CN115350723A - Waste cotton fabric superfine powder-TiO 2 Preparation method and application of composite photocatalytic material - Google Patents
Waste cotton fabric superfine powder-TiO 2 Preparation method and application of composite photocatalytic material Download PDFInfo
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- 229920000742 Cotton Polymers 0.000 title claims abstract description 102
- 239000004744 fabric Substances 0.000 title claims abstract description 102
- 239000002699 waste material Substances 0.000 title claims abstract description 95
- 229910010413 TiO 2 Inorganic materials 0.000 title claims abstract description 51
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 43
- 239000002131 composite material Substances 0.000 title claims abstract description 40
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
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- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
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- 239000012634 fragment Substances 0.000 claims 2
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- 239000007789 gas Substances 0.000 description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 4
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 4
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- 238000001878 scanning electron micrograph Methods 0.000 description 2
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
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Abstract
The invention provides waste cotton fabric ultrafine powder-TiO 2 The preparation method of the composite photocatalytic material comprises the steps of preparing waste cotton fabric into superfine powder, and respectively preparing the superfine powder and TiO 2 Dispersing nano particles in distilled water to obtain suspension, and mixing to obtain superfine TiO powder of waste cotton fabric 2 Mixing the solution, spraying the mixture on a foam net to prepare the waste cotton fabric ultrafine powder-TiO 2 The invention also discloses a composite photocatalytic material and the waste cotton fabric ultrafine powder-TiO 2 Degradation of composite photocatalytic materialThe application in formaldehyde; the waste cotton fabric is prepared into superfine powder to realize recycling of the waste cotton fabric, and the superfine powder of the waste cotton fabric can disperse TiO 2 Agglomeration of nanoparticles to TiO 2 The nano particles are uniformly dispersed, the photocatalysis effect of the composite material is improved, meanwhile, the waste cotton fabric ultrafine powder has larger adsorption and capture capacity to formaldehyde gas, and the formaldehyde and TiO are prolonged 2 Contact time of (2), synergistically enhancing the TiO 2 The degradation effect on formaldehyde.
Description
Technical Field
The invention relates to TiO 2 The technical field of photocatalysis, in particular to waste cotton fabric ultrafine powder-TiO 2 A preparation method and application of the composite photocatalytic material.
Background
Formaldehyde is a main pollutant in interior decoration, has a strong stimulation effect on skin mucosa, can induce bronchial asthma attack and allergic asthma attack, aggravation or acute attack of allergic dermatitis and the like, and is determined as a suspicious carcinogen by international cancer institutions. The existing common formaldehyde purification methods mainly comprise a green plant adsorption method, a ventilation method, an active carbon adsorption method and a light-contact reaction method, and the adsorption method only transfers formaldehyde but not degrades the formaldehyde and utilizes TiO 2 The photo-catalytic method is used for catalyzing and degrading formaldehyde, so that the method has a good application prospect.
But due to TiO 2 The nano particles are easy to agglomerate to influence the catalytic effect, and the independent TiO 2 The nano particles are not easy to be recycled and regenerated, so that the TiO capable of being uniformly dispersed is prepared 2 The nano particles can synergistically improve the catalytic effect of the photocatalyst, and the photocatalyst is of great significance in easy recovery and regeneration.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides waste cotton fabric ultrafine powder-TiO 2 Preparation method and application of composite photocatalytic material, and preparation methodSimple and easy operation, less working procedures, low energy consumption and easy industrial production, and the waste cotton fabrics are recycled to be made into waste cotton fabric ultrafine powder which is dispersed with TiO 2 Nanoparticles, reduction of TiO 2 The agglomeration effect of the nano particles increases the specific surface area of the material, and meanwhile, a large number of microporous structures on the surface of the ultrafine powder have capturing and adsorbing properties on formaldehyde, so that the photocatalytic effect of the material is synergistically enhanced.
