CN112501705B - Anti-counterfeiting viscose fiber, preparation method and anti-counterfeiting method - Google Patents
Anti-counterfeiting viscose fiber, preparation method and anti-counterfeiting method Download PDFInfo
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- CN112501705B CN112501705B CN202011254984.8A CN202011254984A CN112501705B CN 112501705 B CN112501705 B CN 112501705B CN 202011254984 A CN202011254984 A CN 202011254984A CN 112501705 B CN112501705 B CN 112501705B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/447—Systems using electrophoresis
- G01N27/44704—Details; Accessories
- G01N27/44717—Arrangements for investigating the separated zones, e.g. localising zones
- G01N27/4473—Arrangements for investigating the separated zones, e.g. localising zones by electric means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
Abstract
The invention relates to a preparation method of anti-counterfeiting viscose fiber, which comprises the following steps: soaking pulp in an alkali aqueous solution, then performing squeezing, crushing and ageing treatment, cooling, performing sulfonation treatment, and dissolving in a dilute alkali solution to obtain a rough viscose; mixing the crude viscose with various amino acid metal chelates, defoaming, and aging to obtain spinning solution; carrying out wet spinning on the spinning solution, carrying out acid bath, and then carrying out drawing, cutting, refining, oiling and drying treatment to obtain the anti-counterfeiting viscose; wherein the sum of the metal elements in the amino acid metal chelate accounts for 0.3-1.1 per mill of the mass fraction of the anti-counterfeiting viscose fiber. The anti-counterfeiting viscose fiber disclosed by the invention utilizes various amino acid metal chelates to perform anti-counterfeiting encryption treatment on the viscose fiber, and performs anti-counterfeiting identification through detection and encoding of metal elements and amino acid types, so that the anti-counterfeiting viscose fiber is high in anti-counterfeiting degree and good in anti-counterfeiting concealment.
Description
Technical Field
The invention relates to anti-counterfeiting fibers, in particular to anti-counterfeiting viscose fibers, a preparation method and an anti-counterfeiting method.
Background
With the development and progress of society, chemical fibers become an indispensable part of human life, and the anti-counterfeiting identification of the chemical fibers becomes important gradually, and at present, the anti-counterfeiting of the chemical fibers is mainly realized by monochromatic fluorescent fibers, but the anti-counterfeiting characteristics are single, and the anti-counterfeiting is easy to forge and is not concealed.
Chinese patent CN110042490A discloses a viscose fiber containing tracer labels and a preparation method thereof, which adopts rare earth metal chelate as tracer, and mixes tracer dispersion liquid and spinning viscose stock solution to prepare viscose staple fibers containing tracer labels; chinese patent CN111394822A discloses a fluorescent fiber and a manufacturing method thereof, wherein fluorescent substances and spinning oil are mixed to prepare oil solution, and then the oil solution is coated on the surface of the fiber in a spinning and oiling manner; chinese patent CN202881745U discloses an ultraviolet double-wave anti-counterfeiting fluorescent fiber, which is provided with ultraviolet fluorescent coating layers with different wavelengths.
The anti-counterfeiting fiber has a certain anti-counterfeiting effect and is suitable for being used in certain environments, but the anti-counterfeiting characteristic is too single, the anti-counterfeiting concealment is not good, the anti-counterfeiting characteristic is easy to counterfeit, and the anti-counterfeiting characteristic is easy to damage, so that an anti-counterfeiting method with high anti-counterfeiting degree and good concealment is required to be used in fiber production.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide an anti-counterfeiting viscose fiber, a preparation method and an anti-counterfeiting method.
The first purpose of the invention is to disclose the application of amino acid metal chelate as anti-counterfeiting tracing agent of anti-counterfeiting viscose fiber.
The application refers to that in the preparation process of the viscose fiber, the amino acid metal chelate is added as an anti-counterfeiting tracking agent to prepare the anti-counterfeiting viscose fiber.
