CN111945420A - Green and environment-friendly silver fiber fabric and preparation method thereof - Google Patents
Green and environment-friendly silver fiber fabric and preparation method thereof Download PDFInfo
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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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- D06M2101/02—Natural fibres, other than mineral fibres
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Abstract
The invention relates to the technical field of fabrics, and particularly relates to a green 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 biomass raw material with water and drying; crushing the dried biomass raw material to obtain biomass powder; y2 mixing the biomass powder with water, boiling; cooling to room temperature; centrifuging and filtering to obtain a biomass extracting solution; y3, immersing the fiber fabric into a silver nitrate water solution; and slowly adding the biomass extracting solution for dipping, washing and drying to obtain the green environment-friendly silver fiber fabric. The silver fiber fabric prepared from the biomass extracting solution is green and environment-friendly, has good antibacterial, deodorizing, radiation-proof and anti-static performances, is good in stability, is not easy to oxidize, and does not turn yellow or turn dark 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 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 combining a layer of pure silver on the surface of a fiber through a special process. Silver is used as metal with the best conductivity, and the silver fiber fabric has good radiation shielding effect and is the most ideal radiation-proof clothing fabric at present; meanwhile, the silver fiber fabric is also the best antibacterial and deodorant fabric by utilizing the natural antibacterial property of silver. The silver fiber fabric is soft, light and thin, has excellent air permeability and is very suitable for wearing. However, metal silver is very easy to be oxidized, and is easy to react with substances in the air after being exposed in the air for a long time, so that the fabric turns yellow and dark after being oxidized, and the performance of the silver fiber fabric is reduced.
Currently, silver fibers include nano silver fibers and silver-plated fibers. The nano silver fiber is prepared by adding superfine silver particles in the fiber forming process; the silver-plated fiber is obtained by plating a silver layer on the surface of the fiber through various metallization technologies such as chemical plating or electroplating. In the preparation process of the nano-silver fiber, the nano-silver is easy to agglomerate and is dispersed unevenly, so that the effective utilization rate of the nano-silver fiber is reduced, and the application of the nano-silver fiber is limited. Therefore, the research on silver-plated fibers is mainly focused.
Electroless silver plating is a highly selective process that utilizes a suitable reducing agent in solution to reduce silver ions and deposit them on the surface of the fibers under the action of certain metal catalysts or other processes. The traditional chemical silver plating method has the defects of potential safety hazard, environmental pollution and the like in the production and processing process. The problem to be solved urgently is to find an environment-friendly silver plating method to replace the traditional method in the field of textiles.
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 green environment-friendly silver fiber fabric and the preparation method thereof are provided.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a green environment-friendly silver fiber fabric comprises the following steps:
y1 washing biomass raw material with water and drying; crushing the dried biomass raw material to obtain biomass powder;
y2 mixing the biomass powder with water, boiling; cooling to room temperature; centrifuging and filtering to obtain a biomass extracting solution;
y3, immersing the fiber fabric into a silver nitrate water solution; slowly adding the biomass extracting solution; stirring thoroughly, and soaking for 30-90 min; rinsing with water for 1-3 times, and drying at room temperature.
Further, the preparation method of the green environment-friendly silver fiber fabric comprises the following steps:
y1 washing biomass raw material with water and drying; crushing the dried biomass raw material by using a universal crusher, and sieving by using a 50-100-mesh sieve; then, crushing the biomass powder to 1500-fold 3500 meshes by using an ultrafine crusher to obtain biomass powder;
y2 mixing the biomass powder with water, wherein the mass ratio of the biomass powder to the water is (1-10): 100, respectively; stirring, heating to 50-80 deg.C, and soaking for 10-40 min; continuously heating to 100 deg.C, boiling for 5-20 min; cooling to 50-80 deg.C, and soaking for 10-40 min; cooling to room temperature and standing for 5-20 min; centrifuging and filtering to obtain a biomass extracting solution;
y3, 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 a biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1: (1-20); adjusting pH to 6-10 with sodium hydroxide solution; gradually heating to 50-90 deg.C, stirring, and soaking for 30-90 min; rinsing with water for 1-3 times, and drying at room temperature.
Further, the preparation method of the green environment-friendly silver fiber fabric comprises the following steps:
y1 washing biomass raw material with water and drying; crushing the dried biomass raw material by using a universal crusher, and sieving by using a 50-100-mesh sieve; then, crushing the biomass powder to 1500-fold 3500 meshes by using an ultrafine crusher to obtain biomass powder;
y2 mixing the biomass powder with water, wherein the mass ratio of the biomass powder to the water is (1-10): 100, respectively; stirring, heating to 50-80 deg.C, and soaking for 10-40 min; continuously heating to 100 deg.C, boiling for 5-20 min; cooling to 50-80 deg.C, and soaking for 10-40 min; cooling to room temperature and standing for 5-20 min; centrifuging and filtering to obtain a biomass extracting solution;
y3, soaking 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) soaking for 10-48 h; taking out, curing at the temperature of 100-150 ℃ for 1-10min, and airing to obtain the pretreated fiber fabric; the treatment fluid is one of chitosan solution, functionalized chitosan solution and glycine aqueous solution;
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 a biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1: (1-20); adjusting pH to 6-10 with sodium hydroxide solution; gradually heating to 50-90 deg.C, stirring, and soaking for 30-90 min; rinsing with water for 1-3 times, and drying at room temperature.
