CN114592377A - Bacterial cellulose anti-counterfeiting paper and preparation method thereof - Google Patents
Bacterial cellulose anti-counterfeiting paper and preparation method thereof Download PDFInfo
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- CN114592377A CN114592377A CN202011396862.2A CN202011396862A CN114592377A CN 114592377 A CN114592377 A CN 114592377A CN 202011396862 A CN202011396862 A CN 202011396862A CN 114592377 A CN114592377 A CN 114592377A
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/21—Macromolecular organic compounds of natural origin; Derivatives thereof
- D21H17/24—Polysaccharides
- D21H17/25—Cellulose
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/40—Agents facilitating proof of genuineness or preventing fraudulent alteration, e.g. for security paper
- D21H21/44—Latent security elements, i.e. detectable or becoming apparent only by use of special verification or tampering devices or methods
- D21H21/48—Elements suited for physical verification, e.g. by irradiation
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Abstract
The invention discloses bacterial cellulose anti-counterfeiting paper and a preparation method thereof, and belongs to the technical field of anti-counterfeiting paper product preparation. Purifying and dispersing a bacterial cellulose hydrogel film cultured by bacterial strain fermentation to obtain a uniformly dispersed bacterial cellulose microfiber suspension system; mixing a precursor solution containing europium ions with bacterial cellulose microfiber, and reacting at high temperature and high pressure to obtain a ligand composite microfiber of bacterial cellulose and europium ions; and mixing the composite microfiber with papermaking wood pulp, papermaking and drying to obtain the bacterial cellulose anti-counterfeiting paper. The paper has good mechanical strength and printing performance, shows visible pink fluorescence under the illumination of excitation wavelength 254nm or 365nm, has good anti-counterfeiting performance and fluorescence tolerance, and has good stability to light, heat, acid, alkali, ethanol, gasoline and the like.
Description
Technical Field
The invention relates to anti-counterfeiting paper and a preparation method thereof, in particular to bacterial cellulose anti-counterfeiting paper and a preparation method thereof, and belongs to the technical field of anti-counterfeiting paper product preparation.
Background
Bacterial cellulose is a natural nano-cellulose material fermented by microorganisms, has the same molecular structural unit as other plant celluloses, and simultaneously has a plurality of unique properties and structures. The bacterial cellulose is composed of natural fermented nano-fibers, the average diameter of the nano-fibers is 20-50nm, the mechanical strength of the fibers is high, and the fibers have high tensile strength and elastic modulus; compared with plant cellulose, the bacterial cellulose does not contain associated products such as lignin, pectin, hemicellulose and the like, and has high crystallinity (up to 95 percent and 65 percent of plant cellulose) and high polymerization degree; the bacterial cellulose has high water absorption, water retention and high wet strength due to a large amount of hydroxyl on the surface of the nano fiber; meanwhile, the fermentation period of the bacterial cellulose is short, the fermentation process is mild and green, and the growth period and energy consumption of the bacterial cellulose are far less than those of wood; as well as plant fibers, are completely biodegradable.
Due to the unique properties, the bacterial cellulose becomes a research hotspot of novel materials at home and abroad as a biological material with great application potential. The function characteristics of the bacteria cellulose are internationally researched for only about 10 years, and the bacteria cellulose is applied and researched in the aspects of sound vibration membranes, wound dressing materials and the like. In the paper industry, bacterial cellulose can improve the physical properties of paper such as strength, folding resistance, tearing strength and the like. The bacterial cellulose is introduced into the paper pulp, so that the ink absorption uniformity and the adhesiveness of the high-grade writing paper are obviously improved. The bacterial cellulose suspension is coated on paper in a coating mode, so that the paper has better smoothness and printability and brightness and glossiness of the base paper. In the paper industry of japan, bacterial cellulose is added to secondary fibers to solve the problem of strength reduction during recycling of the secondary fibers, and the secondary fibers can be used to weave high-quality paper.
