CN103881471A - Preparation method of rare earth florescent LOGO anti-forgery ink - Google Patents
Preparation method of rare earth florescent LOGO anti-forgery ink Download PDFInfo
- Publication number
- CN103881471A CN103881471A CN201410048362.8A CN201410048362A CN103881471A CN 103881471 A CN103881471 A CN 103881471A CN 201410048362 A CN201410048362 A CN 201410048362A CN 103881471 A CN103881471 A CN 103881471A
- Authority
- CN
- China
- Prior art keywords
- preparation
- stirring
- rare
- coordination compound
- earth
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 32
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 238000003756 stirring Methods 0.000 claims description 55
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 150000001875 compounds Chemical class 0.000 claims description 30
- 239000003795 chemical substances by application Substances 0.000 claims description 25
- 239000006185 dispersion Substances 0.000 claims description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 229910052693 Europium Inorganic materials 0.000 claims description 15
- 241000237502 Ostreidae Species 0.000 claims description 15
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- 238000012986 modification Methods 0.000 claims description 15
- 230000004048 modification Effects 0.000 claims description 15
- 235000020636 oyster Nutrition 0.000 claims description 15
- 229910052710 silicon Inorganic materials 0.000 claims description 15
- 239000010703 silicon Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 239000003995 emulsifying agent Substances 0.000 claims description 10
- 239000003921 oil Substances 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 claims description 7
- YNPNZTXNASCQKK-UHFFFAOYSA-N Phenanthrene Natural products C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 230000003252 repetitive effect Effects 0.000 claims description 5
- 238000005201 scrubbing Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 238000007639 printing Methods 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000000295 emission spectrum Methods 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 239000000123 paper Substances 0.000 description 15
- 238000004519 manufacturing process Methods 0.000 description 10
- 238000004806 packaging method and process Methods 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- CMGDVUCDZOBDNL-UHFFFAOYSA-N 4-methyl-2h-benzotriazole Chemical compound CC1=CC=CC2=NNN=C12 CMGDVUCDZOBDNL-UHFFFAOYSA-N 0.000 description 1
- 241000519996 Teucrium chamaedrys Species 0.000 description 1
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000001815 facial effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000002211 ultraviolet spectrum Methods 0.000 description 1
Abstract
The invention relates to anti-forgery ink, particularly relates to a preparation method of rare earth florescent LOGO anti-forgery ink, and belongs to the technical field of ink printing. The preparation method comprises the steps of EUCL3 preparation, Eu(BA)(TTA)2Phen quaternary complex preparation and synthesis treatment. The preparation method of the rare earth florescent LOGO anti-forgery ink has the advantages of narrow emission spectrum, high color purity, good monochromaticity, high luminous intensity, high fluorescence efficiency, good product quality stability and good environmental protection property.
Description
Technical field
The present invention relates to a kind of anti-forgery ink, relate in particular to a kind of preparation method of rare-earth fluorescent LOGO anti-forgery ink, belong to ink printing technical field.
Background technology
The mechanical propertys such as corruggted wrapping case has light weight, resistance to compression, resistance toly exposes, anti tear and buffering, shockproof, easy machine-shaping, there is good embellish and pressing adaptability simultaneously, can cycling and reutilization, the advantages such as environmentally safe, both economical, light and easily stacking again.Its use range is more and more wider, and tempo is piece more and more, is most popular packaging vessel in modern packaging, is also one of most important packaged form of adopting of world.
China packaging industry has been brought into play vital role in national economy at present.China's wrapping paper goods output value accounts for total package industrial output 40%, accounts for more than 45% in developed country.And the Corrugated Box output value accounts for the more than 60% of the paper wrapper goods gross output value.Although world economy repeatedly faced adjustment in recent years, in world's packed in cases industry, Asia still keeps the fastest rate of growth, and in all states in Asia, the rate of growth of China is the fastest.The far super world average level of growth of China's Corrugated Box packaging.
