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CN117090052A - Preparation method of antigen fibrillated lyocell fibers - Google Patents

Preparation method of antigen fibrillated lyocell fibers Download PDF

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Publication number
CN117090052A
CN117090052A CN202310798190.5A CN202310798190A CN117090052A CN 117090052 A CN117090052 A CN 117090052A CN 202310798190 A CN202310798190 A CN 202310798190A CN 117090052 A CN117090052 A CN 117090052A
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antigen
cross
linking agent
acid
fibrillating
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CN117090052B (en
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王景
梁永标
张金波
黄尚东
陈卓越
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DYMATIC CHEMICALS Inc
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DYMATIC CHEMICALS Inc
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    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/35—Heterocyclic compounds
    • D06M13/355—Heterocyclic compounds having six-membered heterocyclic rings
    • D06M13/358—Triazines
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
    • D06M11/55—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
    • D06M11/56—Sulfates or thiosulfates other than of elements of Groups 3 or 13 of the Periodic Table
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
    • D06M11/76—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon oxides or carbonates
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/192—Polycarboxylic acids; Anhydrides, halides or salts thereof
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
    • D06M13/248—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing sulfur
    • D06M13/256—Sulfonated compounds esters thereof, e.g. sultones
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    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/402—Amides imides, sulfamic acids
    • D06M13/418—Cyclic amides, e.g. lactams; Amides of oxalic acid
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    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
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    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/53—Polyethers
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    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic

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Abstract

The application discloses a preparation method of an antigen fibrillating lyocell fiber, which comprises the following steps of S1) adding the fiber into the fiber at room temperature according to a bath ratio of 1:4-10, and preparing a cross-linking agent aqueous solution according to an antigen fibrillating composition of 2-5g/L and anhydrous sodium sulphate of 30-50 g/L; s2) heating to 60-80 ℃, preserving heat for 20min, adding 15-30g/L of sodium carbonate, adjusting pH to 11-12 with 30% caustic soda solution after 10min of operation, and continuing to operate for 30 min; s3) taking out of the tank, washing, neutralizing, washing and drying; the antigen fibrillation composition comprises a cross-linking agent, a dispersing agent and a buffering agent, wherein the cross-linking agent comprises the following components in parts by weight: 60-90% of dispersing agent: 30-50%, buffer: 1-5, mixing the components and spray drying to obtain the solid antigen fibrillating composition. The application adopts the mixture of the multi-active-group cross-linking agent as a main body, the structure of the multi-active-group cross-linking agent has better stability under neutral conditions, one active group is hydrolyzed, the other active group still reacts with the fiber, the reactivity is higher, and the fiber-cross-linking agent bond stability after cross-linking is good due to two active groups with different acid and alkali resistance.

Description

Preparation method of antigen fibrillated lyocell fibers
Technical Field
The application relates to the technical field of dyeing and finishing, in particular to a preparation method of antigen fibrillated lyocell fibers.
Background
Currently, reducing the fibrillation propensity of Lyocell fibers is achieved primarily by antigen-fibrillating cross-linkers. The patent publication No. WO95/28516A discloses a crosslinking agent having a plurality of acrylamide groups, preferably 1,3, 5-triacrylate-hexahydrotriazine, which effectively reduces the fibrillation tendency of solvent-spun cellulose fibers, but the crosslinking agent is cumbersome to synthesize, expensive, poorly water-soluble and unstable to alkali after crosslinking; the patent publication WO99/19555A reports that substituted dichlorotriazine cross-linking agents, preferably 2, 4-dichloro-6-hydroxytriazine sodium salt, have good antigen fibrillation performance, have higher liquid content and large dosage, are not easy to store for a long time, are easy to hydrolyze and are unstable to acid. The patent CN103306136A takes the composition of oligomeric polybasic acid and C2-C6 polybasic acid as a cross-linking agent, improves the fibrillation performance of the fiber antigen by high-temperature heating, but has the defects of yellowing and strong damage of the finished fabric and large industrialization difficulty due to complex use process.
