CN105970611A - Supercritical fluid preparation method of nano-silver-coated textile fabric - Google Patents
Supercritical fluid preparation method of nano-silver-coated textile fabric Download PDFInfo
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- CN105970611A CN105970611A CN201610380007.XA CN201610380007A CN105970611A CN 105970611 A CN105970611 A CN 105970611A CN 201610380007 A CN201610380007 A CN 201610380007A CN 105970611 A CN105970611 A CN 105970611A
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- 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
- D06M11/83—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 metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
-
- 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
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
-
- 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
- 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
- D06M2101/10—Animal fibres
- D06M2101/12—Keratin fibres or silk
-
- 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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
-
- 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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Chemically Coating (AREA)
Abstract
The invention belongs to the field of multifunctional textile fabrics, and particularly relates to a nano-silver-coated textile fabric which has the multiple functions such as the catalytic degradation property, the ultraviolet resistance and the water repellency. The invention further provides a preparation method of the nano-silver-coated textile fabric. The nano-silver-coated textile fabric is prepared from silver nitrate, a reducing agent, a stabilizing agent and a textile fabric, wherein the mass ratio of the reducing agent to silver nitrate is 500-50, the mass ratio of the stabilizing agent to silver nitrate is 0.1-10, and 5 g-50 g of silver nitrate is used in every square meter of the textile fabric. According to the preparation method, the nano-silver-coated textile fabric is prepared by adopting a supercritical fluid technique, the textile fabric is treated for 10-100 min under the condition that the pressure is 7 Mpa-30 Mpa and the temperature is 20 DEG C-100 DEG C and then taken out, washed and dried. The textile surface is obtained by depositing nano-silver in supercritical carbon dioxide, the advantages of being environmentally friendly, high in production efficiency and nano-silver binding force, good in repeatability and the like are achieved, and the obtained nano-silver-coated textile fabric as the functions such as the catalytic degradation property, the ultraviolet resistance and the water repellency.
Description
Technical field
The invention belongs to that there is multifunctional textile lining field, be specifically related to supercritical carbon dioxide and prepare nanometer silver plating
Functional textile fabric.
Background technology
Nanometer silver plating textile refers at textile surface by the method plating nano-Ag particles such as physics, chemistry.By
In Nano silver grain, except possessing, the skin effect of general nano material, small-size effect, catalytic efficiency be strong and macroscopic quantum tunnel
Outside the character of many special chemicals such as channel effect and physical property, also there is the catalytic property of uniqueness, excellent biocompatibility
With preferable sensitivities, therefore by nanometer silver plating to textile surface, textile is made to have low-temperature superconducting, antistatic, catalysis
The effect such as degraded, antibacterial, uvioresistant, water repellent, electromagnetic shielding, thus increase the application of textile, such as military electromagnetic screen
Cover, medical antibacterial, domestic surpass water repellent, outdoor activity uvioresistant, environmental and ecological catalytic degradation dyestuff etc. aspect.
The method preparing nanometer silver plating textile at present mainly has vacuum deposition method, in-situ synthesis, chemical reduction method
And supercritical methanol technology etc..Wherein supercritical fluid is widely used because of the physical and chemical performance of its excellence.Supercritical fluid
Surface tension is low, good diffusing, wettability are good, is applied in recent years in the process of textile.Supercritical carbon dioxide
Process reduces pressure after terminating, and carbon dioxide gasifies rapidly, both environmentally safe, and processing speed is fast, processes uniformly, expands
Property is good, has high diffusion coefficient, easily allows nano-particle quickly diffuse in the space of fiber, can reach uniform adsorption
Effect；Carbon dioxide itself is the most nontoxic, tasteless, do not fire, processing procedure safety, and cost is relatively low, and used additives scope can be answered wide.Surpass and face
It is simple and environmentally-friendly, quick, stable that boundary's carbon dioxide process prepares nanometer silver plating textile.
Therefore, weaving face fabric using supercritical carbon dioxide process one step prepare nanometer silver plating textile, formation has
The nanometer silver weaving face fabric of excellent properties, it will have the functions such as antistatic, uvioresistant, antibacterial, water repellent, catalytic degradation simultaneously.