The second purpose of the invention is to provide a preparation method of anti-counterfeiting viscose fiber, which comprises the following steps:
(1) soaking pulp in an alkali aqueous solution, then performing squeezing, crushing and ageing treatment, cooling, performing sulfonation treatment, and dissolving in a dilute alkali solution to obtain a rough viscose;
(2) mixing the crude viscose with various amino acid metal chelates, defoaming, and aging to obtain spinning solution;
(3) carrying out wet spinning on the spinning solution, carrying out acid bath, and then carrying out drawing, cutting, refining, oiling and drying treatment to obtain the anti-counterfeiting viscose; wherein the sum of the metal elements in the amino acid metal chelate accounts for 0.3-1.1 per mill of the mass fraction of the anti-counterfeiting viscose fiber.
Further, in the step (1), the pulp is wood pulp or cotton pulp, and the degree of polymerization of the pulp is 200-600.
Further, in the step (1), the pH value of the crude viscose is 7-10, so that the crude viscose is prevented from being too alkaline, and the stability of the amino acid metal chelate added later is damaged.
Further, in the step (1), the pulp is soaked in an aqueous solution of NaOH, the concentration of the aqueous solution of NaOH is 15-20%, and the soaking bath ratio is 1: 15-20.
Further, in the step (1), the concentration of the dilute alkali solution is 5% -10%.
Further, in the step (2), the amino acid metal chelate is at least two of magnesium glycine chelate, copper methionine chelate and calcium aspartate chelate.
Further, the mass ratio of the glycine chelated magnesium to the methionine chelated copper is 1-3: 1-4; the mass ratio of the glycine chelated magnesium to the aspartic acid chelated calcium is 1-3: 1-5; the mass ratio of the methionine chelated copper to the aspartic acid chelated calcium is 1-4: 1-5.
Further, the molar ratio of glycine to magnesium elements in the glycine chelated magnesium is 2: 1; the mol ratio of methionine to copper element in the methionine chelated copper is 2: 1; the molar ratio of aspartic acid to calcium in the aspartic acid chelated calcium is 1: 1.
Further, the glycine iron chelate contains 30-70% by mass of glycine and 12-13% by mass of iron; the mass fraction of methionine in the methionine chelated copper is 35-65%, and the mass fraction of copper is 15-20%; the aspartic acid in the aspartic acid chelated calcium accounts for 28-70% by mass, and the calcium accounts for 10-25% by mass. In the present invention, the amino acid chelate metal to be added is preferably high in purity, and interference of impurities can be reduced.
Further, in the step (2), the sum of the metal elements in the amino acid metal chelate accounts for 0.5-1.5 per mill of the mass fraction of the spinning solution.
Further, in the step (2), the temperature of the aging treatment is 12 ℃ to 24 ℃.
Further, in the step (3), the coagulation bath used in the acid bath includes sulfuric acid, sodium sulfate and zinc sulfate, and the temperature of the acid bath is 40 ℃ to 55 ℃.
The third purpose of the invention is to provide the anti-counterfeiting viscose fiber prepared by the preparation method, which comprises viscose fiber and a plurality of amino acid metal chelates distributed in the viscose fiber, wherein the sum of the metal elements in the amino acid metal chelates accounts for 0.3-1.1 per mill of the mass fraction of the anti-counterfeiting viscose fiber.
The fourth purpose of the invention is to provide an anti-counterfeiting method of anti-counterfeiting viscose fiber, which comprises the steps of encryption, decryption and authentication:
the encryption step comprises: according to the type and the dosage of the amino acid metal chelate, the anti-counterfeiting viscose fiber is coded to send out encryption information;
the decryption and authentication steps comprise: obtaining encrypted information, and testing the types and the use amounts of amino acid and metal ions in the viscose; then comparing with the obtained encrypted information to identify the authenticity of the viscose fiber.
Further, the encryption step can be performed simultaneously with the preparation process of the anti-counterfeiting viscose fiber, and simultaneously, a coding information table is designed: coding according to the types and the dosage of the amino acid and the metal ions contained in the amino acid metal chelate, coding different serial numbers for different amino acids and different metal ions, for example, numbering the amino acids by using different English letters, and numbering the metal ions by using different Arabic numerals; the combination of the two sequences can obtain a string of true fiber numbers according to the sequence of the usage of amino acid and metal ion, such as the sequence from high content to low content.
