CN112426979B - Waste textile metal nanoparticle composite carbon fiber aerogel and preparation method thereof - Google Patents
Waste textile metal nanoparticle composite carbon fiber aerogel and preparation method thereof Download PDFInfo
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- CN112426979B CN112426979B CN202011271588.6A CN202011271588A CN112426979B CN 112426979 B CN112426979 B CN 112426979B CN 202011271588 A CN202011271588 A CN 202011271588A CN 112426979 B CN112426979 B CN 112426979B
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
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- H—ELECTRICITY
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- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
- H05K9/0083—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive non-fibrous particles embedded in an electrically insulating supporting structure, e.g. powder, flakes, whiskers
Abstract
The invention relates to a preparation method of metal nanoparticle composite carbon fiber aerogel, belonging to the technical field of materials. The preparation method of the waste textile metal nanoparticle composite carbon fiber aerogel comprises the following steps: a. cleaning, bleaching and crushing the waste textiles to obtain textile powder, wherein the size of the textile powder is 0.2-1 mm; b. mixing the textile powder and the metal nanoparticle precursor solution to obtain a mixed solution, treating the mixed solution by at least one of stirring, ultrasound and microwave to enhance metal ion adhesion, dewatering and drying to obtain waste spinning fiber aerogel; c. and calcining the waste spinning fiber aerogel to obtain the metal nanoparticle composite carbon fiber aerogel. High production efficiency, simple process, good repeatability and easy mass production, and solves the pollution problem caused by waste textiles.
Description
Technical Field
The invention relates to a preparation method of metal nanoparticle composite carbon fiber aerogel, belonging to the technical field of materials.
Background
The overall improvement in living standards has led to an increased demand for textile production and consumption, bringing about a large amount of industrial fiber waste and waste clothes with extremely fast renewal speed, producing a large amount of textile waste which is not properly disposed of. The recycling of the waste textiles can become a sustainable solution, the solid waste of the refuse landfill is reduced, the production and energy consumption of raw materials are reduced, less environmental pollution is generated, resources are saved, and the cost is reduced.
At present, the treatment of waste textiles mainly comprises a mechanical method, a thermal energy method, a chemical method and a mixture of the three methods. The mechanical method cannot be classified according to values in the recovery process, so that the added value is not high; the thermal energy method is used for thermal power generation by converting waste textiles into heat through a combustion mode, but the incineration efficiency is low, ash and toxic gas are generated, and the human body and the environment are harmed. The chemical method is a new method in recent years, can realize the recycling of high polymers and monomers, and can create high value-added products. The cellulose fiber is one of the most important textile raw materials, occupies a great share in waste textiles, and has great value potential in the aspect of researching high added value utilization of waste cellulose fabrics.
In the prior art, when the aerogel is prepared by using fibers, alkali treatment is required, for example, patent applications with publication numbers of CN108212089A and CN110983492A use sodium hydroxide to treat the fibers, CN111205506A using waste textile fibers also uses an alkali/urea dissolving system to prepare the aerogel, and in addition, crosslinking agents are required to be used for crosslinking, generally, the crosslinking agents are toxic, and in addition, the aerogel prepared by using the method needs to consume a large amount of time and increase the cost.
And the method for treating the waste textiles by adopting CN111205506A is used for preparing the cellulose aerogel from the waste textiles by utilizing an alkali/urea dissolving system, the heat resistance is poor, the high-temperature calcination at 600-1300 ℃ cannot be tolerated, and after the carbonization treatment at 300 ℃, the aerogel has extremely serious volume shrinkage, poor flexibility and non-conductivity and basically has no electromagnetic shielding performance and electric heating performance.
Disclosure of Invention
The first purpose of the invention is to provide a new method for recycling waste textiles.
In order to achieve the first object of the invention, the preparation method of the waste textile metal nanoparticle composite carbon fiber aerogel comprises the following steps:
a. cleaning, bleaching and crushing the waste textiles to obtain textile powder, wherein the size of the textile powder is 0.2-1 mm;
b. mixing the textile powder and the metal nanoparticle precursor solution to obtain a mixed solution, treating the mixed solution by at least one of stirring, ultrasound and microwave to enhance metal ion adhesion, dewatering and drying to obtain waste spinning fiber aerogel; the concentration of the metal nanoparticle precursor solution is preferably 0.1-1 g/L;
c. and calcining the waste spinning fiber aerogel to obtain the metal nanoparticle composite carbon fiber aerogel.
