CN112206725A - Preparation method of titanium dioxide nanofiber aerogel - Google Patents

Preparation method of titanium dioxide nanofiber aerogel Download PDF

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CN112206725A
CN112206725A CN202011170463.4A CN202011170463A CN112206725A CN 112206725 A CN112206725 A CN 112206725A CN 202011170463 A CN202011170463 A CN 202011170463A CN 112206725 A CN112206725 A CN 112206725A
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何雅贵
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Abstract

The invention discloses a preparation method of titanium dioxide nanofiber aerogel, which comprises the steps of adding polyacrylonitrile into a mixed solvent I, adding tetrabutyl titanate to obtain colloid, adjusting pH with urea, and performing spin coating to obtain TiO2A nanofiber membrane; adding TiO into the mixture2Shearing the nanofiber membrane into small pieces, adding the small pieces into deionized water, stirring vigorously, and adding SiO2Stirring the sol and the graphene oxide at room temperature, pouring the mixture into a mold, and freeze-drying the mixture in a liquid nitrogen environment to obtain TiO2A nanofiber aerogel; washing the titanium dioxide nano-fiber aerogel with hydrochloric acid, placing the washed titanium dioxide nano-fiber aerogel in a tubular furnace, calcining at high temperature, reducing with hydrogen,cooling to obtain the TiO2A nanofiber aerogel. The TiO being2The nanofiber aerogel has excellent conductivity and mechanical properties.

Description

Preparation method of titanium dioxide nanofiber aerogel
Technical Field
The invention belongs to the field of aerogel, and particularly relates to a preparation method of titanium dioxide nanofiber aerogel.
Background
Titanium dioxide is an important raw material widely used in conventional industries related to human life, such as paints, sun cream, food additives, and the like. In 2019, its global market value is $ 166.4 billion, and its compound annual growth rate is expected to be as high as 7.16% in the next five years. When the size is reduced to the nano-scale, a higher charge transfer rate and more active sites can be achieved due to the surface effect of the nanomaterial. Thus, over the past decade, various TiO materials have been used2Nanostructures have great potential in new industries such as energy conversion and storageLeading to extensive research. However, these particulate nanomaterials exist only in powder form, which easily enter the human body through the respiratory system and pose health risks.
In view of the health risks that nanomaterials, when present in powder form, are liable to pass through the respiratory system, in this case "mixtures in powder form containing 1% or more of titanium dioxide, in the form or incorporated in particles having an aerodynamic diameter of < 10 μm", are formally classified by the european union as two classes of carcinogens. In addition, these particulate nanomaterials are difficult to recycle and once released into the environment, can be toxic to organisms. Thus, self-supporting TiO was developed2Construction to ensure safe use and easy recycling is an attractive but challenging task.
Disclosure of Invention
The invention aims to provide a preparation method of titanium dioxide nanofiber aerogel, which comprises the following steps:
s1: adding polyacrylonitrile into a mixed solvent I, stirring for 0.5-1 h, then adding tetrabutyl titanate, carrying out ultrasonic treatment to obtain uniform colloid, adding urea to adjust the pH of the colloid to be 7.5-9, standing and aging for 1-5 h, coating the aged colloid on the surface of a glass substrate by adopting a spin-coating method to obtain a film layer with the thickness of 50-200 mu m, and then drying by using hot air to obtain TiO2The nanofiber membrane comprises 2-5 g of polyacrylonitrile, 100mL of mixed solvent I and 10-30 g of tetrabutyl titanate in a mass-volume ratio.
S2: adding tetraethyl orthosilicate into a mixed solvent II, uniformly stirring by using ultrasonic waves, adding phosphoric acid, mixing and stirring for 2-4 hours, wherein the mass ratio of tetraethyl orthosilicate to phosphoric acid is (4-5): (0.02-0.04), and obtaining SiO2And (3) sol.