China's Corrugated Box packaging is started late, and since reform and opening-up, China's Corrugated Box packaging develops rapidly, and rate of growth is the highest in each big producing country.Nineteen ninety-five, output was 7,400,000,000 square metres, and 2000 annual production are 12,300,000,000 square metres, 134.58 hundred million square metres, Japan, 12,300,000,000 square metres, China.China is since nineteen ninety-five, and corrugated board production amount occupies the 3rd, the world always, is only second to the U.S. and Japan.Within 2010, our corrugated board production amount has exceeded the U.S., leaps to the 1st, the world.
Zhejiang Province is the large province of China's packaging.Large city of Hangzhou and the industry region, Qian Tang gulf of adjoining thereof are the important bases of Zhejiang Province's production, more than 1,000 ten thousand tons of the packing board annual production including coated manila, the important production base of Hangzhou Ye Shi China Packaging Box and packing board.In addition Hangzhou or Asia package centre.Therefore, the development of Packaging Box industry is for the Economic Contribution of Hangzhou, all have great importance for the labour employment of Hangzhou and the induced effect of other industries.
As most important Transport Package form, " false proof " of Corrugated Box is that one of Chinese commodity packaging field has to face all the time, but very heavy topic.The commodity of some reputable brands and high added value often can suffer the infringement of illegal " Lee's ghost ", and " false proof " measure of common tr in the market, mainly contains following several: when cardboard box printing, adopt " anti-forgery ink "; On carton, stick on " laser anti-counterfeit label "; Print additional or stick on " barcode " etc.
The effect of above method is all not satisfactory, and easily, processing is simple in the former " anti-forgery ink " source, and star is as the little carton factory of scattereding all over like men on a chessboard, and almost every household can be done.And " laser anti-counterfeit label " that the second is produced is also that midget plant and family workshop are made mostly, management and control is lax, and it is very convenient that bad personnel will obtain these labels.And be finally " dedicated decoders " or the Help by Phone etc. of commonly using, formality trouble, program are loaded down with trivial details, and anti-counterfeiting performance is poor, is difficult to popularize.For this reason, many scientific research institutions and manufacturing enterprise are all carrying out unremitting research and probe, as: adopt flexible printing technology antiforge pattern on carton; Between fluting board and core paper, embed three colo(u)r streak material marks; ; Between fluting board and printing facial tissue, intelligent electronic tag (being provided with microchip and antenna etc.) is set; In conventional cardboard, integrate again into the ultra-fine corrugated cardboard of one deck, as false proof means, i.e. so-called " false seven layers ", " false nine layers " etc.The false proof measure that these new inventions, new technology have is too simple, there is no characteristic, some production cost costlinesses, and what have is difficult to carry out industrialization volume production, does not therefore have industrial applicibility.
Summary of the invention
The present invention solves the deficiencies in the prior art, provide a kind of rare-earth fluorescent ink formulation of producing in the water color ink of conventional Corrugated Box production use, by flexographic presses, the LOGO of enterprise or the security pattern that is equipped with are printed, pattern after printing is recessive, in fake certification, adopt the UV spectrum of 383nm left and right to excite its LOGO or security pattern, inspire the ruddiness of the 614nm that intensity is stronger, demonstrate the preparation method of a kind of rare-earth fluorescent LOGO anti-forgery ink of security pattern.