Further, in the decryption and identification steps, after the types and the amounts of the amino acid and the metal ions in the viscose fiber are tested, the types and the amounts can be compared with the obtained encrypted information (comprising a real fiber number and a coding information table), if the types and the amounts are matched with the real fiber number, the viscose fiber is identified as a real fiber, otherwise, the viscose fiber is identified as a false fiber.
Furthermore, the type and content of the amino acid are measured by adopting a capillary electrophoresis/mass spectrometry combined technology, and the type and content of the metal element are detected by adopting an inductively coupled plasma spectrometry.
By the scheme, the invention at least has the following advantages:
the invention discloses an anti-counterfeiting viscose fiber and a preparation method thereof, wherein an amino acid metal chelate is used as an anti-counterfeiting tracer to perform anti-counterfeiting encryption on the viscose fiber, the anti-counterfeiting tracer is added in the preparation process of the viscose fiber, the preparation method has simple and convenient process and low energy consumption, the viscose fiber containing specific metal elements and specific amino acid types is obtained, the fiber source can be tracked and identified by detecting the metal elements and the amino acid types, and the anti-counterfeiting tracking is completed. Because two anti-counterfeiting encryption means of metal elements and amino acid are adopted, the anti-counterfeiting degree is high, the anti-counterfeiting viscose fiber is not easy to counterfeit, and meanwhile, the added amino acid chelated metal has good concealment in the prepared anti-counterfeiting viscose fiber and is not easy to find, so that the anti-counterfeiting concealment is good.
The invention utilizes the types and the contents of metal elements and amino acids as the anti-counterfeiting marks, and the anti-counterfeiting marks of the anti-counterfeiting viscose fibers are arranged in the fibers, thereby not influencing the overall fiber performance of the viscose fibers, and the anti-counterfeiting marks of the anti-counterfeiting viscose fibers are easy to detect and identify, have long time effect, effective encryption and traceability, can trace the fiber source according to the anti-counterfeiting code, have high anti-counterfeiting strength, can not increase the complexity of the viscose fiber preparation process, and have good market application prospect.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following description is made with reference to the preferred embodiments of the present invention and the accompanying detailed drawings.
Drawings
Fig. 1 is a process diagram of a preparation method of the anti-counterfeiting viscose fiber.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
In the following embodiments of the present invention, the method for detecting metal elements includes the following steps:
(1) sampling the anti-counterfeiting viscose fiber, putting 0.1 g of the anti-counterfeiting viscose fiber into a test tube, adding a proper amount of deionized water for wetting, and then gradually adding 6.0-10.0mL of concentrated nitric acid;
(2) placing the test tube treated in the step (1) in a digestion instrument for digestion for 4-6 h until concentrated nitric acid is evaporated to dryness, adding 0.3-0.6% nitric acid for dissolution, filtering, and then performing constant volume by using 0.3-0.6% nitric acid to prepare a constant volume solution;
(3) and (3) carrying out quantitative analysis on the constant volume solution prepared in the step (2) by adopting an inductively coupled plasma spectrometer.
The method for detecting amino acid comprises the following steps:
(1) sampling the anti-counterfeiting viscose fiber, putting 0.1 g of the anti-counterfeiting viscose fiber into a 20mL hydrolysis tube, adding 10mL of acidolysis agent, and filling N2And sealing.
(2) Placing the hydrolysis tube in a constant-temperature drying box at the temperature of 105-;
(3) and (3) analyzing the amino acid components of the constant volume solution prepared in the step (2) by adopting an amino acid automatic analyzer, and rapidly detecting the type and the content of the amino acid.
All starting materials are either commercially available or prepared by methods conventional in the art unless otherwise specified. Wherein the CAS number of the glycine chelated magnesium is 14783-68-7, and the manufacturer is Xiamen domino Biotechnology Co., Ltd; the CAS number of the methionine chelated copper is 15170-74-8, and the manufacturer is Wuhan Wooxuan science and technology limited company; the CAS number of the aspartic acid chelated calcium is 39162-75-9, and the manufacturer is Shandong Pu Zheng Biotech limited.
