CN112832020A - Preparation method of immersion or supercritical fluid pretreatment assisted metal plating textile - Google Patents

Preparation method of immersion or supercritical fluid pretreatment assisted metal plating textile Download PDF

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Publication number
CN112832020A
CN112832020A CN202110180360.4A CN202110180360A CN112832020A CN 112832020 A CN112832020 A CN 112832020A CN 202110180360 A CN202110180360 A CN 202110180360A CN 112832020 A CN112832020 A CN 112832020A
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China
Prior art keywords
textile
coupling agent
supercritical
metal
treatment
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Pending
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CN202110180360.4A
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Chinese (zh)
Inventor
王毓
郭荣辉
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Sichuan Police College
Sichuan University
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Sichuan Police College
Sichuan University
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Priority to CN202110180360.4A priority Critical patent/CN112832020A/en
Publication of CN112832020A publication Critical patent/CN112832020A/en
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating 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
    • D06M11/83Treating 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 metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/50Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms

Abstract

The invention relates to a preparation method of a dipping or supercritical fluid auxiliary metal plating textile, belonging to the technical field of textiles. The method of the invention comprises the following steps: a, pretreating a textile; b, impregnation or supercritical treatment by a coupling agent: the dipping is to soak the textile in acetone solution of a coupling agent, treat the textile for 0.5 to 3 hours at the temperature of between 20 and 80 ℃ and then dry the textile; the supercritical treatment comprises the following steps: soaking the textile in an ethanol solution of a coupling agent, performing supercritical static treatment for 10-60 min under the conditions of 5-20 Mpa and 10-80 ℃, and taking out and drying; c, preparing metal-plated textile: mixing a stabilizer, a metal salt and a reducing agent to obtain a solution A; and c, placing the textile dried in the step b into the solution A for microwave treatment, taking out, washing with water, and drying. The product obtained by the method has the functions of static resistance, ultraviolet resistance, electric conduction, electromagnetic shielding and the like, and has better ultraviolet resistance. The method is environment-friendly, high in production efficiency and simple in process.