The invention is realized by the following steps:
the invention provides waste cotton fabric ultrafine powder-TiO 2 The preparation method of the composite photocatalytic material comprises the following steps:
s1, crushing waste cotton fabrics into coarse fiber powder;
s2, freezing and grinding the coarse fiber powder in a liquid nitrogen environment to obtain waste cotton fabric ultrafine powder;
s3, dispersing a certain amount of waste cotton fabric ultrafine powder in distilled water, stirring to prepare a waste cotton fabric ultrafine powder suspension, and taking a certain amount of TiO 2 Dispersing nano particles in distilled water, stirring to prepare TiO 2 A nanoparticle suspension;
s4, preparing the waste cotton fabric superfine powder suspension prepared in the step S3 and TiO 2 Mixing the nano particle suspension according to a certain volume ratio, stirring, and carrying out ultrasonic treatment to obtain the waste cotton fabric ultrafine powder-TiO 2 Mixing the solution;
s5, spraying the adhesive on the front and back surfaces of the cleaned foam net, and then spraying the waste cotton fabric superfine powder-TiO prepared in the step S4 2 Placing the mixed solution at room temperature for a period of time, and drying to obtain the waste cotton fabric ultrafine powder-TiO 2 A composite photocatalytic material.
The method makes full use of the waste cotton fabrics, and utilizes the freeze grinding to prepare the waste cotton fabric ultrafine powder, the waste cotton fabric ultrafine powder and TiO 2 Fully and uniformly mixing nano particles, and dispersing TiO by using waste cotton fabric ultrafine powder 2 Nanoparticles, reduction of TiO 2 The agglomeration effect of the nano particles is that the nano particles are sprayed on a foam net to prepare the foam net with high specific surface areaMeanwhile, the waste cotton fabric ultrafine powder has a large number of microporous structures and strong adsorption capacity to formaldehyde, and can greatly strengthen the waste cotton fabric ultrafine powder-TiO 2 The photocatalytic degradation effect of the nano particle composite material.
Further, the step S1 comprises the steps of cutting the waste cotton fabrics into pieces of 10-20 cm multiplied by 10-20 cm, placing the pieces into a cutting and crushing machine with a screen mesh diameter of 2-5 mm for crushing for 3-5 min, and collecting fiber coarse powder after crushing.
Further, the step S2 comprises the steps of putting a certain amount of the fiber coarse powder prepared in the step S1 into a sample barrel of a freezing grinder, putting 6-10 zirconium oxide grinding balls with the grain diameter of 3-5 mm into the sample barrel, grinding for 3-5 min in a liquid nitrogen environment, and obtaining the waste cotton fabric superfine powder after grinding.
The liquid nitrogen freezing grinding only needs 3-5 min, the traditional dry grinding needs dozens of hours, and the wet ball milling needs 5-6 h, so that the production efficiency is improved.
Further, the specific surface area of the waste cotton fabric ultrafine powder is 80-120 m 2 (iii) a mean particle diameter of 1 to 3 μm.
Further, in the step S3, the concentration of the waste cotton fabric ultrafine powder in the waste cotton fabric ultrafine powder suspension is 1-3 mg/mL, and TiO is added 2 TiO in nanoparticle suspensions 2 The concentration is 10-30 mg/mL.
Further, in step S4, tiO 2 The volume ratio of the nano particle suspension to the waste cotton fabric ultrafine powder suspension is 1.5-1:2.
Further, in step S5, the material of the foam net is one of metal nickel, metal copper, or melamine.
Further, in step S5, waste cotton fabric ultrafine powder-TiO 2 The spraying volume of the mixed solution is 0.01-0.03 mL/cm 2 。
The invention also provides waste cotton fabric ultrafine powder-TiO prepared by the method 2 The application of the composite photocatalytic material in degrading formaldehyde.
Placing the composite photocatalytic material in a formaldehyde environment, irradiating for 30-60 min by using an ultraviolet lamp, determining the concentration of formaldehyde by using a Fourier infrared spectrometer, and comparing the concentrations of the formaldehyde before and after the comparison to calculate the degradation rate of the composite photocatalytic material to the formaldehyde; after the composite photocatalytic material is used for degrading formaldehyde, the composite photocatalytic material is placed in the air and irradiated by an ultraviolet lamp for 2 hours, and the composite photocatalytic material is regenerated, has catalytic activity again and can be used for multiple times.
