolidone carboxylic acid's glyceryl monooleate or
In the mixture of one or more arbitrary proportions, and
In substituent R be that carbonatoms is the alkyl of 5-20.
Preferably, the ester class of described N-acylamino acid is the mixture of one or both arbitrary proportions in N-alkyloyl glutamate or N-lauroyl glutamate dibutyl acid amides.
The dual wavelength extinction aqueous anti-counterfeiting easer that contains zinc oxide of method preparation of the present invention has absorption at the infrared band of 1000-1200nm and the ultraviolet band of 310-340nm; So the dual wavelength extinction aqueous anti-counterfeiting easer that contains zinc oxide of the present invention's preparation is a kind of light absorbing material of dual wavelength; Simultaneously, this dual wavelength light absorbing material can strengthen the anti-counterfeit capability of anti-forgery ink as extinction aqueous anti-counterfeiting easer, can be used as a kind of high-end false proof means and uses, and makes anti-counterfeit capability more reliable.In addition, the tensio-active agent that the present invention adds not only can improve the security feature of printing ink, but also the printing ink of the dual wavelength extinction anti-forgery ink additive that can make the present invention contain zinc oxide after adding has good levelling property and good film forming properties.
Description of drawings
Fig. 1 is the illuminated diagram of the dual wavelength extinction aqueous anti-counterfeiting easer that contains zinc oxide for preparing of the present invention, and wherein ordinate zou is absorbancy, and X-coordinate is wavelength, and unit is nm.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further elaborated.
Embodiment 1:
1) be the deionized water that the zinc oxide of 80-200nm is placed in 100g with the 4g particle diameter, then add the polysorbate60 of 0.30g, more at room temperature utilize ultrasonic wave with the mixed system ultra-sonic dispersion 120min that obtains, namely obtain nano oxidized zinc solution;
2) be that the poly-ethylenedioxy thiophene solution of the polystyrolsulfon acid doping of 1.3-1.7% mixes with the deionization water of 10g with the 10g solid content, then add the sodium laurylsulfonate of 0.02g, then utilize ultrasonic wave dispersion 80min under 20 ℃, obtain solution A;
3) nano oxidized zinc solution is mixed with the mass ratio of solution A with 1:1, obtain mixing solutions B; Then mixing solutions B is heated to 40 ℃, then to add ethylene glycol and particle diameter in the mixing solutions B under high-speed stirring be the polynite of 200-1000nm, reacted 60 minutes, finally obtain containing the dual wavelength extinction anti-forgery ink additive of zinc oxide; Wherein, the ethylene glycol that adds account for step 3) the nano zine oxide solution quality 40%, the particle diameter that adds is 5% of the polynite of the 200-1000nm nano zine oxide solution quality that accounts for step 3).
Embodiment 2:
1) with the 4g particle diameter be the deionized water that the zinc oxide of 80-200nm is placed in 100g, then the polyoxyethylene xylitan monostearate and the glycerine monopalmitate that add 0.30g, at room temperature utilize again ultrasonic cleaner with the mixed system ultra-sonic dispersion 120min that obtains, namely obtain nano oxidized zinc solution;
2) be that the poly-ethylenedioxy thiophene solution of the polystyrolsulfon acid doping of 1.3-1.7% mixes with the deionization water of 10g with the 10g solid content, then add the sodium laurylsulfonate of 0.02g, then utilize ultrasonic echography dispersion 60min to obtain solution A under 20 ℃;
3) nano oxidized zinc solution is mixed with the mass ratio of solution A with 1:1, obtain mixing solutions B; Then mixing solutions B is heated to 40 ℃, then to add ethylene glycol and particle diameter in the mixing solutions B under high-speed stirring be the polynite of 200-1000nm, reacted 60 minutes, finally obtain containing the dual wavelength extinction anti-forgery ink additive of zinc oxide; Wherein, the ethylene glycol that adds account for step 3) the nano zine oxide solution quality 40%, the particle diameter that adds is 5% of the polynite of the 200-1000nm nano zine oxide solution quality that accounts for step 3).