Further, the preparation method of the green environment-friendly silver fiber fabric comprises the following steps:
y1 washing biomass raw material with water and drying; crushing the dried biomass raw material by using a universal crusher, and sieving by using a 50-100-mesh sieve; then, crushing the biomass powder to 1500-fold 3500 meshes by using an ultrafine crusher to obtain biomass powder;
y2 mixing the biomass powder with water, wherein the mass ratio of the biomass powder to the water is (1-10): 100, respectively; stirring, heating to 50-80 deg.C, and soaking for 10-40 min; continuously heating to 100 deg.C, boiling for 5-20 min; cooling to 50-80 deg.C, and soaking for 10-40 min; cooling to room temperature and standing for 5-20 min; centrifuging and filtering to obtain a biomass extracting solution;
y3, soaking the fiber fabric into the chitosan solution or the 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) soaking for 10-48 h; taking out, curing at 100-150 deg.C for 1-10min, and air drying;
y4, soaking 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) soaking for 10-48 h; taking out, curing at the temperature of 100-150 ℃ for 1-10min, and airing to obtain the pretreated fiber fabric;
y5, 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 a biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1: (1-20); adjusting pH to 6-10 with sodium hydroxide solution; gradually heating to 50-90 deg.C, stirring, and soaking for 30-90 min; rinsing with water for 1-3 times, and drying at room temperature.
Preferably, the preparation method of the chitosan solution is as follows: adding chitosan into 0.5-3.5 wt% acetic acid water solution with the mass ratio of chitosan to acetic acid water solution being (0.5-5):100, heating to 50-80 deg.C, and stirring for 0.5-5 h.
In some embodiments of the present application, the method for preparing the green environment-friendly silver fiber fabric comprises the following steps:
y1 washing biomass raw material with water and drying; crushing the dried biomass raw material by using a universal crusher, and sieving by using a 50-100-mesh sieve; then, crushing the biomass powder to 1500-fold 3500 meshes by using an ultrafine crusher to obtain biomass powder;
y2 mixing the biomass powder with water, wherein the mass ratio of the biomass powder to the water is (1-10): 100, respectively; stirring, heating to 50-80 deg.C, and soaking for 10-40 min; continuously heating to 100 deg.C, boiling for 5-20 min; cooling to 50-80 deg.C, and soaking for 10-40 min; cooling to room temperature and standing for 5-20 min; centrifuging and filtering to obtain a biomass extracting solution;
y3, soaking the fiber fabric into the functionalized chitosan solution at room temperature, wherein the mass ratio of the fiber fabric to the functionalized chitosan solution is (0.5-2): (20-100) soaking for 10-48 h; taking out, curing at 100-150 deg.C for 1-10min, and air drying;
y4, soaking 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) soaking for 10-48 h; taking out, curing at the temperature of 100-150 ℃ for 1-10min, and airing to obtain the pretreated fiber fabric;
y5, 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 a biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1: (1-20); adjusting pH to 6-10 with sodium hydroxide solution; gradually heating to 50-90 deg.C, stirring, and soaking for 30-90 min; rinsing with water for 1-3 times, and drying at room temperature.
Preferably, the preparation method of the functionalized chitosan solution is as follows:
treatment liquid a 1: adding chitosan into 0.5-3.5 wt% acetic acid water solution, the mass ratio of chitosan to acetic acid water solution is (0.5-5):100, heating to 50-80 ℃, stirring for 0.5-5h, and cooling to room temperature;
treatment liquid a 2: adding a functional reagent into water, wherein the mass ratio of the functional reagent to the water is (0.5-5) to 100, and performing ultrasonic treatment to fully dissolve the functional reagent; under the ice-bath condition, sequentially adding carbodiimide and N-hydroxysuccinimide, wherein the mass ratio of the carbodiimide to the water is (0.3-5) to 100, and the mass ratio of the N-hydroxysuccinimide to the water is (0.2-5) to 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 for 5-10h at room temperature to obtain the product.
Preferably, the functional reagent is any one of ferulic acid, catechin, caffeic acid and gallic acid.
More preferably, the functionalizing agent is a mixture of catechin and gallic acid, and the mass ratio of the catechin to the gallic acid is (1-5): (1-5).
