CN113201801B - Preparation method and application of amino acid chelated zinc modified ramie tencel fiber - Google Patents
Preparation method and application of amino acid chelated zinc modified ramie tencel fiber Download PDFInfo
- Publication number
- CN113201801B CN113201801B CN202110404933.7A CN202110404933A CN113201801B CN 113201801 B CN113201801 B CN 113201801B CN 202110404933 A CN202110404933 A CN 202110404933A CN 113201801 B CN113201801 B CN 113201801B
- Authority
- CN
- China
- Prior art keywords
- amino acid
- reaction
- fiber
- chelated zinc
- acid chelated
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- 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
- D01F2/24—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives
- D01F2/28—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives from organic cellulose esters or ethers, e.g. cellulose acetate
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0212—Face masks
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/731—Cellulose; Quaternized cellulose derivatives
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B3/00—Preparation of cellulose esters of organic acids
- C08B3/14—Preparation of cellulose esters of organic acids in which the organic acid residue contains substituents, e.g. NH2, Cl
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Medicinal Chemistry (AREA)
- Materials Engineering (AREA)
- Textile Engineering (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Biochemistry (AREA)
- Gerontology & Geriatric Medicine (AREA)
- Dermatology (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a preparation method and application of amino acid chelated zinc modified ramie tencel fiber, which is obtained by esterification reaction of amino acid chelated zinc and ramie tencel fiber, ligand amino acid and zinc nitrate are subjected to chelation reaction at the reaction temperature of 50-65 ℃ and the pH value of 4-7, absolute ethyl alcohol is added to precipitate a reaction product, the reaction product is centrifugally separated and dried to obtain amino acid chelated zinc, the amino acid chelated zinc and cellulose pulp are dissolved in a fiber solvent aqueous solution, the esterification reaction is carried out for 3-4 hours under the conditions of 100 ℃ plus organic solvent and 130 ℃ and vacuum stirring to obtain a spinning solution, wet spinning is carried out after filtration and deaeration, and the spinning solution is solidified and formed in a spinning bath to obtain the amino acid chelated zinc modified ramie tencel fiber. The amino acid chelated zinc modified ramie tencel fiber can improve the oxidation resistance, has a good effect of removing free radicals, and can be used in the field of mask base cloth.
Description
Technical Field
The invention belongs to the technical field of fibers for mask base cloth, and particularly relates to a preparation method and application of amino acid chelated zinc modified Laplace tencel fibers.
Background
The cellulose fiber is a fiber for mask base cloth commonly used in the market, a non-woven fabric made of viscose fiber has performance problems, the alginate fiber is a biological base fiber with good hygroscopicity, biocompatibility and degradability, but the breaking strength of the alginate fiber is low, the cohesive force of the fiber is not high, the lyocell fiber is a novel regenerated cellulose fiber, the fiber surface of the lyocell fiber is provided with a plurality of grooves, the air permeability and the hygroscopicity of the fiber are enhanced, and meanwhile, the lyocell fiber has the advantages of natural antibiosis, skin beautifying and the like.
At present, an amino acid chelate is used as an additive of animal feed to promote the growth and development of animals and is mainly used in the field of aquaculture feed, the in-vitro antioxidant capacity of oyster amino acid chelate zinc is researched, the oyster amino acid chelate zinc has better in-vitro antioxidant capacity, the scavenging capacity of the oyster amino acid chelate zinc on three common free radicals, namely DPPH free radicals, superoxide anion free radicals and hydroxyl free radicals, is gradually enhanced along with the increase of the concentration, and the antioxidant value is increased along with the increase of the concentration. Zinc is one of the essential trace elements in human body, and has important physiological function and wide pharmacological action. Zinc has effects in promoting growth, stimulating appetite, promoting wound healing, promoting brain development and intelligence, promoting sexual organ development, improving sexual function, and enhancing immunity. The aspartic acid has strong affinity and can be used as a carrier of certain metal ions to help the aspartic acid enter cells to be absorbed by organisms. The amino acid microelement chelate is easy to absorb, has anti-interference and strong stability, can enhance the immunity of organisms, can fully meet the requirements of life bodies on microelements, and can achieve the double effects of supplementing amino acid. In the prior art, common modifications of cellulose materials comprise flame retardance, antibiosis, ultraviolet resistance, water resistance, moisture permeability and the like, and few researches on the aspect of oxidation resistance are carried out.
