CN111945420B - Environment-friendly silver fiber fabric and preparation method thereof - Google Patents
Environment-friendly silver fiber fabric and preparation method thereof Download PDFInfo
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- CN111945420B CN111945420B CN202010830597.8A CN202010830597A CN111945420B CN 111945420 B CN111945420 B CN 111945420B CN 202010830597 A CN202010830597 A CN 202010830597A CN 111945420 B CN111945420 B CN 111945420B
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- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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- 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
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- 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
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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
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- D06M2101/06—Vegetal fibres cellulosic
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Abstract
The invention relates to the technical field of fabrics, in particular to a green and environment-friendly silver fiber fabric and a preparation method thereof. The preparation method of the green environment-friendly silver fiber fabric comprises the following steps: y1, washing the biomass raw material with water and airing; pulverizing the dried biomass raw material to obtain biomass powder; y2, mixing biomass powder with water and boiling; cooling to room temperature; centrifuging and filtering to obtain biomass extract; y3, immersing the fiber fabric into a silver nitrate aqueous solution; and slowly adding the biomass extract for soaking, washing with water, and drying to obtain the green environment-friendly silver fiber fabric. The silver fiber fabric prepared by the biomass extracting solution is green and environment-friendly, and the obtained fiber fabric has good antibacterial, deodorizing, radiation-proof and antistatic properties, is good in stability and not easy to oxidize, and does not develop Huang Faan after being used for a period of time.
Description
Technical Field
The invention relates to the technical field of fabrics, in particular to a green and environment-friendly silver fiber fabric and a preparation method thereof.
Background
The metallic silver has excellent optical, electrical, catalytic and antibacterial properties and is widely applied to the field of functional fiber textiles. The silver fiber fabric is a high-tech textile obtained by permanently bonding a layer of pure silver on the surface of the fiber through a special process. Silver is used as metal with the best conductivity, the radiation shielding effect of the silver fiber fabric is good, and the silver fiber fabric is the most ideal radiation protection clothing fabric at present; meanwhile, the silver fiber fabric is also the optimal antibacterial and deodorant fabric by utilizing the natural antibacterial performance of silver. The silver fiber fabric is soft, light and thin, has excellent air permeability and is very suitable for wearing. However, metallic silver is extremely easy to oxidize, and is easy to react with substances in the air after being exposed in the air for too long, so that the oxidized fabric is yellow and dark, and the performance of the silver fiber fabric is reduced.
The silver fiber comprises nano silver fiber and silver-plated fiber. The nano silver fiber is prepared by adding ultra-fine silver particles in the fiber forming process; silver-plated fibers are obtained by plating silver layers on the surfaces of fibers through various metallization technologies such as chemical plating or electroplating. Because the nano silver is easy to agglomerate and uneven in dispersion in the preparation process of the nano silver fiber, the effective utilization rate of the nano silver fiber is reduced, and the application of the nano silver fiber is limited. Therefore, silver-plated fibers are mainly studied.
Electroless silver plating is a highly selective process in which silver ions are reduced and deposited on the surface of the fiber by the catalytic or other process of certain metals using a suitable reducing agent in solution. The traditional chemical silver plating method has the defects of potential safety hazard, environmental pollution and the like in the production and processing process. Finding a green and environment-friendly silver plating method to replace the traditional method in the textile field is a problem to be solved urgently.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the technical problems to be solved by the present invention are: aiming at the defects of the prior art, the environment-friendly silver fiber fabric and the preparation method thereof are provided.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the preparation method of the green and environment-friendly silver fiber fabric comprises the following steps:
y1, washing the biomass raw material with water and airing; pulverizing the dried biomass raw material to obtain biomass powder;
y2, mixing biomass powder with water and boiling; cooling to room temperature; centrifuging and filtering to obtain biomass extract;
y3, immersing the fiber fabric into a silver nitrate aqueous solution; slowly adding the biomass extract; stirring thoroughly, soaking for 30-90min; rinsing with water for 1-3 times, and drying at room temperature.
Further, the preparation method of the green and environment-friendly silver fiber fabric comprises the following steps:
y1, washing the biomass raw material with water and airing; pulverizing the dried biomass raw material by a universal pulverizer, and sieving with a 50-100 mesh sieve; pulverizing to 1500-3500 mesh with superfine pulverizer to obtain biomass powder;
y2 mixing biomass powder with water, wherein the mass ratio of the biomass powder to the water is (1-10): 100; fully stirring, heating to 50-80 ℃ and soaking for 10-40min; heating to 100deg.C, and boiling for 5-20min; cooling to 50-80deg.C, soaking for 10-40min; cooling to room temperature and standing for 5-20min; centrifuging and filtering to obtain biomass extract;
immersing the fiber fabric into 0.5-3.5 wt% of silver nitrate aqueous solution, wherein the mass ratio of the fiber fabric to the silver nitrate aqueous solution is (0.5-2): (15-50); slowly adding the biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1: (1-20); adjusting the pH to 6-10 with sodium hydroxide solution; gradually heating to 50-90deg.C, stirring thoroughly, and soaking at constant temperature for 30-90min; rinsing with water for 1-3 times, and drying at room temperature.