S3: the TiO obtained in the step S12Shearing the nanofiber membrane into small pieces, adding the small pieces into deionized water, and violently stirring for 20-30 min, wherein TiO is2The mass ratio of the nanofiber membrane to the deionized water is 1: 90-96, and then the SiO in the step S2 is added2Stirring the sol and graphene oxide at room temperature for 2-3 h, and pouring the sol and graphene oxideAnd (4) in the mold, carrying out freeze drying for 50-60 h in a liquid nitrogen environment to obtain the nanofiber aerogel precursor.
S4: washing the nanofiber aerogel with hydrochloric acid, airing, taking out, placing in a tubular furnace, and introducing into the tubular furnace according to the volume ratio of 30%: 70% of H2And N2Heating the mixed gas at the flow rate of 3L/min from room temperature to 650-750 ℃, calcining for 1.5-2 h, and cooling to obtain TiO2A nanofiber aerogel.
Preferably, the mixed solvent I is a mixed solvent of absolute ethyl alcohol and N, N-dimethylformamide.
More preferably, the volume ratio of the absolute ethyl alcohol to the N, N-dimethylformamide in the mixed solvent I is (8-9): 0.5-2.
Preferably, the mixed solvent II is a mixed solvent of absolute ethyl alcohol and deionized water.
More preferably, the volume ratio of the absolute ethyl alcohol to the deionized water in the mixed solvent II is (9-12): 4-5.5.
Preferably, the TiO is2Nanofiber film, SiO2The mass ratio of the sol to the graphene oxide is 1 (4.8-5.4) to (0.63-0.88).
Preferably, the temperature increase rate during heating in the step S4 is 2 to 2.5 ℃/min.
The invention has the following beneficial effects:
TiO in the invention2The nanofiber aerogel has a layered ordered cellular structure consisting of nanofibers elastically bonded by elastic Si-O-Si bonds, which can overcome TiO2Inherently brittle and withstands repeated compression at 40% strain without significant deformation. TiO 22The electronic structure of the nanofiber aerogel is adjusted by generating a large number of Oxygen Vacancies (OVs), and the electrical conductivity is significantly improved.
Drawings
FIG. 1 is a diagram of TiO prepared in example 1 of the present invention2XRD pattern of nanofiber aerogel;
FIG. 2 is a diagram of TiO prepared in example 1 of the present invention2SEM spectra of nanofiber aerogels.
Detailed Description
The following examples are provided for the purpose of illustration, and the present invention is not limited to the following examples.
Example 1
A preparation method of titanium dioxide nanofiber aerogel specifically comprises the following steps:
s1: adding polyacrylonitrile into a mixed solvent I of absolute ethyl alcohol and N, N-dimethylformamide with a volume ratio of 8:0.5, stirring for 0.5h, adding tetrabutyl titanate, performing ultrasonic treatment to obtain uniform colloid, adding urea to adjust the pH of the colloid to 7.5, standing and aging for 1h, coating the aged colloid on the surface of a glass substrate by a spin-coating method to obtain a film layer with a thickness of 50 mu m, and drying by hot air to obtain TiO2The nanofiber membrane comprises polyacrylonitrile, a mixed solvent I and tetrabutyl titanate, wherein the mass-volume ratio of the polyacrylonitrile to the mixed solvent I to the tetrabutyl titanate is 2g:100mL:10 g.
S2: adding tetraethyl orthosilicate into absolute ethyl alcohol and deionized water in a volume ratio of 9:4, ultrasonically stirring uniformly, adding phosphoric acid, mixing and stirring for 2 hours, wherein the mass ratio of the tetraethyl orthosilicate to the phosphoric acid is 4:0.02, and obtaining SiO2And (3) sol.
S3: the TiO obtained in the step S12Shearing the nanofiber membrane into small pieces, adding the small pieces into deionized water, and violently stirring for 20min, wherein TiO is2The mass ratio of the nanofiber membrane to the deionized water is 1:90, and then SiO in the step S2 is added2And stirring the sol and the graphene oxide at room temperature for 2-3 h, then pouring the sol and the graphene oxide into a mold, and freeze-drying the sol and the graphene oxide in a liquid nitrogen environment for 50h to obtain the nanofiber aerogel precursor.