Disclosure of Invention
The application aims to provide a preparation method of an antigen fibrillated lyocell fiber, which overcomes the defects of the prior art, and prepares an antigen fibrillating composition to carry out antigen fibrillating treatment on the lyocell fiber by selecting a proper cross-linking agent and an auxiliary agent, and the lyocell fiber finished by adopting the composition has the characteristics of excellent antigen fibrillating performance, good acid and alkali resistance stability, low fabric strength damage, safety, no formaldehyde and the like, and can be used for dipping and steaming processes, dyeing and antigen fibrillating can be carried out in one bath, and the process flow is greatly shortened.
In order to solve the technical problems, the application is realized by the following technical scheme:
the preparation method of the antigen fibrillated lyocell fiber is characterized by comprising the following steps of: s1) adding fiber at room temperature with a bath ratio of 1:4-10, and preparing a cross-linking agent aqueous solution according to 2-5g/L of an antigen fibrillating composition and 30-50g/L of anhydrous sodium sulphate; s2) heating to 60-80 ℃, preserving heat for 20min, adding 15-30g/L of sodium carbonate, preserving heat and running for 30-60min; s3) taking out of the tank, washing, neutralizing, washing and drying;
the antigen fibrillation composition comprises a cross-linking agent, a dispersing agent and a buffering agent, wherein the cross-linking agent comprises the following components in parts by weight: 60-90% of dispersing agent: 20-50%, buffer: 1-5, mixing the components and spray drying to prepare a solid antigen fibrillating composition;
the cross-linking agent is one or more multi-functional triazine compounds which are compounded and used, and the molecular structural general formula is as follows:
wherein the active groups X and Y are the same or different and are selected from one or more of F, cl, nicotinic acid, isonicotinic acid, triethylenediamine, 4-beta-hydroxyethylsulfonyl sulfate aniline-2-sulfonic acid, p-aminophenyl-beta-hydroxyethylsulfonyl sulfate, m-aminophenyl-beta-hydroxyethylsulfonyl sulfate, 2- (2-aminoethyl) sulfonyl ethanol sulfate and 2- [ (chloroethyl) sulfonyl ] ethanol hydrochloride;
r is a modifying group or an active group and is selected from one or more of F, cl, OH, sulfanilic acid, m-sulfanilic acid, p-aminobenzoic acid and 2, 5-disulfonic aniline;
a is a linking group or a bridging group, and is selected from one or more of p-phenylenediamine, m-phenylenediamine, o-phenylenediamine, 2, 4-diaminobenzenesulfonic acid, 2, 5-diaminobenzenesulfonic acid, m-phenylenediamine disulfonic acid, ethylenediamine, propylenediamine, hexamethylenediamine, polyethylene glycol and polyether amine.
The dispersing agent is one or more of alkylphenol ethoxylates, fatty amine ethoxylates, fatty alcohol polyoxyethylene ether sodium sulfate, fatty alcohol polyoxyethylene ether sodium carboxylate, isomeric alcohol polyoxyethylene ether, sodium secondary alkyl sulfonate, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, methyl naphthalene sulfonate formaldehyde condensate, methylene dinaphthyl sulfonate sodium, benzyl naphthalene sulfonate formaldehyde condensate, alkylbenzene sulfonate formaldehyde condensate and sodium lignin sulfonate.