Step a, when the textile powder exceeds 1mm, the conditions of uneven thickness of the aerogel and uneven attachment of metal nano particles can occur; the particle size is less than 0.2mm, and the aerogel has poor flexibility and large brittleness.
In a specific embodiment, the cleaning in the step a is to perform ultrasonic treatment on the waste textiles in an organic solvent, remove impurities and dry the waste textiles; the organic solvent is preferably at least one of acetone and ethanol, and more preferably the volume ratio of the acetone to the ethanol is 1-3: 1;
and a, the ultrasonic treatment time in the step a is 20-35 min.
In one embodiment, the dewatering and drying in step b is: filtering, molding, washing with at least one of ethanol or dimethylformamide, and drying.
In a specific embodiment, the drying in the step b is at least one of freeze drying, supercritical drying and drying; for example, the drying can be carried out in an oven at 50-80 ℃ for 4-6 h.
In one embodiment, the time for treating the mixed solution in the step b is 1 to 2 hours.
In a specific embodiment, the temperature of the calcination in the step c is 600-1300 ℃; preferably, the calcination is: in N2Or in Ar atmosphere, heating to 600-1300 ℃ at the heating rate of 2-5 ℃/min, and keeping for 2-3 h.
In one embodiment, the metal is at least one of silver, copper, nickel, iron, cobalt, potassium, nickel-cobalt alloy, iron-cobalt alloy;
preferably, the metal nanoparticle precursor solution is at least one of silver nitrate, cobalt nitrate, ferric nitrate, nickel nitrate, copper nitrate, potassium hydroxide, nickel cobaltate and cobalt ferrite.
In one embodiment, the bleaching agent used in the bleaching is at least one of sodium chlorite, sodium hypochlorite or hydrogen peroxide; preferably, the bleaching system used is sodium chlorite; more preferably, the method of bleaching comprises: soaking the waste textiles in 3-12 wt% sodium chlorite solution, adjusting the pH value to 4-4.5 by using glacial acetic acid, and treating for 4-16 h at 70-80 ℃; preferably, the mass ratio of the sodium chlorite dosage to the waste textiles is 3-6: 1.
In a specific embodiment, the waste textile is at least one of natural cellulose fiber, cellulose fiber and synthetic fiber blended textile fabric; preferably, the waste textile is at least one of cotton, hemp, bamboo, polyester-cotton blended fabric, polyester-hemp or polyester-bamboo.
The invention aims to achieve a second purpose and provides a waste textile metal nanoparticle composite carbon fiber aerogel.
In order to achieve the second purpose of the invention, the waste textile metal nanoparticle composite carbon fiber aerogel is prepared by the method;
preferably, the density of the waste textile metal nanoparticle composite carbon fiber aerogel is 28-100 mg/cm3；
More preferably, the electromagnetic shielding value of the waste textile metal nanoparticle composite carbon fiber aerogel is 20-50 dB.
Has the advantages that:
the carbon fiber aerogel prepared by taking the waste cellulose fabric as the raw material can effectively avoid the problems of large use and environment in the process of preparing the cellulose aerogel by a dissolving/regenerating method, and has the advantages of high mechanical property, good chemical stability, excellent conductivity, low price, easy acquisition, no harm to human bodies and the like. The introduction of the metal nanoparticles can enhance the interaction with electromagnetic waves and effectively attenuate the electromagnetic waves, and the preparation report of the waste textile and metal nanoparticle composite carbon fiber aerogel is not seen at present. The invention creatively explores the advantages of the whole process flow for preparing the composite carbon fiber aerogel with good performance from the waste textiles:
1) the method for preparing the metal nanoparticle composite carbon fiber aerogel from the waste textiles has the characteristics of high production efficiency, simple and convenient process, good repeatability and easiness in batch production, and solves the problem of pollution caused by the waste textiles.
2) The metal nanoparticle composite carbon fiber aerogel prepared by the invention is light and high in conductivity, and the square resistance of the metal nanoparticle composite carbon fiber aerogel is reduced to 4-15 times that of a pure carbon fiber aerogel.
3) The metal nanoparticle composite carbon fiber aerogel prepared by the invention has the total electromagnetic shielding efficiency of 20-50 dB, reaches the commercial and even military standards, and can be widely applied to high-valued fields such as commercial, high-end information technology, national defense safety technology and the like.