S4: washing the nanofiber aerogel with hydrochloric acid, airing, taking out, placing in a tubular furnace, and introducing into the tubular furnace according to the volume ratio of 30%: 70% of H2And N2Mixing gas at flow rate of 3L/min, heating at temperature rising rate of 2 deg.C/min from room temperature to 650 deg.CCalcining for 2h, and cooling to obtain the conductive TiO2A nanofiber aerogel.
Example 2
A preparation method of titanium dioxide nanofiber aerogel specifically comprises the following steps:
s1: adding polyacrylonitrile into a mixed solvent I of absolute ethyl alcohol and N, N-dimethylformamide with a volume ratio of 9:2, stirring for 1h, adding tetrabutyl titanate, performing ultrasonic treatment to obtain uniform colloid, adding urea to adjust the pH of the colloid to 9, standing and aging for 5h, coating the aged colloid on the surface of a glass substrate by using a spin-coating method to obtain a film layer with the thickness of 200 mu m, and drying by using hot air to obtain TiO2The nanofiber membrane comprises polyacrylonitrile, a mixed solvent I and tetrabutyl titanate, wherein the mass-volume ratio of the polyacrylonitrile to the mixed solvent I to the tetrabutyl titanate is 5g to 100mL to 10-30 g.
S2: adding tetraethyl orthosilicate into absolute ethyl alcohol and deionized water in a volume ratio of 12:5.5, uniformly stirring by ultrasonic waves, adding phosphoric acid, mixing and stirring for 4 hours, wherein the mass ratio of the tetraethyl orthosilicate to the phosphoric acid is 5:0.04, and obtaining SiO2And (3) sol.
S3: the TiO obtained in the step S12Shearing the nanofiber membrane into small pieces, adding the small pieces into deionized water, and violently stirring for 30min, wherein TiO is2The mass ratio of the nanofiber membrane to the deionized water is 1:96, and then SiO in the step S2 is added2And stirring the sol and the graphene oxide at room temperature for 3 hours, then pouring the mixture into a mold, and freeze-drying the mixture in a liquid nitrogen environment for 60 hours to obtain the nanofiber aerogel precursor.
S4: washing the nanofiber aerogel with hydrochloric acid, airing, taking out, placing in a tubular furnace, and introducing into the tubular furnace according to the volume ratio of 30%: 70% of H2And N2Heating the mixed gas from room temperature to 750 ℃ at a heating rate of 2.5 ℃/min at a flow rate of 3L/min, calcining for 2h, and cooling to obtain the conductive TiO2A nanofiber aerogel.
Example 3
A preparation method of titanium dioxide nanofiber aerogel specifically comprises the following steps:
s1: mixing polypropyleneAdding the alkene nitrile into a mixed solvent I of absolute ethyl alcohol and N, N-dimethyl formamide with the volume ratio of 8.2:1, stirring for 1h, then adding tetrabutyl titanate, carrying out ultrasonic treatment to obtain uniform colloid, adding urea to adjust the pH value of the colloid to 8, standing and aging for 3h, coating the aged colloid on the surface of a glass substrate by adopting a spin coating method to obtain a film layer with the thickness of 100 mu m, and drying by using hot air to obtain TiO2The nanofiber membrane comprises polyacrylonitrile, a mixed solvent I and tetrabutyl titanate, wherein the mass-volume ratio of the polyacrylonitrile to the mixed solvent I to the tetrabutyl titanate is 3g to 100mL to 20 g.
S2: adding tetraethyl orthosilicate into absolute ethyl alcohol and deionized water in a volume ratio of 10:4.5, uniformly stirring by ultrasonic waves, adding phosphoric acid, mixing and stirring for 3 hours, wherein the mass ratio of the tetraethyl orthosilicate to the phosphoric acid is 4.4:0.03, and obtaining SiO2And (3) sol.
S3: the TiO obtained in the step S12Shearing the nanofiber membrane into small pieces, adding the small pieces into deionized water, and violently stirring for 25min, wherein TiO is2The mass ratio of the nanofiber membrane to the deionized water is 1:92, and then SiO in the step S2 is added2And stirring the sol and the graphene oxide at room temperature for 2.5h, then pouring the mixture into a mold, and freeze-drying the mixture in a liquid nitrogen environment for 55h to obtain the nanofiber aerogel precursor.