Preparing nanometer silver plating weaving face fabric by supercritical carbon dioxide one-step method, method is simple, and fastness is good, and environmental protection is anhydrous, saves
Cost.At present, great majority research is concentrated mainly in nano silver particles conventional chemical preparation technology, not yet has been reported that and uses supercritical
Fluid one-step method prepares nanometer silver plating textile.
Summary of the invention
It is an object of the invention to provide a kind of supercritical carbon dioxide one-step method and prepare the side of nanometer silver plating weaving face fabric
Method, gained textile material has the functions such as catalytic degradation dyestuff, uvioresistant, water repellent, antistatic.
Technical scheme:
The present invention provides a kind of nanometer silver plating weaving face fabric supercritical carbon dioxide preparation method, it is characterised in that its raw material
Including silver salt, reducing agent, stabilizer and weaving face fabric, wherein, reducing agent and silver salt mass ratio are 500 ~ 50, stabilizer and silver salt
Mass ratio is 0.1 ~ 10, and the quality of every square metre of weaving face fabric use silver salt is 5g～50g.
Described weaving face fabric is at least one in natural fabric material or chemosynthesis weaving face fabric.
Preferably, at least one during described weaving face fabric is cotton, hair, fiber crops, silk, terylene, viscose glue, polyester or acrylon.
Described silver salt is silver nitrate, silver oxalate, succinimide silver.
Described reducing agent is sodium citrate, sodium borohydride, ethylene glycol, reducing sugar, organophosphor.
Described stabilizer is sodium citrate, polyvinylpyrrolidone, sodium lauryl sulphate, polyamide-amide (PAMAM) tree
Shape macromole, polydimethylsiloxane.
Described preparation method uses supercritical carbon dioxide process.
The present invention provides described nanometer silver plating weaving face fabric preparation method, first by molten to weaving face fabric ethanol and acetone
In liquid, ultrasound wave respectively cleans 15min, then silver salt and stabilizer is dissolved in a certain amount of reducing agent, adds supercritical titanium dioxide
In carbon equipment, add a certain size textile, react a period of time under suitable pressure, temperature conditions, finally by weaving face fabric warp
Wash, be dried.
The preparation method of the present invention above-mentioned nanometer silver plating weaving face fabric, comprises the steps:
1) weaving face fabric pre-treatment: in weaving face fabric ethanol and acetone soln, ultrasound wave respectively cleans 15min taking-up, dries；
2) preparation of nanometer silver plating textile: then silver salt and stabilizer (mass ratio 0.1 ~ 10) are dissolved in a certain amount of
In reducing agent (reducing agent and silver salt mass ratio are 500 ~ 50), add in supercritical carbon dioxide equipment, put into textile, suitable
When 7 ~ 30Mpa pressure, temperature be 20 ~ 100 DEG C under the conditions of take out after supercritical reaction 10 ~ 100min, finally by weaving face fabric
Through washing, it is dried.
Beneficial effects of the present invention:
The present invention uses super critical CO 2 technology plating nanometer silver on the textile, has environmental protection, production efficiency height, nanometer
The silver features such as adhesion is high, reproducible, and the nanometer silver plating weaving face fabric obtained has antibacterial, uvioresistant, catalytic degradation
The functions such as dyestuff, water repellent, antistatic.The method technique is simple, low cost, it is possible to formed on weaving face fabric surface uniformly, fastness
High functional coating.
Accompanying drawing explanation
Fig. 1 is the supercritical carbon dioxide nanometer silver plating wool fabric scanning electron microscope of inventive embodiments 1 preparation
(SEM) photo (amplifying 30000 times).As seen from Figure 1, nano silver particles deposits wool surface, nanometer silver visibly homogeneously
Particle graininess spherical in shape.