Above-mentioned technical problem of the present invention is mainly solved by following technical proposals:
A preparation method for rare-earth fluorescent LOGO anti-forgery ink, carries out according to the following steps:
(1), EUCL
3preparation:
By EU
2o
3join in dilute hydrochloric acid, dilute hydrochloric acid concentration is 2.0～3.0 mol/L, is provided with the EU of 350g in the dilute hydrochloric acid of every 2～3L
2o
3, then stir, after stirring, solution becomes transparent liquid by muddiness, and adding weak base to regulate pH value is 6.5～7, makes EUCL
3the aqueous solution;
(2), Eu (BA) (TTA)
2the preparation of Phen quaternary coordination compound:
To make EuCl
3the aqueous solution mix than 1:2 according to amount of substance with TTA, again Phen, BA are added drop-wise in mixed solution, filter with the middling speed industrial filter paper of 30～50um, after filtering, wash with the warm water of 25 degree～35 degree, be at 50～60 DEG C, to carry out freeze-day with constant temperature 24 hours by the solid matter on industrial filter paper in temperature, make quaternary coordination compound;
(3), synthetic processing:
First by Synolac, Dormant oils alcohol liquid, nonionic emulsifying agent and PEO dispersion agent carry out mixing and stirring, after stirring, carry out milled processed, the fineness of grinding distribution is 16～19um, add again the quaternary coordination compound in step (2), modification polydimethyl silicon, PEO dispersion agent, quaternary coordination compound, modification polydimethyl silicon and PEO dispersion agent account for 1～2% of total mass ratio, addition sequence is followed successively by quaternary coordination compound, PEO dispersion agent, modification polydimethyl silicon, in the process adding, need to continue to stir, add the churning time of new material to be not less than 20 minutes at every turn, obtain shallow oyster white rare-earth europium Antiforge fluorescent ink.
As preferably, in step (1), dilute hydrochloric acid slowly splashes into, and the speed splashing into is 3.5ml/min, stirs while splashing into, and solution is become transparent by muddiness; The time of stirring is not less than 30 min, and the speed of stirring is 500～1000 rpm.
As preferably, in step (2), the time that middling speed industrial filter paper filters is 15～20min, and with carrying out warm water washing in electric-heated thermostatic water bath, the time of warm water washing is 30～40min, and stirring velocity when warm water washs is 500～1000rpm.
As preferably, the stirring velocity that adds new material in step (3) is 100～500 rpm, and the time of stirring is 80～130min; The shallow oyster white rare-earth europium Antiforge fluorescent ink obtaining is proceeded in encloses container, under 130 DEG C of high temperature, react 8h, cooling rear taking-up product, first with carrying out repetitive scrubbing 2 times with distilled water after dehydrated alcohol, the time of each washing is about 20～30min, and freeze-day with constant temperature obtains light orange look pressed powder.
As preferably, in step (3), making viscosity is 18～25pa.s, the shallow oyster white rare-earth europium Antiforge fluorescent ink that degree of mobilization is 37～40mm; Synolac: Dormant oils alcohol liquid: nonionic emulsifying agent: quaternary coordination compound: the mass ratio of PEO dispersion agent equals 73～76:15～16:1～1.2:6～7:2～2.5.
TTA refers to tolyltriazole.Phen refers to o-phenanthroline.BA refers to phenylformic acid.
Anti-forgery ink, under the exciting of UV-light 383nm, produces the ruddiness of 614nm.
Therefore, the preparation method of a kind of rare-earth fluorescent LOGO anti-forgery ink of the present invention, has emmission spectrum narrow, and purity of color is high, and monochromaticity is good, and luminous intensity is high, and fluorescence efficiency is high, and constant product quality is good, and the feature of environmental protection is strong.
Embodiment
Below by embodiment,, technical scheme of the present invention is described in further detail.
Embodiment 1: a kind of preparation method of rare-earth fluorescent LOGO anti-forgery ink, carries out according to the following steps:
(1), EUCL
3preparation:
By EU
2o
3join in dilute hydrochloric acid, dilute hydrochloric acid concentration is 2.0 mol/L, is provided with the EU of 350g in the dilute hydrochloric acid of every 2L
2o
3, then stir, after stirring, solution becomes transparent liquid by muddiness, and adding weak base to regulate pH value is 6.5, makes EUCL
3the aqueous solution;
(2), Eu (BA) (TTA)
2the preparation of Phen quaternary coordination compound:
To make EuCl
3the aqueous solution mix than 1:2 according to amount of substance with TTA, again Phen, BA are added drop-wise in mixed solution, filter with the middling speed industrial filter paper of 30um, after filtering, wash with the warm water of 25 degree, be at 50 DEG C, to carry out freeze-day with constant temperature 24 hours by the solid matter on industrial filter paper in temperature, make quaternary coordination compound;
(3), synthetic processing:
First by Synolac, Dormant oils alcohol liquid, nonionic emulsifying agent and PEO dispersion agent carry out mixing and stirring, after stirring, carry out milled processed, the fineness of grinding distribution is 16um, add again the quaternary coordination compound in step (2), modification polydimethyl silicon, PEO dispersion agent, quaternary coordination compound, modification polydimethyl silicon and PEO dispersion agent account for 1% of total mass ratio, addition sequence is followed successively by quaternary coordination compound, PEO dispersion agent, modification polydimethyl silicon, in the process adding, need to continue to stir, add the churning time of new material to be not less than 20 minutes at every turn, obtain shallow oyster white rare-earth europium Antiforge fluorescent ink.