S4: washing the nanofiber aerogel with hydrochloric acid, airing, taking out, placing in a tubular furnace, and introducing into the tubular furnace according to the volume ratio of 30%: 70% of H2And N2Heating the mixed gas from room temperature to 700 ℃ at a heating rate of 2 ℃/min at a flow rate of 3L/min, calcining for 1.5h, and cooling to obtain the conductive TiO2A nanofiber aerogel.
Example 4
A preparation method of titanium dioxide nanofiber aerogel specifically comprises the following steps:
s1: adding polyacrylonitrile into a mixed solvent I of absolute ethyl alcohol and N, N-dimethylformamide with a volume ratio of 8.6:1.5, stirring for 1h, adding tetrabutyl titanate, performing ultrasonic treatment to obtain uniform colloid, adding urea to adjust the pH of the colloid to 8.5, standing and aging for 4h, and coating the aged colloid on the surface of a glass substrate by a spin-coating methodCoating to obtain a film layer with a thickness of 150 μm, and drying with hot air to obtain TiO2The nanofiber membrane comprises polyacrylonitrile, a mixed solvent I and tetrabutyl titanate, wherein the mass-volume ratio of the polyacrylonitrile to the mixed solvent I to the tetrabutyl titanate is 4g:100mL:25 g.
S2: adding tetraethyl orthosilicate into absolute ethyl alcohol and deionized water in a volume ratio of 11:5.1, uniformly stirring by ultrasonic waves, adding phosphoric acid, mixing and stirring for 4 hours, wherein the mass ratio of the tetraethyl orthosilicate to the phosphoric acid is 4:0.03, and obtaining SiO2And (3) sol.
S3: the TiO obtained in the step S12Shearing the nanofiber membrane into small pieces, adding the small pieces into deionized water, and violently stirring for 30min, wherein TiO is2The mass ratio of the nanofiber membrane to the deionized water is 1:94, and then SiO in the step S2 is added2And stirring the sol and the graphene oxide at room temperature for 2.6h, then pouring the mixture into a mold, and freeze-drying the mixture in a liquid nitrogen environment for 50h to obtain the nanofiber aerogel precursor.
S4: washing the nanofiber aerogel with hydrochloric acid, airing, taking out, placing in a tubular furnace, and introducing into the tubular furnace according to the volume ratio of 30%: 70% of H2And N2Heating the mixed gas from room temperature to 750 ℃ at a heating rate of 2.5 ℃/min at a flow rate of 3L/min, calcining for 2h, and cooling to obtain the conductive TiO2A nanofiber aerogel.
Performance test experiments:
TiO prepared in example 1 to 42The nanofiber aerogel is tested for conductivity, the conductivity is tested by an ST-2258C digital four-probe tester to characterize the conductivity, the results are shown in Table 1,
TiO prepared in example 1 to 42The nanofiber aerogels were tested for tensile properties, tensile strength was measured by a tensile tester (XQ-1C), and the results are shown in Table 1,
testing the mechanical properties of the aerogels prepared in examples 1-4, and subjecting the TiO prepared in examples 1-4 to2Repeatedly rolling the nanofiber aerogel under 40% strain for 10 times, and obtaining the TiO aerogel2The nanofiber aerogel has no obvious deformation, and compared with the original aerogel which is not rolled,the deformation rates are all below 0.05 percent,
deformation rate is (aerogel thickness before ten rolling times-aerogel thickness after ten rolling times)/aerogel thickness before ten rolling times x 100%;
TABLE 1 test results
Figure BDA0002747129040000051
Figure BDA0002747129040000061
As can be seen from Table 1, the conductivity of the nanofiber aerogel prepared in the embodiments 1 to 4 of the present invention is 49.1mS cm-1The nano aerogel disclosed by the invention has good conductivity, and the tensile strength of the nano fiber aerogel prepared in the embodiments 1 to 4 is higher than 2.82MPa, so that the nano aerogel disclosed by the invention has very high strength.