Disclosure of Invention
The invention mainly aims to provide a preparation method of a zinc amino acid chelate modified ramie tencel fiber, which is obtained by esterification reaction of the zinc amino acid chelate and the ramie tencel fiber and comprises the following steps:
(1) carrying out chelation reaction on ligand amino acid and zinc nitrate at the reaction temperature of 50-65 ℃ and the pH value of 4-7, adding absolute ethyl alcohol to precipitate a reaction product, carrying out centrifugal separation, and drying to obtain amino acid chelated zinc;
(2) dissolving the amino acid chelated zinc and the cellulose pulp obtained in the step (1) in a fiber solvent aqueous solution, and carrying out esterification reaction for 3-4 hours at the temperature of 100-130 ℃ under the condition of vacuum stirring to obtain a spinning solution;
(3) and (3) filtering and defoaming the spinning solution obtained in the step (2), then carrying out wet spinning, and coagulating and forming in a spinning bath to obtain the amino acid chelated zinc modified Lemie tencel fiber, wherein the amino acid chelated zinc accounts for 1% -3% of the total amount of the product.
In some embodiments, in step (1), the molar ratio of zinc nitrate to ligand amino acid is 1-2: 1-3.
Preferably, in the step (1), the ligand amino acid is L-aspartic acid, and the amino acid chelated zinc is L-aspartic acid chelated zinc, and the preparation method comprises the following steps: adding 0.538g L-asparagus amino acid and 20mL of distilled water into a round bottom flask, heating to 40-55 ℃ in an oil bath, slowly adding a zinc nitrate aqueous solution under the condition of magnetic stirring, recording the reaction starting time, adjusting the pH of a reaction solution to be within the range of 4-7 by using 6mol/L NaOH solution, heating to 50-65 ℃ for carrying out heat preservation reaction for 1 hour, adding absolute ethyl alcohol to precipitate a reaction product, carrying out centrifugal separation, and drying to obtain the L-asparagus amino acid chelated zinc, wherein the reaction formula is as follows:
wherein n is [1,1000000000 ].
In some embodiments, in step (2), the fiber solvent is selected from N-methylmorpholine-N-oxide (NMMO), and the mass fraction of the aqueous fiber solvent solution is 45% to 55%.
In some embodiments, in step (2), the cellulose pulp is selected from one or a combination of two or more of hemp fiber, wood fiber and bamboo fiber, and the mass volume ratio of the cellulose pulp to the fiber solvent aqueous solution is 1: 15-25 (g/mL).
In some embodiments, the wet-spun product of step (3) further comprises the steps of alcohol washing, water washing, oil bath, drying and post-processing.
The invention also provides the amino acid chelated zinc modified ramie tencel fiber, which is obtained by the preparation method of the amino acid chelated zinc modified ramie tencel fiber.
The invention also provides application of the amino acid chelated zinc modified Laplace tencel fiber in an antioxidant mask base cloth. The Laplace tencel fiber modified by the amino acid chelated zinc has good capability of eliminating free radicals (DPPH free radicals, superoxide anion free radicals and hydroxyl free radicals), and can be used for improving facial aging when being used for facial mask base cloth.
Compared with the prior art, the invention has the beneficial effects that: the amino acid chelated zinc modified lyocell fiber is obtained by wet spinning of the spinning solution obtained by dissolving the amino acid chelated zinc and the cellulose pulp in the fiber solvent water solution, so that the inoxidizability of the fiber can be improved, the removal effect on free radicals (DPPH free radicals, superoxide anion free radicals and hydroxyl free radicals) is good, amino acid and trace elements can be supplemented, the production process is relatively simple and convenient, and the lyocell fiber can be used in the field of mask base cloth by combining the advantages of liquid retention rate, air permeability, stability, bacteriostasis, softness and the like of the lyocell fiber.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the invention without limiting the invention to the right. It is obvious that the drawings in the following description are only some embodiments, and that for a person skilled in the art, other drawings can be derived from them without inventive effort. In the drawings:
FIG. 1 is a flow chart of a process for preparing a lyocell fiber modified with zinc amino acid chelate according to an embodiment of the present invention.