Description

Preparation method of immersion or supercritical fluid pretreatment assisted metal plating textile
Technical Field
The invention relates to a preparation method of a dipping or supercritical fluid auxiliary metal plating textile, belonging to the technical field of textiles.
Background
Metal-coated textiles refer to the coating of metal particles on the textile surface by physical, chemical, etc. methods. The metal is plated on the surface of the textile, so that the textile has the functions of static resistance, electric conduction, electromagnetic shielding, ultraviolet resistance and the like, the added value of the textile is improved, and the application fields of the textile are increased, such as the fields of clothing, household textiles, industrial textiles and the like.
The existing methods for preparing metal-plated textiles mainly include physical deposition methods, chemical deposition methods, supercritical fluid chemical deposition methods and the like. Among them, the supercritical fluid chemical deposition method has potential application because of its excellent physicochemical properties. Supercritical fluids have low surface tension, good diffusion capability, and good wetting properties, and have been used in recent years for dyeing textiles. After the supercritical carbon dioxide treatment is finished, the pressure is reduced, and the carbon dioxide is quickly gasified, so that the method has the advantages of no pollution to the environment, high treatment speed, uniform treatment, good expansibility and extremely high diffusion coefficient, is easy to quickly diffuse metal on the surface of the fiber and in the fiber, can achieve the effect of uniform deposition, and improves the bonding strength of the metal coating and the fiber; the carbon dioxide is non-toxic, tasteless and non-combustible, the treatment process is safe, the cost is lower, and the applicable auxiliary agent range is wide.
Therefore, the metal plated textile prepared by the supercritical carbon dioxide deposition method has excellent performance, and has the functions of static resistance, ultraviolet resistance, electric conduction, electromagnetic shielding and the like. The metal plated textile is prepared by a supercritical carbon dioxide one-step method, the method is simple, environment-friendly and water-free, and the cost is saved. Although the ultraviolet-resistant coating has a certain ultraviolet-resistant function, the requirement cannot be met, and the ultraviolet-resistant function needs to be further improved.
Disclosure of Invention
The invention aims to solve the first technical problem of providing a novel supercritical fluid-assisted metal plating textile preparation method.
To solve the first technical problem of the present invention, the method includes:
a. textile pretreatment: cleaning and drying the textile;
b. impregnation with a coupling agent or supercritical treatment: the dipping is to soak the textile in acetone solution of a coupling agent, treat the textile for 0.5 to 3 hours at the temperature of between 20 and 80 ℃ and then dry the textile; the supercritical treatment comprises the following steps: soaking the textile in an ethanol solution of a coupling agent, performing supercritical static treatment for 10-60 min under the conditions of 5-20 Mpa and 10-80 ℃, and taking out and drying;
c. preparation of metal-plated textiles: mixing a stabilizer, a metal salt and a reducing agent to obtain a solution A; putting the textile dried in the step b into the solution A for microwave treatment, taking out, washing with water and drying; wherein the microwave treatment temperature is 30-80 ℃, and the treatment time is 5-10 min; the mass ratio of the stabilizer to the metal salt to the reducing agent is as follows: 0.1-1: 1: 1-100;
preferably, the microwave treatment in step c further comprises turning over every 1 min.
In one embodiment, the cleaning in step a is: and respectively ultrasonically cleaning the textile in ethanol and acetone solution for 10-30 min.
In a specific embodiment, the textile is a natural fiber facing or a chemical synthetic textile fiber, or at least one of a natural fiber yarn or a chemical synthetic textile yarn or a fabric thereof.
In one embodiment, the textile is at least one of cotton, hemp, wool, bamboo pulp fiber, regenerated fiber, polyester, chinlon or spandex.
In a specific embodiment, the volume ratio of acetone to the coupling agent in the acetone solution of the coupling agent in the step b is 50-200; the volume ratio of ethanol in the ethanol solution of the coupling agent to the coupling agent is 5-20; the coupling agent is preferably a silane.
In one embodiment, the metal salt is at least one of silver salt, copper salt, nickel salt and cobalt salt; preferably a silver salt; more preferably silver nitrate, wherein the mass of the silver nitrate used per square meter of textile is 1-50 g.
In a specific embodiment, the reducing agent is at least one of sodium citrate, sodium borohydride, ethylene glycol and reducing sugar.
In one embodiment, the stabilizer is at least one of sodium citrate, polyvinylpyrrolidone, sodium lauryl sulfate, and polydimethylsiloxane.
In one embodiment, the mass ratio of the stabilizer, the metal salt and the reducing agent is as follows: 0.1-1: 1: 1-10.
A second technical problem to be solved by the present invention is to provide a metal-plated textile.
In order to solve the second technical problem of the invention, the metal-plated textile is prepared by the method.
Advantageous effects
The product obtained by the method has the functions of static resistance, ultraviolet resistance, electric conduction, electromagnetic shielding and the like, and has better ultraviolet resistance.
The method has the characteristics of environmental protection, high production efficiency, high bonding force between the metal and the textile, good repeatability and the like.
The method has simple process and low cost, and can form a uniform and high-fastness functional coating on the surface of the textile.
Drawings
FIG. 1 is a scanning electron microscope image (magnified 30000 times) of the surface of the nano-silver fabric prepared in example 1;
fig. 2 shows the uv transmittance of the original bamboo fiber fabric and the nano-silver fabric pretreated with supercritical silane under the same other conditions of example 1 of the present invention.
Detailed Description
To solve the first technical problem of the present invention, the method includes:
a. textile pretreatment: cleaning and drying the textile;