Claims (7)

1. The preparation method of the titanium dioxide nanofiber aerogel is characterized by comprising the following steps of:
s1: adding polyacrylonitrile into a mixed solvent I, stirring for 0.5-1 h, then adding tetrabutyl titanate, carrying out ultrasonic treatment to obtain uniform colloid, adding urea to adjust the pH of the colloid to be 7.5-9, standing and aging for 1-5 h, coating the aged colloid on the surface of a glass substrate by adopting a spin-coating method to obtain a film layer with the thickness of 50-200 mu m, and then drying by using hot air to obtain TiO2The nanofiber membrane comprises a polyacrylonitrile membrane, a mixed solvent I and tetrabutyl titanate, wherein the mass-volume ratio of the polyacrylonitrile membrane to the mixed solvent I to the tetrabutyl titanate is 2-5 g, 100mL and 10-30 g;
s2: adding tetraethyl orthosilicate into a mixed solvent II, uniformly stirring by using ultrasonic waves, adding phosphoric acid, mixing and stirring for 2-4 hours, wherein the mass ratio of tetraethyl orthosilicate to phosphoric acid is (4-5): (0.02-0.04), and obtaining SiO2Sol;
s3: the TiO obtained in the step S12The nanofiber membrane is cut into small pieces, and thenAdding the mixture into deionized water, and violently stirring for 20-30 min, wherein TiO2The mass ratio of the nanofiber membrane to the deionized water is 1: 90-96, and then the SiO in the step S2 is added2Stirring the sol and graphene oxide at room temperature for 2-3 h, then pouring the mixture into a mold, and freeze-drying the mixture in a liquid nitrogen environment for 50-60 h to obtain a nanofiber aerogel precursor;
s4: washing the nanofiber aerogel with hydrochloric acid, airing, taking out, placing in a tubular furnace, and introducing into the tubular furnace according to the volume ratio of 30%: 70% of H2And N2Heating the mixed gas at the flow rate of 3L/min from room temperature to 650-750 ℃, calcining for 1.5-2 h, and cooling to obtain TiO2A nanofiber aerogel.
2. The method for preparing the titanium dioxide nanofiber aerogel according to claim 1, wherein the mixed solvent I is a mixed solvent of absolute ethyl alcohol and N, N-dimethylformamide.
3. The method for preparing the titanium dioxide nanofiber aerogel according to claim 1 or 2, wherein the volume ratio of absolute ethyl alcohol to N, N-dimethylformamide in the mixed solvent I is (8-9): 0.5-2.
4. The method for preparing the titanium dioxide nano fiber aerogel according to claim 1, wherein the mixed solvent II is a mixed solvent of absolute ethyl alcohol and deionized water.
5. The method for preparing the titanium dioxide nanofiber aerogel according to claim 1 or 4, wherein the volume ratio of the absolute ethyl alcohol to the deionized water in the mixed solvent II is (9-12) to (4-5.5).
6. The method for preparing titanium dioxide nano fiber aerogel according to claim 1, wherein the TiO is2Nanofiber film, SiO2The mass ratio of the sol to the graphene oxide is 1 (4.8)～5.4):(0.63～0.88)。
7. The method for preparing titanium dioxide nanofiber aerogel according to claim 1, wherein the heating rate in the step S4 is 2-2.5 ℃/min.
CN202011170463.4A 2020-10-28 2020-10-28 Preparation method of titanium dioxide nanofiber aerogel Withdrawn CN112206725A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113171769A (en) * 2021-05-12 2021-07-27 周口师范学院 Nano composite photocatalytic material and preparation method thereof
CN113831581A (en) * 2021-09-23 2021-12-24 航天特种材料及工艺技术研究所 High-elasticity anti-radiation nanofiber aerogel material and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113171769A (en) * 2021-05-12 2021-07-27 周口师范学院 Nano composite photocatalytic material and preparation method thereof
CN113831581A (en) * 2021-09-23 2021-12-24 航天特种材料及工艺技术研究所 High-elasticity anti-radiation nanofiber aerogel material and preparation method thereof

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