CN104988793A - Reversible photochromic anti-counterfeit paper and preparation method thereof - Google Patents
Reversible photochromic anti-counterfeit paper and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of anti-counterfeit paper manufacturing, and particularly discloses reversible photochromic anti-counterfeit paper and a preparation method thereof. The reversible photochromic anti-counterfeit paper is composed of a reversible color-shifting coating and paper-base carrier materials, the reversible color-shifting coating is composed of paint including reversible photochromic substances, and the paper-base carrier materials are formed by one or two fibrous materials of bleached softwood or bleached broadleaf wood through perpermaking. The preparation method comprises the steps that the reversible photochromic substances are added into the paint to be made into the reversible photochromic paint; the surfaces of the paper-base carrier materials are coated with a reversible photochromic paint, a reversible photochromic coating is formed after drying is conducted, and the reversible photochromic anti-counterfeit paper is obtained. According to the reversible photochromic anti-counterfeit paper and the preparation method thereof, the reversible photochromic substances are added into the paint to be applied to anti-counterfeit paper, and the reversible photochromic anti-counterfeit paper and the preparation method thereof have the advantages of being fast in detection, good in thermal stability, long in retention cycle, good in reversibility of color change and strong in anti-counterfeit capacity.
Description
Technical field
The invention belongs to cheque paper manufacturing technology field, be specifically related to a kind of photo-induced reversible color-changing anti-counterfeit paper and preparation method thereof.
Background technology
Along with development that is economic and society, kind and the demand of speciality paper product constantly increase, competition between commodity is also more and more fierce, and in order to prevent illegal competitor from copying independent research product, anti-counterfeiting technology is applied in the middle of the exploitation of new product more and more.With regard to existing anti-counterfeiting technology, be divided into physical security, chemistry is false proof and biology is false proof.Optical means wherein in physical method is widely used because of simple to operate, and wherein photochromism is comparatively common, and ultraviolet light induced variable color detects easy, and can repeatedly operate, and is current most widely used general and the most ripe photochromism anti-forging technology.But at photochromism anti-forging technical elements, the research in past makes coating or ink mainly with the form of microcapsules, the shortcomings such as realize multilayer reversible color, there is poor durability, aberration is few, and retention cycle is short.
Spiro-pyrans is as photochromic organic monomer, by illumination isomerization, form the reversible transition of colourless closed loop body spiro-pyrans and coloured open loop body, owing to having special photosensitive effect and fluorescent effect, become one of attractive host molecule in anti-fake material field.Spiropyran compounds closed loop configuration is relatively stable, and be not subject to extraneous factor (temperature, concentration, pH etc.) impact, and open loop structure is comparatively subject to extraneous factor impact, especially temperature influence is larger.Due to spiropyran compounds open loop structure poor heat stability, limit its large-scale application in field of photovoltaic materials.Therefore the current research to spiropyran compounds mainly concentrates on and solves heat irreversible.
Summary of the invention
For solving the shortcoming and defect part of prior art, primary and foremost purpose of the present invention is to provide a kind of photo-induced reversible color-changing anti-counterfeit paper.This photo-induced reversible color-changing anti-counterfeit paper, by adding photo-induced reversible electrochromic substance in coating, is coated in paper substrate surfaces of carrier materials and forms photo-induced reversible discoloration coating, gives paper photo-induced reversible color shifting properties, thus reaches false proof object.
Another object of the present invention is to the preparation method that above-mentioned photo-induced reversible color-changing anti-counterfeit paper is provided.
For achieving the above object, the present invention adopts following technical scheme:
A kind of photo-induced reversible color-changing anti-counterfeit paper, this photo-induced reversible color-changing anti-counterfeit paper is made up of photo-induced reversible discoloration coating and paper substrate carrier material, described photo-induced reversible discoloration coating is made up of the coating containing photo-induced reversible electrochromic substance, and paper substrate carrier material is manufactured paper with pulp by the one in bleached softwood wood or bleaching broad-leaved wood fiber raw material or two kinds and formed.