Embodiment 3:
1) with the 4g particle diameter be the deionized water that the zinc oxide of 80-200nm is placed in 100g, then the lactic acid glycerol mono fatty acid ester and the lactic acid dialycerides fat acid esters that add 0.30g, at room temperature utilize ultrasonic wave with the mixed system ultra-sonic dispersion 120min that obtains, namely obtain nano oxidized zinc solution;
2) be that the poly-ethylenedioxy thiophene solution of the polystyrolsulfon acid doping of 1.3-1.7% mixes with the deionization water of 10g with the 10g solid content, add the sodium laurylsulfonate of 0.02g, then utilize ultrasonic wave dispersion 40min to obtain solution A under 20 ℃;
3) nano oxidized zinc solution is mixed with the mass ratio of solution A with 1:1, obtain mixing solutions B; Then mixing solutions B is heated to 40 ℃, then to add ethylene glycol and particle diameter in the mixing solutions B under high-speed stirring be the polynite of 200-1000nm, reacted 60 minutes, finally obtain containing the dual wavelength extinction anti-forgery ink additive of zinc oxide; Wherein, the ethylene glycol that adds account for step 3) the nano zine oxide solution quality 40%, the particle diameter that adds is 5% of the polynite of the 200-1000nm nano zine oxide solution quality that accounts for step 3).
Embodiment 4:
1) with the 4.2g particle diameter be the deionized water that the zinc oxide of 80-200nm is placed in 200g, then the quaternized poly 4 vinyl pyridine and the polysorbas20 that add 0.20g, at room temperature utilize again ultrasonic wave that the mixed system that obtains is disperseed 120min, namely obtain nano oxidized zinc solution;
2) be that the poly-ethylenedioxy thiophene solution of the polystyrolsulfon acid doping of 1.3-1.7% mixes with the deionization water of 10g with the 10g solid content, then add the benzene sulfonic acid sodium salt of 0.02g, then utilize ultrasonic wave dispersion 80min to obtain solution A under 70 ℃;
3) nano oxidized zinc solution is mixed with the mass ratio of solution A with 1:1.5, obtain mixing solutions B; Then mixing solutions B is heated to 65 ℃, then to add glycerol and particle diameter in the mixing solutions B under high-speed stirring be the carboxymethyl starch of 200-1000nm, reacted 50 minutes, finally obtain containing the dual wavelength extinction anti-forgery ink additive of zinc oxide; Wherein, the glycerol that adds account for step 3) the nano zine oxide solution quality 30%, the particle diameter that adds is 7% of the carboxymethyl starch of the 200-1000nm nano zine oxide solution quality that accounts for step 3).
Embodiment 5:
1) be the deionized water that the zinc oxide of 80-200nm is placed in 200g with the 4.2g particle diameter, then add the coconut amine hydrochloride of 0.20g, more at room temperature utilize ultrasonic wave that the mixed system that obtains is disperseed 120min, namely obtain nano oxidized zinc solution;
2) be that the poly-ethylenedioxy thiophene solution of the polystyrolsulfon acid doping of 1.3-1.7% mixes with the deionization water of 10g with the 10g solid content, then add the sodium laurylsulfonate of 0.02g, utilize ultrasonic wave dispersion 60min to obtain solution A under 35 ℃;
3) nano oxidized zinc solution is mixed with the mass ratio of solution A with 1:1.5, obtain mixing solutions B; Then mixing solutions B is heated to 65 ℃, then to add glycerol and particle diameter in the mixing solutions B under high-speed stirring be the carboxymethyl starch of 200-1000nm, reacted 50 minutes, finally obtain containing the dual wavelength extinction anti-forgery ink additive of zinc oxide; Wherein, the glycerol that adds account for step 3) the nano zine oxide solution quality 30%, the particle diameter that adds is 7% of the carboxymethyl starch of the 200-1000nm nano zine oxide solution quality that accounts for step 3).