The preparation method of the antigen fibrillated lyocell fiber, wherein the buffer is selected from one of tris (hydroxymethyl) aminomethane+ethylenediamine tetraacetic acid, tris (hydroxymethyl) aminomethane+ethylenediamine tetraacetic acid disodium salt, triethanolamine+ethylenediamine tetraacetic acid disodium salt, succinic acid+caprolactam, disodium hydrogen phosphate+sodium dihydrogen phosphate, disodium hydrogen phosphate+potassium dihydrogen phosphate
The application has the following beneficial effects:
(1) The application adopts the mixture of the multi-active-group cross-linking agent as a main body, has alkali-resistant monochloro/dichloro-s-triazine/quaternary ammonium cations and acid-resistant vinyl sulfone functional groups after cross-linking, has better stability under neutral conditions, has one active group hydrolyzed, has higher reactivity with fiber, and has better stability of the fiber-cross-linking agent bond after cross-linking due to the acid-resistant and alkali-resistant active groups.
(2) According to the application, the cross-linking agent and the dispersing agent are combined, so that the structural hydrophilicity and diffusivity of the cross-linking agent are increased, and the cross-linking agent and the inside of the fiber are fully contacted and reacted, so that the cross-linking rate is improved. And the steric hindrance and electrostatic repulsion provided by the dispersing agent are beneficial to the saline-alkali resistance stability of the crosslinking agent molecules, and the working solution can be kept clear and transparent within one hour, so that the conditions of insufficient water solubility of the crosslinking agent or precipitation due to increased association degree after encountering saline alkali and uneven treatment effect are prevented.
(3) The antigen fibrillating composition is suitable for impregnation and steaming processes, the crosslinking equipment is conventional equipment, the existing equipment of a factory does not need to be refitted, and the antigen fibrillating composition is convenient to use and easy to operate for customers.
(4) The cross-linking agent used in the application has simple synthesis process and low price, the cross-linking agent solution just prepared is added with a dispersing agent and a buffering agent for pulping treatment, and is stored after standardized spray drying, the storage shelf life of the cross-linking agent is prolonged, and the cross-linking agent can be stored for one year or even longer, and the strength of the product is basically unchanged.
(5) The antigen has good fibrillation effect, good washing resistance and no formaldehyde release, and avoids harm to human body and environment.
Detailed Description
The following description of the embodiments of the present application will be made clearly and completely, and it is apparent that the described embodiments are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Example 1:
1. an antigen-fibrillating composition:
(1) The raw materials are selected according to the following weight percentages:
wherein the structural formula of the cross-linking agent A is shown in Table 6.
(2) The preparation method of the antigen fibrosis composition specifically comprises the following steps: firstly, regulating the pH value of the slurry of the cross-linking agent A reacted to the end point to be 5-6 by using sodium carbonate, then adding sodium dodecyl benzene sulfonate, sodium methylenedinaphthyl sulfonate NNO, succinic acid and caprolactam into the reaction solution of the cross-linking agent A with the content of 22%, fully stirring for 1 hour at 15-20 ℃, transferring the slurry into a spray tower storage tank, and packaging after spray drying, thus obtaining the antigen fibrillating composition I-1.
2. Antigen fibrillation crosslinking finishing:
bath ratio 1:8, adding fiber at room temperature, and preparing a cross-linking agent aqueous solution according to 3g/L of the antigen fibrillating composition and 40g/L of anhydrous sodium sulphate; heating to 60 ℃, preserving heat for 20min, adding 20g/L of sodium carbonate, preserving heat and running for 40min, taking out of a cylinder, washing with water, neutralizing, washing with water and drying to obtain the antigen fibrillated lyocell fiber.
Examples 2 to 6:
the antigen-fibrillating composition of the present application can be prepared according to the method described in the above example 1, except that the components of example 1 are replaced with the raw material components of crosslinking agent, dispersant, and buffer, respectively, in the following table 1 in mass fractions:
table 1 antigen-fibrillating compositions of examples 2 to 6
Example 7
1. An antigen-fibrillating composition:
(1) The raw materials are selected according to the following weight percentages:
wherein the structural formulas of the cross-linking agent A and the cross-linking agent G are shown in the table 6.