The described coating containing photo-induced reversible electrochromic substance is: comprise the pigment that 60 ~ 80 parts by mass kaolin and 20 ~ 40 parts by mass grinding calcium carbonates (GCC) form, and account for pigment gross mass 1% ~ 2% photo-induced reversible electrochromic substance, account for pigment gross mass 10% ~ 20% styrene-butadiene latex, account for pigment gross mass 0.2% ~ 1% dispersant, account for the oxidized starch of pigment gross mass 0 ~ 5% and account for the defoamer of pigment gross mass 0.2% ~ 0.5%.
Described photo-induced reversible electrochromic substance is shitosan spiro-pyrans graft copolymer.
Described shitosan spiro-pyrans graft copolymer can obtain in accordance with the following methods:
(1) according to document (Lin Youwen, Xu Chen, Lu Canhui. cm-chitosan synthesis condition research [J]. chemistry world, 2000,41 (8): 415-417.DOI:10.3969/j.issn.0367-6358.2000.08.006.) method described in prepares cm-chitosan: in there-necked flask, add shitosan 1 part of (parts by mass, down together), isopropyl alcohol 15 parts, mass concentration are 30%NaOH aqueous slkali 25 parts, heating water bath, stir and drip the acetic acid 6 parts (adding in 30min) be dissolved in 20 parts of isopropyl alcohols down, at 65 DEG C, react 8h; Reaction is finished, cooling, and point water-yielding stratum sticky matter, adds 50 parts of distilled water, fully stirs and uses mass fraction 10%HCl to regulate pH=7, elimination insoluble matter; The methyl alcohol adding 4 times amount in filtrate fully precipitates, and filters, and absolute ethanol washing precipitates, and solid, in the oven dry of 100 DEG C, baking oven, is ground to 200 orders, obtains cm-chitosan after oven dry;
(2) according to document (Liu Maodong. the research [D] of chitosan graft/doping spiro-pyrans, spiral shell oxazine and photochromic properties. Northwest Normal University, method 2005.DOI:10.7666/d.y721789.) prepares shitosan spiro-pyrans graft copolymer: take a certain amount of cm-chitosan, adds excessive SOCl
2, backflow 48h, NaOH solution is except tail gas; Distillation removing SOCl
2, obtain yellowish-brown powder chloride shitosan; Finally, get the spiro-pyrans of chloride shitosan and triplication, join in the excessive propanone solution containing a small amount of NaOH respectively, backflow 15h, after having reacted, in apparatus,Soxhlet's, use acetone, water washing respectively to cleaning solution no longer variable color, obtain shitosan spiro-pyrans graft copolymer.
Described dispersant is one or several the mixing in calgon, sodium pyrophosphate or Sodium Polyacrylate.
Described defoamer is polyoxyethylene ether.
The preparation method of above-mentioned photo-induced reversible color-changing anti-counterfeit paper, comprises the following steps:
(1) take raw material according to following ratio: comprise the pigment that 60 ~ 80 parts by mass kaolin and 20 ~ 40 parts by mass grinding calcium carbonates (GCC) form, and account for pigment gross mass 1% ~ 2% photo-induced reversible electrochromic substance, account for pigment gross mass 10% ~ 20% styrene-butadiene latex, account for pigment gross mass 0.2% ~ 1% dispersant, account for the oxidized starch of pigment gross mass 0 ~ 5% and account for the defoamer of pigment gross mass 0.2% ~ 0.5%;
(2) the photo-induced reversible electrochromic substance that step (1) weighs up is added in kaolin, grinding calcium carbonate (GCC), styrene-butadiene latex, dispersant, oxidized starch and defoamer the coating made containing photo-induced reversible electrochromic substance;
(3) paint containing photo-induced reversible electrochromic substance step (2) obtained, at paper substrate carrier surface, forms photo-induced reversible discoloration coating after drying, obtains described photo-induced reversible color-changing anti-counterfeit paper.
The concrete steps of described step (2) are: join in the water of 100 parts by mass by kaolin and grinding calcium carbonate (GCC), then add dispersant high speed dispersion 10 ~ 15min under 8000 ~ 15000r/min rotating speed; Add a part of defoamer again, stir 2 ~ 5min in 800 ~ 1500r/min; Add styrene-butadiene latex and oxidized starch again, stir 5 ~ 10min in 8000 ~ 15000r/min; Add another part defoamer again, stir 2 ~ 5min in 800 ~ 1500r/min; Finally add photo-induced reversible electrochromic substance, stir 5 ~ 10min in 8000 ~ 15000r/min, obtain the described coating containing photo-induced reversible electrochromic substance.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) the invention provides a kind of photo-induced reversible color-changing anti-counterfeit paper and manufacture method thereof, the method adopts shitosan and spiro-pyrans graft copolymer to be used as photo-induced reversible electrochromic substance, conventional means is adopted to add in the middle of coating by this material, to the coatings of this material be contained on paper substrate again by conventional papermaking coating technique, produce the cheque paper with photo-induced reversible color shifting properties, simple to operate, be convenient to industrial applications.