Embodiment 6:
1) be the deionized water that the zinc oxide of 80-200nm is placed in 200g with the 4.2g particle diameter, then add the high fatty amine salt of 0.20g, more at room temperature utilize ultrasonic wave that the mixed system that obtains is disperseed 120min, namely obtain nano oxidized zinc solution; High fatty amine salt is by in hydrochloric acid and the product that obtains of tallow amine and rosin Amine D;
2) be that the poly-ethylenedioxy thiophene solution of the polystyrolsulfon acid doping of 1.3-1.7% mixes with the deionization water of 10g with the 10g solid content, then add the sodium laurylsulfonate of 0.02g, then utilize ultrasonic wave dispersion 80min to obtain solution A under 20 ℃;
3) nano oxidized zinc solution is mixed with the mass ratio of solution A with 1:1.5, obtain mixing solutions B; Then mixing solutions B is heated to 65 ℃, then to add glycerol and particle diameter in the mixing solutions B under high-speed stirring be the carboxymethyl starch of 200-1000nm, reacted 50 minutes, finally obtain containing the dual wavelength extinction anti-forgery ink additive of zinc oxide; Wherein, the glycerol that adds account for step 3) the nano zine oxide solution quality 30%, the particle diameter that adds is 7% of the carboxymethyl starch of the 200-1000nm nano zine oxide solution quality that accounts for step 3).
High fatty amine salt in embodiment 6 step 1) can also adopt in hydrochloric acid, formic acid or acetic acid and high fatty amine is made, and acid and the high fatty amine specifically selected are as shown in table 1:
Table 1
Embodiment 13
1) be the deionized water that the zinc oxide of 80-200nm is placed in 150g with the 5g particle diameter, then add the A Keweier A of 0.35g, at room temperature utilize ultrasonic wave with the mixed system ultra-sonic dispersion 120min that obtains, namely obtain nano oxidized zinc solution;
2) be that the poly-ethylenedioxy thiophene solution of the polystyrolsulfon acid doping of 1.3-1.7% mixes with the deionization water of 10g with the 10g solid content, then the sulfonated α-olefin that adds 0.02g, utilize again ultrasonic wave to disperse 40min to obtain solution A under 42 ℃, wherein, the general formula of described sulfonated α-olefin is RCH=CHCH
2SO
3Na, and RCH=CHCH
2SO
3Substituent R in Na is that carbonatoms is the alkyl of 5-20;
3) nano oxidized zinc solution is mixed with the mass ratio of solution A with 1:1.2, obtain mixing solutions B; Then mixing solutions B is heated to 70 ℃, then to add glycerol and particle diameter in the mixing solutions B under high-speed stirring be the carboxymethyl starch of 200-1000nm, reacted 40 minutes, finally obtain containing the dual wavelength extinction aqueous anti-counterfeiting easer of zinc oxide; Wherein, the glycerol that adds account for step 3) the nano zine oxide solution quality 25%, the particle diameter that adds is 10% of the carboxymethyl starch of the 200-1000nm nano zine oxide solution quality that accounts for step 3).
Embodiment 14:
1) with the 5g particle diameter be the deionized water that the zinc oxide of 80-200nm is placed in 150g, then the rope Luo Ming A and the octadecyl trimethyl ammonium chloride that add 0.35g, at room temperature utilize again ultrasonic cleaner that the mixed system ultra-sonic dispersion that obtains is even, namely obtain nano oxidized zinc solution;
2) be that the poly-ethylenedioxy thiophene solution of the polystyrolsulfon acid doping of 1.3-1.7% mixes with the deionization water of 10g with the 10g solid content, then add the sodium laurylsulfonate of 0.02g, then utilize ultrasonic wave dispersion 40min to obtain solution A under 20 ℃;
3) nano oxidized zinc solution is mixed with the mass ratio of solution A with 1:1.2, obtain mixing solutions B; Then mixing solutions B is heated to 70 ℃, then to add glycerol and particle diameter in the mixing solutions B under high-speed stirring be the carboxymethyl starch of 200-1000nm, reacted 40 minutes, finally obtain containing the dual wavelength extinction anti-forgery ink additive of zinc oxide; Wherein, the glycerol that adds account for step 3) the nano zine oxide solution quality 25%, the particle diameter that adds is 10% of the carboxymethyl starch of the 200-1000nm nano zine oxide solution quality that accounts for step 3).
