CN104789000B - The high yield preparation method of micro-structural security pigment - Google Patents
The high yield preparation method of micro-structural security pigment Download PDFInfo
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Abstract
The invention discloses a kind of high yield preparation method of micro-structural security pigment, comprise the following steps：(1) the b coatings that can be peeled off with base material are coated in substrate surface；(2) anti-counterfeiting function film layer s is coated or deposited on b coatings；(3) side of the product obtained in step (2), coating or layer deposited isolating d；(4) separation layer d side, according to the method for step (2), is coated with or deposits anti-counterfeiting function film layer s；The step of repeat step (3)~(4) n times, n is the integer more than or equal to 0；(5) etching coating and the band base material pigment that the stratified film of deposition is three-dimensional regular shape；(6) it is impregnated in organic solvent, peels off pigment；(7) it is placed in separating liquid, dissolves separation layer d, filter, drying obtains described micro-structural security pigment.The present invention can realize high yield, the preparation method of the micro-structural security pigment of high efficiency, preparation process non-secondary pollution, safety and environmental protection.
Description
Technical field
The present invention relates to the preparation method of the false proof metallic pigments of micro-structural.
Background technology
In pigment, metallic pigments are a special kinds, and metallic pigments can make the thing being coated as ornamental pigment
Product are bright and colourful, with bright metallic luster and metallic travel.What consumption was maximum in metallic pigments is zinc powder, the conjunction of copper zinc
Bronze and aluminium powder (including aluminum paste).Flake aluminum is one of very important metallic pigments, and initial people mainly use it
Metal form and aspect and plate finish effect, but with science and technology and modern industry development, the kind of aluminium pigment is increasingly
It is many, high reflectance of the aluminium pigment to visible ray, ultraviolet light and infrared light so that insulation can be played by its obtained coating, prevented
The effect of light and heat radiation, makees while the laminated structure of aluminium pigment can play reduction vapor, oxygen and the infiltration of other corrosive mediums
With being widely used in the industries such as ink, coating, building, automobile and chemical industry, its glossiness to product, uniformity, planarization
And fastness is all played a very important role.These special performances of aluminium pigment, it is turned into numerous metallic pigments should
With most wide, the class that development is fast and research is more.
Metallic flake pigment has down flop property, and with the difference of observer's viewing angle, pigment is showed by bright
The bright change different to dimness.Equally, the glossiness and shade of aluminium silver powder are with the incident angle of incident light and the change at visual angle
Change the change for occurring light and color.Aluminium silver powder is arranged in carrier film with different levels, when incident light is radiated at each layer aluminium flake reflection
The obvious brightness of light gone out is also different.When light injects aluminium silver powder of the film layer containing transparent pigment and aluminium silver powder Jing Guo different levels
Reflect, occur the change of tone and metal light, the visual angle of incident light is moved from vertical gradually generation angular displacement, and light is then passed through
The aluminium silver powder of the pigment and different-grain diameter of the pigment of different number of particles and different number of particles, the light and tone reflected and
Metal light also changes.This characteristic of aluminium silver powder, has been widely used in ink, coating industry, its changeable colors along with angle
Characteristic can be used for ink antiforge by design.
Most metallic pigments powder, is produced by physical method, i.e., turn from solid-liquid or gaseous metal
Powder is turned to, is allowed to be processed as specific metal dust：Powder, such as sublimed method are converted into by the gas phase state of metal；By metal
Liquid phase state be converted into powder, such as atomization：Powder, such as ball-milling method are converted into by the solid state shape of metal.
Research with anti-fraud functional metallic pigments is less at present, Shanghai Zige Optical Membrane Material Co., Ltd.
CN201110145270.8 discloses a kind of anti-counterfeiting microstructure pigment and its manufacturing process, micro- by being molded acquisition particle diameter 1-200
Rice, the micro-structural individual layer sheet aluminium pigment of regular shape (such as character pattern, geometry), can be used as security pigment, should
Invention fabrication process is less efficient, and during pigment screening, there is irregular little particle and adhere on regular targets pigment,
So that there is more irregular little particle in final finished pigment, it is greatly affected product quality.
CIBA corporation in 2006 US20100062244 discloses a kind of preparation side of plane-parallel flake-like pigment particles
Method, is related to the separation layer between deposited on substrates separating agent layer, at least one gas producing formation and gas producing formation, gas producing formation is from base material
After separating, then by solvent by between product separation layer dissolve, by aluminum slice elution, filtering by way of isolate
Come, particle diameter is then adjusted by ultrasonication.The invention is improved prepares flake pigment work in deposited on substrates and then stripping
The production efficiency of skill, but the finished pigment that the invention is related to only is controlled particle diameter by ultrasound, is not related to pigment
The formation and control of regular shape.
