CN109174095B - Preparation method of monatomic catalyst for degrading VOCs (volatile organic compounds) - Google Patents

Preparation method of monatomic catalyst for degrading VOCs (volatile organic compounds) Download PDF

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CN109174095B
CN109174095B CN201811033761.1A CN201811033761A CN109174095B CN 109174095 B CN109174095 B CN 109174095B CN 201811033761 A CN201811033761 A CN 201811033761A CN 109174095 B CN109174095 B CN 109174095B
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丁辉
崔家浩
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    • 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
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Abstract

The invention discloses a preparation method of a monatomic catalyst for degrading VOCs (volatile organic compounds), which comprises the following steps: step one, heating a solution added with a cerium-containing compound and ammonium chloroplatinate in a microwave reactor; step two, centrifuging the solution to obtain a precipitate product; step four, washing the precipitated product with deionized water or absolute ethyl alcohol, and then calcining in a muffle furnace to obtain the single-atom catalyst Pt/CeO2. The invention utilizes the microwave radiation condition for heating, has high heating speed, uniformly heats the solution in the reaction cavity, leads metal atoms to be loaded on the carrier in a more dispersed way, improves the utilization rate of the metal and has higher catalytic activity.

Description

Preparation method of monatomic catalyst for degrading VOCs (volatile organic compounds)
Technical Field
The invention belongs to the field of catalysts, and relates to a preparation method of a normal-temperature monatomic catalyst for degrading VOCs (volatile organic compounds) by a microwave method.
Background
Volatile Organic compounds (vocs) are a class of important air pollutants, and the world health organization defines that Organic compounds with a boiling point of 50-260 ℃ and a saturated vapor pressure of over 133Pa at room temperature include alkanes, alkenes, aromatic hydrocarbons and derivatives thereof, alcohols, aldehydes, ketones, amines, amides, acids, anhydrides, and the like. VOCs are important atmospheric pollutants, are harmful to human bodies, can cause the human bodies to have various uncomfortable feelings, and have toxicity and irritation. It is known that many VOCs have neurotoxicity, renal and hepatic toxicity, and even carcinogenic effects, can damage the cardiovascular system, cause gastrointestinal disorders, induce diseases of the immune system, endocrine system and hematopoietic system, cause metabolic disorders, are also important factors in the formation of photochemical smog and PM2.5, and can also cause the production of greenhouse gases and the destruction of the ozone layer.
Compared with the traditional technology, the technology for catalyzing and degrading the VOCs at the normal temperature can greatly reduce the temperature and cost for treating the VOCs, reduce the energy consumption loss of equipment, improve the safety factor, has simple and convenient operation process, and meets the requirement of green chemistry. Microwaves are electromagnetic waves having a frequency between 300MHz and 300 GHz. Different from the traditional heating that heat is transferred from outside to inside in the modes of heat conduction, heat radiation and the like, the microwave is heated simultaneously from inside to outside through two modes of dipole rotation and ion conduction. The microwave heating has the characteristics of high heating speed, uniform heating, selective heating and easy control. Under the condition of microwave radiation, the chemical reaction has fast reaction rate, high conversion rate and high selectivity. The rare earth element has good wave-absorbing property, the unique electronic structure of the rare earth element improves the peak value capability of absorbing electromagnetic waves, widens the absorption frequency band, and can increase the reaction times of microwaves in the propagation of the base material by matching with a microwave auxiliary heating mode, so that the reaction is more fully carried out, the rare earth element is more uniformly distributed in the material synthesis, and the production energy consumption and the cost are reduced. Compared with the traditional supported catalyst, the single atom catalyst realizes that a single atom becomes a reaction active point, the load capacity of the catalyst is greatly reduced, and the catalytic effect is also obviously improved. However, the monatomic catalyst is easy to migrate and agglomerate, so that the initiation activity is reduced and even the catalyst is deactivated. At present, the preparation method of the monatomic catalyst comprises an atomic layer deposition method, an immersion method, a mass separation soft landing method, a solid phase melting method, a strong electrostatic adsorption method and the like, but the process for preparing the monatomic catalyst for degrading VOCs by a microwave method has not been reported so far.
Patent CN108057455A discloses an ozone catalytic oxidation catalyst and a preparation method thereof. This patent is with raw materials coal crocus, after adding active ingredient, shaping, carbomorphism and activation, and the pore structure of the ozone catalytic oxidation catalyst who makes changes, makes the diplopore distribution structure that mesopore and micropore coexist, and catalyst catalytic activity improves, but the catalyst need add ozone and just can high-efficient degradation, has the problem that structural stability is poor, noble metal dispersibility is not high.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of a monatomic catalyst for degrading VOCs (volatile organic compounds).
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a monatomic catalyst for degrading VOCs comprises the following steps:
(1) dissolving a cerium-containing compound in deionized water, adding an alkaline substance into a cerium-containing compound solution to enable the pH of the solution to be 8-9, adding ammonium chloroplatinate into the solution, wherein the mass ratio of the ammonium chloroplatinate added into the solution to the cerium-containing compound is 1: 10-30;
(2) putting the solution into a microwave reactor, and heating for 10-30 min at 150-300 ℃;
(3) after the reaction is finished, carrying out centrifugal separation on the solution on a high-speed centrifuge at the rotating speed of 6000-10000 rpm for 5-15 minutes, and removing the solution in the centrifuge tube to obtain a precipitation product;
(4) washing the precipitated product with deionized water or absolute ethyl alcohol, then placing the precipitated product in a muffle furnace, calcining the product in air at 150-300 ℃ for 1.5-2.5 hours, and finally obtaining the monatomic catalyst Pt/CeO2。
Compared with the prior art, the invention has the following beneficial effects:
1. the monatomic catalyst prepared by the method has the advantages of good dispersibility, high structural stability, high atom utilization rate, low use cost, good catalytic effect and long service life.
2. The preparation process is simple and convenient to operate, and VOCs can be degraded at normal temperature without ozone oxidation.
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FIG. 1 is a simple schematic diagram of the process of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it should be apparent that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A preparation method of a monatomic catalyst for degrading VOCs comprises the following steps:
(1) dissolving a cerium-containing compound in deionized water, adding an alkaline substance into a cerium-containing compound solution to enable the pH of the solution to be 8-9, adding ammonium chloroplatinate into the solution, wherein the mass ratio of the ammonium chloroplatinate added into the solution to the cerium-containing compound is 1: 10-30;
(2) putting the solution into a microwave reactor, and heating for 10-30 min at 150-300 ℃;
(3) after the reaction is finished, carrying out centrifugal separation on the solution on a high-speed centrifuge at the rotating speed of 6000-10000 rpm for 5-15 minutes, and removing the solution in the centrifuge tube to obtain a precipitation product;
(4) washing the precipitated product with deionized water or absolute ethyl alcohol, then placing the precipitated product in a muffle furnace, calcining the product in air at 150-300 ℃ for 1.5-2.5 hours, and finally obtaining the monatomic catalyst Pt/CeO2。
The cerium-containing compound in the step (1) is one or more of cerium nitrate, cerium acetate or ammonium cerium nitrate.
The alkaline substance in the step (1) is one or two of ammonia water or ammonium carbonate.
The microwave power of the microwave reactor in the step (2) is 200W-700W. Microwave heating belongs to internal heating, the heating speed is high, the solution in the reaction cavity is uniformly heated, platinum is more dispersedly loaded on cerium dioxide, and the efficiency of degrading VOCs is higher.
The catalyst of the invention can be used for purifying various low-concentration organic waste gases and other combustible component waste gases, such as industrial tail gas, automobile tail gas and the like.
Example 1
(1) Dissolving cerous nitrate in deionized water, then adding ammonia water into a cerous nitrate solution to enable the pH of the solution to be 8, adding ammonium chloroplatinate into the solution, wherein the mass ratio of the ammonium chloroplatinate to the cerous nitrate added into the solution is 1: 10;
(2) putting the solution into a microwave reactor, and heating for 30min at 150 ℃, wherein the microwave power of the microwave reactor is 200W;
(3) after the reaction is finished, centrifugally separating the solution on a high-speed centrifuge at the rotating speed of 6000 rpm for 5 minutes, and removing the solution in a centrifugal tube to obtain a precipitation product;
(4) washing the precipitated product with absolute ethanol, placing the precipitated product in a muffle furnace, and calcining the product in air at 150 ℃ for 2.5 hours to obtain the final productSingle atom catalyst Pt/CeO2。
The test of the catalytic performance was carried out in a plasma reactor at a voltage of 25KV and the gas content of VOCs was determined by gas chromatography. The concentration of formaldehyde is 1000mg/m3The space velocity is 20000h-1The concentrations of the reactants and products were measured by gas chromatograph, and the inlet and outlet concentrations of ozone were measured by ozone analyzer. The formaldehyde removal rate # 1 is shown in Table 1.
The formaldehyde in the detection process is replaced by toluene, the content is 300ppm, other detection conditions are unchanged, and the removal rate of toluene # 1 is shown in Table 2.
Example 2
(1) Dissolving cerium acetate in deionized water, then adding ammonia water and ammonium carbonate into a cerium acetate solution to enable the pH of the solution to be 8.5, adding ammonium chloroplatinate into the solution, wherein the mass ratio of the ammonium chloroplatinate to the cerium acetate added into the solution is 1: 15;
(2) putting the solution into a microwave reactor, and heating for 20min at 200 ℃, wherein the microwave power of the microwave reactor is 300W;
(3) after the reaction is finished, centrifugally separating the solution on a high-speed centrifuge at the rotating speed of 7000 rpm for 8 minutes, and removing the solution in the centrifuge tube to obtain a precipitation product;
(4) washing the precipitated product with deionized water, then placing the precipitated product in a muffle furnace, and then calcining the product in air at 200 ℃ for 2 hours to finally obtain the monatomic catalyst Pt/CeO2。
The test of the catalytic performance was carried out in a plasma reactor at a voltage of 25KV and the gas content of VOCs was determined by gas chromatography. The concentration of formaldehyde is 1000mg/m3The space velocity is 20000h-1The concentrations of the reactants and products were measured by gas chromatograph, and the inlet and outlet concentrations of ozone were measured by ozone analyzer. The formaldehyde removal rate of # 2 is shown in Table 1.
The formaldehyde in the detection process is replaced by toluene, the content is 300ppm, other detection conditions are unchanged, and the removal rate of toluene # 2 is shown in Table 2.
Example 3
(1) Dissolving ammonium ceric nitrate and cerous nitrate in deionized water, then adding ammonium carbonate into a cerium-containing compound solution to make the pH of the solution equal to 9, and adding ammonium chloroplatinate into the solution, wherein the mass ratio of the ammonium chloroplatinate added into the solution to the cerium-containing compound is 1: 20;
(2) putting the solution into a microwave reactor, and heating for 15min at 250 ℃, wherein the microwave power of the microwave reactor is 500W;
(3) after the reaction is finished, centrifugally separating the solution on a high-speed centrifuge for 10 minutes at the rotating speed of 8000 rpm, and removing the solution in a centrifugal tube to obtain a precipitate;
(4) washing the precipitated product with deionized water, placing the precipitated product in a muffle furnace, and calcining the product in air at 250 ℃ for 1.5 hours to obtain the monatomic catalyst Pt/CeO2。
The test of the catalytic performance was carried out in a plasma reactor at a voltage of 25KV and the gas content of VOCs was determined by gas chromatography. The concentration of formaldehyde is 1000mg/m3The space velocity is 20000h-1The concentrations of the reactants and products were measured by gas chromatograph, and the inlet and outlet concentrations of ozone were measured by ozone analyzer. The formaldehyde removal rate of # 3 is shown in Table 1.
The formaldehyde in the detection process is replaced by toluene, the content is 300ppm, other detection conditions are unchanged, and the 3# toluene removal rate is shown in table 2.
Example 4
(1) Dissolving cerium acetate in deionized water, then adding ammonium carbonate into a cerium acetate solution to enable the pH of the solution to be 9, and adding ammonium chloroplatinate into the solution, wherein the mass ratio of the ammonium chloroplatinate to the cerium acetate added into the solution is 1: 30;
(2) putting the solution into a microwave reactor, and heating for 10min at 300 ℃, wherein the microwave power of the microwave reactor is 700W;
(3) after the reaction is finished, centrifugally separating the solution on a high-speed centrifuge at the rotating speed of 10000 rpm for 15 minutes, and removing the solution in a centrifugal tube to obtain a precipitate;
(4) washing the precipitated product with absolute ethanol, then placing the precipitated product in a muffle furnace, then calcining in air at 300 ℃ for 2.5 hours,finally obtaining the single-atom catalyst Pt/CeO2。
The test of the catalytic performance was carried out in a plasma reactor at a voltage of 25KV and the gas content of VOCs was determined by gas chromatography. The concentration of formaldehyde is 1000mg/m3The space velocity is 20000h-1The concentrations of the reactants and products were measured by gas chromatograph, and the inlet and outlet concentrations of ozone were measured by ozone analyzer. The 4# formaldehyde removal is shown in Table 1.
The formaldehyde in the detection process is replaced by toluene, the content is 300ppm, other detection conditions are unchanged, and the 4# toluene removal rate is shown in table 2.
TABLE 1 catalytic Formaldehyde purification reactivity on catalyst
Figure GDA0002776310300000061
TABLE 2 catalytic purification reaction performance of toluene on catalyst
Figure GDA0002776310300000071

Claims (4)

1. A preparation method of a monatomic catalyst for degrading VOCs is characterized by comprising the following steps:
(1) dissolving a cerium-containing compound in deionized water, adding an alkaline substance into a cerium-containing compound solution to enable the pH of the solution to be 8-9, adding ammonium chloroplatinate into the solution, wherein the mass ratio of the ammonium chloroplatinate added into the solution to the cerium-containing compound is 1: 10-30;
(2) putting the solution into a microwave reactor, and heating for 10-30 min at 150-300 ℃;
(3) after the reaction is finished, carrying out centrifugal separation on the solution on a high-speed centrifuge at the rotating speed of 6000-10000 rpm for 5-15 minutes, and removing the solution in the centrifuge tube to obtain a precipitation product;
(4) washing the precipitated product with deionized water or absolute ethanol, and then placing the precipitated product in a muffle furnace, and then washing the product at 150E to ECalcining the mixture for 1.5 to 2.5 hours in air at the temperature of 300 ℃ to finally obtain the monatomic catalyst Pt/CeO2。
2. The method of claim 1 for preparing a monatomic catalyst for the degradation of VOCs, wherein: the cerium-containing compound is one or more of cerium nitrate, cerium acetate or ammonium cerium nitrate.
3. The method of claim 1 or 2, wherein the monatomic catalyst is selected from the group consisting of: the alkaline substance in the step (1) is one or two of ammonia water or ammonium carbonate.
4. The method of claim 3, wherein the monatomic catalyst is selected from the group consisting of: the microwave power of the microwave reactor in the step (2) is 200W-700W.
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CN110026186A (en) * 2019-04-30 2019-07-19 太原氦舶新材料有限责任公司 A kind of monatomic catalyst of metal of activated carbon from activated sludge load and its preparation and application
CN110465291B (en) * 2019-08-09 2022-02-25 太原理工大学 Monoatomic noble metal type catalyst Ru/Cr2O3And preparation method and application thereof

Citations (5)

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CN102836712A (en) * 2011-06-24 2012-12-26 上海牛翼新能源科技有限公司 Catalyst for completely removing formaldehyde in indoor air at room temperature
CN103551180A (en) * 2013-11-19 2014-02-05 中国海洋石油总公司 Preparation method of C10+ bicyclo-heavy aromatics selective hydrogenation cracking catalyst
CN103706358A (en) * 2013-12-02 2014-04-09 唐雅蓉 Preparation method of Pt-CeO2 catalyst
CN104162425A (en) * 2014-07-21 2014-11-26 贝谷科技股份有限公司 Catalyst for complete catalytic oxidation of indoor low concentration formaldehyde at room temperature
CN106622227A (en) * 2016-12-29 2017-05-10 天津大学 Preparation method of monoatomic catalyst for indoor air purification

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102836712A (en) * 2011-06-24 2012-12-26 上海牛翼新能源科技有限公司 Catalyst for completely removing formaldehyde in indoor air at room temperature
CN103551180A (en) * 2013-11-19 2014-02-05 中国海洋石油总公司 Preparation method of C10+ bicyclo-heavy aromatics selective hydrogenation cracking catalyst
CN103706358A (en) * 2013-12-02 2014-04-09 唐雅蓉 Preparation method of Pt-CeO2 catalyst
CN104162425A (en) * 2014-07-21 2014-11-26 贝谷科技股份有限公司 Catalyst for complete catalytic oxidation of indoor low concentration formaldehyde at room temperature
CN106622227A (en) * 2016-12-29 2017-05-10 天津大学 Preparation method of monoatomic catalyst for indoor air purification

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