(2) The preparation method of the antigen fibrosis composition specifically comprises the following steps: firstly, regulating the pH value of the slurry of the cross-linking agent A reacted to the end point to be 5-6 by using sodium carbonate, then adding the solid of the cross-linking agent G, sodium dodecyl benzene sulfonate, sodium methylene dinaphthyl sulfonate NNO, succinic acid and caprolactam into the reaction solution of the cross-linking agent A with the content of 15 percent, fully stirring for 1 hour at 15-20 ℃, then transferring the slurry into a spray tower storage tank, and packaging after spray drying, thus obtaining the antigen fibrillating composition I-7.
2. Antigen fibrillation crosslinking finishing:
bath ratio 1:8, adding fiber at room temperature, and preparing a cross-linking agent aqueous solution according to 3g/L of the antigen fibrillating composition and 40g/L of anhydrous sodium sulphate; heating to 60 ℃, preserving heat for 20min, adding 20g/L of sodium carbonate, running for 30min, taking out of a cylinder, washing with water, neutralizing, washing with water, and drying to obtain the antigen fibrillated lyocell fiber.
Examples 8 to 12:
the antigen-fibrillating composition of the present application can be prepared according to the method described in example 7 above, except that the components of example 7 are replaced with the raw material components of crosslinking agent, dispersant, and buffer, respectively, in the following table 2 in mass fractions:
TABLE 2 antigen-fibrillating compositions of examples 8 to 12
Comparative example 1
The comparative example differs from example 7 in that the composition of the comparative example is made from the following raw materials in parts by weight:
1. an antigen-fibrillating composition:
(1) The raw materials are selected according to the following weight percentages:
(2) The preparation method of the antigen fibrosis composition specifically comprises the following steps: firstly, regulating the pH value of the cross-linking agent A slurry reacted to the end point to be 5-6 by using sodium carbonate, then adding cross-linking agent G, succinic acid and caprolactam into the cross-linking agent A reaction liquid with the content of 15%, fully stirring for 1 hour at 15-20 ℃, then transferring the slurry into a spray tower storage tank, spray drying and packaging to obtain the antigen fibrillating composition I-13.
2. Antigen fibrillation crosslinking finishing:
bath ratio 1:8, adding fiber at room temperature, and preparing a cross-linking agent aqueous solution according to 2.4g/L (the cross-linking agent content is the same as the ratio) of the antigen fibrillating composition and 40g/L of anhydrous sodium sulphate; heating to 60 ℃, preserving heat for 20min, adding 20g/L of sodium carbonate, running for 45min, taking out of a cylinder, washing with water, neutralizing, washing with water, and drying to obtain the antigen fibrillated lyocell fiber.
Comparative examples 2 to 6:
the antigen-fibrillating composition of the present application can be prepared by the method described in the above comparative example 1, except that the components in proportion 1 are replaced with the raw material components crosslinking agent, dispersant, buffer, etc. in the following table 3, respectively, in mass fractions:
table 3 antigen-fibrillating compositions of comparative examples 2 to 6
Performance test
1. And (3) salt and alkali resistance test: to 100ml of deionized water, 2g of the antigen-fibrillating compositions obtained in examples 1 to 12 and comparative examples 1 to 6, respectively, were added, and the temperature was raised to 60℃and kept for 10 minutes to dissolve. Sampling was performed at a constant temperature, saline-alkali (20 g/L sodium carbonate and 40g/L sodium sulfate were added to the solution) was added with stirring, and pH=12 was adjusted using 30% caustic soda solution. The dissolution was observed by spot method at 60℃for every 5min until the composition had a significant halo on the filter paper, and the saline-alkali tolerance time was calculated and the results are shown in Table 4:
TABLE 4 saline-alkali tolerance test results of antigen-fibrillated compositions (stability test of compositions)
As shown in Table 4, the antigen-fibrillating composition prepared by the method of the present application can obviously prolong the salt and alkali tolerance time of the crosslinking agent and improve the solubility of the crosslinking agent.