The excellent Ni Fusi companies CN200610091187.6 of JDS disclose the week in the opaque flakes applied for concealed anti-false
The manufacturing process that framework or border are provided is enclosed, is related to a kind of thin film flakes of concealed anti-false application, it has by mechanical system
Compacting or embossment or etching or the mark or invisible symbol that are formed by laser mode, wherein invisible symbol can use aobvious
Micro mirror is seen.To keep the integrality of symbol, framework is provided around all or part of invisible symbols so as to when single thin
When being removed in the supporting construction that piece is deposited from them, most of thin slice along the framework thread breakage provided rather than with it is a kind of not
Controllable unforeseen mode is broken.The specific method of stripping and the post processing of pigment is not directed in the invention, face is only provided
The moulding process of tablet.
Dupont Teijin Films U. S. Ltd PA's CN200780017716.0 patents are related to one kind as false proof face
The preparation method of the particle with controlled dimensions of purposes is expected, by providing the micro-relief for including one or more separate units
The laminate substrate of repeat patterns, each unit is made up of bottom parts with the wall with height (HW)；By organic or inorganic material
It is deposited on substrate (thickness T, T≤HW), deposited organic or inorganic material is peeled off, by solvent transfer techniques in peel groove
Particle is peeled off and settled, the final particle for obtaining default controlled dimensions.The invention equally exists the relatively low shortcoming of production efficiency, together
When the manufacture method in by the size of the wall pigment set in advance with certain altitude, this is resulted in is peeled off using solvent
When, the pigment that presence can not be peeled off in hole reduces yield, while unstripped pigment can also influence laminate substrate next
The use of preparation process.
The content of the invention
It is an object of the invention to provide a kind of high yield preparation method of micro-structural security pigment, to overcome prior art to deposit
Defect.
The high yield preparation method of described micro-structural security pigment, comprises the following steps：
(1) the b coatings that can be peeled off with base material are coated in substrate surface, thickness is 0.5 μm~4 μm after drying；
Described base material is plastics, preferably BOPP, PE, PET or PA, or surface is BOPP, PE or PA composite plastic
Planarizing material；
Described b layers are obtained by the way of coating glue coating, and coating method is coated with for heliogravure full version, and coating glue makes
Resin, selection low molecular weight solvent type can redissolve resin, such as ethyl cellulose, hydroxyl modification binary vinyl chloride-vinyl acetate resin, chlorination
Polyolefin or styrene acrylic；
Described low molecular weight solvent is selected from alcohol, ester or ether, ethyl acetate, butyl acetate, isopropanol, propane diols first
One or more of ether, ethoxy-c acid ether, dimethyl succinate, dimethyl glutarate, dimethyl adipate, wherein low point
Son amount can redissolve resin content account for coating glue percentage by weight be 3%-40%；
(2) anti-counterfeiting function film layer s is coated or deposited on b coatings；
The Multi-layer anti-counterfeit that described anti-counterfeiting function film layer s is single metal level or be made up of metal level and antiforge function layer
Function film layer；
It is preferred that, described anti-counterfeiting function film layer s is made up of the metal level being combined successively with antiforge function layer；
Described anti-counterfeiting function film layer s gross thickness is 200nm-2000nm, and the thickness of metal film layer is gross thickness
2.5%~50.0%, antiforge function layer thickness be gross thickness 50.0~97.5%；
The material of the metal film layer be selected from lower boiling metal material, such as aluminium, magnesium, chromium or nickel, preferably metallic aluminium,
Deposited by way of vacuum evaporation；
Described antiforge function layer material is selected from fluorescent material, twilight sunset fluorescent material, metamerism filter, Raman material
It is one or more of in material or magnetic anti-counterfeit functional material；
Described magnetic functional material is formed by way of intaglio plate coating or vacuum evaporation deposition；
The described fluorescent material contained, twilight sunset fluorescent material, metamerism filter and raman material passes through photograph
Intaglio printing mode is coated；
It is preferred that, the method for coating or depositing anti-counterfeiting function film layer s on described b coatings comprises the following steps：First
Coating or deposited metal film layer on b coatings, then coat or deposit pseudo- functional layer on metal film layer；