Further, the preparation method of the green and environment-friendly silver fiber fabric comprises the following steps:
y1, washing the biomass raw material with water and airing; pulverizing the dried biomass raw material by a universal pulverizer, and sieving with a 50-100 mesh sieve; pulverizing to 1500-3500 mesh with superfine pulverizer to obtain biomass powder;
y2 mixing biomass powder with water, wherein the mass ratio of the biomass powder to the water is (1-10): 100; fully stirring, heating to 50-80 ℃ and soaking for 10-40min; heating to 100deg.C, and boiling for 5-20min; cooling to 50-80deg.C, soaking for 10-40min; cooling to room temperature and standing for 5-20min; centrifuging and filtering to obtain biomass extract;
immersing the fiber fabric into the treatment liquid at room temperature, wherein the mass ratio of the fiber fabric to the treatment liquid is (0.5-2): (20-100), dipping for 10-48h; taking out, curing for 1-10min at 100-150 ℃, and airing to obtain pretreated fiber fabric; the treatment fluid is one of chitosan solution, functional chitosan solution and glycine aqueous solution;
and Y4, immersing the pretreated fiber fabric into 0.5-3.5 wt% of silver nitrate aqueous solution, wherein the mass ratio of the fiber fabric to the silver nitrate aqueous solution is (0.5-2): (15-50); slowly adding the biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1: (1-20); adjusting the pH to 6-10 with sodium hydroxide solution; gradually heating to 50-90deg.C, stirring thoroughly, and soaking at constant temperature for 30-90min; rinsing with water for 1-3 times, and drying at room temperature.
Further, the preparation method of the green and environment-friendly silver fiber fabric comprises the following steps:
y1, washing the biomass raw material with water and airing; pulverizing the dried biomass raw material by a universal pulverizer, and sieving with a 50-100 mesh sieve; pulverizing to 1500-3500 mesh with superfine pulverizer to obtain biomass powder;
y2 mixing biomass powder with water, wherein the mass ratio of the biomass powder to the water is (1-10): 100; fully stirring, heating to 50-80 ℃ and soaking for 10-40min; heating to 100deg.C, and boiling for 5-20min; cooling to 50-80deg.C, soaking for 10-40min; cooling to room temperature and standing for 5-20min; centrifuging and filtering to obtain biomass extract;
immersing the fiber fabric into a chitosan solution or a functionalized chitosan solution at room temperature, wherein the mass ratio of the fiber fabric to the chitosan solution or the functionalized chitosan solution is (0.5-2): (20-100), dipping for 10-48h; taking out, solidifying at 100-150deg.C for 1-10min, and air drying;
immersing the fiber fabric in the step Y3 into glycine aqueous solution at room temperature, wherein the mass ratio of the fiber fabric to the glycine aqueous solution is (0.5-2): (20-100), dipping for 10-48h; taking out, curing for 1-10min at 100-150 ℃, and airing to obtain pretreated fiber fabric;
the pretreated fiber fabric is immersed into 0.5 to 3.5 weight percent of silver nitrate aqueous solution, and the mass ratio of the fiber fabric to the silver nitrate aqueous solution is (0.5 to 2): (15-50); slowly adding the biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1: (1-20); adjusting the pH to 6-10 with sodium hydroxide solution; gradually heating to 50-90deg.C, stirring thoroughly, and soaking at constant temperature for 30-90min; rinsing with water for 1-3 times, and drying at room temperature.
Preferably, the preparation method of the chitosan solution comprises the following steps: adding chitosan into 0.5-3.5 wt% acetic acid water solution with the mass ratio of chitosan to acetic acid water solution of (0.5-5) 100, heating to 50-80 deg.c, and stirring for 0.5-5 hr.
In some embodiments of the present application, the method for preparing the green and environment-friendly silver fiber fabric includes the following steps:
y1, washing the biomass raw material with water and airing; pulverizing the dried biomass raw material by a universal pulverizer, and sieving with a 50-100 mesh sieve; pulverizing to 1500-3500 mesh with superfine pulverizer to obtain biomass powder;
y2 mixing biomass powder with water, wherein the mass ratio of the biomass powder to the water is (1-10): 100; fully stirring, heating to 50-80 ℃ and soaking for 10-40min; heating to 100deg.C, and boiling for 5-20min; cooling to 50-80deg.C, soaking for 10-40min; cooling to room temperature and standing for 5-20min; centrifuging and filtering to obtain biomass extract;
immersing the fiber fabric into the functionalized chitosan solution at the room temperature, wherein the mass ratio of the fiber fabric to the functionalized chitosan solution is (0.5-2): (20-100), dipping for 10-48h; taking out, solidifying at 100-150deg.C for 1-10min, and air drying;
immersing the fiber fabric obtained in the step Y3 into glycine aqueous solution at room temperature, wherein the mass ratio of the fiber fabric to the glycine aqueous solution is (0.5-2): (20-100), dipping for 10-48h; taking out, curing for 1-10min at 100-150 ℃, and airing to obtain pretreated fiber fabric;
the pretreated fiber fabric is immersed into 0.5 to 3.5 weight percent of silver nitrate aqueous solution, and the mass ratio of the fiber fabric to the silver nitrate aqueous solution is (0.5 to 2): (15-50); slowly adding the biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1: (1-20); adjusting the pH to 6-10 with sodium hydroxide solution; gradually heating to 50-90deg.C, stirring thoroughly, and soaking at constant temperature for 30-90min; rinsing with water for 1-3 times, and drying at room temperature.