Preferably, the concentration of the glycine aqueous solution is 0.5 wt% to 3.5 wt%.
Preferably, the fiber fabric is any one of a pure cotton fiber fabric, a polyester fiber fabric, a wool fiber fabric, a silk fiber fabric and a polyamide fiber fabric.
Preferably, the biomass raw material is any one of dried leaves of aegle marmelos, dried leaves of mangoes and peanut shells.
The invention also provides a green environment-friendly silver fiber fabric prepared by the method.
As a renewable green resource, how to effectively utilize biomass is always a research hotspot. According to the invention, the biomass is used as a raw material, and active molecules in the biomass are reduced in situ on the surface of the fiber fabric to generate silver nanoparticles, so that the silver fiber fabric is obtained. The biomass raw material is subjected to primary crushing by adopting a universal crusher and secondary crushing treatment by combining an ultrafine crusher; meanwhile, the biomass extracting solution is prepared by adopting a segmented temperature-controlled extraction method, so that active molecules in the biomass are fully dissolved, the in-situ reduction capability 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 reason is that the preparation method of the biomass extracting solution is suitable, effective plant active molecules in the biomass raw material, such as dihydroxy chromone, eriodictyol, trihydroxy flavanone, luteolin and the like in peanut shells, or flavonoid compounds, terpenoids, thiamine and the like in mango leaves are more dissolved in the biomass extracting solution, and the reducing capability is stronger.
The invention further improves the performance of the silver fiber fabric by pretreating the fiber fabric in two steps. 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 fabric; on the other hand, after the glycine in the glycine aqueous solution is combined with the fabric fibers, the nano silver particles generated on the surface of the fiber fabric by reduction can be stabilized, the nano silver particles are prevented from being oxidized, and the function of a protective agent is achieved. Furthermore, the invention adopts a functionalized chitosan solution, and the chitosan is coupled with a functionalized reagent of gallic acid or/and catechin, so that the capability of capturing and adsorbing silver ions is obviously improved; and after the 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 invention has the advantages of
The invention provides a novel preparation method of a green environment-friendly fiber fabric by adopting a biomass extracting solution to prepare a silver fiber fabric. Pretreating the fiber fabric by adopting a two-step method, (1) combining chitosan in a chitosan solution with fabric fibers, so that silver ions are easily captured and adsorbed by the fiber fabric, and more nano silver particles are generated; (2) the glycine in the glycine aqueous solution is combined with the fabric fibers to protect the nano silver particles generated on the surface of the fiber fabric 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 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 environment-friendly fiber fabric disclosed by the invention is good in 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 general popularization and application.
Detailed Description
Some of the raw materials in the examples and comparative examples are as follows:
the peanut shells in the examples and comparative examples were provided by the plant industries of futokadsura, california.
The universal pulverizer used in the examples and comparative examples was a 130B model universal pulverizer available from Tazhou King Cheng pharmaceutical machinery, Inc., and the main shaft rotation speed was 7000 r/min.
The pure cotton fiber fabrics of the examples and comparative examples were manufactured by Shaoxing Kobridal textile Co., Ltd, a grammage of 265g/m2。
In the examples and comparative examples, the ultrafine pulverizer of CWF-300 type, model number, spindle speed 1450r/min, was used.
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 Aladdin, product number: A110749.
carbodiimide in examples and comparative examples: CAS number: 151-51-9; purchased from Junrui, Shanghai.
N-hydroxysuccinimide in examples and comparative examples: CAS number: 6066-82-6; purchased from michelin, shanghai.
Gallic acid in examples and comparative examples: CAS number: 149-91-7; is purchased from chemical engineering of fertilizer combination and Tianjian.
Catechins in examples and comparative examples: CAS number: 18829-70-4; purchased from Shanghai Aladdin.
Comparative example 1
A preparation method of a green environment-friendly silver fiber fabric comprises the following steps:
y1 washing biomass raw material with water and drying; crushing the dried biomass raw material by using a universal crusher, and sieving by using a 80-mesh sieve to obtain biomass powder;
y2 mixing the biomass powder with water, wherein the mass ratio of the biomass powder to the water is 7:100, respectively; stirring thoroughly, heating to 62 deg.C, soaking for 32 min; continuously heating to 100 deg.C, boiling for 12 min; cooling to 62 deg.C, and soaking for 28 min; cooling to room temperature and standing for 8 min; centrifuging and filtering to obtain a biomass extracting solution;
y3, immersing the fiber fabric into 1.6 wt% of silver nitrate aqueous solution, wherein the mass ratio of the fiber fabric to the silver nitrate aqueous solution is 1: 45, a first step of; slowly adding a biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1: 6; adjusting the pH to 8.8 with sodium hydroxide solution; gradually heating to 86 deg.C, stirring, and soaking for 52 min; rinsing with water for 2 times, and drying at room temperature.