Fig. 2 is the supercritical carbon dioxide nanometer silver plating wool fabric ultraviolet-visible spectrum of inventive embodiments 1 preparation
Figure.Fig. 2 a, b, the c respectively original Pilus Caprae seu Ovis of present example 1, the silver-plated wool fabric prepared by traditional method and with supercritical two
Nanometer silver plating wool fabric UV, visible light light transmission rate prepared by carbonoxide technology.As shown in Figure 2, supercritical carbon dioxide is used
The silver-plated wool fabric transmitance of preparation is minimum, i.e. supercritical carbon dioxide preparation method has actively work for Nano silver deposition
With, it is seen that the nanometer silver plating wool fabric using super critical CO 2 technology to prepare has best UVResistant effect.
Fig. 3 is the supercritical carbon dioxide nanometer silver plating wool fabric catalytic degradation effect of the embodiment of the present invention 1 preparation
Figure.After Fig. 3 a, b are respectively methylene blue solution addition sodium borohydride solution, all in blueness, i.e. represent after adding sodium borohydride,
Methylene blue not degraded；And Fig. 3 c, d respectively methylene blue solution does not adds nanometer silver plating wool fabric and addition is received
After rice silver plating wool fabric, under natural light after 20s, the latter is become clear, colorless by blueness, i.e. represents, is adding nanometer
After silver plating wool fabric, methylene blue is by sodium borohydride and nanometer silver plating wool fabric catalytic degradation, and solution becomes colourless
State.Nanometer silver plating wool fabric prepared by visible supercritical carbon dioxide process has good catalytic effect.
Fig. 4 is the embodiment of the present invention 2 nanometer silver plating fabric of preparation under the conditions of different pressure carbon dioxides.
Fig. 5 is the nanometer silver plating fabric contact angle of the deposition preparation under the embodiment of the present invention 2 differential responses time conditions.
Detailed description of the invention
The present invention provides a kind of nanometer silver plating weaving face fabric supercritical carbon dioxide preparation method, it is characterised in that its
Raw material includes silver nitrate, reducing agent, stabilizer and weaving face fabric, and wherein, reducing agent and silver nitrate mass ratio are 500 ~ 50, stable
Agent and silver nitrate mass ratio are 0.1 ~ 10, and the quality of every square metre of weaving face fabric use silver nitrate is 5g～50g.
Described weaving face fabric is at least one in natural fabric material or chemosynthesis weaving face fabric.
Preferably, at least one during described weaving face fabric is cotton, hair, fiber crops, silk, terylene, viscose glue, polyester or acrylon.
Described silver salt is silver nitrate, silver oxalate, succinimide silver.
Described reducing agent is sodium citrate, sodium borohydride, ethylene glycol, reducing sugar, organophosphor.
Described stabilizer is sodium citrate, polyvinylpyrrolidone, sodium lauryl sulphate, polyamide-amide (PAMAM) tree
Shape macromole, polydimethylsiloxane.
Described preparation method uses supercritical carbon dioxide process.
The present invention provides the preparation method of described nanometer silver plating weaving face fabric, first by weaving face fabric ethanol and acetone
In solution, ultrasound wave respectively cleans 15min, then silver salt and stabilizer is dissolved in a certain amount of reducing agent, adds supercritical two
In carbon monoxide plants, add a certain size textile, react a period of time under suitable pressure, temperature conditions, finally will spin
Knitted fabric is through washing, being dried.
The preparation method of the present invention above-mentioned nanometer silver plating weaving face fabric, comprises the steps:
1) weaving face fabric pre-treatment: in weaving face fabric ethanol and acetone soln, ultrasound wave respectively cleans 15min taking-up, dries；
2) preparation of nanometer silver plating textile: then silver salt and stabilizer (mass ratio 0.1 ~ 10) are dissolved in a certain amount of
In reducing agent (reducing agent and silver salt mass ratio are 500 ~ 50), add in supercritical carbon dioxide equipment, put into textile, suitable
When 7 ~ 30Mpa pressure, temperature be 20 ~ 100 DEG C under the conditions of take out after supercritical reaction 10 ~ 100min, finally by weaving face fabric
Through washing, it is dried.
Below by embodiment, the present invention is specifically described, it is necessary to be pointed out that embodiment is served only for the present invention
Further illustrate, it is impossible to be interpreted as limiting the scope of the invention, these those skilled in the art can according to this
Some nonessential improvement and adjustment are made in invention.