Embodiment 15:
1) with the 4.5g particle diameter be the deionized water that the zinc oxide of 80-200nm is placed in 120g, then the sucrose fatty ester and the stearyl dimethyl benzyl ammonium chloride that add 0.25g, at room temperature utilize again ultrasonic wave that the mixed system ultra-sonic dispersion that obtains is even, namely obtain nano oxidized zinc solution;
2) be that the poly-ethylenedioxy thiophene solution of the polystyrolsulfon acid doping of 1.3-1.7% mixes with the deionization water of 10g with the 10g solid content, then add the sodium laurylsulfonate of 0.02g, then utilize ultrasonic wave dispersion 80min to obtain solution A under 20 ℃;
3) nano oxidized zinc solution is mixed with the mass ratio of solution A with 1:1.5, obtain mixing solutions B; Then mixing solutions B is heated to 50 ℃, then to add glycerol and particle diameter in the mixing solutions B under high-speed stirring be the carboxymethyl starch of 200-1000nm, reacted 55 minutes, finally obtain containing the dual wavelength extinction anti-forgery ink additive of zinc oxide; Wherein, the glycerol that adds account for step 3) the nano zine oxide solution quality 25%, the particle diameter that adds is 8% of the carboxymethyl starch of the 200-1000nm nano zine oxide solution quality that accounts for step 3).
Sucrose fatty ester in embodiment 15 step 1) and stearyl dimethyl benzyl ammonium chloride can also adopt other cats product and/or nonionogenic tenside to replace, and cats product and/or the nonionogenic tenside specifically selected are as shown in table 2:
Table 2
Embodiment 26:
1) with the 4g particle diameter be the deionized water that the zinc oxide of 80-200nm is placed in 100g, then add the 1-hydroxyethyl of 0.30g-2-heptadecyl-tetrahydroglyoxaline, at room temperature utilize again ultrasonic wave that the mixed system ultra-sonic dispersion that obtains is even, namely obtain nano oxidized zinc solution;
2) be that the poly-ethylenedioxy thiophene solution of the polystyrolsulfon acid doping of 1.3-1.7% mixes with the deionization water of 10g with the 10g solid content, then add the alpha-sulfo monocarboxylic acid of 0.02g, then utilize ultrasonic wave dispersion 40min to obtain solution A under 20 ℃;
3) nano oxidized zinc solution is mixed with the mass ratio of solution A with 1:1, obtain mixing solutions B; Then mixing solutions B is heated to 40 ℃, then to add ethylene glycol and particle diameter in the mixing solutions B under high-speed stirring be the polynite of 200-1000nm, reacted 60 minutes, finally obtain containing the dual wavelength extinction anti-forgery ink additive of zinc oxide; Wherein, the ethylene glycol that adds account for step 3) the nano zine oxide solution quality 40%, the particle diameter that adds is 5% of the polynite of the 200-1000nm nano zine oxide solution quality that accounts for step 3).
Embodiment 27:
1) with the 4.2g particle diameter be the deionized water that the zinc oxide of 80-200nm is placed in 200g, then add the stearoyl of 0.20g for aminoethyl diethyl benzyl ammonium chloride and 1-hydroxyethyl-1-benzyl-2-tridecyl tetrahydroglyoxaline ammonium chloride, at room temperature utilize again ultrasonic wave that the mixed system ultra-sonic dispersion that obtains is even, namely obtain nano oxidized zinc solution;
2) be that the poly-ethylenedioxy thiophene solution of the polystyrolsulfon acid doping of 1.3-1.7% mixes with the deionization water of 10g with the 10g solid content, add the sodium laurylsulfonate of 0.02g, then utilize ultrasonic wave dispersion 60min to obtain solution A under 20 ℃;
3) nano oxidized zinc solution is mixed with the mass ratio of solution A with 1:1.5, obtain mixing solutions B; Then mixing solutions B is heated to 65 ℃, then to add glycerol and particle diameter in the mixing solutions B under high-speed stirring be the carboxymethyl starch of 200-1000nm, reacted 50 minutes, finally obtain containing the dual wavelength extinction aqueous anti-counterfeiting easer of zinc oxide; Wherein, the glycerol that adds account for step 3) the nano zine oxide solution quality 30%, the particle diameter that adds is 7% of the carboxymethyl starch of the 200-1000nm nano zine oxide solution quality that accounts for step 3).