The fiber fabric is a pure cotton fiber fabric.
The biomass raw material is peanut shells.
Comparative example 2
A preparation method of a green environment-friendly silver fiber fabric comprises the following steps:
y1 washing biomass raw material with water and drying; crushing the dried biomass raw material by using a universal crusher, and sieving by using a 80-mesh sieve; then crushing the biomass powder to 3000 meshes by using an ultrafine crusher to obtain biomass powder;
y2 mixing the biomass powder with water, wherein the mass ratio of the biomass powder to the water is 7:100, respectively; stirring, heating to 100 deg.C, boiling for 12 min; cooling to 62 deg.C, and soaking for 60 min; cooling to room temperature and standing for 8 min; centrifuging and filtering to obtain a biomass extracting solution;
y3, immersing the fiber fabric into 1.6 wt% of silver nitrate aqueous solution, wherein the mass ratio of the fiber fabric to the silver nitrate aqueous solution is 1: 45, a first step of; slowly adding a biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1: 6; adjusting the pH to 8.8 with sodium hydroxide solution; gradually heating to 86 deg.C, stirring, and soaking for 52 min; rinsing with water for 2 times, and drying at room temperature.
The fiber fabric is a pure cotton fiber fabric.
The biomass raw material is peanut shells.
Comparative example 3
A preparation method of a green environment-friendly silver fiber fabric comprises the following steps:
y1 washing biomass raw material with water and drying; crushing the dried biomass raw material by using a universal crusher, and sieving by using a 80-mesh sieve; then crushing the biomass powder to 3000 meshes by using an ultrafine crusher to obtain biomass powder;
y2 mixing the biomass powder with water, wherein the mass ratio of the biomass powder to the water is 7:100, respectively; stirring thoroughly, heating to 62 deg.C, and soaking for 60 min; continuously heating to 100 deg.C, boiling for 12 min; cooling to room temperature and standing for 8 min; centrifuging and filtering to obtain a biomass extracting solution;
y3, immersing the fiber fabric into 1.6 wt% of silver nitrate aqueous solution, wherein the mass ratio of the fiber fabric to the silver nitrate aqueous solution is 1: 45, a first step of; slowly adding a biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1: 6; adjusting the pH to 8.8 with sodium hydroxide solution; gradually heating to 86 deg.C, stirring, and soaking for 52 min; rinsing with water for 2 times, and drying at room temperature.
The fiber fabric is a pure cotton fiber fabric.
The biomass raw material is peanut shells.
Example 1
A preparation method of a green environment-friendly silver fiber fabric comprises the following steps:
y1 washing biomass raw material with water and drying; crushing the dried biomass raw material by using a universal crusher, and sieving by using a 80-mesh sieve; then crushing the biomass powder to 3000 meshes by using an ultrafine crusher to obtain biomass powder;
y2 mixing the biomass powder with water, wherein the mass ratio of the biomass powder to the water is 7:100, respectively; stirring thoroughly, heating to 62 deg.C, soaking for 32 min; continuously heating to 100 deg.C, boiling for 12 min; cooling to 62 deg.C, and soaking for 28 min; cooling to room temperature and standing for 8 min; centrifuging and filtering to obtain a biomass extracting solution;
y3, immersing the fiber fabric into 1.6 wt% of silver nitrate aqueous solution, wherein the mass ratio of the fiber fabric to the silver nitrate aqueous solution is 1: 45, a first step of; slowly adding a biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1: 6; adjusting the pH to 8.8 with sodium hydroxide solution; gradually heating to 86 deg.C, stirring, and soaking for 52 min; rinsing with water for 2 times, and drying at room temperature.
The fiber fabric is a pure cotton fiber fabric.
The biomass raw material is peanut shells.
Comparative example 4
A preparation method of a green environment-friendly silver fiber fabric comprises the following steps:
y1 washing biomass raw material with water and drying; crushing the dried biomass raw material by using a universal crusher, and sieving by using a 80-mesh sieve; then crushing the biomass powder to 3000 meshes by using an ultrafine crusher to obtain biomass powder;
y2 mixing the biomass powder with water, wherein the mass ratio of the biomass powder to the water is 7:100, respectively; stirring thoroughly, heating to 62 deg.C, soaking for 32 min; continuously heating to 100 deg.C, boiling for 12 min; cooling to 62 deg.C, and soaking for 28 min; cooling to room temperature and standing for 8 min; centrifuging and filtering to obtain a biomass extracting solution;
y3, immersing the fiber fabric into the chitosan solution at room temperature, wherein the mass ratio of the fiber fabric to the chitosan solution is 1: 60, soaking for 25 h; taking out, curing for 8min at 121 ℃, and airing to obtain a pretreated fiber fabric;
y4, immersing the pretreated fiber fabric into 1.6 wt% of silver nitrate aqueous solution, wherein the mass ratio of the fiber fabric to the silver nitrate aqueous solution is 1: 45, a first step of; slowly adding a biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1: 6; adjusting the pH to 8.8 with sodium hydroxide solution; gradually heating to 86 deg.C, stirring, and soaking for 52 min; 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 2.0 wt% acetic acid water solution with the mass ratio of chitosan to acetic acid water solution being 0.7:100, heating to 62 ℃, and stirring for 1h to obtain the chitosan-acetic acid water-based coating.