Embodiment 1
The wool fabric of a size of 5cm × 5cm is cleaned 15min with acetone and EtOH Sonicate ripple respectively, takes out and dry；By 0.1g
Silver nitrate and 0.1g polyvinylpyrrolidone are dissolved in 30ml ethylene glycol solution, stir 30min.Gained solution adds and Pilus Caprae seu Ovis
Cloth specimen together adds reactor, and at 10Mpa, temperature is taken out after supercritical carbon dioxide stir process 60min under the conditions of being 70 DEG C,
Washing is dried.
The microstructure of gained nanometer silver plating wool fabric is as follows with macro property:
1, the pattern of nano-Ag particles:
Fig. 1 is nanometer silver plating wool fabric scanning electron microscope (SEM) photo.As seen from Figure 1, nano silver particles is very
Deposit wool surface equably, nano silver particles graininess spherical in shape.
2, ultraviolet permeability under different preparation methoies:
Fig. 2 a, b, c are respectively original Pilus Caprae seu Ovis, the silver-plated wool fabric prepared by traditional method and prepare with supercritical carbon dioxide
The UV, visible light light transmission rate of silver-plated wool fabric.As shown in Figure 2, the silver-plated wool fabric prepared with supercritical carbon dioxide
Ultraviolet permeability minimum, i.e. supercritical carbon dioxide preparation method has positive role for the deposition of nanometer silver, it is seen that use
Nanometer silver plating wool fabric prepared by supercritical carbon dioxide has best UVResistant effect.
3, nanometer silver plating wool fabric catalytic degradation methylene blue performance prepared by supercritical carbon dioxide:
As it is shown on figure 3, after Fig. 3 a, b are respectively methylene blue solution addition sodium borohydride solution, all in blueness, i.e. represent and add
After entering sodium borohydride, methylene blue not degraded；And Fig. 3 c, d are respectively methylene blue solution and do not add nanometer silver plating
After wool fabric and addition nanometer silver plating wool fabric, under natural light after 20s, the latter is become clear, colorless by blueness,
I.e. representing, after adding nanometer silver plating wool fabric, methylene blue is catalyzed by sodium borohydride and nanometer silver plating wool fabric
Degraded, solution becomes colorless state.Result shows, the nanometer silver plating wool fabric using supercritical carbon dioxide to prepare has
Excellent catalytic effect.
4, the resistance to performance of soaping of nanometer silver plating wool fabric prepared by supercritical carbon dioxide:
Table 1 show supercritical carbon dioxide preparation and traditional method is prepared nanometer silver plating wool fabric and soaped before and after's K/S value.
Use nanometer silver plating wool fabric K/S value prepared by supercritical carbon dioxide method more than traditional method, i.e. color depth before soaping
Degree is apparently higher than traditional method.This also indicates that, the nanometer silver plating wool fabric prepared by supercritical carbon dioxide has more
Nano silver deposition, thus cause fabric color deeper.By comparing the K/S value after soaping, by supercritical carbon dioxide side
The color depth of nanometer silver plating wool fabric prepared by method remains above traditional method.Contrast K/S value reduces percent, traditional method
After the nanometer silver plating wool fabric of preparation is soaped, K/S reduces 17.5%, and nanometer silver plating Pilus Caprae seu Ovis prepared by supercritical carbon dioxide
After the soaping of fabric, K/S reduces only 3.6%, and result shows, the nanometer silver plating wool fabric prepared by supercritical carbon dioxide
There is the most resistance to soaping property.
The preparation of table 1. supercritical carbon dioxide and traditional method are prepared nanometer silver plating wool fabric and are soaped before and after's K/S value
Embodiment 2
The wool fabric of a size of 5cm × 5cm is cleaned 15min with acetone and EtOH Sonicate ripple respectively, takes out and dry；By 0.1g
Silver nitrate and 0.1g polyvinylpyrrolidone are dissolved in 30ml ethylene glycol solution, stir 30min.Gained solution adds and Pilus Caprae seu Ovis
Cloth specimen together adds reactor, at 8 ~ 14Mpa, temperature be 70 DEG C under the conditions of after supercritical carbon dioxide stir process 20 ~ 80min
Taking out, washing is dried.