In addition, the bacterial cellulose also has an active effect on improving the performance of the special paper. Bacterial cellulose, for example, has also been reported for use in currency paper for currency, which has good print quality, high strength, and excellent water resistance. Chinese patent CN103103882B discloses anti-counterfeiting paper containing a transparent bacterial cellulose film, wherein in the papermaking process of paper, the bacterial cellulose film is added into paper pulp to be made into the anti-counterfeiting paper containing the bacterial cellulose, or a positioning application device is utilized to apply the bacterial cellulose film to a preset position of a wet paper sheet, and then the anti-counterfeiting paper containing the bacterial cellulose is prepared through subsequent steps.
Disclosure of Invention
In view of the above, the invention provides the bacterial cellulose anti-counterfeiting paper obtained by compounding the bacterial cellulose nanofiber effect and the fluorescent color-changing material on the basis of the existing papermaking performance of the bacterial cellulose fiber.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of bacterial cellulose anti-counterfeiting paper comprises the following steps:
1) sequentially purifying and dispersing the hydrogel film of the bacterial cellulose cultured by bacterial fermentation to obtain a microfiber suspension system;
2) adding a precursor solution containing europium ions into a microfiber suspension system, and mixing and reacting to obtain a composite microfiber;
3) and uniformly mixing the composite microfiber and papermaking wood pulp, and papermaking and drying to obtain the bacterial cellulose anti-counterfeiting paper.
Further, the bacteria used in the fermentation culture in the step 1) are any one or a mixture of several bacteria of acetobacter xylinum, rhizobium, sarcina, pseudomonas, achromobacter, alcaligenes, aerobacter and azotobacter, and the number of the viable bacteria of the bacteria is 103-109One per ml.
Further, the purification treatment in step 1) is performed by: cutting a hydrogel film of the bacterial cellulose into a cuboid with the size of 1-2cm multiplied by 0.1-0.5cm multiplied by 0.1cm, soaking the cuboid in a NaOH aqueous solution with the weight of 1-5% at the temperature of 20-26 ℃ for 6-24h, taking out the cuboid, washing the cuboid with water until the pH value is 7 so as to remove mycoprotein on the bacterial cellulose and residual culture medium adhered on the cellulose film;
the dispersion treatment operation is as follows: dispersing the hydrogel membrane of the purified bacterial cellulose by a fiber dissociator at 10000-20000rpm for 10-30min, filtering out excessive water, adding ethanol water solution, carboxymethyl cellulose and silane coupling agent to the bacterial cellulose microfiber suspension system, wherein the mass of the bacterial cellulose is 3-10wt%, the content of the carboxymethyl cellulose is 0.2-0.4wt%, and the content of the silane coupling agent is 0.01-1wt%, filtering out excessive water by a filter bag after the bacterial cellulose membrane is dispersed, taking 100ml of the mixed system, drying, the mass of the bacterial cellulose and the water content can be calculated, the mass of the bacterial cellulose in the system is controlled to be 10-20wt%, then adding an ethanol water solution, simultaneously adding carboxymethyl cellulose and a silane coupling agent, and adjusting the mass ratio of the bacterial cellulose.
Wherein, the silane coupling agent is one or a mixture of more of aminosilane, vinyl silane, epoxy silane and mercapto silane;
the ethanol content in the ethanol water solution is 30-70 wt%.
Further, the precursor solution containing europium ions in step 2) is a trivalent europium ion compound solution, and specifically is a mixed solution of one or more of europium trichloride, europium sulfate, europium nitrate, europium acetate and europium carbonate.
Further, in the step 2), the mixing reaction is to add 0.001-0.1mmol of precursor solution containing europium ions into each 1000g of microfiber suspension system, and perform mixing reaction for 10-30min at the temperature of 120-150 ℃.
Further, the diameter of the bacterial cellulose microfiber in the composite microfiber in the step 2) is 1-20 μm, and europium ion nanoparticles with the particle size of 80-200nm are distributed on the bacterial cellulose microfiber.