The fiber fabric is a pure cotton fiber fabric.
The biomass raw material is peanut shells.
Comparative example 5
A preparation method of a green environment-friendly silver fiber fabric comprises the following steps:
y1 washing biomass raw material with water and drying; crushing the dried biomass raw material by using a universal crusher, and sieving by using a 80-mesh sieve; then crushing the biomass powder to 3000 meshes by using an ultrafine crusher to obtain biomass powder;
y2 mixing the biomass powder with water, wherein the mass ratio of the biomass powder to the water is 7:100, respectively; stirring thoroughly, heating to 62 deg.C, soaking for 32 min; continuously heating to 100 deg.C, boiling for 12 min; cooling to 62 deg.C, and soaking for 28 min; cooling to room temperature and standing for 8 min; centrifuging and filtering to obtain a biomass extracting solution;
y3, soaking 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, soaking for 25 h; taking out, curing for 8min at 121 ℃, and airing to obtain a pretreated fiber fabric;
y4, immersing the pretreated fiber fabric into 1.6 wt% of silver nitrate aqueous solution, wherein the mass ratio of the fiber fabric to the silver nitrate aqueous solution is 1: 45, a first step of; slowly adding a biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1: 6; adjusting the pH to 8.8 with sodium hydroxide solution; gradually heating to 86 deg.C, stirring, and soaking for 52 min; rinsing with water for 2 times, and drying at room temperature.
The concentration of the glycine aqueous solution was 0.7 wt%.
The fiber fabric is a pure cotton fiber fabric.
The biomass raw material is peanut shells.
Example 2
A preparation method of a green environment-friendly silver fiber fabric comprises the following steps:
y1 washing biomass raw material with water and drying; crushing the dried biomass raw material by using a universal crusher, and sieving by using a 80-mesh sieve; then crushing the biomass powder to 3000 meshes by using an ultrafine crusher to obtain biomass powder;
y2 mixing the biomass powder with water, wherein the mass ratio of the biomass powder to the water is 7:100, respectively; stirring thoroughly, heating to 62 deg.C, soaking for 32 min; continuously heating to 100 deg.C, boiling for 12 min; cooling to 62 deg.C, and soaking for 28 min; cooling to room temperature and standing for 8 min; centrifuging and filtering to obtain a biomass extracting solution;
y3, immersing the fiber fabric into the chitosan solution at room temperature, wherein the mass ratio of the fiber fabric to the chitosan solution is 1: 60, soaking for 25 h; taking out, curing at 121 deg.C for 8min, and air drying;
y4, soaking 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, soaking for 25 h; taking out, curing for 8min at 121 ℃, and airing to obtain a pretreated fiber fabric;
y5, immersing the pretreated fiber fabric into 1.6 wt% of silver nitrate aqueous solution, wherein the mass ratio of the fiber fabric to the silver nitrate aqueous solution is 1: 45, a first step of; slowly adding a biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1: 6; adjusting the pH to 8.8 with sodium hydroxide solution; gradually heating to 86 deg.C, stirring, and soaking for 52 min; 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 2.0 wt% acetic acid water solution with the mass ratio of chitosan to acetic acid water solution being 0.7:100, heating to 62 ℃, and stirring for 1h to obtain the chitosan-acetic acid water-based coating.
The concentration of the glycine aqueous solution was 0.7 wt%.
The fiber fabric is a pure cotton fiber fabric.
The biomass raw material is peanut shells.