b. impregnation with a coupling agent or supercritical treatment: the dipping is to soak the textile in acetone solution of a coupling agent, treat the textile for 0.5 to 3 hours at the temperature of between 20 and 80 ℃ and then dry the textile; the supercritical treatment comprises the following steps: soaking the textile in an ethanol solution of a coupling agent, performing supercritical static treatment for 10-60 min under the conditions of 5-20 Mpa and 10-80 ℃, and taking out and drying;
c. preparation of metal-plated textiles: mixing a stabilizer, a metal salt and a reducing agent to obtain a solution A; putting the textile dried in the step b into the solution A for microwave treatment, taking out, washing with water and drying; wherein the microwave treatment temperature is 30-80 ℃, and the treatment time is 5-10 min; the mass ratio of the stabilizer to the metal salt to the reducing agent is as follows: 0.1-1: 1: 1-100;
preferably, the microwave treatment in step c further comprises turning over every 1 min.
In one embodiment, the cleaning in step a is: and respectively ultrasonically cleaning the textile in ethanol and acetone solution for 10-30 min.
The invention carries out coupling agent pretreatment on the textile fabric to enhance the binding force between the coating and the textile fabric.
In a specific embodiment, the textile is a natural fiber facing or a chemical synthetic textile fiber, or at least one of a natural fiber yarn or a chemical synthetic textile yarn or a fabric thereof.
In one embodiment, the textile is at least one of cotton, hemp, wool, bamboo pulp fiber, regenerated fiber, polyester, chinlon or spandex.
In a specific embodiment, the volume ratio of acetone to the coupling agent in the acetone solution of the coupling agent in the step b is 50-200; the volume ratio of ethanol in the ethanol solution of the coupling agent to the coupling agent is 5-20; the coupling agent is preferably a silane.
In one embodiment, the metal salt is at least one of silver salt, copper salt, nickel salt and cobalt salt; preferably a silver salt; more preferably silver nitrate, wherein the mass of the silver nitrate used per square meter of textile is 1-50 g.
In a specific embodiment, the reducing agent is at least one of sodium citrate, sodium borohydride, ethylene glycol and reducing sugar.
In one embodiment, the stabilizer is at least one of sodium citrate, polyvinylpyrrolidone, sodium lauryl sulfate, and polydimethylsiloxane.
In one embodiment, the mass ratio of the stabilizer, the metal salt and the reducing agent is as follows: 0.1-1: 1: 1-10.
In order to solve the second technical problem of the invention, the metal-plated textile is prepared by the method.
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the scope of the present invention.
Example 1
Ultrasonically cleaning the bamboo pulp fiber fabric with the size of 5cm multiplied by 5cm for 30min by using acetone and ethanol respectively, taking out the fabric, and naturally drying the fabric in a ventilated place; in a fume hood, flatly laying and placing bamboo pulp fiber fabrics cleaned by ethanol acetone, dissolving 5ml of silane in 45ml of ethanol, adding the solution into a dye kettle, adding a cloth sample into a reaction kettle, performing supercritical static treatment for 10min under the conditions of 10Mpa and 40 ℃, taking out, and airing; 0.08g of AgNO3Respectively dissolving in 40ml of deionized water, adding 6ml of 1% sodium citrate, and uniformly stirring; and then putting the bamboo pulp fiber fabric subjected to silane treatment into the silver nitrate solution, performing microwave heating treatment for 8min, turning over every 1min, washing with water, and drying in an oven at 80 ℃.
The microstructure and the macroscopic performance of the obtained nano-silver plated bamboo pulp fiber fabric are as follows:
fig. 1 is a Scanning Electron Microscope (SEM) photograph of nano silver. As can be seen from FIG. 1, the silver nanoparticles are relatively uniformly distributed on the surface of the fiber, and the silver nanoparticles are spherical;
2. ultraviolet transmittance under different pretreatment methods:
fig. 2 shows the ultraviolet transmittance of the original bamboo fiber fabric and the bamboo pulp fiber fabric pretreated by the supercritical silane under the same other conditions, and it can be seen from fig. 2 that the bamboo pulp fiber fabric is pretreated by the supercritical silane, and the ultraviolet transmittance is the lowest, i.e. the bamboo pulp fiber fabric treated by the nano silver silane has a positive effect on the deposition of nano silver, and it can be seen that the nano silver bamboo pulp fiber fabric pretreated by the supercritical fluid has the best ultraviolet resistance effect.
Example 2
Ultrasonically cleaning the bamboo pulp fiber fabric with the size of 5cm multiplied by 5cm for 30min by using acetone and ethanol respectively, taking out the fabric, and naturally drying the fabric in a ventilated place; in a fume hood, 10 pieces of bamboo pulp fiber fabrics cleaned by ethanol and acetone are flatly laid, 5ml of silane is dissolved in 45ml of ethanol, the solution is added into a dye kettle, a cloth sample is added into a reaction kettle, and the bamboo pulp fiber fabrics are taken out after supercritical static treatment is carried out for 10 minutes under the conditions of 10Mpa and the temperature of 40 ℃ and are dried; 0.08g of AgNO3Dissolving in 40ml deionized water, respectively adding 1% sodium citrate 2ml, 4ml, 6ml, 8ml and 10ml, and stirring; and then putting the bamboo pulp fiber fabric subjected to silane treatment into the silver nitrate solution, performing microwave heating treatment for 8min, turning over every 1min, washing with water, and drying in an oven at 80 ℃.
Deposition rates under different pretreatment and different sodium citrate content conditions:
the deposition rate of the nano-silver fabric prepared in the embodiment 2 of the invention under the conditions of different pretreatments and different sodium citrate contents is the same as that of the nano-silver fabric prepared in the embodiment 2 of the invention under the conditions of different sodium citrate contents without silane pretreatment, silane pretreatment and supercritical silane pretreatment. The results show that the deposition rate of the bamboo pulp fiber is the largest at different amounts of sodium citrate when the bamboo pulp fiber is subjected to the supercritical silane pretreatment, the deposition of nano silver of the bamboo pulp fiber fabric treated by the supercritical silane is better than that of the bamboo pulp fiber fabric treated by the common method or untreated bamboo pulp fiber fabric treated by the supercritical silane, and the bamboo pulp fiber fabric treated by the supercritical silane has a positive effect on the deposition of nano silver.