The invention has the following beneficial effects:
1. the method takes the waste cotton fabrics as raw materials to prepare the superfine powder, realizes the recycling of the waste cotton fabrics, utilizes the liquid nitrogen grinding technology to prepare the superfine powder of the waste cotton fabrics, and has simple process and greatly shortened preparation time; the prepared waste cotton fabric superfine powder has small grain diameter, the average grain diameter is 1-3 mu m, the grain diameter is uniform, and the specific surface area is larger.
2. Prepared waste cotton fabric superfine powder dispersible TiO 2 Agglomeration of nanoparticles to TiO 2 The nano particles are uniformly dispersed, the photocatalysis effect of the composite material is improved, meanwhile, the waste cotton fabric ultrafine powder has larger adsorption and capture capacity to formaldehyde gas, and the formaldehyde gas and TiO are prolonged 2 The contact time of (2) increases the reaction concentration of the formaldehyde gas.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a sample diagram of ultrafine powder of waste cotton fabric provided in embodiment 1 of the present invention;
FIG. 2 is an SEM image of ultrafine powder of waste cotton fabric provided in embodiment 1 of the present invention;
FIG. 3 shows superfine TiO powder of waste cotton fabric provided in embodiment 1 of the present invention 2 Mixing the solution;
FIG. 4 is a waste provided in example 1 of the present inventionSuperfine powder-TiO of used cotton fabric 2 SEM image of nanoparticle mixture.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, it is obvious to those skilled in the art that other drawings can be obtained based on these drawings without creative efforts.
Example 1
Cutting waste cotton fabrics into pieces of 10-20 cm multiplied by 10-20 cm, putting the pieces into a cutting and crushing machine with a sieve mesh of 2mm, crushing for 3min, wherein the rotating speed of the cutting and crushing machine is 2500rpm, and taking out crushed fiber coarse powder from a collecting tank after crushing;
placing 2g of fiber coarse powder into a sample barrel of a freezing grinder, simultaneously placing 6 zirconia grinding balls with the particle size of 5mm into the sample barrel, grinding for 5min in a liquid nitrogen environment at the grinding frequency of 30Hz, and obtaining waste cotton fabric ultrafine powder after grinding (see figure 1);
scanning electron microscope test is carried out on the waste cotton fabric ultrafine powder (the result is shown in figure 2), as can be seen from figure 2, the waste cotton fabric ultrafine powder is in a spherical shape and is divided into steps after being frozen and ground, the particle size is about 2 mu m, the particle size distribution is relatively uniform, a large number of micropores exist on the surface of the powder, the specific surface area of the powder is increased by the micropores, the adsorption of formaldehyde gas is guaranteed, the loading of titanium dioxide nanoparticles is facilitated, the average particle size of the waste cotton fabric ultrafine powder is measured to be 2 mu m by a Malvern particle sizer, the average particle size is consistent with the SEM test result, and the average specific surface area of the waste cotton fabric ultrafine powder is measured to be 112m by a BET method 2 /g；
Weighing 0.2g of waste cotton fabric ultrafine powder, dispersing the waste cotton fabric ultrafine powder in 100mL of distilled water, and stirring (the rotating speed is controlled to be 600-800 rpm) for 15min to obtain a waste cotton fabric ultrafine powder suspension; weighing 2gTiO 2 Dispersing the nano particles in 100mL of distilled water, stirring (controlling the rotating speed to be 200 rpm) for 10min to obtain TiO 2 A nanoparticle suspension;
taking 10ml of TiO 2 Mixing the nanoparticle suspension with 10mL waste cotton fabric ultrafine powder suspension, stirring at 600rpm for 15min, and performing ultrasonic treatment for 30min to obtain waste cotton fabric ultrafine powder-TiO 2 Mixed solution (see fig. 3);
taking superfine powder-TiO 2 The nanoparticle mixture was subjected to scanning electron microscopy (see FIG. 4 for results), and from FIG. 4, tiO was determined 2 The nano particles are loaded on the surface of the ultrafine powder, the aggregation phenomenon of the nano particles does not occur, the ultrafine powder not only provides a large surface area for the nano particles, but also promotes the dispersion of the nano particles, and the agglomeration is reduced;
scrubbing a metal nickel foam net (30 cm multiplied by 50 cm) with methanol, naturally drying, spraying 3M adhesive spraying agent for 5s on the front and back surfaces respectively, and spraying 90mL of the prepared waste cotton fabric ultrafine powder-TiO on the front and back surfaces immediately 2 Drying the nano particle mixed solution for 2h at room temperature, and transferring the nano particle mixed solution into an oven for drying for 20h at the temperature of 60 ℃ to obtain waste cotton fabric ultrafine powder-TiO 2 A composite photocatalytic material.