Example 3
A preparation method of a green environment-friendly silver fiber fabric comprises the following steps:
y1 washing biomass raw material with water and drying; crushing the dried biomass raw material by using a universal crusher, and sieving by using a 80-mesh sieve; then crushing the biomass powder to 3000 meshes by using an ultrafine crusher to obtain biomass powder;
y2 mixing the biomass powder with water, wherein the mass ratio of the biomass powder to the water is 7:100, respectively; stirring thoroughly, heating to 62 deg.C, soaking for 32 min; continuously heating to 100 deg.C, boiling for 12 min; cooling to 62 deg.C, and soaking for 28 min; cooling to room temperature and standing for 8 min; centrifuging and filtering to obtain a biomass extracting solution;
y3, soaking the fiber fabric into the functionalized chitosan solution at room temperature, wherein the mass ratio of the fiber fabric to the functionalized chitosan solution is 1: 60, soaking for 25 h; taking out, curing at 121 deg.C for 8min, and air drying;
y4, soaking 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, soaking for 25 h; taking out, curing for 8min at 121 ℃, and airing to obtain a pretreated fiber fabric;
y5, immersing the pretreated fiber fabric into 1.6 wt% of silver nitrate aqueous solution, wherein the mass ratio of the fiber fabric to the silver nitrate aqueous solution is 1: 45, a first step of; slowly adding a biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1: 6; adjusting the pH to 8.8 with sodium hydroxide solution; gradually heating to 86 deg.C, stirring, and soaking for 52 min; 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 a 1: adding chitosan into 2.0 wt% acetic acid aqueous solution, wherein the mass ratio of the chitosan to the acetic acid aqueous solution is 1.4:100, heating to 62 ℃, stirring for 1h, and cooling to room temperature; treatment liquid a 2: adding a functional reagent into water, wherein the mass ratio of the functional reagent to the water is 1.4:100, and fully dissolving by ultrasonic; sequentially adding carbodiimide and N-hydroxysuccinimide under an 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, wherein the volume ratio of the treatment liquid A1 to the treatment liquid A2 is 1:1, stirring for 40min under an ice bath condition, taking out, and standing at room temperature for 8h to obtain the composition.
The functional reagent is gallic acid.
The concentration of the glycine aqueous solution was 0.7 wt%.
The fiber fabric is a pure cotton fiber fabric.
The biomass raw material is peanut shells.
Example 4
A preparation method of a green environment-friendly silver fiber fabric comprises the following steps:
y1 washing biomass raw material with water and drying; crushing the dried biomass raw material by using a universal crusher, and sieving by using a 80-mesh sieve; then crushing the biomass powder to 3000 meshes by using an ultrafine crusher to obtain biomass powder;
y2 mixing the biomass powder with water, wherein the mass ratio of the biomass powder to the water is 7:100, respectively; stirring thoroughly, heating to 62 deg.C, soaking for 32 min; continuously heating to 100 deg.C, boiling for 12 min; cooling to 62 deg.C, and soaking for 28 min; cooling to room temperature and standing for 8 min; centrifuging and filtering to obtain a biomass extracting solution;
y3, soaking the fiber fabric into the functionalized chitosan solution at room temperature, wherein the mass ratio of the fiber fabric to the functionalized chitosan solution is 1: 60, soaking for 25 h; taking out, curing at 121 deg.C for 8min, and air drying;
y4, soaking 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, soaking for 25 h; taking out, curing for 8min at 121 ℃, and airing to obtain a pretreated fiber fabric;
y5, immersing the pretreated fiber fabric into 1.6 wt% of silver nitrate aqueous solution, wherein the mass ratio of the fiber fabric to the silver nitrate aqueous solution is 1: 45, a first step of; slowly adding a biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1: 6; adjusting the pH to 8.8 with sodium hydroxide solution; gradually heating to 86 deg.C, stirring, and soaking for 52 min; 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 a 1: adding chitosan into 2.0 wt% acetic acid aqueous solution, wherein the mass ratio of the chitosan to the acetic acid aqueous solution is 1.4:100, heating to 62 ℃, stirring for 1h, and cooling to room temperature; treatment liquid a 2: adding a functional reagent into water, wherein the mass ratio of the functional reagent to the water is 1.4:100, and fully dissolving by ultrasonic; sequentially adding carbodiimide and N-hydroxysuccinimide under an 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, wherein the volume ratio of the treatment liquid A1 to the treatment liquid A2 is 1:1, stirring for 40min under an ice bath condition, taking out, and standing at room temperature for 8h to obtain the composition.
The functional reagent is catechin.
The concentration of the glycine aqueous solution was 0.7 wt%.
The fiber fabric is a pure cotton fiber fabric.
The biomass raw material is peanut shells.