In step (1), dilute hydrochloric acid slowly splashes into, and the speed splashing into is 3.5ml/min, stirs while splashing into, and solution is become transparent by muddiness; The time of stirring is not less than 30 min, and the speed of stirring is 500rpm.
In step (2), the time that middling speed industrial filter paper filters is 15～20min, and with carrying out warm water washing in electric-heated thermostatic water bath, the time of warm water washing is 30～40min, and stirring velocity when warm water washing is 500～1000rpm.
The stirring velocity that adds new material in step (3) is 100rpm, and the time of stirring is 80min; The shallow oyster white rare-earth europium Antiforge fluorescent ink obtaining is proceeded in encloses container, under 130 DEG C of high temperature, react 8h, cooling rear taking-up product, first with carrying out repetitive scrubbing 2 times with distilled water after dehydrated alcohol, the time of each washing is about 20min, and freeze-day with constant temperature obtains light orange look pressed powder.
In step (3), making viscosity is 18pa.s, the shallow oyster white rare-earth europium Antiforge fluorescent ink that degree of mobilization is 37mm; Synolac: Dormant oils alcohol liquid: nonionic emulsifying agent: quaternary coordination compound: the mass ratio of PEO dispersion agent equals 73:15:1:6:2.
Embodiment 2: a kind of preparation method of rare-earth fluorescent LOGO anti-forgery ink, carries out according to the following steps:
(1), EUCL
3preparation:
By EU
2o
3join in dilute hydrochloric acid, dilute hydrochloric acid concentration is 2.5 mol/L, is provided with the EU of 350g in the dilute hydrochloric acid of every 2.5L
2o
3, then stir, after stirring, solution becomes transparent liquid by muddiness, and adding weak base to regulate pH value is 6.8, makes EUCL
3the aqueous solution;
(2), Eu (BA) (TTA)
2the preparation of Phen quaternary coordination compound:
To make EuCl
3the aqueous solution mix than 1:2 according to amount of substance with TTA, again Phen, BA are added drop-wise in mixed solution, filter with the middling speed industrial filter paper of 40um, after filtering, wash with the warm water of 30 degree, be at 55 DEG C, to carry out freeze-day with constant temperature 24 hours by the solid matter on industrial filter paper in temperature, make quaternary coordination compound;
(3), synthetic processing:
First by Synolac, Dormant oils alcohol liquid, nonionic emulsifying agent and PEO dispersion agent carry out mixing and stirring, after stirring, carry out milled processed, the fineness of grinding distribution is 18um, add again the quaternary coordination compound in step (2), modification polydimethyl silicon, PEO dispersion agent, quaternary coordination compound, modification polydimethyl silicon and PEO dispersion agent account for 1～2% of total mass ratio, addition sequence is followed successively by quaternary coordination compound, PEO dispersion agent, modification polydimethyl silicon, in the process adding, need to continue to stir, add the churning time of new material to be not less than 20 minutes at every turn, obtain shallow oyster white rare-earth europium Antiforge fluorescent ink.
In step (1), dilute hydrochloric acid slowly splashes into, and the speed splashing into is 3.5ml/min, stirs while splashing into, and solution is become transparent by muddiness; The time of stirring is not less than 30 min, and the speed of stirring is 800rpm.