Preferably, the preparation method of the functionalized chitosan solution comprises the following steps:
treatment liquid A1: adding chitosan into 0.5-3.5 wt% acetic acid water solution with the mass ratio of chitosan to acetic acid water solution of (0.5-5) 100, heating to 50-80 ℃, stirring for 0.5-5h, and cooling to room temperature;
treatment liquid A2: adding a functionalization reagent into water, wherein the mass ratio of the functionalization reagent to the water is (0.5-5): 100, and performing ultrasonic treatment to fully dissolve; sequentially adding carbodiimide and N-hydroxysuccinimide under ice bath condition, wherein the mass ratio of the carbodiimide to the water is (0.3-5) 100, and the mass ratio of the N-hydroxysuccinimide to the water is (0.2-5) 100, and fully stirring;
adding the treatment solution A2 into the treatment solution A1, wherein the volume ratio of the treatment solution A1 to the treatment solution A2 is (0.5-5): 1, stirring for 30-60min under ice bath condition, taking out, and standing at room temperature for 5-10 h.
Preferably, the functionalizing agent is any one of ferulic acid, catechin, caffeic acid and gallic acid.
Further preferably, the functionalizing agent is a mixture of catechin and gallic acid, and the mass ratio of catechin to gallic acid is (1-5): (1-5).
Preferably, the concentration of the glycine aqueous solution is 0.5wt% to 3.5wt%.
Preferably, the fiber fabric is any one of pure cotton fiber fabric, polyester fiber fabric, wool fiber fabric, silk fiber fabric and polyamide fiber fabric.
Preferably, the biomass raw material is any one of dried tangerine leaves, dried mango leaves and peanut shells.
The invention also provides a green and environment-friendly silver fiber fabric which is prepared by adopting the method.
How to effectively utilize biomass as a renewable green resource has been a research hotspot. According to the method, biomass is used as a raw material, and active molecules in the biomass are used for in-situ reduction on the surface of the fiber fabric to generate silver nano particles, so that the silver fiber fabric is obtained. The invention adopts a universal pulverizer to pulverize for the first time, and then combines a superfine pulverizer to pulverize for the second time to treat biomass raw materials; meanwhile, a sectional temperature control extraction method is adopted to prepare a biomass extracting solution, so that active molecules in biomass are fully dissolved, the in-situ reduction capacity is stronger, the silver content of the produced silver fiber fabric is higher, and the performance of the silver fiber fabric is obviously improved; the preparation method of the biomass extract is suitable in conditions, and effective plant active molecules in biomass raw materials, such as dihydroxychromone, eriodictyol, trihydroxyflavanone, luteolin and the like in peanut shells, or flavonoid compounds, terpenoid compounds, thiamine and the like in mango leaves are more dissolved in the biomass extract, so that the reduction capability is stronger.
According to the invention, the performance of the silver fiber fabric is further improved by two-step pretreatment of the fiber fabric. On one hand, after chitosan in the chitosan solution is combined with fabric fibers, silver ions are easy to capture and adsorb, so that more nano silver particles are generated on the surface of the fiber fabric; on the other hand, after glycine in the glycine aqueous solution is combined with fabric fibers, nano silver particles which are reduced on the surfaces of the fiber fabrics can be stabilized, the nano silver particles are prevented from being oxidized, and the protective agent is used. Furthermore, the invention adopts the functionalized chitosan solution, and the capability of capturing and adsorbing silver ions of chitosan is obviously improved by coupling the chitosan with the functionalized reagent gallic acid or/and catechin; after pretreatment of the functionalized chitosan solution, the nano silver particles on the surface of the fiber fabric are more stable, and unexpected technical effects are achieved.
The beneficial effects of the invention are that
The invention provides a novel green environment-friendly fiber fabric preparation method by adopting biomass extract to prepare silver fiber fabric. Pretreating the fiber fabric by adopting a two-step method, (1) combining chitosan of chitosan solution with fabric fibers to enable silver ions to be easily captured and adsorbed by the fiber fabric, and generating more nano silver particles; (2) Glycine of glycine aqueous solution is combined with fabric fibers to protect nano silver particles generated on the surfaces of the fiber fabrics and prevent the nano silver particles from being oxidized. Furthermore, the invention adopts the functionalized chitosan solution, and the chitosan is coupled with the functionalized reagent gallic acid or/and catechin, so that silver ions are more easily captured and adsorbed by the fiber fabric; in addition, after the functionalized chitosan solution is adopted for pretreatment, the nano silver particles on the surface of the fiber fabric are more stable, and unexpected technical effects are achieved. The environment-friendly fiber fabric disclosed by the invention has good antibacterial performance, and the silver fiber fabric is more stable and is not easy to oxidize. The preparation method is simple and convenient, has high production efficiency and is beneficial to popularization and application.
Detailed Description
Some of the raw materials in the examples and comparative examples are described below:
peanut hulls in examples and comparative examples were supplied by the company, inc. of the Loose Teng Korea, jiaxiang county.
The universal pulverizer of the examples and comparative examples used a universal pulverizer of model 130B type from jinzhong pharmaceutical machinery, thai, spindle speed 7000r/min.