(2) the present invention adopts shitosan spiro-pyrans graft copolymer as photo-induced reversible electrochromic substance, overcome spiropyran compounds open loop structure to heat-labile shortcoming, obtained photo-induced reversible color-changing anti-counterfeit paper has thermal reversibility, not by the impact of environment temperature, develop the color sensitive, easy to use, retention cycle is long.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
A preparation method for photo-induced reversible color-changing anti-counterfeit paper, comprises the following steps:
(1) take each raw material according to following ratio: the pigment be made up of 70 parts by mass kaolin and 30 parts by mass grinding calcium carbonates (GCC), and account for pigment gross mass 1% photo-induced reversible electrochromic substance shitosan spiro-pyrans graft copolymer, account for pigment gross mass 15% styrene-butadiene latex, account for pigment gross mass 0.5% sodium hexametaphosphate dispersant, account for the oxidized starch of pigment gross mass 3% and account for the defoamer polyoxyethylene ether of pigment gross mass 0.2%;
(2) kaolin step (1) weighed up and grinding calcium carbonate (GCC) join in the water of 100 parts by mass, then add sodium hexametaphosphate dispersant high speed dispersion 13min under 10000r/min rotating speed; Add half polyoxyethylene ether again, stir 3min in 1000r/min; Add styrene-butadiene latex and oxidized starch again, stir 8min in 10000r/min; Add second half polyoxyethylene ether again, stir 3min in 1000r/min; Finally add photo-induced reversible electrochromic substance shitosan spiro-pyrans graft copolymer, stir 8min in 10000r/min, obtain the coating containing photo-induced reversible electrochromic substance;
(3), on the paper base material of being manufactured paper with pulp to full bleaching softwood pulp by coater by the coating containing photo-induced reversible electrochromic substance obtained for step (2), photo-induced reversible color-changing anti-counterfeit paper after oven dry, is obtained.Under ultra violet lamp, this cheque paper is aobvious red, and under visible light illumination, this cheque paper reverts to rapidly again colourless.Be placed in by this cheque paper at 45 DEG C of temperature and take out after 24h, under ultra violet lamp, this cheque paper is aobvious red, and under visible light illumination, this cheque paper reverts to rapidly again colourless.After this cheque paper normal temperature is preserved 100 days, under ultra violet lamp, this cheque paper is aobvious red, and under visible light illumination, this cheque paper reverts to rapidly again colourless.
Embodiment 2
A preparation method for photo-induced reversible color-changing anti-counterfeit paper, comprises the following steps:
(1) take each raw material according to following ratio: the pigment be made up of 70 parts by mass kaolin and 30 parts by mass grinding calcium carbonates (GCC), and account for pigment gross mass 2% photo-induced reversible electrochromic substance shitosan spiro-pyrans graft copolymer, account for pigment gross mass 20% styrene-butadiene latex, account for the dispersant sodium pyrophosphate of pigment gross mass 0.5% and account for the defoamer polyoxyethylene ether of pigment gross mass 0.5%;
(2) kaolin step (1) weighed up and grinding calcium carbonate (GCC) join in the water of 100 parts by mass, then add dispersant sodium pyrophosphate high speed dispersion 10min under 15000r/min rotating speed; Add half polyoxyethylene ether again, stir 2min in 1500r/min; Add styrene-butadiene latex again, stir 10min in 8000r/min; Add second half polyoxyethylene ether again, stir 2min in 1500r/min; Finally add photo-induced reversible electrochromic substance shitosan spiro-pyrans graft copolymer, stir 5min in 15000r/min, obtain the coating containing photo-induced reversible electrochromic substance;
(3), on the paper base material of being manufactured paper with pulp to full bleaching softwood pulp by coater by the coating containing photo-induced reversible electrochromic substance obtained for step (2), photo-induced reversible color-changing anti-counterfeit paper after oven dry, is obtained.Under ultra violet lamp, this cheque paper is aobvious red, and under visible light illumination, this cheque paper reverts to rapidly again colourless.Be placed in by this cheque paper at 45 DEG C of temperature and take out after 24h, under ultra violet lamp, this cheque paper is aobvious red, and under visible light illumination, this cheque paper reverts to rapidly again colourless.After this cheque paper normal temperature is preserved 100 days, under ultra violet lamp, this cheque paper is aobvious red, and under visible light illumination, this cheque paper reverts to rapidly again colourless.