2. Wet abrasion times: the application aims at a method for measuring the fibrillation degree, which is used for testing the wet abrasion times of fibers, and specific detection methods and performance indexes refer to the standard FZ/T52019-2018 and T/CCFA 01026-2016. The resulting fibers were measured for wet abrasion values, and the blank was fibers that were not crosslinked, and the results are shown in Table 5.
3. Acid and alkali resistance test after crosslinking: 130/100/60℃test method: bath ratio 1:10, adding fibrillated and finished fibers at room temperature, and adjusting different pH values by using a working solution: ph=2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13; heating to 130/100/60 ℃, preserving heat for 40min, washing with water, drying, and testing the wet abrasion value. Alkali resistance test method at room temperature (25 ℃): adding the fibers into caustic soda solutions with different concentrations, soaking for 1min, washing in dilute alkali, washing with water, drying, and testing the wet abrasion value. The wet abrasion value was retained by 80% or more, which means that the acid-base number was maintained under this condition, and the results are shown in Table 5.
TABLE 5 results of testing for antigen fibrosis related properties
In combination with examples 1-12 and comparative examples 1-6, it can be seen from Table 1 that the number of wet abrasion times of Lyocell fibers after finishing the crosslinked composition is significantly increased, and the crosslinking agent and the dispersing agent cooperate with each other to increase the structural hydrophilicity and diffusivity of the crosslinking agent, so that the fibers react with the crosslinking agent and crosslink more sufficiently, and the wet abrasion value of the finished fibers is increased more significantly than that of the comparative examples without the dispersing agent. In addition, the combination of two active groups with different acid and alkali resistance ensures that the fiber-cross-linking agent bond after cross-linking has good stability, has excellent acid and alkali resistance, and can meet the requirements of various application scenes of dyeing and finishing.
Table 6: keySubstancesin patent
The preferred embodiments of the application disclosed above are intended only to assist in the explanation of the application. The preferred embodiments are not exhaustive or to limit the application to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the application and the practical application, to thereby enable others skilled in the art to best understand and utilize the application. The application is limited only by the claims and the full scope and equivalents thereof.

Claims (3)

1. The preparation method of the antigen fibrillated lyocell fiber is characterized by comprising the following steps of: s1) adding fiber at room temperature with a bath ratio of 1:4-10, and preparing a cross-linking agent aqueous solution according to 2-5g/L of an antigen fibrillating composition and 30-50g/L of anhydrous sodium sulphate; s2) heating to 60-80 ℃, preserving heat for 20min, adding 15-30g/L of sodium carbonate, preserving heat and running for 30-60min; s3) taking out of the tank, washing, neutralizing, washing and drying;
the antigen fibrillation composition comprises a cross-linking agent, a dispersing agent and a buffering agent, wherein the cross-linking agent comprises the following components in parts by weight: 60-90% of dispersing agent: 20-50%, buffer: 1-5, mixing the components and spray drying to prepare a solid antigen fibrillating composition;
the cross-linking agent is one or more multi-functional triazine compounds which are compounded and used, and the molecular structural general formula is as follows:
wherein the active groups X and Y are the same or different and are selected from one or more of F, cl, nicotinic acid, isonicotinic acid, triethylenediamine, 4-beta-hydroxyethylsulfonyl sulfate aniline-2-sulfonic acid, p-aminophenyl-beta-hydroxyethylsulfonyl sulfate, m-aminophenyl-beta-hydroxyethylsulfonyl sulfate, 2- (2-aminoethyl) sulfonyl ethanol sulfate and 2- [ (chloroethyl) sulfonyl ] ethanol hydrochloride;
r is a modifying group or an active group and is selected from one or more of F, cl, OH, sulfanilic acid, m-sulfanilic acid, p-aminobenzoic acid and 2, 5-disulfonic aniline;
a is a linking group or a bridging group, and is selected from one or more of p-phenylenediamine, m-phenylenediamine, o-phenylenediamine, 2, 4-diaminobenzenesulfonic acid, 2, 5-diaminobenzenesulfonic acid, m-phenylenediamine disulfonic acid, ethylenediamine, propylenediamine, hexamethylenediamine, polyethylene glycol and polyether amine.