Pure cotton fiber fabrics of examples and comparative examples, manufactured by Shaoxing Ke Qiaojian mol textile Co., ltd., have a gram weight of 265g/m 2 。
In the examples and comparative examples, the ultrafine pulverizer was adopted, and the spindle rotation speed was 1450r/min, with the model of CWF-300, a company of Jinan Tianyu special equipment Co., ltd.
Chitosan in examples and comparative examples: CAS number: 9012-76-4; purchased from sigma aldrich (Shanghai), low molecular weight, product number: 448869.
glycine in examples and comparative examples: CAS number: 56-40-6; purchased from Shanghai Ala, product number: A110749.
carbodiimide in examples and comparative examples: CAS number: 151-51-9; purchased from Shanghai junrui.
N-hydroxysuccinimide in examples and comparative examples: CAS number: 6066-82-6; purchased from Shanghai Meilin.
Gallic acid in examples and comparative examples: CAS number: 149-91-7; is purchased from the chemical industry of the fertilizer combination.
Catechin in examples and comparative examples: CAS number: 18829-70-4; purchased from Shanghai Ala.
Comparative example 1
The preparation method of the green and environment-friendly silver fiber fabric comprises the following steps:
y1, washing the biomass raw material with water and airing; pulverizing the dried biomass raw material by a universal pulverizer, and sieving with an 80-mesh sieve to obtain biomass powder;
y2 mixing biomass powder with water, wherein the mass ratio of the biomass powder to the water is 7:100; fully stirring, heating to 62 ℃ and soaking for 32min; heating to 100deg.C, and boiling for 12min; cooling to 62 ℃ and soaking for 28min; cooling to room temperature and standing for 8min; centrifuging and filtering to obtain biomass extract;
immersing the fiber fabric into a 1.6wt% silver nitrate aqueous solution, wherein the mass ratio of the fiber fabric to the silver nitrate aqueous solution is 1:45; slowly adding the biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1:6, preparing a base material; adjusting the pH to 8.8 with sodium hydroxide solution; gradually heating to 86 ℃, fully stirring, and preserving heat and soaking for 52min; rinsing with water for 2 times, and drying at room temperature.
The fiber fabric is pure cotton fiber fabric.
The biomass raw material is peanut shells.
Comparative example 2
The preparation method of the green and environment-friendly silver fiber fabric comprises the following steps:
y1, washing the biomass raw material with water and airing; pulverizing the dried biomass raw material by a universal pulverizer, and sieving with an 80-mesh sieve; pulverizing to 3000 mesh with superfine pulverizer to obtain biomass powder;
y2 mixing biomass powder with water, wherein the mass ratio of the biomass powder to the water is 7:100; fully stirring, heating to 100 ℃ and boiling for 12min; cooling to 62 ℃ and soaking for 60min; cooling to room temperature and standing for 8min; centrifuging and filtering to obtain biomass extract;
immersing the fiber fabric into a 1.6wt% silver nitrate aqueous solution, wherein the mass ratio of the fiber fabric to the silver nitrate aqueous solution is 1:45; slowly adding the biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1:6, preparing a base material; adjusting the pH to 8.8 with sodium hydroxide solution; gradually heating to 86 ℃, fully stirring, and preserving heat and soaking for 52min; rinsing with water for 2 times, and drying at room temperature.
The fiber fabric is pure cotton fiber fabric.
The biomass raw material is peanut shells.
Comparative example 3
The preparation method of the green and environment-friendly silver fiber fabric comprises the following steps:
y1, washing the biomass raw material with water and airing; pulverizing the dried biomass raw material by a universal pulverizer, and sieving with an 80-mesh sieve; pulverizing to 3000 mesh with superfine pulverizer to obtain biomass powder;
y2 mixing biomass powder with water, wherein the mass ratio of the biomass powder to the water is 7:100; fully stirring, heating to 62 ℃ and soaking for 60min; heating to 100deg.C, and boiling for 12min; cooling to room temperature and standing for 8min; centrifuging and filtering to obtain biomass extract;
immersing the fiber fabric into a 1.6wt% silver nitrate aqueous solution, wherein the mass ratio of the fiber fabric to the silver nitrate aqueous solution is 1:45; slowly adding the biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1:6, preparing a base material; adjusting the pH to 8.8 with sodium hydroxide solution; gradually heating to 86 ℃, fully stirring, and preserving heat and soaking for 52min; rinsing with water for 2 times, and drying at room temperature.
The fiber fabric is pure cotton fiber fabric.
The biomass raw material is peanut shells.
Example 1
The preparation method of the green and environment-friendly silver fiber fabric comprises the following steps:
y1, washing the biomass raw material with water and airing; pulverizing the dried biomass raw material by a universal pulverizer, and sieving with an 80-mesh sieve; pulverizing to 3000 mesh with superfine pulverizer to obtain biomass powder;
y2 mixing biomass powder with water, wherein the mass ratio of the biomass powder to the water is 7:100; fully stirring, heating to 62 ℃ and soaking for 32min; heating to 100deg.C, and boiling for 12min; cooling to 62 ℃ and soaking for 28min; cooling to room temperature and standing for 8min; centrifuging and filtering to obtain biomass extract;
immersing the fiber fabric into a 1.6wt% silver nitrate aqueous solution, wherein the mass ratio of the fiber fabric to the silver nitrate aqueous solution is 1:45; slowly adding the biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1:6, preparing a base material; adjusting the pH to 8.8 with sodium hydroxide solution; gradually heating to 86 ℃, fully stirring, and preserving heat and soaking for 52min; rinsing with water for 2 times, and drying at room temperature.