Further, the mass of the composite micro-fiber in the step 3) is 0.1-1wt% of the sum of the mass of the composite micro-fiber and the mass of the papermaking wood pulp.
Further, the papermaking pulp in the step 3) is one or a mixture of any more of wood pulp, bamboo pulp, straw pulp, cotton pulp and secondary recycled pulp.
The invention also provides the bacterial cellulose anti-counterfeiting paper prepared by the method, and the paper has stable ultraviolet-excited fluorescence anti-counterfeiting performance.
The invention has the beneficial effects that: the bacterial cellulose is nano-scale fiber, while the common papermaking fiber is micro-scale, in order to enable the bacterial cellulose fiber to be matched with papermaking slurry, the dispersibility is improved by introducing carboxymethyl cellulose, the binding capacity among nano-fibers is increased by adding the silane coupling agent, and the bacterial cellulose nano-fibers become micro-fibers. Is easy to be mixed with papermaking pulp for processing and is convenient for the observation of anti-counterfeiting fiber.
The silane coupling agent can be combined with a large number of hydroxyl groups on the surface of the bacterial cellulose, the ligand capacity of europium ions is improved under the action of a bridge, and the density of a large number of negative charges generated by the hydroxyl groups is reduced. The surface negative charge density of the bacterial cellulose is 10 times that of the common plant fiber.
Europium ions are quickly reacted on the surfaces of the microfibers of the bacterial cellulose to form europium nano-particles in a hydro-thermal synthesis mode, and the europium nano-particles are stable in fluorescence effect and high in intensity.
According to the invention, on the basis of the existing papermaking performance of the bacterial cellulose fiber, the bacterial cellulose nanofiber effect is compounded with the fluorescent color-changing material to obtain the bacterial cellulose anti-counterfeiting paper. The paper has good mechanical strength and printing performance, shows visible pink fluorescence under the illumination of excitation wavelength 254nm or 365nm, has good anti-counterfeiting performance and fluorescence tolerance, and has good stability to light, heat, acid, alkali, ethanol, gasoline and the like.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the following examples, the fiber debonder manufacturer model is: the model ZB-JLQ standard fiber dissociator produced by Hangzhou Paopon Automation technology limited company has the basic parameters of 6.5 x 6.5-4 equal parts of an inner spiral line; leaf convolution frequency of 48.3 + -1.6655-1(ii) a Power AC220V ± 10% 50 HZ.
Example 1
The preparation method of the bacterial cellulose anti-counterfeiting paper comprises the following steps:
1) fermenting with Acetobacter xylinum to obtain natural bacterial cellulose hydrogel membrane (wherein the volume ratio of the strain to the fermentation medium is 1:1, and the number of viable bacteria is 103Piece/ml), cutting the hydrogel film into pieces with the length of 1cm and the width of 0.1 cm; a cuboid of uniform shape having a thickness of 0.1 cm; soaking in 1wt% NaOH water solution at room temperature for 24h, washing with water to neutralityRemoving mycoprotein on the bacterial cellulose and residual culture medium adhered to the cellulose membrane;
dispersing the purified bacterial cellulose by a fiber dissociator at the speed of 10000rpm for 30 min; then filtering out excessive water, adding ethanol water solution, carboxymethyl cellulose and silane coupling agent until the mass of the bacterial cellulose in the bacterial cellulose microfiber suspension system is 3wt%, the content of the carboxymethyl cellulose is 0.2wt%, the content of the silane coupling agent is 0.01wt%, and the ethanol content of the ethanol water solution is 70 wt%;
2) europium trichloride is added into a prepared bacterial cellulose microfiber suspension system, 0.01mmol of europium ion compound is added into every 1000g of the prepared bacterial cellulose microfiber suspension system, and the mixture is heated in a high-temperature high-pressure kettle for 10min at 120 ℃ to obtain a bacterial cellulose and europium ion ligand composite microfiber; the finally obtained bacterial cellulose and europium ion ligand composite microfiber is obtained, wherein the diameter of the bacterial cellulose microfiber is 1 micron, europium ion nano-particles are distributed on the microfiber, and the particle size of the particles is 80 nm;
3) and mixing the composite microfiber with papermaking wood pulp, papermaking and drying to obtain the bacterial cellulose anti-counterfeiting paper. The mass of the ligand composite microfiber containing bacterial cellulose and europium ions in the paper accounts for 1wt% of the whole, the paper has stable ultraviolet excitation fluorescence anti-counterfeiting performance, and visible pink fluorescence is displayed under the illumination of excitation wavelength 254nm or 365 nm.