4) The invention does not need alkali to treat the waste fiber, does not need a cross-linking agent and has low cost.
Drawings
Fig. 1 is a flow chart of a preparation method of the waste textile metal nanoparticle composite carbon fiber aerogel in example 2 of the present invention.
Fig. 2 is a schematic diagram of an embodiment of the waste textile metal nanoparticle composite carbon fiber aerogel in example 2 of the present invention.
Fig. 3 is a scanning electron microscope image of the waste textile metal nanoparticle composite carbon fiber aerogel in example 2 of the present invention.
Fig. 4 is a graph of electromagnetic shielding performance of the waste textile metal nanoparticle composite aerogel in example 2 of the present invention.
Detailed Description
In order to achieve the first object of the invention, the preparation method of the waste textile metal nanoparticle composite carbon fiber aerogel comprises the following steps:
a. cleaning, bleaching and crushing the waste textiles to obtain textile powder, wherein the size of the textile powder is 0.2-1 mm;
b. mixing the textile powder and the metal nanoparticle precursor solution to obtain a mixed solution, treating the mixed solution by at least one of stirring, ultrasound and microwave to enhance metal ion adhesion, dewatering and drying to obtain waste spinning fiber aerogel; the concentration of the metal nanoparticle precursor solution is preferably 0.1-1 g/L;
c. and calcining the waste spinning fiber aerogel to obtain the metal nanoparticle composite carbon fiber aerogel.
The pulverization in step a can adopt a conventional pulverization machine, such as a household crusher or a grinder.
In a specific embodiment, the cleaning in the step a is to perform ultrasonic treatment on the waste textiles in an organic solvent, remove impurities and dry the waste textiles; the organic solvent is preferably at least one of acetone and ethanol, and more preferably the volume ratio of the acetone to the ethanol is 1-3: 1;
and a, the ultrasonic treatment time in the step a is 20-35 min.
In one embodiment, the dewatering and drying in step b is: filtering, shaping, washing with ethanol to replace water, and drying.
In a specific embodiment, the drying in the step b is at least one of freeze drying, supercritical drying and oven drying; for example, the drying can be carried out in an oven at 50-80 ℃ for 4-6 h.
In one embodiment, the time for treating the mixed solution in the step b is 1 to 2 hours.
In a specific embodiment, the temperature of the calcination in the step c is 600-1300 ℃; preferably, the calcination is: in N2Or in Ar atmosphere, heating to 600-1300 ℃ at the heating rate of 2-5 ℃/min, and keeping for 2-3 h.
In one embodiment, the metal is at least one of silver, copper, nickel, iron, cobalt, potassium, nickel-cobalt alloy, iron-cobalt alloy;
preferably, the metal nanoparticle precursor solution is at least one of silver nitrate, cobalt nitrate, ferric nitrate, nickel nitrate, copper nitrate, potassium hydroxide, nickel cobaltate and cobalt ferrite.
In one embodiment, the bleaching agent used in the bleaching is at least one of sodium chlorite, sodium hypochlorite or hydrogen peroxide; preferably, the bleaching system used is sodium chlorite; more preferably, the method of bleaching comprises: soaking the waste textiles in 3-12 wt% sodium chlorite solution, adjusting the pH value to 4-4.5 by using glacial acetic acid, and treating for 4-16 h at 70-80 ℃; preferably, the mass ratio of the sodium chlorite dosage to the waste textiles is 3-6: 1.
In a specific embodiment, the waste textile is at least one of natural cellulose fiber, cellulose fiber and synthetic fiber blended textile fabric; preferably, the waste textile is at least one of cotton, hemp, bamboo, polyester-cotton blended fabric, polyester-hemp or polyester-bamboo.
In order to achieve the second purpose of the invention, the waste textile metal nanoparticle composite carbon fiber aerogel is prepared by the method;
preferably, the density of the waste textile metal nanoparticle composite carbon fiber aerogel is 28-100 mg/cm3；
More preferably, the electromagnetic shielding value of the waste textile metal nanoparticle composite carbon fiber aerogel is 20-50 dB.
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the scope of the present invention.