It is preferred that, then it is coated with or deposited metal film layer, obtains described anti-counterfeiting function film layer s；It is preferred that, respectively
Layer is deposited by way of vacuum evaporation；
(3) the anti-counterfeiting function film layer s obtained in step (2) side, coating or layer deposited isolating d, thickness is 50nm
~4000nm；
Described separation layer d material selection is selected from inorganic salts or water-soluble polymer；
The preferred water-soluble metal nitrate of described inorganic salts, metal chloride, metal sulfate or metal phosphate, institute
The metal stated is selected from sodium, potassium, magnesium or calcium, and most preferred inorganic salts are sodium nitrate, potassium nitrate, potassium chloride or sodium chloride；
Described low-molecular weight polymer preferred cellulose, hydroxyl starch, carboxy starch, polyacrylamide or polyethylene pyrrole
Alkanone；
Separation layer d is prepared using the method for coating, during coating, and water-soluble inorganic salt weight concentration is 1%~10%, water-soluble
Property polymer weight concentration be 3~15%, the layer coating after, through hot blast or infra-red drying；
(4) in described separation layer d side, according to the method for step (2), it is coated with or deposits anti-counterfeiting function film layer
S, thickness is 200nm~4000nm；
As needed, step (3)~(4) can be carried out n times, and coating or deposition, n are the integer more than or equal to 0；
When n is 0, described separation layer d is one layer, and when n is 1, described separation layer d is two layers, by that analogy；It is excellent
Choosing, the integer of n=0~20, industrially, typically using the integer of n=0~4；
(5) using the method for laser ablation, the stratified film with deposition will be coated, is etched into the tape base of three-dimensional regular shape
Material pigment, base material is not etched, the regular shape such as letter in uniform thickness, numeral, triangle, rhombus；
(6) by the band base material pigment of step (5), 10-30min in organic solvent is impregnated in, pigment is peeled off from base material；
Described organic solvent is one or more of in ethyl acetate, butyl acetate, n-propyl acetate, isopropanol,
It is preferred that n-propyl acetate, butyl acetate；
(7) by the product of step (6), it is placed in separating liquid, dissolves separation layer d, can be filtered using ultrasound, separated and dissolved,
In inert atmosphere, 50 DEG C~85 DEG C drying obtain described micro-structural security pigment, are a kind of three-dimensional regular shape, such as thick
The micro-structural security pigment of the regular shapes such as degree uniform letter, numeral, triangle, rhombus；
Described separating liquid is the aqueous solution of polyphosphate sodium, polyethers or polyester-type that weight concentration is 0.1~1%.
The method of the present invention, is that a kind of can realize high yield, the making side of the micro-structural security pigment of high efficiency
Method, preparation process non-secondary pollution, safety and environmental protection.
Embodiment
Embodiment 1
(1) selection surfacing material BOPP is base material, and ethyl acetate, n-propyl acetate and isopropanol are coated on its surface
For the b coatings that can be peeled off with base material of mixed solvent, wherein mixed solvent accounts for the 85% of coating glue, and coating glue is using 85 DEG C of hot blasts
The mode of drying is dried；
In mixed solvent, the weight ratio of ethyl acetate, n-propyl acetate and isopropanol is：
Ethyl acetate: n-propyl acetate: isopropanol=45: 45: 10；
The resin that coating glue is used is selected from ethyl cellulose；
The dried thickness of b coatings is 2 μm；
(2) one layer of aluminium film (200nm ± 5nm, when thickness is by depositing is deposited by way of vacuum evaporation on b coatings
Between be controlled), magnetic material (Magnetic is then carried out by way of vacuum evaporation in the aluminium film of deposition
Pig.340, BASF) deposition (100nm ± 5nm), then redeposited one layer of aluminium lamination (200nm ± 5nm), completes antiforge function
Film layer s preparation；
(3) 5% Alkitrate is coated on to anti-counterfeiting function film layer s side, separation layer d is formed, thickness is
0.7μm；
(4) method for and then again using step (2), second anti-counterfeiting function film layer s is prepared in separation layer d side；
(5) laser is used, each film layer with deposition will be coated, be etched into equilateral triangular shape；
(6) by the pigment intermediate product containing two s layers of a d layer, it is impregnated in butyl acetate, by pigment intermediate product
Stripped down from BOPP base materials；
(7) it is subsequently placed in the separation liquid that polyphosphate sodium weight concentration is 1%, ultrasonic dissolution separation layer d, filtering,
Dried in blanket of nitrogen, obtain three layers of equilateral triangle micro-structural security pigment.