Embodiment 28:
1) with the 4.2g particle diameter be the deionized water that the zinc oxide of 80-200nm is placed in 200g, then the octadecyl dimethyl hydroxyethyl quaternary ammonium nitrate that adds 0.20g, at room temperature utilize again ultrasonic wave that the mixed system ultra-sonic dispersion that obtains is even, namely obtain nano oxidized zinc solution;
2) be that the poly-ethylenedioxy thiophene solution of the polystyrolsulfon acid doping of 1.3-1.7% mixes with the deionization water of 10g with the 10g solid content, then add the sodium laurylsulfonate of 0.02g, more at room temperature utilize ultrasonic wave dispersion 80min to obtain solution A;
3) nano oxidized zinc solution is mixed with the mass ratio of solution A with 1:1.5, obtain mixing solutions B; Then mixing solutions B is heated to 65 ℃, then to add glycerol and particle diameter in the mixing solutions B under high-speed stirring be the carboxymethyl starch of 200-1000nm, reacted 50 minutes, finally obtain containing the dual wavelength extinction anti-forgery ink additive of zinc oxide; Wherein, the glycerol that adds account for step 3) the nano zine oxide solution quality 30%, the particle diameter that adds is 7% of the carboxymethyl starch of the 200-1000nm nano zine oxide solution quality that accounts for step 3).
Embodiment 29:
1) with the 4.2g particle diameter be the deionized water that the zinc oxide of 80-200nm is placed in 200g, then the N that adds 0.20g, N-double hydroxyethyl laurylamide, more at room temperature utilize ultrasonic wave that the mixed system ultra-sonic dispersion that obtains is even, namely obtain nano oxidized zinc solution;
2) just the 10g solid content is that the poly-ethylenedioxy thiophene solution of the polystyrolsulfon acid doping of 1.3-1.7% mixes with the deionization water of 10g, then adds the sodium laurylsulfonate of 0.02g, more at room temperature utilizes ultrasonic wave dispersion 50min to obtain solution A;
3) nano oxidized zinc solution is mixed with the mass ratio of solution A with 1:1.5, obtain mixing solutions B; Then mixing solutions B is heated to 65 ℃, then to add glycerol and particle diameter in the mixing solutions B under high-speed stirring be the carboxymethyl starch of 200-1000nm, reacted 50 minutes, finally obtain containing the dual wavelength extinction aqueous anti-counterfeiting easer of zinc oxide; Wherein, the glycerol that adds account for step 3) the nano zine oxide solution quality 30%, the particle diameter that adds is 7% of the carboxymethyl starch of the 200-1000nm nano zine oxide solution quality that accounts for step 3).
Embodiment 30:
1) with the 4.2g particle diameter be the deionized water that the zinc oxide of 80-200nm is placed in 200g, then polyoxyethylene two (dodecyl) phosphoric acid ester that adds 0.20g, at room temperature utilize again ultrasonic wave that the mixed system that obtains is uniformly dispersed, namely obtain nano oxidized zinc solution;
2) be that the poly-ethylenedioxy thiophene solution of the polystyrolsulfon acid doping of 1.3-1.7% mixes with the deionization water of 10g with the 10g solid content, then add the Yi Jiebang A of 0.02g, then utilize ultrasonic wave dispersion 70min to obtain solution A under 20 ℃;
3) nano oxidized zinc solution is mixed with the mass ratio of solution A with 1:1.5, obtain mixing solutions B; Then mixing solutions B is heated to 65 ℃, then to add glycerol and particle diameter in the mixing solutions B under high-speed stirring be the carboxymethyl starch of 200-1000nm, reacted 50 minutes, finally obtain containing the dual wavelength extinction aqueous anti-counterfeiting easer of zinc oxide; Wherein, the glycerol that adds account for step 3) the nano zine oxide solution quality 30%, the particle diameter that adds is 7% of the carboxymethyl starch of the 200-1000nm nano zine oxide solution quality that accounts for step 3).