The fiber fabric is pure cotton fiber fabric.
The biomass raw material is peanut shells.
Comparative example 4
The preparation method of the green and environment-friendly silver fiber fabric comprises the following steps:
y1, washing the biomass raw material with water and airing; pulverizing the dried biomass raw material by a universal pulverizer, and sieving with an 80-mesh sieve; pulverizing to 3000 mesh with superfine pulverizer to obtain biomass powder;
y2 mixing biomass powder with water, wherein the mass ratio of the biomass powder to the water is 7:100; fully stirring, heating to 62 ℃ and soaking for 32min; heating to 100deg.C, and boiling for 12min; cooling to 62 ℃ and soaking for 28min; cooling to room temperature and standing for 8min; centrifuging and filtering to obtain biomass extract;
immersing the fiber fabric into chitosan solution at room temperature, wherein the mass ratio of the fiber fabric to the chitosan solution is 1:60, dipping for 25h; taking out, curing for 8min at 121 ℃, and airing to obtain pretreated fiber fabric;
and Y4, immersing the pretreated fiber fabric into a 1.6wt% silver nitrate aqueous solution, wherein the mass ratio of the fiber fabric to the silver nitrate aqueous solution is 1:45; slowly adding the biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1:6, preparing a base material; adjusting the pH to 8.8 with sodium hydroxide solution; gradually heating to 86 ℃, fully stirring, and preserving heat and soaking for 52min; rinsing with water for 2 times, and drying at room temperature.
The preparation method of the chitosan solution comprises the following steps: adding chitosan into 2.0wt% acetic acid aqueous solution, heating to 62 ℃ and stirring for 1h, wherein the mass ratio of the chitosan to the acetic acid aqueous solution is 0.7:100.
The fiber fabric is pure cotton fiber fabric.
The biomass raw material is peanut shells.
Comparative example 5
The preparation method of the green and environment-friendly silver fiber fabric comprises the following steps:
y1, washing the biomass raw material with water and airing; pulverizing the dried biomass raw material by a universal pulverizer, and sieving with an 80-mesh sieve; pulverizing to 3000 mesh with superfine pulverizer to obtain biomass powder;
y2 mixing biomass powder with water, wherein the mass ratio of the biomass powder to the water is 7:100; fully stirring, heating to 62 ℃ and soaking for 32min; heating to 100deg.C, and boiling for 12min; cooling to 62 ℃ and soaking for 28min; cooling to room temperature and standing for 8min; centrifuging and filtering to obtain biomass extract;
immersing the fiber fabric into glycine aqueous solution at room temperature, wherein the mass ratio of the fiber fabric to the glycine aqueous solution is 1:60, dipping for 25h; taking out, curing for 8min at 121 ℃, and airing to obtain pretreated fiber fabric;
and Y4, immersing the pretreated fiber fabric into a 1.6wt% silver nitrate aqueous solution, wherein the mass ratio of the fiber fabric to the silver nitrate aqueous solution is 1:45; slowly adding the biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1:6, preparing a base material; adjusting the pH to 8.8 with sodium hydroxide solution; gradually heating to 86 ℃, fully stirring, and preserving heat and soaking for 52min; rinsing with water for 2 times, and drying at room temperature.
The concentration of the glycine aqueous solution was 0.7wt%.
The fiber fabric is pure cotton fiber fabric.
The biomass raw material is peanut shells.
Example 2
The preparation method of the green and environment-friendly silver fiber fabric comprises the following steps:
y1, washing the biomass raw material with water and airing; pulverizing the dried biomass raw material by a universal pulverizer, and sieving with an 80-mesh sieve; pulverizing to 3000 mesh with superfine pulverizer to obtain biomass powder;
y2 mixing biomass powder with water, wherein the mass ratio of the biomass powder to the water is 7:100; fully stirring, heating to 62 ℃ and soaking for 32min; heating to 100deg.C, and boiling for 12min; cooling to 62 ℃ and soaking for 28min; cooling to room temperature and standing for 8min; centrifuging and filtering to obtain biomass extract;
immersing the fiber fabric into chitosan solution at room temperature, wherein the mass ratio of the fiber fabric to the chitosan solution is 1:60, dipping for 25h; taking out, curing at 121deg.C for 8min, and air drying;
immersing the fiber fabric obtained in the step Y3 into glycine aqueous solution at room temperature, wherein the mass ratio of the fiber fabric to the glycine aqueous solution is 1:60, dipping for 25h; taking out, curing for 8min at 121 ℃, and airing to obtain pretreated fiber fabric;
the pretreated fiber fabric is immersed into a 1.6wt% silver nitrate aqueous solution, and the mass ratio of the fiber fabric to the silver nitrate aqueous solution is 1:45; slowly adding the biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1:6, preparing a base material; adjusting the pH to 8.8 with sodium hydroxide solution; gradually heating to 86 ℃, fully stirring, and preserving heat and soaking for 52min; rinsing with water for 2 times, and drying at room temperature.