Example 5
A preparation method of a green environment-friendly silver fiber fabric comprises the following steps:
y1 washing biomass raw material with water and drying; crushing the dried biomass raw material by using a universal crusher, and sieving by using a 80-mesh sieve; then crushing the biomass powder to 3000 meshes by using an ultrafine crusher to obtain biomass powder;
y2 mixing the biomass powder with water, wherein the mass ratio of the biomass powder to the water is 7:100, respectively; stirring thoroughly, heating to 62 deg.C, soaking for 32 min; continuously heating to 100 deg.C, boiling for 12 min; cooling to 62 deg.C, and soaking for 28 min; cooling to room temperature and standing for 8 min; centrifuging and filtering to obtain a biomass extracting solution;
y3, soaking the fiber fabric into the functionalized chitosan solution at room temperature, wherein the mass ratio of the fiber fabric to the functionalized chitosan solution is 1: 60, soaking for 25 h; taking out, curing at 121 deg.C for 8min, and air drying;
y4, soaking 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, soaking for 25 h; taking out, curing for 8min at 121 ℃, and airing to obtain a pretreated fiber fabric;
y5, immersing the pretreated fiber fabric into 1.6 wt% of silver nitrate aqueous solution, wherein the mass ratio of the fiber fabric to the silver nitrate aqueous solution is 1: 45, a first step of; slowly adding a biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1: 6; adjusting the pH to 8.8 with sodium hydroxide solution; gradually heating to 86 deg.C, stirring, and soaking for 52 min; 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 a 1: adding chitosan into 2.0 wt% acetic acid aqueous solution, wherein the mass ratio of the chitosan to the acetic acid aqueous solution is 1.4:100, heating to 62 ℃, stirring for 1h, and cooling to room temperature; treatment liquid a 2: adding a functional reagent into water, wherein the mass ratio of the functional reagent to the water is 1.4:100, and fully dissolving by ultrasonic; sequentially adding carbodiimide and N-hydroxysuccinimide under an 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, wherein the volume ratio of the treatment liquid A1 to the treatment liquid A2 is 1:1, stirring for 40min under an ice bath condition, taking out, and standing at room temperature for 8h to obtain the composition.
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 0.7 wt%.
The fiber fabric is a pure cotton fiber fabric.
The biomass raw material is peanut shells.
Test example 1
Test for Oxidation resistance
ABTS method is adopted. Dissolving ABTS in distilled water to prepare a stock solution 1 of 7.4 mmol/L; dissolving potassium persulfate in distilled water to prepare a stock solution 2 of 2.6 mmol/L; then mixing the stock solution 1 and the stock solution 2 in equal volume, and reacting for 15h at room temperature in a dark place to obtain ABTS working mother liquor; before use, the ABTS 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). And under the same condition, taking the fabric to be tested for testing, and paralleling 5 groups.
Antioxidant activity (%) - (A-B)/Cx 100
Wherein A is the absorbance value of the sample to be detected after reaction, and B is the absorbance value of the blank of the sample to be detected; c is the absorbance value of the ABTS working solution without sample application.
TABLE 1 Oxidation resistance test Table
As can be seen from Table 1, the silver fiber fabric of the fiber fabric pretreated by the two-step method in the example 2 has the oxidation resistance obviously higher than that of the silver fiber fabric of the comparative examples 4-5 (the fiber fabric is pretreated by the chitosan solution or the glycine aqueous solution); in the embodiments 3-5, the oxidation resistance of the silver fiber fabric is further improved by adopting the functionalized chitosan solution.
Test example 2
Test of antibacterial Property
And (4) performing an 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 C8739) were selected as test strains. The specific method comprises the following steps: the reference sample and the fabric to be measured are cut into pieces with the size of 5mm multiplied by 5mm, 0.75g is weighed as a sample, all the fabrics to be measured are weighed in the same method, three groups are paralleled and wrapped by small paper sheets, and the fabrics to be measured are sterilized for standby use under the same condition. Inoculating the bacterial liquid, placing on a constant temperature oscillator, and oscillating at 24 ℃ and 150r/min for 18 h. The sample was diluted with 0.03mol/LPBS buffer (sterilized) to an appropriate dilution. Pipette 1mL of the diluted test solution into a sterile plate and pour approximately 15mL of nutrient agar medium. Three plates were made each for parallel sampling. The plate was inverted and incubated at 37 ℃ for 48 h. And (6) counting colonies.
Bacteriostatic rate (%) - (W-Q)/Wx100
Wherein, W and Q are the average values of the test of the reference sample and the fabric to be tested respectively.
Control sample W: the cotton standard interlining fabric specified in the standard GB/T20944.3-2008 is used as a control sample after being steamed 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 in the embodiment 2 by using a two-step method; in the embodiments 3-5, the antibacterial performance of the silver fiber fabric is further improved by adopting the functionalized chitosan solution; and in example 5, the functionalized chitosan solution prepared by coupling and compounding the functionalized reagents gallic acid and catechin is obviously higher than that of examples 3-4, so that the antibacterial performance is remarkably improved.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (10)
1. The preparation method of the green environment-friendly silver fiber fabric is characterized by comprising the following steps of:
y1 washing biomass raw material with water and drying; crushing the dried biomass raw material to obtain biomass powder;
y2 mixing the biomass powder with water, boiling; cooling to room temperature; centrifuging and filtering to obtain a biomass extracting solution;
y3, immersing the fiber fabric into a silver nitrate water solution; and slowly adding the biomass extracting solution for dipping, washing and drying.