The tolerance test is carried out on the bacterial cellulose anti-counterfeiting paper according to the national standard GB/T37074-2018 ultraviolet excitation fluorescence anti-counterfeiting fiber technical condition: after a sample is placed in a 100 ℃ oven for 30min, the relative fluorescence brightness change is 1.2%, which indicates that the sample has good heat resistance; after a sample is exposed for 5 hours under a solarization instrument, the relative fluorescence brightness change is 2.0 percent, which indicates that the sample has good light resistance; after the sample is respectively treated by acid and alkali, the relative fluorescence brightness change is 3.5 percent and 4.6 percent, which shows that the sample has good acid and alkali resistance.
Example 2
The preparation method of the bacterial cellulose anti-counterfeiting paper comprises the following steps:
1) obtained by fermentation of RhizobiumThe natural bacterial cellulose hydrogel membrane (wherein the volume ratio of the bacterial strain to the fermentation medium is 1:10, wherein the viable count of the bacterial strain is 105Piece/ml), cutting the hydrogel film into pieces with the length of 1cm and the width of 0.2 cm; a cuboid of uniform shape having a thickness of 0.1 cm; soaking in 2wt% NaOH aqueous solution at room temperature for 16h, and washing with water to neutrality to remove mycoprotein on the bacterial cellulose and residual culture medium adhered on the cellulose membrane;
dispersing the purified bacterial cellulose by using a fiber dissociator at the speed of 12000rpm for 25 min; then filtering out excessive water, adding an ethanol water solution, carboxymethyl cellulose and a silane coupling agent until the mass of the bacterial cellulose in a bacterial cellulose microfiber suspension system is 5wt%, the content of the carboxymethyl cellulose is 0.3wt%, the content of vinyl silane is 0.03wt%, and the ethanol content of the ethanol water solution is 60 wt%;
2) adding europium sulfate into the prepared bacterial cellulose microfiber suspension system, adding 0.01mmol of europium ion compound into every 1000g of the prepared bacterial cellulose microfiber suspension system, and heating the mixture in a high-temperature high-pressure kettle at 150 ℃ for 30min to obtain a bacterial cellulose and europium ion ligand composite microfiber; the finally obtained bacterial cellulose and europium ion ligand composite microfiber is characterized in that the diameter of the bacterial cellulose microfiber is 12 microns, europium ion nanoparticles are distributed on the microfiber, and the particle size of the particles is 100 nm;
3) and mixing the composite microfiber and papermaking bamboo pulp, papermaking and drying to obtain the bacterial cellulose anti-counterfeiting paper. The mass of the ligand composite microfiber containing bacterial cellulose and europium ions in the paper accounts for 0.6wt% of the whole, the paper has stable ultraviolet excitation fluorescence anti-counterfeiting performance, and visible pink fluorescence is displayed under illumination with an excitation wavelength of 365 nm.
