CN108359124B - Preparation method of waste textile bismuth tungstate composite aerogel - Google Patents
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Abstract
The invention belongs to the field of recycling of waste textiles, and particularly relates to a method for preparing a waste textile bismuth tungstate composite aerogel with photocatalytic degradation performance. The invention provides a preparation method of waste textile bismuth tungstate composite aerogel, which comprises the steps of extracting nano-cellulose by using an acidolysis method, preparing a cellulose solvent system from bismuth tungstate dispersion, dissolving the nano-cellulose in the cellulose solvent system, adding a proper amount of cross-linking agent to obtain hydrogel, and drying to prepare the aerogel. The preparation method of the waste textile bismuth tungstate composite aerogel can provide a new way for solving the problem of recycling of solid wastes, and the prepared aerogel has excellent photocatalytic degradation performance and can be applied to the fields of environmental protection and the like.
Description
Technical Field
The invention belongs to the field of recycling of waste textiles, and particularly relates to a preparation method of a waste textile bismuth tungstate composite aerogel.
Background
China has nearly 14 hundred million population, the application of textiles covers the aspects of production and life of people, and correspondingly, a large amount of waste textile materials are generated. At present, environmental protection and green development are advocated all over the world, and research on recycling of waste textiles has huge value potential in the aspects of chemical economy sustainable development and high added value utilization of solid wastes. At the present time when energy and resources are increasingly tense, the recycling of solid wastes is slow.
At present, three methods, namely a physical method, an energy method and a chemical method, are mainly used for treating waste textiles. However, the above methods all have some disadvantages, the physical method is difficult to classify the blend fiber, the applicability is poor, the recovery technical requirement is high, the cost is high, and the process is complex; the energy method is to burn the fabric to obtain energy, however, the burning method has high investment cost and low resource utilization rate and can cause air pollution. And cellulose fibers are one of the most important textile materials. Especially as an important natural fiber material in the modern textile industry. Cellulose fibers represent a large share in the field of clothing materials for human use. Therefore, the recovery of the waste cellulose fiber has important research and development values.
Aerogel is a special gel, which is a product obtained by drying hydrogel or organogel without changing the three-dimensional network structure of aerogel itself and replacing the liquid in hydrogel with gas, has high porosity and large specific surface area, and is the solid material with minimum density accepted in the world at present. The cellulose aerogel prepared by taking cellulose as a raw material not only has the characteristic of good toughness, but also is easy to process and form; compared with the traditional carbon aerogel, the compression resilience performance of the carbon aerogel is very excellent; is a high-performance adsorption material and is expected to provide a new solution for frequent offshore oil pollution disasters and sewage treatment in recent years. Bismuth tungstate is a material with photocatalytic activity under visible light irradiation, and the preparation process is mature and simple and is widely concerned. The invention creatively explores the whole process flow from extracting the nanocellulose from the waste textiles to preparing the composite aerogel with good performance. Dissolving waste textiles by using a reagent, extracting nanocellulose, preparing a cellulose solvent system in bismuth tungstate dispersion liquid, adding cellulose into the system for crosslinking, and finally drying to obtain the aerogel.
Disclosure of Invention
The invention aims to provide a preparation process method of a waste textile bismuth tungstate composite aerogel, which can effectively recycle waste textiles and prepare the composite aerogel with photocatalytic performance.
The experimental scheme of the invention is as follows:
the invention provides a preparation method of waste textile bismuth tungstate composite aerogel, which comprises the steps of crushing waste textiles, treating the crushed waste textiles with a reagent, stirring, preserving heat, centrifuging and dialyzing to obtain nanocellulose, preparing a cellulose solvent in bismuth tungstate dispersion liquid, uniformly stirring the extracted cellulose in the system, dissolving at a low temperature, adding a cross-linking agent, forming hydrogel under heating, and finally drying to obtain the composite aerogel.
The waste textile is at least one of natural 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 reagent is at least one of sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid and ammonium persulfate.
Preferably, the acid is sulfuric acid or ammonium persulfate.
The system is at least one of sodium hydroxide, potassium hydroxide, sodium hydroxide/urea and sodium hydroxide/thiourea.
Preferably, the system is sodium hydroxide/urea or sodium hydroxide/thiourea.
The cross-linking agent is at least one of epichlorohydrin, pentanediol, sodium alginate, glutaraldehyde, divinylalum and polyethylene glycol glycidyl ether.
Preferably, the epoxy chloropropane is used.