The preparation method of the chitosan solution comprises the following steps: adding chitosan into 2.0wt% acetic acid aqueous solution, heating to 62 ℃ and stirring for 1h, wherein the mass ratio of the chitosan to the acetic acid aqueous solution is 0.7:100.
The concentration of the glycine aqueous solution was 0.7wt%.
The fiber fabric is pure cotton fiber fabric.
The biomass raw material is peanut shells.
Example 3
The preparation method of the green and environment-friendly silver fiber fabric comprises the following steps:
y1, washing the biomass raw material with water and airing; pulverizing the dried biomass raw material by a universal pulverizer, and sieving with an 80-mesh sieve; pulverizing to 3000 mesh with superfine pulverizer to obtain biomass powder;
y2 mixing biomass powder with water, wherein the mass ratio of the biomass powder to the water is 7:100; fully stirring, heating to 62 ℃ and soaking for 32min; heating to 100deg.C, and boiling for 12min; cooling to 62 ℃ and soaking for 28min; cooling to room temperature and standing for 8min; centrifuging and filtering to obtain biomass extract;
immersing the fiber fabric into the functionalized chitosan solution at the room temperature, wherein the mass ratio of the fiber fabric to the functionalized chitosan solution is 1:60, dipping for 25h; taking out, curing at 121deg.C for 8min, and air drying;
immersing the fiber fabric obtained in the step Y3 into glycine aqueous solution at room temperature, wherein the mass ratio of the fiber fabric to the glycine aqueous solution is 1:60, dipping for 25h; taking out, curing for 8min at 121 ℃, and airing to obtain pretreated fiber fabric;
the pretreated fiber fabric is immersed into a 1.6wt% silver nitrate aqueous solution, and the mass ratio of the fiber fabric to the silver nitrate aqueous solution is 1:45; slowly adding the biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1:6, preparing a base material; adjusting the pH to 8.8 with sodium hydroxide solution; gradually heating to 86 ℃, fully stirring, and preserving heat and soaking for 52min; rinsing with water for 2 times, and drying at room temperature.
The preparation method of the functionalized chitosan solution comprises the following steps: treatment liquid A1: adding chitosan into 2.0wt% acetic acid aqueous solution, heating to 62 ℃, stirring for 1h, and cooling to room temperature, wherein the mass ratio of the chitosan to the acetic acid aqueous solution is 1.4:100; treatment liquid A2: adding a functionalization reagent into water, wherein the mass ratio of the functionalization reagent to the water is 1.4:100, and performing ultrasonic treatment to fully dissolve; sequentially adding carbodiimide and N-hydroxysuccinimide under ice bath condition, wherein the mass ratio of the carbodiimide to the water is 0.8:100, and the mass ratio of the N-hydroxysuccinimide to the water is 0.5:100, and fully stirring; and slowly adding the treatment liquid A2 into the treatment liquid A1, stirring for 40min under the ice bath condition, taking out, and standing at room temperature for 8h to obtain the treatment liquid A1.
The functionalizing agent is gallic acid.
The concentration of the glycine aqueous solution was 0.7wt%.
The fiber fabric is pure cotton fiber fabric.
The biomass raw material is peanut shells.
Example 4
The preparation method of the green and environment-friendly silver fiber fabric comprises the following steps:
y1, washing the biomass raw material with water and airing; pulverizing the dried biomass raw material by a universal pulverizer, and sieving with an 80-mesh sieve; pulverizing to 3000 mesh with superfine pulverizer to obtain biomass powder;
y2 mixing biomass powder with water, wherein the mass ratio of the biomass powder to the water is 7:100; fully stirring, heating to 62 ℃ and soaking for 32min; heating to 100deg.C, and boiling for 12min; cooling to 62 ℃ and soaking for 28min; cooling to room temperature and standing for 8min; centrifuging and filtering to obtain biomass extract;
immersing the fiber fabric into the functionalized chitosan solution at the room temperature, wherein the mass ratio of the fiber fabric to the functionalized chitosan solution is 1:60, dipping for 25h; taking out, curing at 121deg.C for 8min, and air drying;
immersing the fiber fabric in the step Y3 into glycine aqueous solution at room temperature, wherein the mass ratio of the fiber fabric to the glycine aqueous solution is 1:60, dipping for 25h; taking out, curing for 8min at 121 ℃, and airing to obtain pretreated fiber fabric;
the pretreated fiber fabric is immersed into a 1.6wt% silver nitrate aqueous solution, and the mass ratio of the fiber fabric to the silver nitrate aqueous solution is 1:45; slowly adding the biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1:6, preparing a base material; adjusting the pH to 8.8 with sodium hydroxide solution; gradually heating to 86 ℃, fully stirring, and preserving heat and soaking for 52min; rinsing with water for 2 times, and drying at room temperature.