Example 2
Cutting waste cotton fabrics into pieces of 10-20 cm multiplied by 10-20 cm, putting the pieces into a cutting crusher with a sieve mesh diameter of 5mm, crushing for 5min, wherein the rotating speed of the cutting crusher is 2500rpm, and taking out crushed fiber coarse powder from a collecting tank after crushing;
placing 2g of fiber coarse powder into a sample barrel of a freezing grinder, simultaneously placing 8 zirconia grinding balls with the grain diameter of 3mm into the sample barrel, grinding for 3min in a liquid nitrogen environment at the grinding frequency of 30Hz to obtain the waste cotton fabric ultrafine powder after grinding is finished, measuring the average grain diameter of the waste cotton fabric ultrafine powder to be 3 mu m by using a Malvern particle sizer, and measuring the average specific surface area of the waste cotton fabric ultrafine powder to be 118m by using a BET method 2 /g；
Weighing 0.3g of waste cotton fabric ultrafine powder, dispersing the waste cotton fabric ultrafine powder in 100mL of distilled water, and stirring (the rotating speed is controlled to be 600-800 rpm) for 20min to obtain a waste cotton fabric ultrafine powder suspension; weighing 4g of TiO 2 Dispersing the nano particles in 100mL of distilled water, stirring (controlling the rotating speed to be 300 rpm) for 15min to obtain TiO 2 A nanoparticle suspension;
taking 10ml of TiO 2 Mixing the nano particle suspension with 20mL waste cotton fabric ultrafine powder suspension, stirring at 800rpm for 20min, and performing ultrasonic treatment for 40min to obtain waste cotton fabric ultrafine powder-TiO 2 And (4) mixing the solution.
Scrubbing a metal copper foam net (30 cm multiplied by 50 cm) with methanol, naturally drying, spraying 3M adhesive spraying agent on the front and back surfaces for 5s, and spraying 30mL of the prepared waste cotton fabric ultrafine powder-TiO on the front and back surfaces 2 Drying the nano particle mixed solution for 2 hours at room temperature, transferring the nano particle mixed solution into an oven for drying for 20 hours at the temperature of 60 ℃ to obtain waste cotton fabric ultrafine powder-TiO 2 A composite photocatalytic material.
Example 3
Placing the composite photocatalytic materials prepared in the embodiments 1 and 2 in a formaldehyde gas environment with the concentration of 50ppm, irradiating the composite photocatalytic materials for 30min by using an ultraviolet lamp, and determining the formaldehyde degradation rates by using a Fourier infrared spectrometer (Gasmet Dx4015, finland) to be 94.8% and 93.45% respectively; placing the used composite photocatalytic material in the air, and treating for 2h by ultraviolet lamp irradiation to obtain regenerated superfine powder-TiO 2 The composite photocatalytic material can be repeatedly used.
Example 1 ultra-fine powder-TiO of waste cotton fabric 2 Composite photocatalytic material and TiO prepared by adding no waste cotton fabric ultrafine powder under the same condition 2 The degradation rate data of the photocatalytic material and the composite photocatalytic material with different regeneration times to formaldehyde are shown in table 1.