Example 1
Ultrasonic cleaning waste cotton cloth with size of 5cm × 5cm with acetone and ethanol for 20min, and oven drying. Preparing a sodium chlorite solution by 6 wt%, completely soaking small pieces of cut waste cotton in the sodium chlorite solution, dropwise adding glacial acetic acid, adjusting the pH value to be 4.5, sealing a container, and treating for 12 hours in a warm water bath at 80 ℃. The mass ratio of the sodium chlorite dosage to the waste spinning is 5: 1, cleaning, drying and crushing for later use. Adding cobalt acetate and nickel acetate into deionized water according to a molar ratio of 1:1, stirring for 120min, performing ultrasonic treatment for 120min, placing the solution in a reaction kettle at 160 ℃ for 24h, performing suction filtration, and drying to obtain the nickel cobaltate powder. Weighing 1g of cotton powder, adding the cotton powder into 50ml of deionized water, adding 40mg of nickel cobaltate powder into the water, mechanically stirring the mixture on a magnetic stirrer for 2 hours, pouring the suspension into a 60ml Buchner funnel, carrying out vacuum filtration molding, replacing the water with ethanol, and drying the mixture in an oven at 60 ℃ to obtain the fiber aerogel. The sample was carbonized in N by moving it to a muffle furnace2In the atmosphere, the temperature rising rate is 2 ℃/min, the carbonization temperature is 1000 ℃, and the carbonization time is 2h, so that the nickel-cobalt alloy composite carbon fiber aerogel is obtained.
The performance of the metal composite carbon fiber aerogel obtained in example 1 is as follows:
average total efficiency of electromagnetic shielding is 33.88dB
The density of the metal nanoparticle composite carbon fiber aerogel is 86mg/cm3
Conductivity 3.4 omega/sq
The temperature of the aerogel at 4V was 43.6 ℃.
Example 2
And (3) ultrasonically cleaning the waste linen with the size of 5cm multiplied by 5cm for 40min by using acetone and ethanol respectively, and drying. Preparing a sodium hypochlorite solution with the concentration of 2g/L, completely soaking the small pieces of the cut waste ramie in the sodium hypochlorite solution, and piling for 2 hours. The mass ratio of the sodium hypochlorite dosage to the waste spinning is 1: and 5, cleaning, drying and crushing for later use. Weighing 1g of hemp, adding the hemp into 50ml of deionized water, adding 50mg of nickel nitrate, placing the mixture in a household microwave oven for 2h, pouring the suspension into a 60ml Buchner funnel, replacing water with ethanol, performing vacuum filtration molding, placing the mixture in supercritical carbon dioxide, uniformly discharging gas for 8h, and drying the mixture to form the fiber aerogel, wherein the supercritical carbon dioxide state is 60 ℃ and 10 MPa. And (3) moving the obtained sample to a muffle furnace for carbonization, and obtaining the nickel nanoparticle composite carbon fiber aerogel in the Ar atmosphere at the temperature rise rate of 4 ℃/min, the carbonization temperature of 800 ℃ and the carbonization time of 2 h.
The performance of the metal composite carbon fiber aerogel obtained in example 2 is as follows:
average total efficiency of electromagnetic shielding is 41.28dB
The density of the metal nanoparticle composite carbon fiber aerogel is 94mg/cm3
Conductivity 1.77 omega/sq
The aerogel was stabilized at 56.4 ℃ at 3V.
The preparation method of the aerogel has the advantages of simple preparation process and good chemical stability, and the obtained aerogel has multiple performances, can be used as a conductive and electromagnetic shielding material, and has wide application prospect.
Claims (16)
1. The preparation method of the waste textile metal nanoparticle composite carbon fiber aerogel is characterized by comprising the following steps of:
a. cleaning, bleaching and crushing the waste textiles to obtain textile powder, wherein the size of the textile powder is 0.2-1 mm;
b. mixing the textile powder and the metal nanoparticle precursor solution to obtain a mixed solution, treating the mixed solution by at least one of stirring, ultrasound and microwave to enhance metal ion adhesion, dewatering and drying to obtain waste spinning fiber aerogel; the concentration of the metal nanoparticle precursor solution is 0.1-1 g/L;
c. calcining the waste spinning fiber aerogel to obtain metal nanoparticle composite carbon fiber aerogel;
and b, treating the mixed solution for 1-2 hours.