Example 1
The present embodiment provides an anti-counterfeit viscose fiber and a preparation method thereof, wherein the process flow is shown in fig. 1, and the raw materials include wood pulp (with a polymerization degree of 200) and an anti-counterfeit tracking agent.
The anti-counterfeiting tracking agent is composed of the following raw materials in parts by weight: 10 parts of glycine chelated magnesium (the content of magnesium element is 1.2 parts, the content of glycine is 4 parts), 10 parts of methionine chelated copper (the content of copper element is 1.5 parts, the content of methionine is 4.5 parts), 10 parts of aspartic acid chelated calcium (the content of calcium element is 1 part, the content of aspartic acid is 5 parts), and 70 parts of deionized water; wherein the magnesium element: copper element: the mass ratio of calcium element is 1.2:1.5: 1; wherein the weight ratio of glycine: methionine: the mass ratio of aspartic acid is 4:4.5: 5. The preparation method of the anti-counterfeiting tracking agent comprises the following steps:
(1) adding glycine chelated magnesium, methionine chelated copper, aspartic acid chelated calcium and deionized water into a reaction kettle provided with a stirring device;
(2) and (3) opening the stirrer at the temperature of 20 ℃, and uniformly stirring for 10min to prepare the anti-counterfeiting tracking agent.
The preparation method of the anti-counterfeiting viscose fiber comprises the following specific steps:
(1) soaking wood pulp in 15 wt% NaOH solution at a bath ratio of 1:15, sequentially squeezing, pulverizing, aging, cooling, adding CS2Sulfonating and grinding, and then uniformly dissolving in dilute alkali solution with the concentration of 5 wt% to prepare crude viscose with the pH value of 8.2;
(2) fully mixing the rough viscose, filtering, adding the anti-counterfeiting tracking agent into the rough viscose, defoaming, and aging at 15 ℃ to prepare a spinning solution;
(3) wet spinning the spinning solution, passing through an acid coagulation bath consisting of sulfuric acid, sodium sulfate and zinc sulfate on a spinning machine, forming cellulose slivers at the acid bath temperature of 40 ℃, then drawing at the drawing rate of 15%, cutting, refining, oiling at the oil content of 0.15%, and finally drying at the drying temperature of 60 ℃ to obtain the anti-counterfeiting viscose.
The anti-counterfeiting viscose fiber is viscose staple fiber, the titer is 1.21dtex, and the length is 30 mm.
Through detection of an inductively coupled plasma spectrometer, the content of magnesium element is 10.988ppm (g), the content of copper element is 13.655ppm (g), the content of calcium element is 8.894ppm (g), and then the content of magnesium element: copper element: calcium element mass ratio is 1.19: 1.48:0.96.
Through the detection of an amino acid automatic analyzer, the glycine content is 0.11%, the methionine content is 0.12%, and the aspartic acid content is 0.14%, then the glycine content is as follows: methionine content: the mass ratio of the aspartic acid content is 3.66: 4: 4.66.
example 2
This example provides an anti-counterfeit viscose fiber and a method for preparing the same, wherein the raw materials include wood pulp (with a polymerization degree of 210) and an anti-counterfeit tracking agent.
The anti-counterfeiting tracking agent is composed of the following raw materials in parts by weight: 10 parts of glycine chelated magnesium (the content of magnesium element is 1.3 parts, the content of glycine is 4.2 parts), 10 parts of methionine chelated copper (the content of copper element is 1.7 parts, the content of methionine is 4.8 parts), 10 parts of aspartic acid chelated calcium (the content of calcium element is 1.5 parts, the content of aspartic acid is 5.2 parts) and 70 parts of deionized water; wherein the magnesium element: copper element: the mass ratio of calcium element is 1.3:1.7: 1.5; wherein the weight ratio of glycine: methionine: the mass ratio of aspartic acid is 4.2:4.8: 5.2. The preparation method of the anti-counterfeiting tracking agent is the same as that of the example 1.