Embodiment 31:
1) with the 4.2g particle diameter be the deionized water that the zinc oxide of 80-200nm is placed in 200g, then add the mnyristoyl of 0.20g for the aminopropyl dimethyl benzyl ammonium chloride, at room temperature utilize again ultrasonic wave that the mixed system that obtains is uniformly dispersed, namely obtain nano oxidized zinc solution;
2) be that the poly-ethylenedioxy thiophene solution of the polystyrolsulfon acid doping of 1.3-1.7% mixes with the deionization water of 10g with the 10g solid content, then add the sodium laurylsulfonate of 0.02g, then utilize ultrasonic wave dispersion 80min to obtain solution A under 20 ℃;
3) nano oxidized zinc solution is mixed with the mass ratio of solution A with 1:1.5, obtain mixing solutions B; Then mixing solutions B is heated to 65 ℃, then to add glycerol and particle diameter in the mixing solutions B under high-speed stirring be the carboxymethyl starch of 200-1000nm, reacted 50 minutes, finally obtain containing the dual wavelength extinction anti-forgery ink additive of zinc oxide; Wherein, the glycerol that adds account for step 3) the nano zine oxide solution quality 30%, the particle diameter that adds is 7% of the carboxymethyl starch of the 200-1000nm nano zine oxide solution quality that accounts for step 3).
Mnyristoyl in step 1) can also be replaced in order to lower cats product and/or nonionogenic tenside for the aminopropyl dimethyl benzyl ammonium chloride, and is specifically as shown in table 3:
Table 3
As seen from Figure 1, the absorbing wavelength of the dual wavelength extinction anti-forgery ink additive that contains zinc oxide of the present invention's preparation is 1000-1200nm and 310-340nm, the absorbancy of 310-340nm part can be measured by the long ultraviolet spectrophotometer of all-wave, as seen, the dual wavelength extinction anti-forgery ink additive that contains zinc oxide all has absorption within ultraviolet, infrared band, show that it is a kind of dual wavelength extinction additive.
The poly-ethylenedioxy thiophene solution of the polystyrolsulfon acid doping in above all embodiment namely gathers (3, the 4-Ethylenedioxy Thiophene)-poly-(styrene sulfonic acid) (PEDOT/PSS), and the cats product of not listing one by one in above-described embodiment and/or nonionogenic tenside, all can replace cats product and/or the nonionogenic tenside specifically selected in above-described embodiment step 1), thereby make the dual wavelength extinction aqueous anti-counterfeiting easer that contains zinc oxide.
Claims (5)
1. a preparation technology who contains the dual wavelength extinction aqueous anti-counterfeiting easer of zinc oxide, is characterized in that, comprises the following steps:
1) nano zine oxide is placed in deionized water, then adds tensio-active agent, at room temperature utilize ultrasonic wave that the mixed system that obtains is uniformly dispersed, namely obtain nano oxidized zinc solution; Wherein, the mass ratio of zinc oxide, deionized water, tensio-active agent is (4-5): (100-200): (0.20-0.35), tensio-active agent is cats product and/or nonionogenic tenside;
2) the poly-ethylenedioxy thiophene solution that is the polystyrolsulfon acid doping of 1.3-1.7% according to the mass ratio of 1:1 with solid content mixes with deionized water, then adds anion surfactant, then utilizes ultrasonic wave to be uniformly dispersed under 20-70 ℃, obtains solution A; Wherein, the poly-ethylenedioxy thiophene solution of polystyrolsulfon acid doping and the mass ratio of anion surfactant are 10:0.02;
3) with nano oxidized zinc solution with solution A with 1:(1-1.5) mass ratio mix, obtain mixing solutions B; Then mixing solutions B is heated to 40-70 ℃, more under agitation to add alcoholic solvent and particle diameter in the mixing solutions B be the powder of 200-1000nm, reacted 40-60 minute, finally obtain containing the dual wavelength extinction aqueous anti-counterfeiting easer of zinc oxide; Wherein, the alcoholic solvent that adds accounts for the 25-40% of the nano zine oxide solution quality of step 3), and alcoholic solvent is ethylene glycol or glycerol; The powder that adds accounts for the 5-10% of the nano zine oxide solution quality of step 3), and powder is polynite or carboxymethyl starch.