In step (2), the time that middling speed industrial filter paper filters is 18min, and with carrying out warm water washing in electric-heated thermostatic water bath, the time of warm water washing is 35min, and stirring velocity when warm water washing is 800rpm.
The stirring velocity that adds new material in step (3) is 300 rpm, and the time of stirring is 100min; The shallow oyster white rare-earth europium Antiforge fluorescent ink obtaining is proceeded in encloses container, under 130 DEG C of high temperature, react 8h, cooling rear taking-up product, first with carrying out repetitive scrubbing 2 times with distilled water after dehydrated alcohol, the time of each washing is about 25min, and freeze-day with constant temperature obtains light orange look pressed powder.
In step (3), making viscosity is 20pa.s, the shallow oyster white rare-earth europium Antiforge fluorescent ink that degree of mobilization is 38mm; Synolac: Dormant oils alcohol liquid: nonionic emulsifying agent: quaternary coordination compound: the mass ratio of PEO dispersion agent equals 75:15.5:1.1:6.5:2.2.
Embodiment 3: a kind of preparation method of rare-earth fluorescent LOGO anti-forgery ink, carries out according to the following steps:
(1), EUCL
3preparation:
By EU
2o
3join in dilute hydrochloric acid, dilute hydrochloric acid concentration is 3.0 mol/L, is provided with the EU of 350g in the dilute hydrochloric acid of every 3L
2o
3, then stir, after stirring, solution becomes transparent liquid by muddiness, and adding weak base to regulate pH value is 7, makes EUCL
3the aqueous solution;
(2), Eu (BA) (TTA)
2the preparation of Phen quaternary coordination compound:
To make EuCl
3the aqueous solution mix than 1:2 according to amount of substance with TTA, again Phen, BA are added drop-wise in mixed solution, filter with the middling speed industrial filter paper of 50um, after filtering, wash with the warm water of 25 degree～35 degree, be at 60 DEG C, to carry out freeze-day with constant temperature 24 hours by the solid matter on industrial filter paper in temperature, make quaternary coordination compound;
(3), synthetic processing:
First by Synolac, Dormant oils alcohol liquid, nonionic emulsifying agent and PEO dispersion agent carry out mixing and stirring, after stirring, carry out milled processed, the fineness of grinding distribution is 19um, add again the quaternary coordination compound in step (2), modification polydimethyl silicon, PEO dispersion agent, quaternary coordination compound, modification polydimethyl silicon and PEO dispersion agent account for 2% of total mass ratio, addition sequence is followed successively by quaternary coordination compound, PEO dispersion agent, modification polydimethyl silicon, in the process adding, need to continue to stir, add the churning time of new material to be not less than 20 minutes at every turn, obtain shallow oyster white rare-earth europium Antiforge fluorescent ink.
In step (1), dilute hydrochloric acid slowly splashes into, and the speed splashing into is 3.5ml/min, stirs while splashing into, and solution is become transparent by muddiness; The time of stirring is not less than 30 min, and the speed of stirring is 1000 rpm.
In step (2), the time that middling speed industrial filter paper filters is 20min, and with carrying out warm water washing in electric-heated thermostatic water bath, the time of warm water washing is 40min, and stirring velocity when warm water washing is 1000rpm.
The stirring velocity that adds new material in step (3) is 500 rpm, and the time of stirring is 130min; The shallow oyster white rare-earth europium Antiforge fluorescent ink obtaining is proceeded in encloses container, under 130 DEG C of high temperature, react 8h, cooling rear taking-up product, first with carrying out repetitive scrubbing 2 times with distilled water after dehydrated alcohol, the time of each washing is about 30min, and freeze-day with constant temperature obtains light orange look pressed powder.
In step (3), making viscosity is 25pa.s, the shallow oyster white rare-earth europium Antiforge fluorescent ink that degree of mobilization is 40mm; Synolac: Dormant oils alcohol liquid: nonionic emulsifying agent: quaternary coordination compound: the mass ratio of PEO dispersion agent equals 76:16:1.2:7:2.5.