1, nanometer silver plating wool fabric contact angle under different pressure carbon dioxides:
Fig. 4 is the embodiment of the present invention 2 nanometer silver plating fabric of preparation under the conditions of different pressure carbon dioxides, as seen from the figure,
Other conditions are identical, and under different carbon dioxide conditions, the contact angle of the nanometer silver plating wool fabric of preparation is along with pressure increase
And first increase and reduce afterwards, reach peak when 10Mpa.This is because along with pressure carbon dioxide increases, supercritical titanium dioxide
Carbon swelling effect increases with diffusion effect, during beneficially nano silver particles is diffused into fiber and fiber gap, blocks fiber gap,
Reduce water to permeate from fiber gap, thus improve contact angle.As can be seen here, supercritical carbon dioxide has for Nano silver deposition
Positive role.
2, the nanometer silver plating wool fabric contact angle of differential responses time:
Fig. 5 is the nanometer silver plating fabric of the deposition preparation under the embodiment of the present invention 2 differential responses time conditions, as seen from the figure,
Other conditions are identical, extend in time, the contact angle of the nanometer silver plating wool fabric of preparation under differential responses time conditions
And first increase and reduce afterwards, reach maximum when the response time is 60min.This is because prolongation over time, nanometer silver granuel
Son preferably spreads and is deposited on wool surface and is diffused into fiber with fiber gap, blocks fiber gap, reduces water
Permeate from fiber gap, thus improve contact angle.As can be seen here, the response time is preferred at 60min.
Claims (5)
1. a nanometer silver weaving face fabric, it is characterised in that its raw material includes silver salt, reducing agent, stabilizer and weaving face fabric, its
In, reducing agent and silver salt mass ratio are 500 ~ 50, and stabilizer and silver salt mass ratio are 0.1 ~ 10, and every square metre of weaving face fabric uses
The quality of silver salt is 5g～50g.
Nanometer silver plating weaving face fabric the most according to claim 1, it is characterised in that described weaving face fabric is natural fiber
At least one in fabric or chemosynthesis weaving face fabric；Preferably, described weaving face fabric is cotton, hair, fiber crops, silk, terylene, glues
At least one in glue, polypropylene or acrylon.
Nanometer silver plating weaving face fabric the most according to claim 1, it is characterised in that described silver salt is silver nitrate, oxalic acid
Silver, succinimide silver；Described reducing agent is sodium citrate, sodium borohydride, ethylene glycol, reducing sugar, organophosphor；Stabilizer is lemon
Lemon acid sodium, polyvinylpyrrolidone, sodium lauryl sulphate, polyamide-amide (PAMAM) dendrimer, polydimethylsiloxanes
Alkane；Described preparation method uses supercritical carbon dioxide process.
4. the preparation method of the nanometer silver plating weaving face fabric described in any one of claim 1-3, it is characterised in that first will weaving
In fabric ethanol and acetone soln, ultrasound wave respectively cleans 15min, then silver salt and stabilizer is dissolved in a certain amount of reducing agent
In, add in supercritical carbon dioxide equipment, add a certain size textile, under suitable pressure, temperature conditions, react one section
Time, finally by weaving face fabric through washing, being dried.
The preparation method of nanometer silver plating weaving face fabric the most according to claim 4, it is characterised in that silver salt and stable
Agent is dissolved in reducing agent, adds reactor together with cloth specimen, and at 7 ~ 30Mpa, under the conditions of temperature is 20 ~ 100 DEG C, supercritical is anti-
Take out after answering 10 ~ 100min, wash, dry.
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Cited By (3)
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| CN108442099A (en) * | 2018-03-28 | 2018-08-24 | 南通大学 | A kind of anti-ultraviolet nano zinc oxide composite textile and preparation method thereof |
| CN112832020A (en) * | 2021-02-08 | 2021-05-25 | 四川警察学院 | Preparation method of immersion or supercritical fluid pretreatment assisted metal plating textile |
| 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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Application publication date: 20160928 |