The preparation method of the anti-counterfeiting viscose fiber comprises the following specific steps:
(1) soaking wood pulp in 15 wt% NaOH solution at a bath ratio of 1:16, sequentially squeezing, pulverizing, aging, cooling, adding CS2Sulfonating and grinding, and uniformly dissolving in 5 wt% dilute alkali solution to obtain crude viscose with pH of 8.5;
(2) fully mixing the rough viscose, filtering, adding the anti-counterfeiting tracking agent into the rough viscose, defoaming, and aging at 15 ℃ to prepare a spinning solution;
(3) wet spinning the spinning solution, passing through an acid coagulation bath consisting of sulfuric acid, sodium sulfate and zinc sulfate on a spinning machine, forming cellulose slivers at the acid bath temperature of 40 ℃, then drawing at the drawing rate of 15%, cutting, refining, oiling at the oil content of 0.15%, and finally drying at the drying temperature of 60 ℃ to obtain the anti-counterfeiting viscose.
The anti-counterfeiting viscose fiber is viscose staple fiber, the titer is 1.26dtex, and the length is 32 mm.
Through detection of an inductively coupled plasma spectrometer, the content of magnesium element is 14.191ppm (g), the content of copper element is 17.897ppm (g), the content of calcium element is 15.886ppm (g), and then the content of magnesium element: copper element: the mass ratio of calcium element is 1.26:1.60: 1.42.
Through the detection of an amino acid automatic analyzer, the glycine content is 0.13%, the methionine content is 0.15%, and the aspartic acid content is 0.16%, so that the glycine content is as follows: methionine content: the mass ratio of the content of the aspartic acid is 3.90:4.50: 4.80.
Example 3
This example provides an anti-counterfeit viscose fiber and a method for preparing the same, wherein the raw materials include wood pulp (with a polymerization degree of 221) and an anti-counterfeit tracking agent.
The anti-counterfeiting tracking agent is composed of the following raw materials in parts by weight: 10 parts of glycine chelated magnesium (the content of magnesium element is 1.2 parts, the content of glycine is 4 parts), 15 parts of methionine chelated copper (the content of copper element is 2.25 parts, the content of methionine is 6.75 parts), 20 parts of aspartic acid chelated calcium (the content of calcium element is 2 parts, the content of aspartic acid is 10 parts), and 80 parts of deionized water; wherein the magnesium element: copper element: the mass ratio of calcium element is 1.2:2.25: 2; wherein the weight ratio of glycine: methionine: the mass ratio of aspartic acid is 4:6.75: 10. The preparation method of the anti-counterfeiting tracking agent is the same as that of the example 1.
The preparation method of the anti-counterfeiting viscose fiber comprises the following specific steps:
(1) soaking wood pulp in 18 wt% NaOH solution at a bath ratio of 1:18, sequentially squeezing, pulverizing, aging, cooling, adding CS2Sulfonating and grinding, and then uniformly dissolving in 8 wt% dilute alkali solution to obtain crude viscose with pH of 9.1;
(2) fully mixing the rough viscose, filtering, adding the anti-counterfeiting tracking agent into the rough viscose, defoaming, and aging at 20 ℃ to obtain spinning stock solution;
(3) wet spinning the spinning solution, passing through an acid coagulation bath consisting of sulfuric acid, sodium sulfate and zinc sulfate on a spinning machine, forming cellulose slivers at the acid bath temperature of 45 ℃, then drawing at the drawing rate of 15%, cutting, refining, oiling at the oil content of 0.16%, and finally drying at the drying temperature of 60 ℃ to obtain the anti-counterfeiting viscose.
The anti-counterfeiting viscose fiber is viscose staple fiber, the titer is 1.38dtex, and the length is 38 mm.
Through detection of an inductively coupled plasma spectrometer, the content of magnesium element is 9.968ppm (g), the content of copper element is 19.435ppm (g), the content of calcium element is 16.744ppm (g), and then the content of magnesium element: copper element: the mass ratio of calcium element is 1.11:2.17: 1.87.
Through the detection of an amino acid automatic analyzer, if the glycine content is 0.09%, the methionine content is 0.16%, and the aspartic acid content is 0.24%, the glycine content is as follows: methionine content: the mass ratio of the content of the aspartic acid is 3.6:6.4: 9.6.
Example 4
This example provides an anti-counterfeit viscose fiber and a method for preparing the same, wherein the raw materials include wood pulp (with a polymerization degree of 245) and an anti-counterfeit tracking agent.