Claims (5)
1. a preparation method for rare-earth fluorescent LOGO anti-forgery ink, is characterized in that carrying out according to the following steps:
(1), EUCL
3preparation:
By EU
2o
3join in dilute hydrochloric acid, dilute hydrochloric acid concentration is 2.0～3.0 mol/L, is provided with the EU of 350g in the dilute hydrochloric acid of every 2～3L
2o
3, then stir, after stirring, solution becomes transparent liquid by muddiness, and adding weak base to regulate pH value is 6.5～7, makes EUCL
3the aqueous solution;
(2), Eu (BA) (TTA)
2the preparation of Phen quaternary coordination compound:
To make EuCl
3the aqueous solution mix than 1:2 according to amount of substance with TTA, again Phen, BA are added drop-wise in mixed solution, filter with the middling speed industrial filter paper of 30～50um, after filtering, wash with the warm water of 25 degree～35 degree, be at 50～60 DEG C, to carry out freeze-day with constant temperature 24 hours by the solid matter on industrial filter paper in temperature, make quaternary coordination compound;
(3), synthetic processing:
First by Synolac, Dormant oils alcohol liquid, nonionic emulsifying agent and PEO dispersion agent carry out mixing and stirring, after stirring, carry out milled processed, the fineness of grinding distribution is 16～19um, add again the quaternary coordination compound in step (2), modification polydimethyl silicon, PEO dispersion agent, quaternary coordination compound, modification polydimethyl silicon and PEO dispersion agent account for 1～2% of total mass ratio, addition sequence is followed successively by quaternary coordination compound, PEO dispersion agent, modification polydimethyl silicon, in the process adding, need to continue to stir, add the churning time of new material to be not less than 20 minutes at every turn, obtain shallow oyster white rare-earth europium Antiforge fluorescent ink.
2. the preparation method of a kind of rare-earth fluorescent LOGO anti-forgery ink according to claim 1, is characterized in that: in step (1), dilute hydrochloric acid slowly splashes into, and the speed splashing into is 3.5ml/min, stirs while splashing into, and solution is become transparent by muddiness; The time of stirring is not less than 30 min, and the speed of stirring is 500～1000 rpm.
3. the preparation method of a kind of rare-earth fluorescent LOGO anti-forgery ink according to claim 1, it is characterized in that: in step (2), the time that middling speed industrial filter paper filters is 15～20min, with carrying out warm water washing in electric-heated thermostatic water bath, the time of warm water washing is 30～40min, and stirring velocity when warm water washing is 500～1000rpm.
4. the preparation method of a kind of rare-earth fluorescent LOGO anti-forgery ink according to claim 1, is characterized in that: the stirring velocity that adds new material in step (3) is 100～500 rpm, and the time of stirring is 80～130min; The shallow oyster white rare-earth europium Antiforge fluorescent ink obtaining is proceeded in encloses container, under 130 DEG C of high temperature, react 8h, cooling rear taking-up product, first with carrying out repetitive scrubbing 2 times with distilled water after dehydrated alcohol, the time of each washing is about 20～30min, and freeze-day with constant temperature obtains light orange look pressed powder.