Embodiment 3
A preparation method for photo-induced reversible color-changing anti-counterfeit paper, comprises the following steps:
(1) take each raw material according to following ratio: the pigment be made up of 60 parts by mass kaolin and 40 parts by mass grinding calcium carbonates (GCC), and account for pigment gross mass 2% photo-induced reversible electrochromic substance shitosan spiro-pyrans graft copolymer, account for pigment gross mass 10% styrene-butadiene latex, account for pigment gross mass 0.2% dispersant Sodium Polyacrylate, account for the oxidized starch of pigment gross mass 5% and account for the defoamer polyoxyethylene ether of pigment gross mass 0.3%;
(2) kaolin step (1) weighed up and grinding calcium carbonate (GCC) join in the water of 100 parts by mass, then add dispersant Sodium Polyacrylate high speed dispersion 15min under 8000r/min rotating speed; Add half polyoxyethylene ether again, stir 5min in 800r/min; Add styrene-butadiene latex and oxidized starch again, stir 5min in 8000r/min; Add second half polyoxyethylene ether again, stir 2min in 1000r/min; Finally add photo-induced reversible electrochromic substance shitosan spiro-pyrans graft copolymer, stir 8min in 10000r/min, obtain the coating containing photo-induced reversible electrochromic substance;
(3), on the paper base material of being manufactured paper with pulp to full bleaching hardwood pulp by coater by the coating containing photo-induced reversible electrochromic substance obtained for step (2), photo-induced reversible color-changing anti-counterfeit paper after oven dry, is obtained.Under ultra violet lamp, this cheque paper is aobvious red, and under visible light illumination, this cheque paper reverts to rapidly again colourless.Be placed in by this cheque paper at 45 DEG C of temperature and take out after 24h, under ultra violet lamp, this cheque paper is aobvious red, and under visible light illumination, this cheque paper reverts to rapidly again colourless.After this cheque paper normal temperature is preserved 100 days, under ultra violet lamp, this cheque paper is aobvious red, and under visible light illumination, this cheque paper reverts to rapidly again colourless.
Embodiment 4
A preparation method for photo-induced reversible color-changing anti-counterfeit paper, comprises the following steps:
(1) take each raw material according to following ratio: the pigment be made up of 80 parts by mass kaolin and 20 parts by mass grinding calcium carbonates (GCC), and account for pigment gross mass 1.5% photo-induced reversible electrochromic substance shitosan spiro-pyrans graft copolymer, account for pigment gross mass 15% styrene-butadiene latex, account for pigment gross mass 1% dispersant Sodium Polyacrylate, account for the oxidized starch of pigment gross mass 2% and account for the defoamer polyoxyethylene ether of pigment gross mass 0.3%;
(2) kaolin step (1) weighed up and grinding calcium carbonate (GCC) join in the water of 100 parts by mass, then add dispersant Sodium Polyacrylate high speed dispersion 10min under 15000r/min rotating speed; Add half polyoxyethylene ether again, stir 3min in 1000r/min; Add styrene-butadiene latex and oxidized starch again, stir 5min in 15000r/min; Add second half polyoxyethylene ether again, stir 3min in 1000r/min; Finally add photo-induced reversible electrochromic substance shitosan spiro-pyrans graft copolymer, stir 5min in 15000r/min, obtain the coating containing photo-induced reversible electrochromic substance;
(3), on the paper base material of being manufactured paper with pulp to 50% bleaching needle-point leaf pulp and 50% bleached hardwood pulp by coater by the coating containing photo-induced reversible electrochromic substance obtained for step (2), photo-induced reversible color-changing anti-counterfeit paper after oven dry, is obtained.Under ultra violet lamp, this cheque paper is aobvious red, and under visible light illumination, this cheque paper reverts to rapidly again colourless.Be placed in by this cheque paper at 45 DEG C of temperature and take out after 24h, under ultra violet lamp, this cheque paper is aobvious red, and under visible light illumination, this cheque paper reverts to rapidly again colourless.After this cheque paper normal temperature is preserved 100 days, under ultra violet lamp, this cheque paper is aobvious red, and under visible light illumination, this cheque paper reverts to rapidly again colourless.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from Spirit Essence of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (7)
1. a photo-induced reversible color-changing anti-counterfeit paper, is characterized in that, this photo-induced reversible color-changing anti-counterfeit paper is made up of photo-induced reversible discoloration coating and paper substrate carrier material; Described photo-induced reversible discoloration coating is made up of the coating containing photo-induced reversible electrochromic substance, and paper substrate carrier material is manufactured paper with pulp by the one in bleached softwood wood or bleaching broad-leaved wood fiber raw material or two kinds and formed.