The preparation method of the functionalized chitosan solution comprises the following steps: treatment liquid A1: adding chitosan into 2.0wt% acetic acid aqueous solution, heating to 62 ℃, stirring for 1h, and cooling to room temperature, wherein the mass ratio of the chitosan to the acetic acid aqueous solution is 1.4:100; treatment liquid A2: adding a functionalization reagent into water, wherein the mass ratio of the functionalization reagent to the water is 1.4:100, and performing ultrasonic treatment to fully dissolve; sequentially adding carbodiimide and N-hydroxysuccinimide under ice bath condition, wherein the mass ratio of the carbodiimide to the water is 0.8:100, and the mass ratio of the N-hydroxysuccinimide to the water is 0.5:100, and fully stirring; and slowly adding the treatment liquid A2 into the treatment liquid A1, stirring for 40min under the ice bath condition, taking out, and standing at room temperature for 8h to obtain the treatment liquid A1.
The functionalizing agent is catechin.
The concentration of the glycine aqueous solution was 0.7wt%.
The fiber fabric is pure cotton fiber fabric.
The biomass raw material is peanut shells.
Example 5
The preparation method of the green and environment-friendly silver fiber fabric comprises the following steps:
y1, washing the biomass raw material with water and airing; pulverizing the dried biomass raw material by a universal pulverizer, and sieving with an 80-mesh sieve; pulverizing to 3000 mesh with superfine pulverizer to obtain biomass powder;
y2 mixing biomass powder with water, wherein the mass ratio of the biomass powder to the water is 7:100; fully stirring, heating to 62 ℃ and soaking for 32min; heating to 100deg.C, and boiling for 12min; cooling to 62 ℃ and soaking for 28min; cooling to room temperature and standing for 8min; centrifuging and filtering to obtain biomass extract;
immersing the fiber fabric into the functionalized chitosan solution at the room temperature, wherein the mass ratio of the fiber fabric to the functionalized chitosan solution is 1:60, dipping for 25h; taking out, curing at 121deg.C for 8min, and air drying;
immersing the fiber fabric in the step Y3 into glycine aqueous solution at room temperature, wherein the mass ratio of the fiber fabric to the glycine aqueous solution is 1:60, dipping for 25h; taking out, curing for 8min at 121 ℃, and airing to obtain pretreated fiber fabric;
the pretreated fiber fabric is immersed into a 1.6wt% silver nitrate aqueous solution, and the mass ratio of the fiber fabric to the silver nitrate aqueous solution is 1:45; slowly adding the biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1:6, preparing a base material; adjusting the pH to 8.8 with sodium hydroxide solution; gradually heating to 86 ℃, fully stirring, and preserving heat and soaking for 52min; rinsing with water for 2 times, and drying at room temperature.
The preparation method of the functionalized chitosan solution comprises the following steps: treatment liquid A1: adding chitosan into 2.0wt% acetic acid aqueous solution, heating to 62 ℃, stirring for 1h, and cooling to room temperature, wherein the mass ratio of the chitosan to the acetic acid aqueous solution is 1.4:100; treatment liquid A2: adding a functionalization reagent into water, wherein the mass ratio of the functionalization reagent to the water is 1.4:100, and performing ultrasonic treatment to fully dissolve; sequentially adding carbodiimide and N-hydroxysuccinimide under ice bath condition, wherein the mass ratio of the carbodiimide to the water is 0.8:100, and the mass ratio of the N-hydroxysuccinimide to the water is 0.5:100, and fully stirring; and slowly adding the treatment liquid A2 into the treatment liquid A1, stirring for 40min under the ice bath condition, taking out, and standing at room temperature for 8h to obtain the treatment liquid A1.
The functionalization reagent is a mixture of catechin and gallic acid, and the mass ratio of the catechin to the gallic acid is 2:3.
the concentration of the glycine aqueous solution was 0.7wt%.
The fiber fabric is pure cotton fiber fabric.
The biomass raw material is peanut shells.
Test example 1
Test of antioxidant Properties
The ABTS method was used. Dissolving ABTS in distilled water to prepare a 7.4mmol/L stock solution 1; dissolving potassium persulfate in distilled water to prepare a 2.6mmol/L stock solution 2; mixing the stock solution 1 with the stock solution 2 in equal volume, and reacting for 15 hours at room temperature in a dark place to obtain an ABTS working mother solution; before use, the solution is diluted to a proper concentration by 80% ethanol (namely, the absorbance value of the diluted ABTS working solution at 734nm is 0.700+/-0.005). Under the same conditions, the fabrics to be tested are taken for testing, and 5 groups are parallel.
Antioxidant activity (%) = (a-B)/c×100
Wherein A is the absorbance value of the sample to be detected after the reaction, and B is the absorbance value of the blank of the sample to be detected; c is the absorbance value of the unsampled ABTS working solution.
Table 1 oxidation resistance test table
As can be seen from Table 1, the oxidation resistance of the silver fiber fabric of example 2 is significantly higher than that of comparative examples 4-5 (pretreatment of the fiber fabric with chitosan solution or glycine aqueous solution); examples 3-5 use functionalized chitosan solution to further improve the oxidation resistance of the silver fiber fabric.
Test example 2
Antibacterial property test
And (3) performing antibacterial performance test on the fabric to be tested according to the standard GB/T20944.3-2008. Gram positive bacteria staphylococcus aureus (ATCC 6538) and gram negative bacteria escherichia coli (ATC 8739) are selected as test strains. The specific method comprises the following steps: cutting the control sample and the fabric to be tested into fragments with the size of 5mm multiplied by 5mm, weighing 0.75g as a sample, weighing all the fabrics to be tested by the same method, wrapping the fabrics in parallel three groups by using small paper sheets, and sterilizing under the same condition for standby. Inoculating the bacterial liquid, placing on a constant temperature oscillator, and oscillating for 18h at 24 ℃ at 150 r/min. The test solution was diluted to an appropriate dilution ratio with 0.03mol/LPBS buffer (sterilized). Pipette 1mL of diluted test solution was transferred to a sterilization plate and poured into about 15mL of nutrient agar medium. Three plates were each made in parallel. Solidifying at room temperature, inverting the plate, and culturing at 37 ℃ for 48h. Colony counts.