The anti-counterfeiting tracking agent is composed of the following raw materials in parts by weight: 10 parts of glycine chelated magnesium (the content of magnesium element is 1.2 parts, the content of glycine is 4 parts), 15 parts of methionine chelated copper (the content of copper element is 3 parts, the content of methionine is 7.5 parts), 20 parts of aspartic acid chelated calcium (the content of calcium element is 4 parts, the content of aspartic acid is 11 parts), and 80 parts of deionized water; wherein the magnesium element: copper element: the mass ratio of calcium element is 1.2:3: 4; wherein the weight ratio of glycine: methionine: the mass ratio of aspartic acid is 4:7.5: 11. The preparation method of the anti-counterfeiting tracking agent is the same as that of the example 1.
The preparation method of the anti-counterfeiting viscose fiber comprises the following specific steps:
(1) soaking wood pulp in 18 wt% NaOH solution at a bath ratio of 1:20, sequentially squeezing, pulverizing, aging, cooling, adding CS2Sulfonating and grinding, and then uniformly dissolving in 9 wt% dilute alkali solution to obtain crude viscose with pH of 9.7;
(2) fully mixing the rough viscose, filtering, adding the anti-counterfeiting tracking agent into the rough viscose, defoaming, and aging at 22 ℃ to obtain spinning stock solution;
(3) wet spinning the spinning solution, passing through an acid coagulation bath consisting of sulfuric acid, sodium sulfate and zinc sulfate on a spinning machine, forming cellulose slivers at the acid bath temperature of 45 ℃, then drawing at the drawing rate of 15%, cutting, refining, oiling at the oil content of 0.16%, and finally drying at the drying temperature of 60 ℃ to obtain the anti-counterfeiting viscose.
The anti-counterfeiting viscose fiber is viscose staple fiber, the titer is 1.49dtex, and the length is 41 mm.
Through detection of an inductively coupled plasma spectrometer, the content of magnesium element is 6.884ppm (g), the content of copper element is 16.755ppm (g), the content of calcium element is 22.988ppm (g), and then the content of magnesium element: copper element: the mass ratio of calcium element is 1.15:2.81: 3.86.
Through the detection of an amino acid automatic analyzer, if the glycine content is 0.09%, the methionine content is 0.18%, and the aspartic acid content is 0.26%, the glycine content is as follows: methionine content: the mass ratio of the content of the aspartic acid is 3.6:7.2: 10.4.
Comparing examples 1-4, it can be seen that the denier of the fibers obtained by different methods are close, indicating that the addition of different amino acid metal chelates does not affect the overall fiber performance of the viscose fibers. The above examples 1-4 and the pure viscose fibres without amino acid metal chelate were subjected to mechanical property tests, the preparation method of the pure viscose fibres was as in example 1, and the test results are shown in table 1.
Table 1 mechanical properties test results of viscose fibers
The content of metal elements and the content of amino acids of the anti-counterfeiting viscose fibers prepared in the examples 1 to 4 are compared, and the results are shown in table 2. The proportions of the respective substances in Table 2 are mass ratios.
TABLE 2 amino acid to Metal element content and ratio
Taking the above embodiment as an example, the anti-counterfeiting method of the invention is as follows:
before the anti-counterfeiting viscose fiber is prepared, according to a formula design, numbers are given to glycine, methionine and aspartic acid by using English letters A, B and C, meanwhile, numbers can be given to magnesium elements, copper elements and calcium elements by using Arabic numerals 1, 2 and 3, and then the anti-counterfeiting viscose fiber can be numbered by sequencing according to the dosage from low to high, for example, the anti-counterfeiting viscose fiber of the embodiment 1 is numbered ABC-312, and the anti-counterfeiting viscose fiber of the embodiment 4 is numbered ABC-123.
After the viscose fiber production is completed, the user obtains the design code of the viscose fiber product and the fiber and decrypts the obtained viscose fiber. And detecting the types and the contents of the amino acids and the types and the contents of the metal elements during decryption, combining the amino acids and the metal elements in sequence to obtain decryption codes, and comparing the decryption codes with the obtained design codes to realize the anti-counterfeiting identification of the viscose fibers. As can be seen from table 1, the ratio of the metal elements to the amino acids is not much different from the actual ratio, so the obtained decryption code is consistent with the design code, and the anti-counterfeiting function can be realized by measuring the mass ratio of the metal elements to the amino acids in the viscose fiber.