5. the preparation method of a kind of rare-earth fluorescent LOGO anti-forgery ink according to claim 1, is characterized in that: in step (3), making viscosity is 18～25pa.s, the shallow oyster white rare-earth europium Antiforge fluorescent ink that degree of mobilization is 37～40mm; Synolac: Dormant oils alcohol liquid: nonionic emulsifying agent: quaternary coordination compound: the mass ratio of PEO dispersion agent equals 73～76:15～16:1～1.2:6～7:2～2.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410048362.8A CN103881471B (en) | 2014-02-12 | 2014-02-12 | A kind of preparation method of rare-earth fluorescent LOGO anti-forgery ink |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410048362.8A CN103881471B (en) | 2014-02-12 | 2014-02-12 | A kind of preparation method of rare-earth fluorescent LOGO anti-forgery ink |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103881471A true CN103881471A (en) | 2014-06-25 |
| CN103881471B CN103881471B (en) | 2016-05-11 |
Family
ID=50950614
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410048362.8A Expired - Fee Related CN103881471B (en) | 2014-02-12 | 2014-02-12 | A kind of preparation method of rare-earth fluorescent LOGO anti-forgery ink |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103881471B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108192598A (en) * | 2017-12-12 | 2018-06-22 | 雷春生 | A kind of preparation method of the compound rare-earth light conversion agent of agricultural film |
| CN109232619A (en) * | 2018-11-05 | 2019-01-18 | 中山大学 | Multicolor fluorescence material based on rare earth metal organic frame and preparation method thereof and anti-counterfeiting ink application |
| CN114702860A (en) * | 2022-05-15 | 2022-07-05 | 宝艺新材料股份有限公司 | Improved water-based anti-counterfeiting ink for paperboard printing and preparation method thereof |
| CN117475356A (en) * | 2023-12-25 | 2024-01-30 | 华南理工大学 | Control method and system for preparing invisible double anti-counterfeit label by corrugated case |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101045200A (en) * | 2007-04-06 | 2007-10-03 | 山东大学 | Method for preparing micro-capsule containing high light-effect rare earth compounding matter |
| CN101070318A (en) * | 2007-06-15 | 2007-11-14 | 北京大学 | Light-sensitive luminous europium complex and light-sensitive ligand molecular and their synthesizing method |
-
2014
- 2014-02-12 CN CN201410048362.8A patent/CN103881471B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101045200A (en) * | 2007-04-06 | 2007-10-03 | 山东大学 | Method for preparing micro-capsule containing high light-effect rare earth compounding matter |
| CN101070318A (en) * | 2007-06-15 | 2007-11-14 | 北京大学 | Light-sensitive luminous europium complex and light-sensitive ligand molecular and their synthesizing method |
Non-Patent Citations (1)
| Title |
|---|
| 孟婕等: "铕配合物的合成及其荧光防伪油墨的制备", 《包装工程》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108192598A (en) * | 2017-12-12 | 2018-06-22 | 雷春生 | A kind of preparation method of the compound rare-earth light conversion agent of agricultural film |
| CN109232619A (en) * | 2018-11-05 | 2019-01-18 | 中山大学 | Multicolor fluorescence material based on rare earth metal organic frame and preparation method thereof and anti-counterfeiting ink application |
| CN109232619B (en) * | 2018-11-05 | 2020-07-24 | 中山大学 | Multicolor fluorescent material based on rare earth metal organic framework, preparation method thereof and application of anti-counterfeiting ink |
| CN114702860A (en) * | 2022-05-15 | 2022-07-05 | 宝艺新材料股份有限公司 | Improved water-based anti-counterfeiting ink for paperboard printing and preparation method thereof |
| CN117475356A (en) * | 2023-12-25 | 2024-01-30 | 华南理工大学 | Control method and system for preparing invisible double anti-counterfeit label by corrugated case |
| CN117475356B (en) * | 2023-12-25 | 2024-03-29 | 华南理工大学 | Control method and system for preparing invisible double anti-counterfeit label by corrugated case |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103881471B (en) | 2016-05-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103881471B (en) | A kind of preparation method of rare-earth fluorescent LOGO anti-forgery ink | |
| CN102154925B (en) | Production method of anti-myopia paper | |
| CN108912843A (en) | Infrared or Fluorescent Falsification-resistant Ink of one kind and preparation method thereof | |