Embodiment 2
(1) selection surfacing material PET is base material, and ethyl acetate, n-propyl acetate and isopropanol are coated on its surface
For the b coatings that can be peeled off with base material of mixed solvent, wherein mixed solvent accounts for the 90% of coating glue, and coating glue is using 90 DEG C of hot blasts
The mode of drying is dried；
In mixed solvent, the weight ratio of ethyl acetate, n-propyl acetate and isopropanol is：
Ethyl acetate: butyl acetate: n-propyl acetate: isopropanol=40: 50: 10
The resin that coating glue is used is selected from chlorinated polypropylene；
The dried thickness of b coatings is 1.0 μm；
(2) one layer of nickel film (250nm ± 5nm, when thickness is by depositing is deposited by way of vacuum evaporation on b coatings
Between be controlled), then carried out on the nickel film of deposition by way of coating fluorescent material (Yttrium Orthovanadate europium) coating (dry
Thickness 2000nm ± 50nm afterwards), complete anti-counterfeiting function film layer s preparation；
(3) by 10% polyethylene pyrrole alkanone solution coating anti-counterfeiting function film layer s side, 85 DEG C of hot blast drying tunnel
Dry, form separation layer d, thickness is 2 μm；
(4) and then again using step (2) and the method for (3), second anti-counterfeiting function film is prepared in separation layer d side
Layer s, is repeated a further three times, formed altogether in PET base material with one layer b layers, 5 layers s layers with 4 layers d layers of structure；
(5) laser is used, each film layer with deposition will be coated, etch diamondwise；
(6) by the pigment intermediate product containing 45 s layers of d layers, be impregnated in butyl acetate, by pigment intermediate product from
Stripped down on PE base materials；
(7) in the separation liquid for being subsequently placed in the aqueous solution that polyphosphate sodium weight concentration is 1%, ultrasonic dissolution separation layer d,
Filtering, is dried in blanket of nitrogen, obtains double-decker rhombus micro-structural security pigment.
Claims (16)
1. the high yield preparation method of micro-structural security pigment, it is characterised in that comprise the following steps：
(1) the b coatings that can be peeled off with base material are coated in substrate surface；
(2) anti-counterfeiting function film layer s is coated or deposited on b coatings；
The Multi-layer anti-counterfeit function that described anti-counterfeiting function film layer s is single metal level or be made up of metal level and antiforge function layer
Film layer；
(3) the anti-counterfeiting function film layer s obtained in step (2) side, coating or layer deposited isolating d；
(4) in described separation layer d side, according to the method for step (2), it is coated with or deposits anti-counterfeiting function film layer s；
The step of step (3)~(4), repeat n times, n is the integer more than or equal to 0；
(5) using the method for laser ablation, the stratified film with deposition will be coated, is etched into the band base material face of three-dimensional regular shape
Material；
(6) by the band base material pigment of step (5), it is impregnated in organic solvent, pigment is peeled off from base material；
(7) by the product of step (6), it is placed in separating liquid, dissolves separation layer d, filter, drying obtains described micro-structural and prevented
Pseudo- pigment；
Described separation layer d material is selected from inorganic salts or water-soluble polymer.
2. according to the method described in claim 1, it is characterised in that thickness is 0.5 μm~4 μm after described b coatings are dried.
3. according to the method described in claim 1, it is characterised in that described b coatings are obtained by the way of coating glue coating,
Coating method is coated with for heliogravure full version, and the resin that coating glue is used can redissolve resin selected from low molecular weight solvent type, described
Low molecular weight solvent type can redissolve resin and be selected from ethyl cellulose, hydroxyl modification binary vinyl chloride-vinyl acetate resin, chloridized polyolefin or benzene second
Allyl olefin(e) acid；
Described low molecular weight solvent is selected from alcohol, ester or ether, and the resin content that coating glue is used accounts for the percentage by weight of coating glue
For 3%-40%.
4. according to the method described in claim 1, it is characterised in that in step (2), described anti-counterfeiting function film layer s's is total
Thickness is 200nm-2000nm, and the thickness of metal level is the 2.5%~50.0% of gross thickness, and the thickness of antiforge function layer is total thickness
The 50.0~97.5% of degree.
5. according to the method described in claim 1, it is characterised in that the material of the metal level is selected from aluminium, magnesium, chromium or nickel, lead to
The mode for crossing vacuum evaporation is deposited.
6. method according to claim 5, it is characterised in that described antiforge function layer material is selected from fluorescent material, remaining
It is one or more of in brightness fluorescent material, metamerism filter, raman material or magnetic anti-counterfeit functional material；
Described magnetic functional material is formed by way of intaglio plate coating or vacuum evaporation deposition；
Described fluorescent material, twilight sunset fluorescent material, metamerism filter and raman material passes through photogravure side
Formula is coated.