2. The method for preparing the waste textile metal nanoparticle composite carbon fiber aerogel according to claim 1, wherein the cleaning in the step a is ultrasonic treatment of the waste textile in an organic solvent, impurity removal and drying;
and a, the ultrasonic treatment time in the step a is 20-35 min.
3. The method for preparing the waste textile metal nanoparticle composite carbon fiber aerogel according to claim 2, wherein the organic solvent is at least one of acetone and ethanol.
4. The preparation method of the waste textile metal nanoparticle composite carbon fiber aerogel according to claim 2, wherein the volume ratio of the organic solvent acetone to ethanol is 1-3: 1.
5. The method for preparing the waste textile metal nanoparticle composite carbon fiber aerogel according to claim 1, wherein the water removal and drying in the step b comprises the following steps: filtering, molding, washing with at least one of ethanol or dimethylformamide, and drying.
6. The preparation method of the waste textile metal nanoparticle composite carbon fiber aerogel according to any one of claims 1 to 3, wherein the drying in the step b is at least one of freeze drying, supercritical drying and oven drying.
7. The preparation method of the waste textile metal nanoparticle composite carbon fiber aerogel according to any one of claims 1 to 3, wherein the calcining temperature in the step c is 600-1300 ℃.
8. The method for preparing the waste textile metal nanoparticle composite carbon fiber aerogel according to claim 7, wherein the calcining in the step c is: in N2Or in Ar atmosphere, heating to 600-1300 ℃ at the heating rate of 2-5 ℃/min, and keeping for 2-3 h.
9. The preparation method of the waste textile metal nanoparticle composite carbon fiber aerogel according to any one of claims 1 to 3, wherein the metal is at least one of silver, copper, nickel, iron, cobalt, potassium, nickel-cobalt alloy and iron-cobalt alloy.
10. The preparation method of the waste textile metal nanoparticle composite carbon fiber aerogel according to claim 9, wherein the metal nanoparticle precursor solution is at least one of silver nitrate, cobalt nitrate, ferric nitrate, nickel nitrate, copper nitrate, potassium hydroxide, nickel cobaltate and cobalt ferrite.
11. The preparation method of the waste textile metal nanoparticle composite carbon fiber aerogel according to any one of claims 1 to 3, wherein a bleaching agent used for bleaching is at least one of sodium chlorite, sodium hypochlorite or hydrogen peroxide.
12. The method for preparing the waste textile metal nanoparticle composite carbon fiber aerogel according to claim 11, wherein the bleaching method comprises the following steps: soaking the waste textiles in 3-12 wt% sodium chlorite solution, adjusting the pH value to 4-4.5 by using glacial acetic acid, and treating for 4-16 h at 70-80 ℃.
13. The preparation method of the waste textile metal nanoparticle composite carbon fiber aerogel according to claim 12, wherein the mass ratio of the sodium chlorite to the waste textile is 3-6: 1.
14. The preparation method of the waste textile metal nanoparticle composite carbon fiber aerogel according to any one of claims 1 to 3, wherein the waste textile is at least one of natural cellulose fibers, cellulose fibers and synthetic fiber blended textile fabrics.
15. The preparation method of the waste textile metal nanoparticle composite carbon fiber aerogel according to claim 14, wherein the waste textile is at least one of cotton, hemp, bamboo, polyester-cotton blended fabric, polyester-hemp or polyester-bamboo.
16. The waste textile metal nanoparticle composite carbon fiber aerogel is characterized by being prepared by the method of any one of claims 1 to 15;
the density of the waste textile metal nanoparticle composite carbon fiber aerogel is 28-100 mg/cm3；
The electromagnetic shielding value of the waste textile metal nanoparticle composite carbon fiber aerogel is 20-50 dB.
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| CN114988904A (en) * | 2022-05-19 | 2022-09-02 | 中国科学院金属研究所 | Preparation method for realizing ultralow-density and ultralow-heat-conductivity carbon aerogel composite material through surface functionalization of cotton fibers |
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Address after: 610065, No. 24, south section of first ring road, Chengdu, Sichuan, Wuhou District Patentee after: SICHUAN University Patentee after: Sichuan Yingu Zhilian Environmental Protection Technology Co., Ltd Address before: 610065, No. 24, south section of first ring road, Chengdu, Sichuan, Wuhou District Patentee before: SICHUAN University Patentee before: Sichuan Yingu Zhilian Environmental Protection Technology Co., Ltd |