FIG. 2 is a flow chart of a preferred embodiment of a process for preparing amino acid chelated zinc modified lyocell fiber.
Detailed Description
As shown in figure 1, the preparation method of the L-aspartic acid chelated zinc modified ramie tencel fiber comprises the following steps:
(1) adding 0.538g L-asparagus amino acid and 20mL of distilled water into a round-bottom flask, heating the flask to 40-55 ℃ in an oil bath, magnetically stirring the flask, slowly adding a zinc nitrate aqueous solution in a corresponding proportion, recording the initial reaction time, adjusting the pH of a reaction solution to 4-7 by using 6mol/L NaOH solution, heating the reaction solution to 50-65 ℃, keeping the temperature for reaction for 1h, adding absolute ethyl alcohol to precipitate a chelate after the reaction is finished, centrifugally separating and drying the chelate, thereby obtaining the L-asparagus amino acid chelated zinc.
(2) Distilling the NMMO aqueous solution with the mass fraction of 45% -55% under reduced pressure to obtain the NMMO aqueous solution with the appropriate concentration, dissolving the amino acid chelated zinc and the cellulose pulp into the NMMO aqueous solution, wherein the bath ratio of the mass (g) of the cellulose pulp to the volume (mL) of the NMMO aqueous solution is 1: 15-20, and carrying out esterification reaction for 3-4 hours in a reaction kettle at the temperature of 100-130 ℃ under the condition of vacuum stirring to obtain uniform spinning solution.
(3) Adding the spinning solution obtained in the step (2) into a screw extruder, dissolving and filtering at the temperature of 100-: the length of the air gap is 6-8cm, the spinning speed is 40-50m/min, the aperture of the spinneret plate is 40 microns, and the length of the pore capillary is 400 microns; the sprayed silk threads are vertically stretched in the air and enter a coagulating bath for coagulation forming, the coagulating bath is an NMMO aqueous solution with the concentration of 15%, and the temperature of the coagulating bath is 0 ℃.
(4) Fiber alcohol washing: immersing the fiber obtained in the step (3) into an ethanol solution with a proper concentration for 3.5-4.5 hours at a bath ratio of 1: 15-20.
(5) fiber washing: immersing the fiber treated in the step (4) in hot water at the temperature of 80-90 ℃ for 2-3 hours at a bath ratio of 1: 20-30.
(6) fiber oil bath: immersing the fiber treated in the step (5) into an oil bath solution with a certain concentration, wherein the oil bath temperature is 80-90 ℃, the time is 2.5-3 hours, and the bath ratio is 1: 20-30.
(7) drying the fibers: and (4) drying the fiber treated in the step (6) to obtain the L-aspartic acid zinc chelate modified ramie tencel fiber.
The following examples are given to illustrate the present invention but not to limit the scope of the present invention.
Example one
The preparation method of the L-aspartic acid chelated zinc modified ramie tencel fiber comprises the following steps:
(1) adding 0.538g L-asparagus amino acid and 20mL of distilled water into a round-bottom flask, heating the flask to 40 ℃ in an oil bath, magnetically stirring the flask, slowly adding a zinc nitrate aqueous solution in a corresponding proportion, recording the initial reaction time, adjusting the pH of a reaction solution to be 6 by using 6mol/L NaOH solution, heating the reaction solution to 60 ℃, keeping the temperature for reaction for 1h, adding absolute ethyl alcohol to precipitate a chelate after the reaction is finished, and performing centrifugal separation and drying to obtain the L-asparagus amino acid chelated zinc.
(2) Distilling 45-55% of NMMO aqueous solution in mass fraction under reduced pressure to obtain an NMMO aqueous solution with a proper concentration, dissolving 10g of the amino acid chelated zinc obtained in the step (1) and 500g of cellulose pulp in the NMMO aqueous solution, wherein the bath ratio of the mass (g) of the cellulose pulp to the volume (mL) of the NMMO aqueous solution is 1: and 15, carrying out esterification reaction for 3 hours in a reaction kettle at the temperature of 100 ℃ under the condition of vacuum stirring to obtain uniform spinning solution.