7. method according to claim 4, it is characterised in that coated on described b coatings or deposition antiforge function is thin
Film layer s method, comprises the following steps：First coating or deposited metal layer on b coatings, then coat or deposit on the metal layer
Antiforge function layer, obtains described anti-counterfeiting function film layer s, and each layer is deposited by way of vacuum evaporation.
8. method according to claim 4, it is characterised in that coated on described b coatings or deposition antiforge function is thin
Film layer s method, comprises the following steps：First coating or deposited metal layer on b coatings, then coat or deposit on the metal layer
Antiforge function layer, is then coated with or deposited metal layer, obtains described anti-counterfeiting function film layer s, and each layer passes through vacuum evaporation
Mode deposit.
9. it is according to the method described in claim 1, it is characterised in that in step (3), thin in the antiforge function of step (2) acquisition
Film layer s side, coating or layer deposited isolating d, thickness are 50nm~4000nm.
10. according to the method described in claim 1, it is characterised in that described inorganic salts are water-soluble metal nitrate, metal
Chloride, metal sulfate or metal phosphate, described metal are selected from sodium, potassium, magnesium or calcium；
Described polymer is cellulose, hydroxyl starch, carboxy starch, polyacrylamide or polyvinylpyrrolidone.
11. method according to claim 10, it is characterised in that separation layer d is prepared using the method for coating, during coating,
Water-soluble inorganic salt weight concentration is 1%~10%, and the weight concentration of water-soluble polymer is 3~15%, after layer coating, warp
Hot blast or infra-red drying.
12. according to the method described in claim 1, it is characterised in that in step (4), in described separation layer d side, press
According to the method for step (2), anti-counterfeiting function film layer s is coated with or deposits, thickness is 200nm~4000nm.
13. method according to claim 12, it is characterised in that the step of step (2)~(4), repeat 0~20.
14. method according to claim 12, it is characterised in that in step (6), described organic solvent is selected from acetic acid second
It is one or more of in ester, butyl acetate, n-propyl acetate, isopropanol.
15. according to the method described in claim 1, it is characterised in that in step (7), by the product of step (6), it is placed in separation
In liquid, separation layer d is dissolved, using ultrasound, separated and dissolved is filtered, in inert atmosphere, 50 DEG C~85 DEG C drying, described in acquisition
Micro-structural security pigment.
16. method according to claim 15, it is characterised in that described separating liquid is that weight concentration is 0.1~1%
The aqueous solution of polyphosphate sodium, polyethers or polyester-type.
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| US11702548B2 (en) * | 2017-09-21 | 2023-07-18 | Giesecke+Devrient Currency Technology Gmbh | Method for producing pigment fragments with a predefined internal and/or external contour, and pigment fragments |
| CN108364055B (en) * | 2018-02-09 | 2021-06-04 | 苗鹏 | Printing ink for multi-dimensional spectrum bar code |
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| DE602006020761D1 (en) * | 2005-11-17 | 2011-04-28 | Basf Se | PROCESS FOR PREPARING SHAMPULAR PARTICLES |
| CN101840524A (en) * | 2009-03-18 | 2010-09-22 | 北京锐兴华盾科技有限公司 | Near-infrared absorption anti-counterfeiting method |
| CN101585978B (en) * | 2009-06-04 | 2011-06-22 | 长沙族兴金属颜料有限公司 | Preparation method for high brightness aluminum pigment |
| CN102269927B (en) * | 2011-05-31 | 2012-12-12 | 上海紫格光学薄膜材料有限公司 | Anti-counterfeiting microstructure pigment and manufacturing process thereof |
| CN102504620B (en) * | 2011-09-21 | 2014-06-25 | 惠州市华阳光学技术有限公司 | Pigment sheet and manufacturing method thereof |
| CN103087555B (en) * | 2012-12-11 | 2014-12-03 | 中钞油墨有限公司 | Microstructure metallic pigment with anti-fake function and preparation method of microstructure metallic pigment |
| CN103818134B (en) * | 2014-02-28 | 2016-05-04 | 佛山市南海区新永泰胶粘制品有限公司 | A kind of manufacturing process of anti-counterfeit printing release liners |
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Address after: 288 Xiuyan Road, Pudong New Area, Shanghai, 201315 Patentee after: CHINA BANKNOTE INK Co.,Ltd. Patentee after: China Banknote Printing and Minting Group Co.,Ltd. Address before: 288 Xiuyan Road, Pudong New Area, Shanghai, 201315 Patentee before: CHINA BANKNOTE INK Co.,Ltd. Patentee before: CHINA BANKNOTE PRINTING AND MINTING Corp. |
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