| CN104085214A (en) | Raw paper for thermal transfer paper and preparation process thereof | |
| CN108070302B (en) | Anti-counterfeiting ink with delayed fluorescence and application thereof | |
| CN104087067A (en) | Novel fluorescent material made gravure table printing fluorescent anti-counterfeit ink | |
| CN102492329A (en) | Preparation of rare earth doped fluorescent anti-counterfeiting offset printing ink | |
| CN106588801A (en) | Dicarboxylic acid heavy calcium carbonate powder fluorescent whitening agent as well as preparation method and application thereof | |
| CN103435943A (en) | Novel lanthanum cyanurate composite PVC (polyvinyl chloride) heat stabilizer | |
| CN107603597A (en) | A kind of calcium carbonate-base fluorescent material and preparation method thereof | |
| Zhang et al. | Switchable up and down-conversion luminescent properties of Nd (III)-nanopaper for visible and near-infrared anti-counterfeiting | |
| Chandana et al. | Simple fabrication of novel Sm3+ doped BaGd2ZnO5 nanophosphors for flexible displays, improved data security applications, and solid-state lighting applications | |
| CN103756485B (en) | Water-based is coated with tin graphed sheet whitewash and preparation method thereof outward | |
| CN106283796B (en) | Old newsprint produces the production method of brown paper | |
| CN106243835A (en) | A kind of aqueous rare earth compounding complex microsphere fluorescent ink and preparation technology thereof | |
| Fan et al. | Wearing an organic “coat” on nanocrystals of LaF3: Eu3+ to generate dynamic luminescence for optical anti-counterfeit | |
| CN102583342A (en) | Purification method of microcrystal graphite | |
| CN106588800A (en) | Tetracarboxylic acid heavy calcium carbonate powder fluorescent whitening agent and preparation method and application thereof | |
| Wu et al. | Tunable multimodal printable up-/down-conversion nanomaterials for gradient information encryption | |
| CN100432164C (en) | Optical disclour printing ink with polarization effect | |
| CN111620906A (en) | Organic ultralong room temperature phosphorescent material, triple anti-counterfeiting organic ink and application | |
| CN1039649C (en) | Photochromism anti-forging printing ink and its prodn. method | |
| CN106237980B (en) | A kind of strong effective decoloring agent and preparation method thereof | |
| CN103881477A (en) | Anti-counterfeiting printing ink based on up-and-down conversion synergistic luminescence material | |
| CN103285806A (en) | Preparation technology for silicon collectors in alkali recovery section green liquor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CB03 | Change of inventor or designer information |
Inventor after: Sun Junjun Inventor after: Hu Kaitang Inventor after: Huang Yuqi Inventor after: Hu Limeng Inventor after: Wang Zhaoxia Inventor before: Hu Kaitang Inventor before: Huang Yuqi Inventor before: Hu Limeng Inventor before: Wang Zhaoxia |
|
| COR | Change of bibliographic data | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 311201 Beitang Road, economic development zone, Xiaoshan, Zhejiang, No. 2, No. Patentee after: ZHEJIANG GREAT SHENGDA PACKING Co.,Ltd. Patentee after: HANGZHOU CITY XIAOHSAN DISTRICT KAIYI PACKAGING INDUSTRY TECHNOLOGY RESEARCH AND DEVELOPMENT CENTER Address before: 311201 Beitang Road, economic development zone, Xiaoshan, Zhejiang, No. 2, No. Patentee before: ZHEJIANG GREAT SHENGDA PACKAGING CO.,LTD. Patentee before: HANGZHOU CITY XIAOHSAN DISTRICT KAIYI PACKAGING INDUSTRY TECHNOLOGY RESEARCH AND DEVELOPMENT CENTER |
|
| CP01 | Change in the name or title of a patent holder | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20170831 Address after: 311200 No. 52, Beitang Road, Xiaoshan economic and Technological Development Zone, Hangzhou, Zhejiang Patentee after: ZHEJIANG GREAT SHENGDA PACKING Co.,Ltd. Address before: 311201 Beitang Road, economic development zone, Xiaoshan, Zhejiang, No. 2, No. Co-patentee before: HANGZHOU CITY XIAOHSAN DISTRICT KAIYI PACKAGING INDUSTRY TECHNOLOGY RESEARCH AND DEVELOPMENT CENTER Patentee before: ZHEJIANG GREAT SHENGDA PACKING Co.,Ltd. |
|
| TR01 | Transfer of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160511 Termination date: 20220212 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |