CN109806765B - Air purification composite material and preparation method thereof - Google Patents
Air purification composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an air purification composite material and a preparation method thereof, wherein the preparation method comprises the following steps: preparing a diatomite-loaded nano titanium dioxide composite material; and depositing carbon quantum dots on the surface of the diatomite-loaded nano titanium dioxide composite material to obtain the air purification composite material. According to the invention, a small amount of pollutants in the air are absorbed and concentrated around the photocatalyst by utilizing the strong adsorbability of the diatomite, so that the photocatalyst can be effectively contacted with the pollutants, the contact area is increased, and the photocatalytic efficiency is improved.
Description
Technical Field
The invention relates to the field of composite material preparation, in particular to an air purification composite material and a preparation method thereof.
Background
With the increasing material culture demands and the demand of good life of people, the safety and no pollution of indoor environment become one of the problems to be solved urgently. Building material, decoration and finishing material, wood system furniture etc. are satisfying people to the basic requirement of room life, but the use of unqualified product can directly aggravate the pollution to the room air, even if use qualified product, along with the increase of use quantity, also can have the pollutant accumulation effect, have great hidden danger to the room air quality. Therefore, from the viewpoint of materials, it is a preferable way to improve the indoor air quality by using the air purification material.
The photocatalysis technology has the characteristics of strong oxidizing ability, low cost, environmental friendliness and the like, and can decompose and mineralize organic pollutants only by illumination and finally release the organic pollutants in the form of water and carbon dioxide. TiO 22As a semiconductor photocatalytic material, the photocatalyst has been studied more deeply, but the photocatalyst can only absorb ultraviolet light with the wavelength of less than 390nm, and the photocatalytic activity under visible light is almost zero. Thus, with TiO2As a matrix, the modification by means of doping, compounding and the like is an effective method for improving the photocatalytic performance of the photocatalyst.
So far, although it relates to modification of TiO2Many researches on the base photocatalyst are carried out, but no report is found about the synthesis of a multielement adsorption-photocatalysis synergistic air purification composite material.
Disclosure of Invention
The invention mainly aims to provide a novel air purification composite material and a preparation method thereof, and aims to solve the technical problem that the composite material has strong adsorbability and high visible light catalytic performance, and has strong purification capacity on pollutants such as formaldehyde, toluene and the like under indoor conditions, so that the composite material is more practical.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme. The preparation method of the air purification composite material provided by the invention comprises the following steps:
preparing a diatomite-loaded nano titanium dioxide composite material;
and depositing carbon quantum dots on the surface of the diatomite-loaded nano titanium dioxide composite material to obtain the air purification composite material.
The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures.
Preferably, the preparation method of the air purification composite material, wherein the preparation of the diatomite-loaded nano titanium dioxide composite material comprises: mixing soluble titanium salt and diatomite, and synthesizing the diatomite-loaded nano titanium dioxide composite material by adopting a hydrothermal method or a hydrolytic precipitation method.
Preferably, the method for preparing the air purification composite material, wherein the depositing of the carbon quantum dots on the surface of the diatomite-loaded nano titanium dioxide composite material comprises: dispersing the diatomite-loaded nano titanium dioxide composite material in a carbon quantum dot precursor solution, stirring, reacting at the temperature of 150-220 ℃ for 10-28h, centrifuging, washing and drying to obtain the air purification composite material.
Preferably, in the preparation method of the air purification composite material, the soluble titanium salt is at least one of tetrabutyl titanate, titanium tetrachloride, titanyl sulfate and titanium sulfate;
the mass ratio of the diatomite to the soluble titanium salt is 1: 0.5-3.
Preferably, in the preparation method of the air purification composite material, the carbon quantum dot precursor is at least one of citric acid, ethylenediamine, glucose, amino acid and adipic acid dihydrazide;
the mass ratio of the diatomite-loaded nano titanium dioxide composite material to the carbon quantum dots is 1: 0.2-2.
The object of the present invention and the technical problem to be solved are also achieved by the following technical means. The air purification composite material provided by the invention is prepared by the method; the removal rate of the air purification composite material to formaldehyde under visible light is more than 70%.
The object of the present invention and the technical problem to be solved are also achieved by the following technical means. The preparation method of the multielement air purification composite material provided by the invention comprises the following steps:
and (2) taking soluble noble metal salt as a precursor, and depositing noble metal on the surface of the air purification composite material by adopting a hydrothermal reduction method or a light deposition reduction method to obtain the multi-element air purification composite material.
The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures.
Preferably, the hydrothermal reduction method comprises: dissolving soluble noble metal salt and ascorbic acid in water, adding the air purification composite material, performing ultrasonic stirring, reacting at the temperature of 120-190 ℃ for 10-24h, centrifuging, washing and drying to obtain a multi-element air purification composite material;
the photo-deposition reduction method comprises the following steps: dissolving soluble noble metal salt in acid, adding the air purification composite material, performing ultrasonic treatment and stirring, reacting for 2-8h under the irradiation of a xenon lamp or a high-pressure mercury lamp, centrifuging, washing and drying to obtain the multi-element air purification composite material.
Preferably, in the preparation method of the multi-element air purification composite material, the mass ratio of the air purification composite material to the soluble precious metal salt is 1: 0.001-0.1.
The object of the present invention and the technical problem to be solved are also achieved by the following technical means. The multi-element air purification composite material is prepared by the method; the removal rate of the multi-element air purification composite material to formaldehyde under visible light is more than 75%.
By the technical scheme, the gas purification composite material and the preparation method thereof at least have the following advantages:
the Carbon Quantum Dots (CQDs) have good photoinduced electron transfer and two-photon absorption performance, and the nano noble metal shows strong absorption in a visible light region due to the plasma resonance effect, so the TiO is doubly modified by the carbon quantum dots and the nano noble metal2The absorption and utilization of visible light can be improved, the effective separation of photon-generated carriers is promoted, and the photocatalytic performance of the photocatalyst is improved. And the Diatomite (DE) serving as a natural porous material has the properties of green, environmental protection and environmental friendliness, and can provide a good growth environment and a photocatalytic reaction bed for the nano photocatalytic material. When the composite material is in a low-concentration organic pollutant environment, a small amount of pollutants in the air are absorbed and concentrated around the photocatalyst by utilizing the strong adsorbability of the diatomite, so that the photocatalyst can be effectively contacted with the pollutants, the contact area is increased, and the photocatalytic efficiency is improved.
The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a detailed description of the preferred embodiments of the present invention.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description of the embodiments, structures, characteristics and effects of the air purification composite material and the preparation method thereof according to the present invention will be made with reference to the preferred embodiments. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
One embodiment of the present invention provides a method for preparing an air purification composite material, which comprises:
dissolving soluble titanium salt in water or ethanol, mixing with Diatomite (DE), and synthesizing the diatomite-loaded nano titanium dioxide composite material (TiO) by adopting a hydrothermal method or a hydrolytic precipitation method2/DE)；
Loading nano titanium dioxide composite material (TiO) on diatomite2/DE) is dispersed in a precursor solution of carbon quantum dots (CODs), stirred, reacted for 10 to 28 hours at the temperature of 150 ℃ and 220 ℃, centrifuged, washed and dried to obtain the air purification composite material (CQDs-TiO)2/DE)。
Preferably, the soluble titanium salt is at least one of tetrabutyl titanate, titanium tetrachloride, titanyl sulfate and titanium sulfate;
the mass ratio of the diatomite to the soluble titanium salt is 1: 0.5-3.
Preferably, the carbon quantum dot precursor is at least one of citric acid, ethylenediamine, glucose, amino acid and adipic acid dihydrazide;
the mass ratio of the diatomite-loaded nano titanium dioxide composite material to the carbon quantum dots is 1: 0.2-2.
The air purification composite material provided by another embodiment of the invention is prepared by the method; the removal rate of the air purification composite material to formaldehyde under visible light is more than 70%.
Another embodiment of the present invention provides a method for preparing a multi-element air purification composite material, comprising:
soluble noble metal salt (M salt) is used as a precursor, and the noble metal is deposited on the surface of the air purification composite material (CQDs-TiO) by adopting a hydrothermal reduction method or a light deposition reduction method2DE) to obtain a multicomponent air purification composite material (M-CQDs-TiO)2/DE)。
Preferably, the hydrothermal reduction method comprises: dissolving a soluble noble metal salt precursor and ascorbic acid in water, adding the air purification composite material, performing ultrasonic stirring, reacting at the temperature of 120-190 ℃ for 10-24h, centrifuging, washing and drying to obtain a multi-element air purification composite material;
the photo-deposition reduction method comprises the following steps: dissolving a soluble precious metal salt precursor in acid, adding the air purification composite material, performing ultrasonic stirring, reacting for 1-8h under the irradiation of a xenon lamp or a high-pressure mercury lamp, centrifuging, washing and drying to obtain the multi-element air purification composite material.
Preferably, the mass ratio of the air-purifying composite material to the noble metal salt is 1: 0.001-0.1.
Preferably, the soluble noble metal salt is a water-soluble silver salt or a water-soluble palladium salt.
Another embodiment of the present invention provides a multi-component air purification composite material, which is prepared by the above method; the removal rate of the multi-element air purification composite material to formaldehyde under visible light is more than 75%.
Example 1
One embodiment of the present invention provides a method for preparing an air purification composite material, which comprises:
preparing 500mL of titanyl sulfate solution with the concentration of 24g/L from 12g of titanyl sulfate, adding 10g of diatomite into the solution, strongly stirring for 30min, adding ammonium carbonate solution with the mass concentration of 100g/L, adjusting the pH value of the slurry to 7, then aging for 2h in a constant temperature environment at 40 ℃, centrifuging, washing, drying, transferring to a muffle furnace, preserving the temperature for 2h at 650 ℃, cooling, and grinding to obtain TiO2a/DE composite material.
10g of adipic acid dihydrazide were dissolved in 100ml of water, and after it was completely dissolved, 10g of the prepared TiO was added to the solution2The composite material/DE is stirred strongly for 30min, transferred into a reaction kettle, reacted for 18h in a constant temperature environment of 190 ℃, centrifuged, washed, dried, cooled and ground to obtain the composite material (CQDs-TiO) for air purification2/DE)。
Another embodiment of the present invention provides an air purification composite material prepared by the method of embodiment 1; the removal rate of formaldehyde from the air cleaning composite of example 1 is shown in table 1.
Example 2
One embodiment of the present invention provides a method for preparing an air purification composite material, which comprises:
preparing 500mL of titanyl sulfate solution with the concentration of 30g/L from 15g of titanyl sulfate, adding 10g of diatomite into the solution, strongly stirring for 30min, adding ammonium carbonate solution with the mass concentration of 100g/L, adjusting the pH value of the slurry to 7, then aging for 2h in a constant temperature environment at 40 ℃, centrifuging, washing, drying, transferring into a muffle furnace, preserving the temperature for 2h at 650 ℃, cooling, and grinding to obtain TiO2a/DE composite material.
12g of adipic acid dihydrazide are dissolved in 100ml of water, and after it is completely dissolved, 10g of the prepared TiO are added to the solution2The composite material/DE is stirred strongly for 30min, transferred into a reaction kettle, reacted for 20h in a constant temperature environment of 185 ℃, centrifuged, washed, dried, cooled and ground to obtain the air purification composite material (CQDs-TiO)2/DE)。
Another embodiment of the present invention provides an air purification composite material prepared by the method of embodiment 2; the removal rate of formaldehyde from the air cleaning composite of example 2 is shown in table 1.
Comparative example 1
The invention provides a preparation method of a diatomite-loaded nano titanium dioxide composite material, which comprises the following steps:
preparing 500mL of titanyl sulfate solution with the concentration of 24g/L from 12g of titanyl sulfate, adding 10g of diatomite into the solution, strongly stirring for 30min, adding ammonium carbonate solution with the mass concentration of 100g/L, adjusting the pH value of the slurry to 7, then aging for 2h in a constant temperature environment at 40 ℃, centrifuging, washing, drying, transferring to a muffle furnace, preserving the temperature for 2h at 650 ℃, cooling, and grinding to obtain TiO2a/DE composite material.
The diatomite-loaded nano titanium dioxide composite material is prepared by the method of the comparative example 1; the removal rate of formaldehyde from the diatomite-supported nano titanium dioxide composite material of comparative example 1 is shown in table 1.
Comparative example 2
The invention provides a preparation method of a quantum dot nano titanium dioxide composite material, which comprises the following steps:
12g of adipic acid dihydrazide are dissolved in 100ml of water, and after it is completely dissolved, 10g of TiO is added to the solution2Stirring strongly for 30min, transferring into a reaction kettle, reacting at 185 deg.C for 20h, centrifuging, washing, drying, cooling, and grinding to obtain quantum dot nanometer titanium dioxide composite material (CQDs-TiO)2)。
The invention also provides a quantum dot nano titanium dioxide composite material, which is prepared by the method of the comparative example 2; the removal rate of formaldehyde from the quantum dot nano titania composite of comparative example 2 is shown in table 1.
Example 3
One embodiment of the invention provides a preparation method of a multi-element air purification composite material, which comprises the following steps:
0.2g of palladium chloride was dissolved in 500ml of 0.1mol/L hydrochloric acid, and 10g of CQDs-TiO of example 1 was added2The DE composite material is subjected to ultrasonic dispersion and strong stirring for 1 hour; reacting for 5h under the irradiation of a 300W xenon lamp, centrifuging, washing, drying, cooling and grinding to obtain the multi-element air purification composite material (Pb-CQDs-TiO)2/DE)。
Another embodiment of the present invention provides a multi-component air purification composite material prepared by the method of embodiment 3; the removal rate of formaldehyde from the air cleaning composite of example 3 is shown in table 1.
Example 4
One embodiment of the invention provides a preparation method of a multi-element air purification composite material, which comprises the following steps:
0.25g of silver nitrate was dissolved in 500ml of 0.1mol/L nitric acid, and after complete dissolution, CQDs-TiO-of example 2 was added2The DE composite material is subjected to ultrasonic dispersion and strong stirring for 1 hour; reacting for 4.5h under the irradiation of a 300W high-pressure mercury lamp, centrifuging, washing, drying, cooling, and grinding to obtain the multi-element air purification composite material (Ag-CQDs-TiO)2/DE)。
Another embodiment of the present invention provides a multi-component air purification composite material prepared by the method of embodiment 4; the removal rate of formaldehyde from the air cleaning composite of example 4 is shown in table 1.
Example 5
One embodiment of the present invention provides a method for preparing an air purification composite material, which comprises:
preparing 14g of titanyl sulfate into 500mL of 28g/L titanyl sulfate solution, adding 10g of diatomite into the solution, strongly stirring for 30min, adding 100g/L ammonium carbonate solution, adjusting the pH value of the slurry to 7, then aging for 2h in a constant-temperature environment at 40 ℃, centrifuging, washing, drying, transferring to a muffle furnace, preserving the temperature for 2h at 650 ℃, cooling, and grinding to obtain TiO2a/DE composite material.
8g of adipic acid dihydrazide were dissolved in 100mL of water, and 10g of the prepared TiO was added2The composite material/DE is stirred strongly for 30min, transferred into a reaction kettle, reacted for 18h in a constant temperature environment of 180 ℃, centrifuged, washed, dried, cooled and ground to obtain the composite material (CQDs-TiO) for air purification2/DE)。
Dissolving 0.1g palladium chloride in 500ml 0.1mol/L hydrochloric acid, adding 10g CQDs-TiO2The DE composite material is subjected to ultrasonic dispersion and strong stirring for 1 hour; reacting for 3.5h under the irradiation of a 300W xenon lamp, centrifuging, washing, drying, cooling and grinding to obtain the multi-element air purification composite material (Pb-CQDs-TiO)2/DE)。
Another embodiment of the present invention provides a multi-component air purification composite material prepared by the method of embodiment 5; the formaldehyde removal rate of the multi-component air purification composite material of example 5 is shown in table 1.
Example 6
One embodiment of the present invention provides a method for preparing an air purification composite material, which comprises:
preparing 500mL of titanyl sulfate solution with the concentration of 18g/L from 9g of titanyl sulfate, adding 10g of diatomite, and stirring strongly for 30min to prepare slurry; adding into the slurryAdjusting the pH value of the slurry to 7 by using an ammonium carbonate solution with the mass concentration of 100g/L, then aging the slurry for 2 hours in a constant temperature environment of 40 ℃, centrifuging, washing, drying, transferring the slurry to a muffle furnace, preserving the temperature for 2 hours at 650 ℃, cooling and grinding to obtain TiO2a/DE composite material.
5g of adipic acid dihydrazide are dissolved in 100ml of water, and after it is completely dissolved, 10g of the prepared TiO are added to the solution2The composite material/DE is stirred strongly for 30min, transferred into a reaction kettle, reacted for 22h in a constant temperature environment of 175 ℃, centrifuged, washed, dried, cooled and ground to obtain the composite material (CQDs-TiO) for air purification2/DE)。
0.03g of palladium chloride was dissolved in 500ml of 0.1mol/L hydrochloric acid, and after complete dissolution, 10g of the prepared CQDs-TiO was added to the solution2The DE composite material is dispersed by ultrasonic and stirred for 1 hour with strong force. The mixed solution reacts for 3 hours under the irradiation of a 300W xenon lamp, and then is ground after being centrifuged, washed, dried and cooled to obtain the multi-element air purification composite material (Pb-CQDs-TiO)2/DE)。
Another embodiment of the present invention provides a multi-component air purification composite material prepared by the method of embodiment 6; the formaldehyde removal rate of the multi-component air purification composite material of example 6 is shown in table 1.
Example 7
One embodiment of the present invention provides a method for preparing an air purification composite material, which comprises:
preparing 500mL of 36g/L titanyl sulfate solution from 18g of titanyl sulfate, adding 10g of diatomite into the solution, strongly stirring for 30min, adding 100g/L ammonium carbonate solution, adjusting the pH value of the slurry to 7, then aging for 2h in a constant-temperature environment at 40 ℃, centrifuging, washing, drying, transferring to a muffle furnace, preserving the temperature for 2h at 650 ℃, cooling, and grinding to obtain TiO2a/DE composite material.
15g of adipic acid dihydrazide were dissolved in 100ml of water, and after complete dissolution, 10g of the prepared TiO was added2The composite material is mixed with DE for 30min, transferred into a reaction kettle and kept at a constant temperature of 190 DEG CReacting for 18h, centrifuging, washing, drying, cooling, and grinding to obtain the composite material (CQDs-TiO) for air purification2/DE)。
Dissolving 0.5g silver nitrate in 500ml 0.1mol/L nitric acid, adding 10g CQDs-TiO2The DE composite material is subjected to ultrasonic dispersion and strong stirring for 1 hour; reacting for 5h under the irradiation of a 300W xenon lamp, centrifuging, washing, drying, cooling and grinding to obtain the multi-element air purification composite material (Ag-CQDs-TiO)2/DE)。
Another embodiment of the present invention provides a multi-component air purification composite material prepared by the method of embodiment 7; the formaldehyde removal rate of the multi-component air purification composite material of example 7 is shown in table 1.
TABLE 1 removal of formaldehyde from composites of examples 1-7
The air purification composite material and the multi-element air purification composite material have strong adsorbability and high visible light photocatalysis, and show strong purification capacity on pollutants such as formaldehyde, toluene and the like under indoor conditions through synergistic action of adsorption and photocatalysis.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are still within the scope of the technical solution of the present invention.