2. the preparation technology who contains the dual wavelength extinction aqueous anti-counterfeiting easer of zinc oxide according to claim 1, it is characterized in that: in described step 1), the particle diameter of nano zine oxide is 80-200nm.
3. the preparation technology who contains the dual wavelength extinction aqueous anti-counterfeiting easer of zinc oxide according to claim 1 is characterized in that: in described step 1), cats product is that rope Luo Ming A, handkerchief Sa Ming A, oleoyl are for aminoethyl diethylamide, A Keweier A, polyethylene polyamines salt, imidazoline surfactant, high fatty amine salt, quaternary ammonium salt cationic surfactant, N
αThe mixture of one or more arbitrary proportions in-coconut acyl arginine ethyl ester, pyridine salt type cats product, quinolinium type cats product, double quaternary ammonium salt type cats product, sulfonium salt type cats product, phosphonium salt type cats product, Arsenic salt type cats product;
Nonionogenic tenside is the mixture of one or more arbitrary proportions in polyoxyethylene-type surfactant, polyoxyethylene polyoxypropylene block type polyethers, EPE polyol EPE, triethanolamine monostearate, phosphorous nonionogenic tenside, amino acid derivative nonionogenic tenside.
4. the preparation technology who contains the dual wavelength extinction aqueous anti-counterfeiting easer of zinc oxide according to claim 3 is characterized in that:
Described polyethylene polyamines salt is quaternized poly 4 vinyl pyridine, poly-sulfuric acid trimethylammonium polyethylene ammonium or polyvinyl lactam hydrochloride;
Described imidazoline surfactant is 1-hydroxyethyl-2-alkyl-tetrahydroglyoxaline, and wherein, in 1-hydroxyethyl-2-alkyl-tetrahydroglyoxaline, the carbonatoms of alkyl is 5-20;
Described high fatty amine salt is to utilize in hydrochloric acid, formic acid or acetic acid and product that senior primary amine, senior secondary amine or senior tertiary amine obtain;
Described quaternary ammonium salt cationic surfactant is that alkyl trimethyl quaternary ammonium salt, alkyl dimethyl benzyl quaternary ammonium salt, alkyl dimethyl ethoxyl quaternary ammonium salt, fatty acyl are for the mixture of one or more arbitrary proportions in amino tri alkyl quaternary ammonium salt, imidazoline type quaternary ammonium salt;
Described polyoxyethylene-type surfactant is the mixture of one or more arbitrary proportions in fatty acyl alkanolamine, Viscotrol C ethylene oxide adduct, long-chain fat polyoxyethylenated alcohol, alkylphenol polyoxyethylene, polyoxyethylene carboxylate, aliphatic amine polyoxyethylene ether, fatty acyl alkanolamine Soxylat A 25-7;
Described polyoxyethylene polyoxypropylene block type polyethers is the mixture of one or more arbitrary proportions in polyoxyethylene polyoxypropylene block type polyethers, polyoxyethylene polyoxypropylene polyoxyethylene blocks type polyethers, polyoxyethylene polyoxypropylene polyoxypropylene block type polyethers;
Described EPE polyol EPE is the mixture of one or more arbitrary proportions in glyceryl ester type tensio-active agent, polyglycerol fatty acid ester, pentaerythritol fatty ester, dehydration Xylitol fatty acid ester, Span, sorbitan fatty acid ester, tween, sucrose fatty ester, alkyl glycoside, Polyglycerine poly monoricinolein;
The acid amides of the nonionogenic tenside that described amino acid derivative nonionogenic tenside is glutamic acid derivatives, the ester class of N-acylamino acid, N-acylamino acid, the mixture of one or more arbitrary proportions in urea groups methylene oleylamide.
5. according to claim 1 or 3 described preparation technologies that contain the dual wavelength extinction aqueous anti-counterfeiting easer of zinc oxide, it is characterized in that: the anion surfactant in described step 3) is sodium laurylsulfonate, benzene sulfonic acid sodium salt, sulfonated α-olefin, alpha-sulfo monocarboxylic acid or Yi Jiebang A.
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