(3) Adding the spinning solution obtained in the step (2) into a screw extruder, dissolving and filtering at 110 ℃, and entering a spinning system for wet spinning, wherein the process parameters are as follows: the length of an air gap is 7cm, the spinning speed is 45m/min, the aperture of a spinneret plate is 40 microns, the length of a pore capillary is 400 microns, the sprayed silk yarn is vertically stretched in the air and enters a coagulation bath for coagulation forming, the coagulation bath is an NMMO aqueous solution with the concentration of 15%, the temperature of the coagulation bath is 0 ℃, and the L-aspartic acid chelated zinc modified ramie tencel fiber capable of resisting oxidation is obtained through post-treatment such as alcohol washing, water washing, oil bath, drying, post-processing and the like.
Example two
The method for preparing the L-aspartic acid zinc chelate modified Laplace silk fiber according to the first embodiment is characterized in that: in the step (1), a zinc-containing metal compound Zn (OH) is selected2And L-aspartic acid according to a molar ratio of 2: 3, mixing the ingredients.
Effect example 1
The L-aspartic acid zinc chelate modified ramie tencel fiber prepared in the first and second embodiments is subjected to metal element content detection according to the following method, and the specific detection method comprises the following steps:
(S1) adding 0.2g of L-aspartic acid zinc chelate modified ramie tencel fiber sample into 10mL of sulfuric acid solution, then carrying out digestion treatment, gradually increasing the digestion temperature to 180 ℃ for 30 minutes, evaporating the digested solution at 135 ℃ for 3 hours to evaporate sulfuric acid, and fixing the volume to obtain 10mL of constant volume solution.
(S2) carrying out element quantitative analysis on the constant volume solution obtained in the step (S1) by using an inductively coupled plasma spectrometer. The total content of metal ions in the L-aspartic acid zinc chelate modified lyocell fiber is shown in Table 1.
The L-aspartic acid zinc chelate modified Laplace silk fiber prepared in the first and second embodiments is used for detecting the amino acid content according to the following method, and the specific detection method is as follows:
(a) sampling: short fibers with the length of the sample being not more than 5mm are selected, and then 0.5000g of the sample is weighed and placed in a hydrolysis tube.
(b) Hydrolysis and deacidification: adding 15.0mL of 6.0mol/L hydrochloric acid solution into a hydrolysis tube with a short fiber sample, cooling the hydrolysis tube in an ice-water mixture for 4min, introducing high-purity nitrogen into the hydrolysis tube for about 2min, quickly covering a bottle cap, sealing a jaw, placing the hydrolysis tube in a constant-temperature drying oven at 110 ℃ for hydrolysis, and taking out and cooling after 22 h. And opening the hydrolysis tube, transferring the hydrolysis liquid into a 50mL volumetric flask, washing the hydrolysis tube with water for multiple times, metering the volume, uniformly mixing, and filtering with filter paper. Transferring 1.0mL of the filtrate into a 5mL beaker by using a pipette, placing the beaker into a drying oven with the constant temperature of 50 ℃ for drying, dissolving and drying the residue by using 2.0mL of water, and repeating the dissolving and drying operations twice until the residue is completely evaporated to dryness. 0.02mol/L hydrochloric acid 1.0mL is removed to fully dissolve the residue in the beaker, the residue is filtered by a water phase filtering membrane with the aperture of 0.45 micrometer, and the filtrate is used for testing of an automatic amino acid analyzer.
(c) Testing an instrument: 0.2mol of amino acid standard solution is absorbed, diluted to 5mL by 0.02mol/L hydrochloric acid solution to be used as the standard solution for the machine test of the automatic amino acid analyzer, the concentration of the diluted amino acid standard solution is 100nmol/L, and the type and the content of the amino acid in the extracting solution are measured by using an external standard method. The results of measuring the total content of amino acids and the total content of metal elements in the L-aspartic acid zinc chelate modified ramie silk fiber prepared in the first and second examples are shown in Table 1, wherein the total content of amino acids and the total content of metal ions refer to the percentage of amino acids or metal ions in the total mass of the L-aspartic acid zinc chelate modified ramie silk fiber.