The preparation method of the waste textile bismuth tungstate composite aerogel comprises the following steps:
1) carrying out ultrasonic treatment on the fabric by adopting an organic solvent, removing impurities, drying, and crushing, wherein the organic solvent is acetone and ethanol, and the volume ratio of the acetone to the ethanol is 1-3: 1, carrying out ultrasonic treatment for 20-35 min;
2) preparing a certain reagent solution, soaking the waste textile in the reagent solution, and fully stirring until the waste textile is dissolved;
3) placing the sample obtained in the step 2) in a constant-temperature water bath or an ultrasonic cleaner, and stirring for 1-16 h at 40-60 ℃;
4) centrifuging and dialyzing the sample obtained in the step 3) by using deionized water, repeating the process until the filtrate is neutral, drying, and collecting the prepared nano cellulose sample;
5) adding bismuth nitrate and sodium tungstate into deionized water at a molar ratio of 1: 1-4: 1, wherein the concentration is 1-4 mol/L, stirring for 30-120 min, performing ultrasonic treatment for 30-120 min, placing the solution in a reaction kettle at a temperature of 120-200 ℃ for 1-24 h, performing suction filtration, and drying to obtain bismuth tungstate powder. The dosage of the bismuth tungstate is 2 to 15 percent according to the mass ratio of the bismuth tungstate to the nano-cellulose.
6) Dispersing the sample obtained in the step 5) in deionized water, stirring at room temperature, performing ultrasonic treatment, adding alkali and urea or thiourea to prepare a solvent system, freezing for 12-24 h, thawing at room temperature, dropwise adding a cross-linking agent, stirring for 1-3 h, and standing in a constant-temperature water bath or an ultrasonic cleaner at 45-55 ℃ for 10-24h to obtain a hydrogel sample;
7) washing the sample obtained in the step 6) with deionized water until the pH value is neutral, and drying to obtain the composite aerogel.
Preferably, in the step 2), the specific implementation method is as follows: the concentration of the reagent sulfuric acid is 55-64%, the concentration of ammonium persulfate is 1-3 mol/L, fabric fragments are added, the solid-to-liquid ratio is 8: 1-20: 1, and stirring is carried out for 5-20 min.
In the step 6), the ratio of the prepared sodium hydroxide, urea, nano-cellulose, deionized water, cross-linking agent and bismuth tungstate is 3:2:1:45: 4-5: 0.02 to 0.15; the dosage ratio of the prepared sodium hydroxide, thiourea, nano-cellulose, deionized water, cross-linking agent and bismuth tungstate is as follows: 9.5:4.5: 2-5: 85: 8-10: 0.02 to 0.15;
in step 6), the method comprises the following steps: pre-freezing for 6-10 h at-20 to-50 ℃, and freeze-drying for 24-48 h under the air pressure of 1-20 Pa; or drying by using supercritical carbon dioxide, firstly soaking the hydrogel in acetone for 24-96 hours to prepare ketone gel, then placing the ketone gel in liquid carbon dioxide for 4-12 hours, and then uniformly deflating to obtain the dried composite aerogel, wherein the state of the supercritical carbon dioxide is 40-80 ℃ and 9-20 MPa.
The invention has the beneficial effects that:
the composite aerogel prepared from the waste textiles has the characteristics of high production efficiency, simple and convenient process, good repeatability and easiness in batch production, and the obtained aerogel has excellent photocatalytic performance and can be widely applied to the fields of environmental protection and the like.
Drawings
FIG. 1 is a physical diagram of a waste textile bismuth tungstate composite aerogel positive electrode prepared in example 1;
FIG. 2 is an absorbance change curve of methylene blue solution respectively immersed in methylene blue, cellulose aerogel and composite aerogel under the irradiation of xenon lamps at different times, and the internal small graph is a graph of different photocatalytic effects.
Detailed Description
The present invention is described in detail below by way of examples, it should be noted that the examples are only for the purpose of further illustration of the present invention and should not be construed as limiting the scope of the present invention, and that those skilled in the art may make insubstantial modifications and adaptations to the present invention.
Example 1
Ultrasonic cleaning waste cotton cloth with size of 5cm × 5cm with acetone and ethanol for 20min, oven drying, and pulverizing. Weighing 3g of cotton, adding the cotton into 24ml of 64% sulfuric acid solution, stirring for 5min, dissolving, placing in a constant-temperature water bath kettle, mechanically stirring at 50 ℃ for 1h, centrifuging with deionized water, dialyzing, repeating for three times until the filtrate is neutral, and drying to obtain the nano-cellulose. Adding bismuth nitrate and sodium tungstate into deionized water at a molar ratio of 2:1, stirring for 30min, performing ultrasonic treatment for 30min, placing the solution in a reaction kettle at 180 ℃ for 24h, performing suction filtration, and drying to obtain bismuth tungstate powder. Weighing 0.2g of bismuth tungstate powder, adding the powder into 90ml of water, stirring for 30min, performing ultrasonic treatment for 30min to obtain a bismuth tungstate dispersion, adding 6g of sodium hydroxide and 4g of urea to dissolve the bismuth tungstate dispersion, adding 2g of the prepared cellulose sample into the bismuth tungstate dispersion, uniformly stirring, and freezing in a refrigerator for 12 h. Unfreezing at room temperature, dropwise adding 9ml of epoxy chloropropane, magnetically stirring for 1h, and placing the whole sample in a constant-temperature water bath kettle at 50 ℃ for 20h to obtain a hydrogel sample. And (3) washing the hydrogel sample with deionized water until the solution is neutral, pre-freezing for 6h at-50 ℃, and then freeze-drying for 48h under the air pressure of 20Pa to obtain the composite aerogel sample. See fig. 1.