TABLE 1 ultrafine powder-TiO 2 Composite photocatalytic material and single TiO 2 Degradation rate of photocatalytic material and composite photocatalytic material with different regeneration times on formaldehyde
The invention takes the waste cotton fabrics as raw materials to prepare the superfine powder, realizes the recycling of the waste cotton fabrics, and the prepared waste cotton fabric superfine powder can disperse TiO 2 Agglomeration of nanoparticles to TiO 2 The nano particles are uniformly dispersed, and the catalysis of the composite material is improvedThe effect is achieved, meanwhile, the waste cotton fabric ultrafine powder has larger adsorption and capture capacity to formaldehyde gas, and the formaldehyde gas and TiO are prolonged 2 The contact time of the formaldehyde gas is prolonged, the reaction concentration of the formaldehyde gas is increased, and the formaldehyde degradation capability is stronger; the composite photocatalytic material prepared by the method is easy to recycle and regenerate, can be placed in the air after being used, is irradiated for 2 hours by an ultraviolet lamp, can have catalytic activity again, and can be used for multiple times.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. Waste cotton fabric superfine powder-TiO 2 The preparation method of the composite photocatalytic material is characterized by comprising the following steps of:
s1, crushing waste cotton fabrics into coarse fiber powder;
s2, freezing and grinding the coarse fiber powder in a liquid nitrogen environment to obtain waste cotton fabric ultrafine powder;
s3, dispersing a certain amount of waste cotton fabric ultrafine powder in distilled water, stirring to prepare a waste cotton fabric ultrafine powder suspension, and taking a certain amount of TiO 2 Dispersing nano particles in distilled water, stirring and preparing TiO 2 A nanoparticle suspension;
s4, the waste cotton fabric ultrafine powder suspension prepared in the step S3 and TiO 2 Mixing the nano particle suspension according to a certain volume ratio, stirring, and performing ultrasonic treatment to obtain waste cotton fabric ultrafine powder-TiO 2 Mixing the solution;
s5, spraying an adhesive on the front surface and the back surface of the cleaned foam net, and then spraying the waste cotton fabric superfine powder-TiO prepared in the step S4 2 Placing the mixed solution at room temperature for a period of time, and drying to obtain the waste cotton fabric ultrafine powder-TiO 2 A composite photocatalytic material.
2. The cotton fabric ultrafine powder-TiO of claim 1 2 The preparation method of the composite photocatalytic material is characterized by comprising the following steps: the step S1 comprises the steps of shearing waste cotton fabrics into fragments of 10-20 cm multiplied by 10-20 cm, placing the fragments into a cutting crusher with a sieve mesh diameter of 2-5 mm to be crushed for 3-5 min, wherein the rotating speed of the crusher is 2500-2800 rpm, and collecting fiber coarse powder after crushing.
3. The cotton fabric ultrafine powder-TiO of claim 1 2 The preparation method of the composite photocatalytic material is characterized by comprising the following steps: and step S2, placing a certain amount of the fiber coarse powder prepared in the step S1 into a sample barrel of a freezing grinder, placing 6-10 zirconia grinding balls with the grain diameter of 3-5 mm into the sample barrel, grinding for 3-5 min in a liquid nitrogen environment, and obtaining the waste cotton fabric superfine powder after grinding.
4. The cotton fabric ultrafine powder-TiO of claim 1 2 The preparation method of the composite photocatalytic material is characterized by comprising the following steps: the specific surface area of the waste cotton fabric ultrafine powder is 80-120 m 2 (iii) a mean particle diameter of 1 to 3 μm.
5. The cotton fabric ultrafine powder-TiO of claim 1 2 The preparation method of the composite photocatalytic material is characterized by comprising the following steps: in the step S3, the concentration of the waste cotton fabric ultrafine powder in the waste cotton fabric ultrafine powder suspension is 1-3 mg/mL, and TiO is added 2 TiO in nanoparticle suspensions 2 The concentration is 10-30 mg/mL.
6. The cotton fabric ultrafine powder-TiO of claim 1 2 The preparation method of the composite photocatalytic material is characterized by comprising the following steps: in step S4, tiO 2 The volume ratio of the nanoparticle suspension to the waste cotton fabric ultrafine powder suspension is 1.5-1:2.
7. The cotton fabric ultrafine powder-TiO of claim 1 2 The preparation method of the composite photocatalytic material is characterized by comprising the following steps: in step S5, the foam net is made of one of metal nickel, metal copper or melamine。
8. The cotton fabric ultrafine powder-TiO of claim 1 2 The preparation method of the composite photocatalytic material is characterized by comprising the following steps: in step S5, waste cotton fabric ultrafine powder-TiO 2 The spraying volume of the mixed solution is 0.01-0.03 mL/cm 2 。
9. Waste cotton fabric ultrafine powder-TiO prepared by the method of any one of claims 1 to 8 2 The composite photocatalytic material is applied to degrading formaldehyde.
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