Claims (7)
1. The preparation method of the air purification composite material is characterized by comprising the following steps:
preparing a diatomite-loaded nano titanium dioxide composite material;
depositing carbon quantum dots on the surface of the diatomite-loaded nano titanium dioxide composite material to obtain an air purification composite material;
the preparation method of the diatomite-loaded nano titanium dioxide composite material comprises the following steps: mixing soluble titanium salt and diatomite, and synthesizing the diatomite-loaded nano titanium dioxide composite material by adopting a hydrothermal method or a hydrolytic precipitation method;
the mass ratio of the diatomite to the soluble titanium salt is 1: 0.5-3;
the method for depositing the carbon quantum dots on the surface of the diatomite-loaded nano titanium dioxide composite material comprises the following steps: dispersing the diatomite-loaded nano titanium dioxide composite material in a carbon quantum dot precursor solution, stirring, reacting at the temperature of 150 ℃ and 220 ℃ for 10-28h, centrifuging, washing and drying to obtain an air purification composite material;
the carbon quantum dot precursor is adipic acid dihydrazide;
the mass ratio of the diatomite-loaded nano titanium dioxide composite material to the carbon quantum dot precursor is 1: 0.2-2.
2. The method for preparing the air purification composite material as claimed in claim 1, wherein the soluble titanium salt is at least one of tetrabutyl titanate, titanium tetrachloride, titanyl sulfate and titanium sulfate.
3. An air-purifying composite material prepared by the method of any one of claims 1 to 2; the removal rate of the air purification composite material to formaldehyde under visible light is more than 70%.
4. The preparation method of the multi-element air purification composite material is characterized by comprising the following steps:
the multi-element air purification composite material is obtained by taking soluble noble metal salt as a precursor and depositing noble metal on the surface of the air purification composite material in the claim 3 by adopting a hydrothermal reduction method or a light deposition reduction method.
5. The method for preparing the multi-element air purification composite material according to claim 4, wherein the hydrothermal reduction method comprises the following steps: dissolving soluble noble metal salt and ascorbic acid in water, adding the air purification composite material, performing ultrasonic stirring, reacting at the temperature of 120-190 ℃ for 10-24h, centrifuging, washing and drying to obtain a multi-element air purification composite material;
the photo-deposition reduction method comprises the following steps: dissolving soluble noble metal salt in acid, adding the air purification composite material, performing ultrasonic treatment and stirring, reacting for 1-8h under the irradiation of a xenon lamp or a high-pressure mercury lamp, centrifuging, washing and drying to obtain the multi-element air purification composite material.
6. The method for preparing the multi-element air purification composite material according to claim 4, wherein the mass ratio of the air purification composite material to the soluble precious metal salt is 1: 0.001-0.1.
7. A multi-element air purification composite material, prepared by the method of any one of claims 4 to 6; the removal rate of the multi-element air purification composite material to formaldehyde under visible light is more than 75%.
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| CN104001537A (en) * | 2014-06-18 | 2014-08-27 | 中国矿业大学(北京) | Method for improving visible-light catalytic activity and antibacterial performance of TiO2/diatomite composite material |
| CN104368338A (en) * | 2014-11-06 | 2015-02-25 | 上海电力学院 | Preparation method of amino-modified Pd/TiO2 photocatalyst |
| CN106492772A (en) * | 2016-09-13 | 2017-03-15 | 富思特新材料科技发展股份有限公司 | A kind of titanium dioxide nanoplate and the preparation method of diatomite composite photocatalytic agent |
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| CN107670664A (en) * | 2017-10-31 | 2018-02-09 | 云南健牛生物科技有限公司 | Titanic oxide composite photochemical catalyst system prepares and its application |
| CN107876035A (en) * | 2017-11-24 | 2018-04-06 | 中国科学院上海硅酸盐研究所 | A kind of carbon quantum dot/titanic oxide composite photochemical catalyst material and its preparation method and application |
| CN108212159A (en) * | 2018-01-18 | 2018-06-29 | 云南健牛生物科技有限公司 | Fe2O3 doping carbon quantum dot/titanium dioxide composite photocatalyst prepares and the method for degradation of formaldehyde |
| CN108246291A (en) * | 2018-02-06 | 2018-07-06 | 中国建筑材料科学研究总院有限公司 | Titanium dioxide sepiolite composite material of snow cover decorations and preparation method thereof |
| CN108311140A (en) * | 2018-03-21 | 2018-07-24 | 长春理工大学 | A kind of preparation method of the optic catalytic composite material of palladium modification |
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