The effect of the composite aerogel on degrading methylene blue is tested, and the test method comprises the following steps: immersing the composite aerogel in 10mg/L methylene blue solution, placing the solution in a lightproof box, carrying out xenon lamp irradiation for every 20min, and testing the absorbance of the solution by using a visible spectrophotometer, wherein the wavelength is set to 664 nm. Then returning to the box to continue the irradiation for 240 min. Meanwhile, the pure methylene blue solution with the same concentration and the methylene blue solution soaked with the pure cellulose aerogel are used as control tests to be tested, and the test results are shown in figure 2.
Example 2
And (3) ultrasonically cleaning waste linen with the size of 5cm multiplied by 5cm for 30min by using acetone and ethanol respectively, drying and crushing for later use. Weighing 3g of linen, adding the linen into 60ml of 1mol/L ammonium persulfate solution, stirring for 15min, dissolving, placing in a constant-temperature water bath, mechanically stirring for 2h at the temperature of 60 ℃, centrifuging with deionized water, dialyzing, repeating for three times until the filtrate is neutral, and vacuum drying to obtain the nano-cellulose. Adding bismuth nitrate and sodium tungstate into deionized water at a molar ratio of 1:1, stirring for 45min with bismuth nitrate concentration of 4mol/L, performing ultrasonic treatment for 60min, placing the solution in a reaction kettle at 200 ℃ for 12h, performing suction filtration, and drying to obtain bismuth tungstate powder. Weighing 0.1g of bismuth tungstate powder, adding the powder into 85ml of water, stirring for 40min, performing ultrasonic treatment for 40min to obtain a bismuth tungstate dispersion, adding 9.5g of sodium hydroxide and 4.5g of urea to dissolve the bismuth tungstate dispersion, adding 3g of prepared cellulose sample into the bismuth tungstate dispersion, uniformly stirring, and freezing in a refrigerator for 6 h. Unfreezing at room temperature, dropwise adding 10ml of epoxy chloropropane, magnetically stirring for 2h, and placing the whole sample in a constant-temperature water bath kettle at 55 ℃ for 10h to obtain a hydrogel sample. And (3) washing the hydrogel sample with deionized water until the solution is neutral, soaking the hydrogel sample in an acetone solution for 2d to obtain ketone gel, placing the obtained ketone gel in supercritical carbon dioxide for 6h, and uniformly deflating to obtain a composite aerogel sample, wherein the supercritical carbon dioxide state is 60 ℃ and 10 MPa.
The preparation method has the advantages of simple preparation process, good chemical stability, good adsorption performance and photocatalytic degradation performance, and wide application prospect in environmental management.