Example 3
The preparation method of the bacterial cellulose anti-counterfeiting paper comprises the following steps:
1) fermenting with Sarcina to obtain natural bacterial cellulose hydrogel membrane (wherein the volume ratio of strain to fermentation medium is 1:50, and the number of viable bacteria is 10)9Piece/ml), cutting the hydrogel film into pieces with the length of 2cm and the width of 0.3 cm; a cuboid of 0.1cm thickness and uniform shape; 3wt% NaOH aqueous solution at room temperatureSoaking in the solution for 12h, and washing with water to neutrality to remove mycoprotein on the bacterial cellulose and residual culture medium adhered on the cellulose membrane;
dispersing the purified bacterial cellulose by a fiber dissociator at the speed of 15000rpm for 20 min; then filtering out excessive water, adding an ethanol water solution, carboxymethyl cellulose and a silane coupling agent until the mass of the bacterial cellulose in a bacterial cellulose microfiber suspension system is 7wt%, the content of the carboxymethyl cellulose is 0.4wt%, the content of epoxy silane is 0.5wt%, and the ethanol content of the ethanol water solution is 30 wt%;
2) europium nitrate is added into a prepared bacterial cellulose microfiber suspension system, 0.1mmol of europium ion compound is added into every 1000g of the prepared bacterial cellulose microfiber suspension system, and the mixture is heated in a high-temperature autoclave at 150 ℃ for 30min to obtain a bacterial cellulose and europium ion ligand composite microfiber; the finally obtained bacterial cellulose and europium ion ligand composite microfiber is characterized in that the diameter of the bacterial cellulose microfiber is 16 microns, europium ion nanoparticles are distributed on the microfiber, and the particle size of the particles is 200 nm;
3) and mixing the composite microfiber and papermaking straw pulp, papermaking and drying to obtain the bacterial cellulose anti-counterfeiting paper. The mass of the ligand composite microfiber containing bacterial cellulose and europium ions in the paper accounts for 0.4wt% of the whole, the paper has stable ultraviolet excitation fluorescence anti-counterfeiting performance, and visible pink fluorescence is displayed under illumination with excitation wavelength of 254 nm.
Example 4
The preparation method of the bacterial cellulose anti-counterfeiting paper comprises the following steps:
1) mixing Acetobacter xylinum and Pseudomonas, and fermenting to obtain natural bacterial cellulose hydrogel membrane (wherein the volume ratio of strain to fermentation medium is 1:100, and the number of viable bacteria is 10)9Piece/ml), cutting the hydrogel film into pieces with the length of 2cm and the width of 0.5 cm; a cuboid of uniform shape having a thickness of 0.1 cm; soaking in 6wt% NaOH aqueous solution at room temperature for 24h, and washing with water to neutrality to remove mycoprotein on the bacterial cellulose and residual culture medium adhered on the cellulose membrane;
dispersing the purified bacterial cellulose by using a fiber dissociator at the speed of 20000rpm for 10 min; then filtering out excessive water, adding an ethanol water solution, carboxymethyl cellulose and a silane coupling agent until the mass of the bacterial cellulose in a bacterial cellulose microfiber suspension system is 10wt%, the content of the carboxymethyl cellulose is 0.4wt%, the content of a mercaptosilane coupling agent is 1wt%, and the ethanol content of the ethanol water solution is 50 wt%;
2) europium acetate and europium carbonate (molar ratio 1:1 mixing), adding 0.03mmol of europium ion compound into each 1000g of the adding system, and heating the mixture in a high-temperature high-pressure kettle at 140 ℃ for 10min to obtain the bacterial cellulose and europium ion ligand composite microfiber; the finally obtained bacterial cellulose and europium ion ligand composite microfiber is characterized in that the diameter of the bacterial cellulose microfiber is 20 microns, europium ion nanoparticles are distributed on the microfiber, and the particle size of the particles is 150 nm;
3) and (3) mixing the composite microfiber with papermaking wood pulp and secondary recycled pulp (the ratio of the wood pulp to the secondary recycled pulp is 5: 1) mixing, papermaking and drying to obtain the bacterial cellulose anti-counterfeiting paper. The mass of the ligand composite microfiber containing bacterial cellulose and europium ions in the paper accounts for 0.1wt% of the whole, the paper has stable ultraviolet excitation fluorescence anti-counterfeiting performance, and visible pink fluorescence is displayed under illumination with excitation wavelength of 254 nm.