2. a kind of photo-induced reversible color-changing anti-counterfeit paper according to claim 1, it is characterized in that, the described coating containing photo-induced reversible electrochromic substance is: the pigment comprising 60 ~ 80 parts by mass kaolin and 20 ~ 40 parts by mass grinding calcium carbonates composition, and account for pigment gross mass 1% ~ 2% photo-induced reversible electrochromic substance, account for pigment gross mass 10% ~ 20% styrene-butadiene latex, account for pigment gross mass 0.2% ~ 1% dispersant, account for the oxidized starch of pigment gross mass 0 ~ 5% and account for the defoamer of pigment gross mass 0.2% ~ 0.5%.
3. a kind of photo-induced reversible color-changing anti-counterfeit paper according to claim 2, is characterized in that, described photo-induced reversible electrochromic substance is shitosan spiro-pyrans graft copolymer.
4. a kind of photo-induced reversible color-changing anti-counterfeit paper according to claim 2, is characterized in that, described dispersant is one or several the mixing in calgon, sodium pyrophosphate or Sodium Polyacrylate.
5. a kind of photo-induced reversible color-changing anti-counterfeit paper according to claim 2, it is characterized in that, described defoamer is polyoxyethylene ether.
6. the preparation method of a kind of photo-induced reversible color-changing anti-counterfeit paper according to claim 2, is characterized in that, comprise the following steps:
(1) take raw material according to following ratio: comprise 60 ~ 80 parts by mass kaolin and 20 ~ 40 parts by mass grinding calcium carbonates composition pigment, and account for pigment gross mass 1% ~ 2% photo-induced reversible electrochromic substance, account for pigment gross mass 10% ~ 20% styrene-butadiene latex, account for pigment gross mass 0.2% ~ 1% dispersant, account for the oxidized starch of pigment gross mass 0 ~ 5% and account for the defoamer of pigment gross mass 0.2% ~ 0.5%;
(2) the photo-induced reversible electrochromic substance that step (1) weighs up is added in kaolin, grinding calcium carbonate, styrene-butadiene latex, dispersant, oxidized starch and defoamer the coating made containing photo-induced reversible electrochromic substance;
(3) paint containing photo-induced reversible electrochromic substance step (2) obtained, at paper substrate carrier surface, forms photo-induced reversible discoloration coating after drying, obtains described photo-induced reversible color-changing anti-counterfeit paper.
7. preparation method according to claim 6, it is characterized in that, the concrete steps of described step (2) are: kaolin and grinding calcium carbonate are joined in the water of 100 parts by mass, then add dispersant high speed dispersion 10 ~ 15min under 8000 ~ 15000r/min rotating speed; Add a part of defoamer again, stir 2 ~ 5min in 800 ~ 1500r/min; Add styrene-butadiene latex and oxidized starch again, stir 5 ~ 10min in 8000 ~ 15000r/min; Add other a part of defoamer again, stir 2 ~ 5min in 800 ~ 1500r/min; Finally add photo-induced reversible electrochromic substance, stir 5 ~ 10min in 8000 ~ 15000r/min, obtain the described coating containing photo-induced reversible electrochromic substance.
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