Antibacterial ratio (%) = (W-Q)/w×100
Wherein W and Q are the average values of the test of the control sample and the fabric to be tested respectively.
Control W: the cotton standard interlining fabric specified in standard GB/T20944.3-2008 is used as a control sample after being steamed and boiled at high temperature and washed by distilled water.
Table 2 antibacterial property test table
As can be seen from table 2, the antibacterial performance of the silver fiber fabric can be improved by pretreating the fiber fabric by a two-step method in the embodiment 2; the embodiment 3-5 adopts the functionalized chitosan solution, so that the antibacterial performance of the silver fiber fabric is further improved; and the functionalized chitosan solution prepared by coupling and compounding the functionalized reagent gallic acid and catechin in the embodiment 5 has the antibacterial property obviously higher than that of the embodiments 3-4, and the remarkable progress is achieved.
The foregoing describes in detail preferred embodiments of the present invention. It should be understood that numerous modifications and variations can be made in accordance with the concepts of the invention by one of ordinary skill in the art without undue burden. Therefore, all technical solutions which can be obtained by logic analysis, reasoning or limited experiments based on the prior art by the person skilled in the art according to the inventive concept shall be within the scope of protection defined by the claims.
Claims (3)
1. The preparation method of the green and environment-friendly silver fiber fabric is characterized by comprising the following steps of:
y1, washing the biomass raw material with water and airing; pulverizing the dried biomass raw material by a universal pulverizer, and sieving with a 50-100 mesh sieve; pulverizing to 1500-3500 mesh with superfine pulverizer to obtain biomass powder;
y2 mixing biomass powder with water, wherein the mass ratio of the biomass powder to the water is (1-10): 100; fully stirring, heating to 50-80 ℃ and soaking for 10-40min; heating to 100deg.C, and boiling for 5-20min; cooling to 50-80deg.C, soaking for 10-40min; cooling to room temperature and standing for 5-20min; centrifuging and filtering to obtain biomass extract;
immersing the fiber fabric into the functionalized chitosan solution at the room temperature, wherein the mass ratio of the fiber fabric to the functionalized chitosan solution is (0.5-2): (20-100), dipping for 10-48h; taking out, solidifying at 100-150deg.C for 1-10min, and air drying;
immersing the fiber fabric obtained in the step Y3 into glycine aqueous solution at room temperature, wherein the mass ratio of the fiber fabric to the glycine aqueous solution is (0.5-2): (20-100), dipping for 10-48h; taking out, curing for 1-10min at 100-150 ℃, and airing to obtain pretreated fiber fabric; the pretreated fiber fabric is immersed into 0.5 to 3.5 weight percent of silver nitrate aqueous solution, and the mass ratio of the fiber fabric to the silver nitrate aqueous solution is (0.5 to 2): (15-50); slowly adding the biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1: (1-20); adjusting the pH to 6-10 with sodium hydroxide solution; gradually heating to 50-90deg.C, stirring thoroughly, and soaking at constant temperature for 30-90min; rinsing with water for 1-3 times, and drying at room temperature to obtain the final product;
the biomass raw material is any one of dried wood orange leaves, dried mango leaves and peanut shells;
the concentration of the glycine aqueous solution is 0.5-3.5 wt%;
the preparation method of the functionalized chitosan solution comprises the following steps:
treatment liquid A1: adding chitosan into 0.5-3.5 wt% acetic acid water solution with the mass ratio of chitosan to acetic acid water solution of (0.5-5) 100, heating to 50-80 ℃, stirring for 0.5-5h, and cooling to room temperature;
treatment liquid A2: adding a functionalization reagent into water, wherein the mass ratio of the functionalization reagent to the water is (0.5-5): 100, and performing ultrasonic treatment to fully dissolve; sequentially adding carbodiimide and N-hydroxysuccinimide under ice bath condition, wherein the mass ratio of the carbodiimide to the water is (0.3-5) 100, and the mass ratio of the N-hydroxysuccinimide to the water is (0.2-5) 100, and fully stirring; the functionalization reagent is a mixture of catechin and gallic acid, and the mass ratio of the catechin to the gallic acid is (1-5);
adding the treatment solution A2 into the treatment solution A1, wherein the volume ratio of the treatment solution A1 to the treatment solution A2 is (0.5-5): 1, stirring for 30-60min under ice bath condition, taking out, and standing at room temperature for 5-10 h.
2. The method for preparing the green and environment-friendly silver fiber fabric as claimed in claim 1, which is characterized in that: the fiber fabric is any one of pure cotton fiber fabric, polyester fiber fabric, wool fiber fabric, silk fiber fabric and polyamide fiber fabric.
3. The utility model provides a green silver fiber surface fabric which characterized in that: prepared by the method of claim 1 or 2.
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