TABLE 1
| Example one | Example two | |
| The total content of L-aspartic acid | 1.1％ | 1.5％ |
| Metal ion total content ratio | 0.2％ | 0.258％ |
Effect example 2
The oxidation resistance of the L-aspartic acid zinc chelate modified lyocell fibers prepared in examples one and two was tested according to the prior art, wherein the comparative group was the lyocell fibers prepared without adding the amino acid zinc chelate, the total mass of the L-aspartic acid zinc chelate modified lyocell fibers prepared in examples one and two was 334g, and the mass of the amino acid zinc chelate was 2% of the total mass of the lyocell fibers, and the results are shown in table 2.
TABLE 2
| Example one | Example two | Control group | |
| Antioxidant value (AOV) (mg/g) | 52.53 | 54.12 | 10 |
| DPPH free radical (%) | 85.1 | 85.9 | 15.31 |
| Superoxide anion radical (%) | 51.21 | 52 | 12.9 |
| Hydroxyl radical (%) | 82.64 | 83.5 | 4.9 |
The present invention has been described in detail with reference to the embodiments, but the contents are only preferred examples of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (7)
1. The application of the amino acid chelated zinc modified ramie tencel fiber in the anti-oxidation mask base cloth comprises the following steps:
(1) carrying out chelation reaction on ligand amino acid and zinc nitrate at the reaction temperature of 50-65 ℃ and the pH value of 4-7, adding absolute ethyl alcohol to precipitate a reaction product, carrying out centrifugal separation, and drying to obtain amino acid chelated zinc;
(2) dissolving the amino acid chelated zinc and the cellulose pulp obtained in the step (1) in a fiber solvent aqueous solution, and carrying out esterification reaction for 3-4 hours at the temperature of 100-130 ℃ under the condition of vacuum stirring to obtain spinning solution;
(3) and (3) filtering and defoaming the spinning solution obtained in the step (2), performing wet spinning, and solidifying and forming in a spinning bath to obtain the amino acid chelated zinc modified ramie tencel fiber, wherein the amino acid chelated zinc accounts for 1% -3% of the total amount of the product.
2. The use according to claim 1, wherein in step (1), the molar ratio of zinc nitrate to ligand amino acid is 1-2: 1-3.
3. The use of claim 1, wherein in step (1), the ligand amino acid is L-aspartic acid, and the amino acid chelated zinc is L-aspartic acid chelated zinc, and is prepared by the following method: adding 0.538g L-asparagus amino acid and 20mL of distilled water into a round-bottom flask, heating the round-bottom flask to 40-55 ℃ in an oil bath, slowly adding a zinc nitrate aqueous solution under the condition of magnetic stirring, recording the initial reaction time, adjusting the pH of a reaction solution to be within the range of 4-7 by using 6mol/L NaOH solution, heating the reaction solution to 50-65 ℃ for heat preservation reaction for 1 hour, adding absolute ethyl alcohol to precipitate a reaction product, performing centrifugal separation, and drying to obtain the compound, wherein the reaction formula is shown as follows:
wherein n is [1,1000000000 ].
4. The use according to claim 1, wherein in step (2), the fiber solvent is selected from N-methylmorpholine-N-oxide (NMMO), and the mass fraction of the fiber solvent aqueous solution is 45% -55%.
5. The use according to claim 1, wherein in step (2), the cellulose pulp is selected from one or a combination of two or more of hemp fibers, wood fibers and bamboo fibers.
6. Use according to claim 5, wherein the mass to volume ratio of the cellulose pulp to the aqueous solution of the fiber-solvent is 1 g: 15-25 mL.