Claims (10)

1. The preparation method of the dipping or supercritical fluid pretreatment auxiliary metal plating textile is characterized by comprising the following steps:
a. textile pretreatment: cleaning and drying the textile;
b. impregnation with a coupling agent or supercritical treatment: the dipping is to soak the textile in acetone solution of a coupling agent, treat the textile for 0.5 to 3 hours at the temperature of between 20 and 80 ℃ and then dry the textile; the supercritical treatment comprises the following steps: soaking the textile in an ethanol solution of a coupling agent, performing supercritical static treatment for 10-60 min under the conditions of 5-20 Mpa and 10-80 ℃, and taking out and drying;
c. preparation of metal-plated textiles: mixing a stabilizer, a metal salt and a reducing agent to obtain a solution A; putting the textile dried in the step b into the solution A for microwave treatment, taking out, washing with water and drying; wherein the microwave treatment temperature is 30-80 ℃, and the treatment time is 5-10 min; the mass ratio of the stabilizer to the metal salt to the reducing agent is as follows: 0.1-1: 1: 1-100;
preferably, the microwave treatment in step c further comprises turning over every 1 min.
2. The method of claim 1, wherein the cleaning step a comprises: and respectively ultrasonically cleaning the textile in ethanol and acetone solution for 10-30 min.
3. The method of preparing a dipped or supercritical fluid pretreated secondary metal-plated textile according to claim 1 or 2 wherein the textile is at least one of a natural fiber fabric or a chemically synthetic textile fiber, or a natural fiber yarn or a chemically synthetic textile yarn or fabric thereof.
4. The method for preparing a dipped or supercritical fluid pre-treated auxiliary metal-plated textile according to claim 3, wherein the textile is at least one of cotton, hemp, wool, bamboo pulp fiber, regenerated fiber, terylene, chinlon or spandex.
5. The method for preparing the dipping or supercritical fluid pretreatment auxiliary metal plated textile according to claim 1 or 2, wherein the volume ratio of acetone and the coupling agent in the acetone solution of the coupling agent in the step b is 50-200; the volume ratio of ethanol in the ethanol solution of the coupling agent to the coupling agent is 5-20; the coupling agent is preferably a silane.
6. The method of claim 1 or 2, wherein the metal salt is at least one of a silver salt, a copper salt, a nickel salt, and a cobalt salt; preferably a silver salt; more preferably silver nitrate, wherein the mass of the silver nitrate used per square meter of textile is 1-50 g.
7. The method for preparing a dipping or supercritical fluid pretreatment auxiliary metal-plated textile according to claim 1 or 2, wherein the reducing agent is at least one of sodium citrate, sodium borohydride, glycol and reducing sugar.
8. The method of claim 1 or 2, wherein the stabilizing agent is at least one of sodium citrate, polyvinylpyrrolidone, sodium dodecyl sulfate, and polydimethylsiloxane.
9. The method for preparing a metal-plated textile product by immersion or supercritical fluid pretreatment as claimed in claim 1 or 2, wherein the mass ratio of the stabilizer, the metal salt and the reducing agent is: 0.1-1: 1: 1-10.
10. A metallized textile prepared by the method of preparing an auxiliary metallized textile by immersion or supercritical fluid pretreatment according to any one of claims 1 to 9.
CN202110180360.4A 2021-02-08 2021-02-08 Preparation method of immersion or supercritical fluid pretreatment assisted metal plating textile Pending CN112832020A (en)

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CN114635285A (en) * 2022-01-20 2022-06-17 上海讯隆益联科技有限公司 Metallized polymer-based non-woven fabric and preparation method and application thereof
CN114875660A (en) * 2022-05-17 2022-08-09 厦门大学 Conductive textile cloth for mediating direct absorption of metal nanowires and preparation method thereof
CN115652623A (en) * 2022-10-11 2023-01-31 四川警察学院 Metal/graphene plated fabric prepared by microwave and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN113622187A (en) * 2021-09-06 2021-11-09 陕西元丰纺织技术研究有限公司 Supercritical carbon dioxide after-finishing process of wave-absorbing electromagnetic shielding fabric
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CN114875660A (en) * 2022-05-17 2022-08-09 厦门大学 Conductive textile cloth for mediating direct absorption of metal nanowires and preparation method thereof
CN115652623A (en) * 2022-10-11 2023-01-31 四川警察学院 Metal/graphene plated fabric prepared by microwave and preparation method thereof

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Application publication date: 20210525