In the above embodiment, the metal element and the amino acid are added in the viscose fiber production process at different charge ratios, and then the prepared anti-counterfeiting viscose fiber is tested for the metal element and the amino acid, so that the content of the metal element and the amino acid in the anti-counterfeiting viscose fiber is slightly reduced compared with the charge amount, but the actual proportion of the metal element and the amino acid is close to the charge ratio, and therefore, the amino acid chelated metal can be used as one of anti-counterfeiting means of the viscose fiber. The amino acid chelated metal is used as an anti-counterfeiting means of the viscose, two anti-counterfeiting means of metal elements and amino acid can be used, the anti-counterfeiting degree is high, the anti-counterfeiting concealment degree is good, the anti-counterfeiting metal is not easy to counterfeit and damage, and the memory tracking property and the recognition function are realized simultaneously.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, it should be noted that, for those skilled in the art, many modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The amino acid metal chelate is used as an anti-counterfeiting tracking agent of the anti-counterfeiting viscose fiber.
2. The preparation method of the anti-counterfeiting viscose fiber is characterized by comprising the following steps:
(1) soaking pulp in an alkali aqueous solution, then performing squeezing, crushing and ageing treatment, cooling, performing sulfonation treatment, and dissolving in an alkali solution to obtain a rough viscose;
(2) uniformly mixing the crude viscose with various amino acid metal chelates, defoaming and curing to obtain a spinning solution;
(3) carrying out wet spinning on the spinning stock solution, and after acid bath, carrying out drawing, cutting, refining, oiling and drying treatment to obtain the anti-counterfeiting viscose; wherein the sum of the mass of the metal elements contained in the amino acid metal chelate accounts for 0.3-1.1 per mill of the mass fraction of the anti-counterfeiting viscose fiber.
3. The method of claim 2, wherein: in the step (1), the pulp is wood pulp or cotton pulp, and the degree of polymerization of the pulp is 200-600.
4. The method of claim 2, wherein: in step (1), the pH value of the crude viscose is 7-10.
5. The method of claim 2, wherein: in the step (2), the amino acid metal chelate is at least two of glycine chelated magnesium, methionine chelated copper and aspartic acid chelated calcium.
6. The method of claim 5, wherein: the mass ratio of the glycine chelated magnesium to the methionine chelated copper is 1-3: 1-4; the mass ratio of the glycine chelated magnesium to the aspartic acid chelated calcium is 1-3: 1-5; the mass ratio of the methionine chelated copper to the aspartic acid chelated calcium is 1-4: 1-5.
7. The method of claim 2, wherein: in the step (2), the sum of the mass of the metal elements contained in the amino acid metal chelate accounts for 0.5-1.5 per mill of the mass fraction of the spinning solution.
8. The method of claim 2, wherein: in the step (2), the temperature of the aging treatment is 12 ℃ to 24 ℃.
9. The anti-counterfeiting viscose fiber prepared by the preparation method according to any one of claims 2 to 8, which comprises viscose fiber and a plurality of amino acid metal chelates distributed in the viscose fiber, wherein the sum of the metal elements in the amino acid metal chelates accounts for 0.3 to 1.1 per mill of the mass fraction of the anti-counterfeiting viscose fiber.
10. A method for preventing forgery of viscose fiber according to claim 9, comprising the steps of encrypting and decrypting, and identifying:
the encrypting step includes: according to the type and the dosage of the amino acid metal chelate, the anti-counterfeiting viscose fiber is coded to send out encryption information;
the decryption and authentication steps comprise: obtaining encrypted information, and testing the types and the use amounts of amino acid and metal ions in the viscose; then comparing with the obtained encrypted information to identify the authenticity of the viscose fiber.
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| CN112609257B (en) * | 2020-11-11 | 2021-09-17 | 南通纺织丝绸产业技术研究院 | Anti-counterfeiting lyocell fiber, preparation method and anti-counterfeiting method |
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