2. The method for preparing the antigen fibrillated lyocell fiber according to claim 1, characterized in that: the dispersing agent is one or more of alkylphenol ethoxylates, fatty amine ethoxylates, fatty alcohol ethoxylate sodium sulfate, fatty alcohol ethoxylate sodium carboxylate, isomeric alcohol ethoxylates, sodium secondary alkyl sulfonate, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, methyl naphthalene sulfonate formaldehyde condensate, methylene dinaphthyl sulfonate, benzyl naphthalene sulfonate formaldehyde condensate, alkyl benzene sulfonate formaldehyde condensate and sodium lignin sulfonate.
3. The method for preparing the antigen fibrillated lyocell fiber according to claim 1, characterized in that: the buffer is selected from one of tris (hydroxymethyl) aminomethane+ethylenediamine tetraacetic acid, tris (hydroxymethyl) aminomethane+ethylenediamine tetraacetic acid disodium salt, triethanolamine+ethylenediamine tetraacetic acid disodium salt, succinic acid+caprolactam, disodium hydrogen phosphate+sodium dihydrogen phosphate, disodium hydrogen phosphate+potassium dihydrogen phosphate.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10013966A1 (en) * 2000-03-21 2001-10-11 Thueringisches Inst Textil Method of increasing ultraviolet absorption and reducing fibrillation of lyocell fibers involves treatment with cross-linking compound containing both UV-absorbing groups and several anchor groups
KR20050030477A (en) * 2003-09-26 2005-03-30 주식회사한일합섬 Continuous process for making anti-fibrillated lyocell fiber
CN111893749A (en) * 2020-08-14 2020-11-06 亚太森博（山东）浆纸有限公司 Crosslinking agent and method for fibrillation-resistant treatment of lyocell fiber
CN112281483A (en) * 2019-07-22 2021-01-29 中国纺织科学研究院有限公司 Rapid crosslinking method of cellulose fibers and preparation method of anti-fibrillation cellulose fibers
CN112458752A (en) * 2020-11-27 2021-03-09 亚太森博（山东）浆纸有限公司 Lyocell fiber, agent for crosslinking antigen fibrillation of Lyocell fiber, and method for treating antigen fibrillation of Lyocell fiber
CN115161989A (en) * 2022-09-02 2022-10-11 青岛大学 Scouring and bleaching process for Lyocell knitted fabric

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10013966A1 (en) * 2000-03-21 2001-10-11 Thueringisches Inst Textil Method of increasing ultraviolet absorption and reducing fibrillation of lyocell fibers involves treatment with cross-linking compound containing both UV-absorbing groups and several anchor groups
KR20050030477A (en) * 2003-09-26 2005-03-30 주식회사한일합섬 Continuous process for making anti-fibrillated lyocell fiber
CN112281483A (en) * 2019-07-22 2021-01-29 中国纺织科学研究院有限公司 Rapid crosslinking method of cellulose fibers and preparation method of anti-fibrillation cellulose fibers
CN111893749A (en) * 2020-08-14 2020-11-06 亚太森博（山东）浆纸有限公司 Crosslinking agent and method for fibrillation-resistant treatment of lyocell fiber
CN112458752A (en) * 2020-11-27 2021-03-09 亚太森博（山东）浆纸有限公司 Lyocell fiber, agent for crosslinking antigen fibrillation of Lyocell fiber, and method for treating antigen fibrillation of Lyocell fiber
CN115161989A (en) * 2022-09-02 2022-10-11 青岛大学 Scouring and bleaching process for Lyocell knitted fabric

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