Claims (7)
1. A preparation method of waste textile bismuth tungstate composite aerogel is characterized in that waste textiles are crushed, treated by a reagent, stirred, kept warm, centrifuged and dialyzed to obtain nanocellulose, a cellulose solvent system is prepared in bismuth tungstate dispersion liquid, the extracted cellulose is added into the system and stirred uniformly, dissolved at low temperature, added with a cross-linking agent, formed into hydrogel under heating conditions, and finally dried to obtain the composite aerogel;
the method comprises the following steps:
1) carrying out ultrasonic treatment on the fabric by adopting an organic solvent, removing impurities, drying, and crushing, wherein the organic solvent is acetone and ethanol, and the volume ratio of the acetone to the ethanol is 1-3: 1, carrying out ultrasonic treatment for 20-35 min;
2) preparing a reagent solution, soaking the waste textiles in the reagent solution, and fully stirring the waste textiles until the waste textiles are dissolved, wherein the reagent is sulfuric acid or ammonium persulfate; in the step 2), adding waste textiles into a solution-solid ratio of 8: 1-20: 1, wherein the concentration of the reagent sulfuric acid is 55-64% and the concentration of ammonium persulfate is 1-3 mol/L, and stirring for 5-20 min;
3) placing the sample obtained in the step 2) in a constant-temperature water bath or an ultrasonic cleaner, and mechanically stirring for 1-16 h at 40-60 ℃;
4) centrifuging and dialyzing the sample obtained in the step 3) by using deionized water, repeating the process until the filtrate is neutral, drying, and collecting the prepared nano cellulose sample;
5) dispersing the prepared bismuth tungstate in an aqueous solution, stirring and ultrasonically treating, and adding alkali and urea or thiourea to prepare a cellulose solvent system; the system is sodium hydroxide/urea or sodium hydroxide/thiourea;
6) dispersing the sample obtained in the step 4) in the system solution obtained in the step 5), stirring at room temperature, freezing for 12-24 h, thawing at room temperature, dropwise adding a cross-linking agent, stirring for 1-3 h, and standing in a constant-temperature water bath or an ultrasonic cleaner at 45-55 ℃ for 10-24h to obtain a hydrogel sample; in the step 6), the dosage ratio of sodium hydroxide, urea, nano-cellulose, deionized water, a crosslinking agent and bismuth tungstate in the prepared solvent system is 3:2:1:45 (4-5) or 0.02-0.15, or the dosage ratio of sodium hydroxide, thiourea, nano-cellulose, deionized water, the crosslinking agent and bismuth tungstate is: 9.5:4.5 (2-5) 85 (8-10) 0.02-0.15;
7) washing the sample obtained in the step 6) with deionized water until the pH value is neutral, and drying to obtain the composite aerogel.
2. The preparation method of the waste textile bismuth tungstate composite aerogel according to claim 1, wherein the waste textile is at least one of natural cellulose fibers and cellulose fiber and synthetic fiber blended textile fabrics.
3. The preparation method of the waste textile bismuth tungstate composite aerogel according to claim 1, wherein the waste textile is at least one of cotton, hemp, bamboo, polyester-cotton blended fabric, polyester-hemp or polyester-bamboo.
4. The preparation method of the waste textile bismuth tungstate composite aerogel according to claim 1, wherein the cross-linking agent is at least one of epichlorohydrin, pentanediol, sodium alginate, glutaraldehyde, divinylalum and polyethylene glycol glycidyl ether.
5. The preparation method of the waste textile bismuth tungstate composite aerogel as claimed in claim 1, wherein the cross-linking agent is epichlorohydrin.
6. The preparation method of the waste textile bismuth tungstate composite aerogel according to claim 1, which is characterized by comprising the following steps of: the preparation of the bismuth tungstate in the step 5) is specifically operated as follows: adding bismuth nitrate and sodium tungstate into deionized water according to a molar ratio of 1: 1-4: 1, wherein the concentration is 1-4 mol/L, stirring for 30-120 min, performing ultrasonic treatment for 30-120 min, placing the solution into a reaction kettle at a temperature of 120-200 ℃ for 1-24 h, performing suction filtration, and drying to obtain bismuth tungstate powder.
7. The preparation method of the waste textile bismuth tungstate composite aerogel according to claim 1, which is characterized by comprising the following steps of: in the step 7), pre-freezing for 6-10 h at-20 to-50 ℃, and freeze-drying for 24-48 h under the air pressure of 1-20 Pa; or drying by using supercritical carbon dioxide, firstly soaking the hydrogel in acetone for 24-96 h, continuously replacing the acetone to prepare ketone gel, then placing the ketone gel in the supercritical carbon dioxide for more than 4-12 h, and then uniformly deflating to obtain the dried aerogel, wherein the state of the supercritical carbon dioxide is 40-80 ℃ and 9-20 MPa.
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| CN109935757B (en) * | 2018-11-28 | 2021-09-07 | 万向一二三股份公司 | Preparation method of composite lithium ion battery diaphragm |
| CN110540187A (en) * | 2019-09-27 | 2019-12-06 | 天津工业大学 | preparation method of clay/carbon aerogel material |
| CN111205506B (en) * | 2020-03-20 | 2021-09-07 | 四川大学 | Preparation method of waste textile flame-retardant aerogel |
| CN112354561B (en) * | 2020-11-10 | 2022-06-14 | 四川大学 | Photocatalytic material based on stable loading of biomass porous base material and method and application thereof |
| CN115069218A (en) * | 2021-03-12 | 2022-09-20 | 四川大学 | Preparation method of metal organic framework composite GO/waste spinning cellulose aerogel |
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| CN102836745A (en) * | 2012-08-24 | 2012-12-26 | 东北林业大学 | Preparation method for photo-catalysis material with aerogel substrate |
| WO2017187152A1 (en) * | 2016-04-25 | 2017-11-02 | The University Of Sussex | Dry coating method for preparing photocatalytic particles |
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