Claims (10)
1. A preparation method of bacterial cellulose anti-counterfeiting paper is characterized by comprising the following steps:
1) sequentially purifying and dispersing the hydrogel film of the bacterial cellulose cultured by bacterial fermentation to obtain a microfiber suspension system;
2) adding a precursor solution containing europium ions into a microfiber suspension system, and mixing and reacting to obtain a composite microfiber;
3) and uniformly mixing the composite microfiber and papermaking wood pulp, papermaking and drying to obtain the bacterial cellulose anti-counterfeiting paper.
2. The method for preparing the bacterial cellulose anti-counterfeiting paper according to claim 1, characterized in that the bacteria used in the fermentation culture in the step 1) are any one or a mixture of several bacteria of acetobacter xylinum, rhizobium, sarcina, pseudomonas, achromobacter, alcaligenes, aerobacter and azotobacter;
the number of viable bacteria of the bacteria is 103-109One per ml.
3. The method for preparing the bacterial cellulose anti-counterfeiting paper according to claim 1, wherein the purification treatment in the step 1) is performed by the following steps: cutting the bacterial cellulose hydrogel film into cuboids with the length of 1-2cm multiplied by 0.1-0.5cm multiplied by 0.1cm, soaking the cuboids in a NaOH aqueous solution with the weight of 1-5wt% for 6-24h at the temperature of 20-26 ℃, taking out and washing with water until the pH value is 7;
the dispersion treatment operation is as follows: dispersing the hydrogel film of the purified bacterial cellulose by a fiber dissociator at 10000-20000rpm for 10-30min, filtering out excessive water, adding ethanol water solution, carboxymethyl cellulose and silane coupling agent until the mass of the bacterial cellulose in a bacterial cellulose microfiber suspension system is 3-10wt%, the content of the carboxymethyl cellulose is 0.2-0.4wt% and the content of the silane coupling agent is 0.01-1 wt%.
4. The preparation method of the bacterial cellulose anti-counterfeiting paper according to claim 3, characterized in that the silane coupling agent is one or a mixture of aminosilane, vinyl silane, epoxy silane and mercapto silane;
the ethanol content in the ethanol water solution is 30-70 wt%.
5. The method for preparing the bacterial cellulose anti-counterfeiting paper according to claim 1, wherein the precursor solution containing the europium ions in the step 2) is a mixed solution of one or more of europium trichloride, europium sulfate, europium nitrate, europium acetate and europium carbonate.
6. The method for preparing the bacterial cellulose anti-counterfeiting paper according to claim 1, wherein the mixing reaction in step 2) is to add 0.001-0.1mmol of europium-containing precursor solution to each 1000g of microfiber suspension system, and perform mixing reaction at 120-150 ℃ for 10-30 min.
7. The preparation method of the bacterial cellulose anti-counterfeiting paper according to claim 1, wherein the diameter of the bacterial cellulose microfiber in the composite microfiber in step 2) is 1-20 μm, europium ion nanoparticles are distributed on the bacterial cellulose microfiber, and the particle size is 80-200 nm.
8. The preparation method of the bacterial cellulose anti-counterfeiting paper according to claim 1, wherein the mass of the composite micro-fibers in the step 3) is 0.1-1wt% of the sum of the mass of the composite micro-fibers and the mass of the papermaking wood pulp.
9. The method for preparing the bacterial cellulose anti-counterfeiting paper according to claim 1, wherein the papermaking pulp in the step 3) is one or a mixture of any of wood pulp, bamboo pulp, straw pulp, cotton pulp and secondary recycled pulp.
10. A bacterial cellulose anti-counterfeiting paper prepared by the method of any one of claims 1-9.
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