2. The preparation method of the green environment-friendly silver fiber fabric as claimed in claim 1, characterized by comprising the following steps:
y1 washing biomass raw material with water and drying; crushing the dried biomass raw material by using a universal crusher, and sieving by using a 50-100-mesh sieve; then, crushing the biomass powder to 1500-fold 3500 meshes by using an ultrafine crusher to obtain biomass powder;
y2 mixing the biomass powder with water, wherein the mass ratio of the biomass powder to the water is (1-10): 100, respectively; stirring, heating to 50-80 deg.C, and soaking for 10-40 min; continuously heating to 100 deg.C, boiling for 5-20 min; cooling to 50-80 deg.C, and soaking for 10-40 min; cooling to room temperature and standing for 5-20 min; centrifuging and filtering to obtain a biomass extracting solution;
y3, 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 a biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1: (1-20); adjusting pH to 6-10 with sodium hydroxide solution; gradually heating to 50-90 deg.C, stirring, and soaking for 30-90 min; rinsing with water for 1-3 times, and drying at room temperature.
3. The preparation method of the green environment-friendly silver fiber fabric as claimed in claim 2, characterized by comprising the following steps:
y1 washing biomass raw material with water and drying; crushing the dried biomass raw material by using a universal crusher, and sieving by using a 50-100-mesh sieve; then, crushing the biomass powder to 1500-fold 3500 meshes by using an ultrafine crusher to obtain biomass powder;
y2 mixing the biomass powder with water, wherein the mass ratio of the biomass powder to the water is (1-10): 100, respectively; stirring, heating to 50-80 deg.C, and soaking for 10-40 min; continuously heating to 100 deg.C, boiling for 5-20 min; cooling to 50-80 deg.C, and soaking for 10-40 min; cooling to room temperature and standing for 5-20 min; centrifuging and filtering to obtain a biomass extracting solution;
y3, soaking 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) soaking for 10-48 h; taking out, curing at the temperature of 100-150 ℃ for 1-10min, and airing to obtain the pretreated fiber fabric;
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 a biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1: (1-20); adjusting pH to 6-10 with sodium hydroxide solution; gradually heating to 50-90 deg.C, stirring, and soaking for 30-90 min; rinsing with water for 1-3 times, and drying at room temperature.
4. The preparation method of the green environment-friendly silver fiber fabric as claimed in claim 3, characterized in that: the treatment fluid is one of chitosan solution, functionalized chitosan solution and glycine aqueous solution.
5. The preparation method of the green environment-friendly silver fiber fabric as claimed in claim 3, characterized by comprising the following steps:
y1 washing biomass raw material with water and drying; crushing the dried biomass raw material by using a universal crusher, and sieving by using a 50-100-mesh sieve; then, crushing the biomass powder to 1500-fold 3500 meshes by using an ultrafine crusher to obtain biomass powder;
y2 mixing the biomass powder with water, wherein the mass ratio of the biomass powder to the water is (1-10): 100, respectively; stirring, heating to 50-80 deg.C, and soaking for 10-40 min; continuously heating to 100 deg.C, boiling for 5-20 min; cooling to 50-80 deg.C, and soaking for 10-40 min; cooling to room temperature and standing for 5-20 min; centrifuging and filtering to obtain a biomass extracting solution;
y3, soaking the fiber fabric into the chitosan solution or the 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) soaking for 10-48 h; taking out, curing at 100-150 deg.C for 1-10min, and air drying;
y4, soaking 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) soaking for 10-48 h; taking out, curing at the temperature of 100-150 ℃ for 1-10min, and airing to obtain the pretreated fiber fabric;
y5, 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 a biomass extracting solution, wherein the mass ratio of the fiber fabric to the biomass extracting solution is 1: (1-20); adjusting pH to 6-10 with sodium hydroxide solution; gradually heating to 50-90 deg.C, stirring, and soaking for 30-90 min; rinsing with water for 1-3 times, and drying at room temperature.
6. The preparation method of the green environment-friendly silver fiber fabric as claimed in claim 4 or 5, wherein the preparation method of the chitosan solution is as follows: adding chitosan into 0.5-3.5 wt% acetic acid water solution with the mass ratio of chitosan to acetic acid water solution being (0.5-5):100, heating to 50-80 deg.C, and stirring for 0.5-5 h.
7. The preparation method of the green environment-friendly silver fiber fabric as claimed in claim 4 or 5, characterized in that: the concentration of the glycine aqueous solution is 0.5-3.5 wt%.
8. The preparation method of the green environment-friendly silver fiber fabric as claimed in any one of claims 1 to 5, 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.
9. The preparation method of the green environment-friendly silver fiber fabric as claimed in any one of claims 1 to 5, characterized in that: the biomass raw material is any one of dried leaves of aegle marmelos, dried leaves of mangoes and peanut shells.
10. The green environment-friendly silver fiber fabric is characterized in that: prepared by the method of any one of claims 1 to 9.
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