7. The use according to claim 1, wherein in step (3), the wet-spun product further comprises the steps of alcohol washing, water washing, oil bath, drying and post-processing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110404933.7A CN113201801B (en) | 2021-04-15 | 2021-04-15 | Preparation method and application of amino acid chelated zinc modified ramie tencel fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110404933.7A CN113201801B (en) | 2021-04-15 | 2021-04-15 | Preparation method and application of amino acid chelated zinc modified ramie tencel fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113201801A CN113201801A (en) | 2021-08-03 |
| CN113201801B true CN113201801B (en) | 2022-07-22 |
Family
ID=77027083
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110404933.7A Active CN113201801B (en) | 2021-04-15 | 2021-04-15 | Preparation method and application of amino acid chelated zinc modified ramie tencel fiber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113201801B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001048056A1 (en) * | 1999-12-28 | 2001-07-05 | Mitsui Chemicals, Incorporated | Process for producing crosslinked polyaspartic acid (salt) |
| CN112609257A (en) * | 2020-11-11 | 2021-04-06 | 南通纺织丝绸产业技术研究院 | Anti-counterfeiting lyocell fiber, preparation method and anti-counterfeiting method |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004050664A1 (en) * | 2002-12-05 | 2004-06-17 | Md Bioalpha Co., Ltd. | Method for preparation of amino acid chelate |
| US20130122140A1 (en) * | 2011-11-16 | 2013-05-16 | Robert Kim | Alkaline Mineral Booster With Antioxidants |
-
2021
- 2021-04-15 CN CN202110404933.7A patent/CN113201801B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001048056A1 (en) * | 1999-12-28 | 2001-07-05 | Mitsui Chemicals, Incorporated | Process for producing crosslinked polyaspartic acid (salt) |
| CN112609257A (en) * | 2020-11-11 | 2021-04-06 | 南通纺织丝绸产业技术研究院 | Anti-counterfeiting lyocell fiber, preparation method and anti-counterfeiting method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113201801A (en) | 2021-08-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101802277B (en) | Lyocell fiber | |
| CN107447297B (en) | A kind of hydrogel alginate fibre and preparation method thereof | |
| CN101250759B (en) | Medical chitosan fibre and preparation method thereof | |
| CN108221081B (en) | High-strength carboxymethyl cellulose/sodium alginate blend fiber and preparation method thereof | |
| CN109234826B (en) | Method for preparing lyocell fibers by using bamboo as raw material | |
| CN101974800B (en) | Method for manufacturing wood-pupa protein viscose staple fibers | |
| US20220411967A1 (en) | Anti-counterfeiting lyocell fiber, preparation method thereof and anti-counterfeiting method | |
| CN109183171A (en) | A kind of wild Flos Lonicerae viscose rayon preparation method with antibacterial action | |
| CN101509156B (en) | Method of preparing soy protein/cellulosic composite fiber with high protein inventory | |
| CN113201801B (en) | Preparation method and application of amino acid chelated zinc modified ramie tencel fiber | |
| CN109321990B (en) | Preparation method of super-hydrophobic lyocell fibers | |
| GB522542A (en) | Improved process for the manufacture of crimped artificial textile filaments, and filaments produced thereby | |
| Kamalha et al. | Analysis of the secondary crystalline structure of regenerated Bombyx mori fibroin | |
| CN102899734A (en) | Silk fibroin hollow fiber and preparation method thereof | |
| CN104358026B (en) | The preparation method of the nitrification cellulose diacetate nano fibrous membrane of adsorbable-desorption protein | |
| CN110699769B (en) | Method for preparing lyocell fibers by using ramie fibers as raw materials | |
| CN105369389A (en) | Collagen fiber and its production process | |
| CN112281231A (en) | Eupatilin-containing wormwood fiber capable of protecting health and preserving health and preparation method thereof | |
| CN107502982B (en) | Preparation method of feather keratin viscose fiber | |
| CN1195109C (en) | Method for manufacturing soybean protein glued fiber | |
| CN112626631B (en) | Sea-buckthorn fiber and preparation method thereof | |
| CN110230111A (en) | A method of Lyocell fibers are prepared by raw material of poplar | |
| CN102558292A (en) | Preparation method of fibroins of different forms | |
| CN111321478B (en) | Preparation process of modified water-resistant fiber | |
| CN112760745A (en) | Textile fiber with radiation protection function and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |