CN114602525B - Aluminum nitride-based ceramic organic matter contaminated soil thermal desorption catalyst and preparation method and application thereof - Google Patents
Aluminum nitride-based ceramic organic matter contaminated soil thermal desorption catalyst and preparation method and application thereof Download PDFInfo
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
- B09C1/08—Reclamation of contaminated soil chemically
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- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/02—Soil-conditioning materials or soil-stabilising materials containing inorganic compounds only
- C09K17/08—Aluminium compounds, e.g. aluminium hydroxide
Abstract
The invention discloses a thermal desorption catalyst for soil polluted by aluminum nitride-based ceramic organic matters and a preparation method thereof. Based on the mass of the carrier, the mass percentage of the catalytic active component is 1% -5%, and the mass percentage of the cocatalyst is 0.5% -1%. After roasting aluminum nitride powder into ceramic wafers at high temperature, modifying the surface of aluminum nitride ceramic by using a plasma surface treatment instrument, then carrying out acid pickling corrosion on activated carbon by using dilute hydrochloric acid to further improve the concentration of hydroxyl on the surface of aluminum nitride ceramic, soaking the aluminum nitride ceramic into a mixed solution of an active component and a promoter precursor, and carrying out adsorption, drying and roasting to obtain the aluminum nitride ceramic. The catalyst is environment-friendly, high in mechanical strength and high in thermal conductivity, 100% desorption of 3-chlorobiphenyl can be realized at 230 ℃, and the thermal desorption energy consumption of 3-chlorobiphenyl is greatly reduced. The product can be widely applied to the field of thermal desorption of soil organic pollutants.
Description
Technical Field
The invention relates to an aluminum nitride-based ceramic organic matter contaminated soil thermal desorption catalyst and a preparation method and application thereof, belonging to the field of environmental protection catalytic materials and soil remediation.
Background
With the rapid development of economic and town construction and the promulgation of national related policies, chemical enterprises leave a large number of organic contaminated sites. The organic matters not only directly cause great harm to soil animals, plants, microorganisms and an ecological system, but also can enter a human body in a steam inhalation mode, a skin contact mode and the like, and the great harm is generated to the human body. The repair and treatment work of the soil of the organic matter polluted site becomes an important problem of unavoidable nationality and relativity civilians, and the treatment and repair requirements have important social value and economic value.
Research on various repair technologies and equipment for organic contaminated sites is widely carried out in recent years, and related research results are also applied to the repair of the contaminated sites. The thermal desorption restoration technology has the advantages of high treatment efficiency, short restoration period, wide application range and the like, and is widely applied to fields such as soil, sludge, sediment and the like containing volatile and semi-volatile organic pollutants. The pollutants which can be treated by thermal desorption comprise polychlorinated biphenyl, nitrobenzene, polybrominated diphenyl ether, chlorobenzene, mercury, polycyclic aromatic hydrocarbon and the like. However, the contaminants in the contaminated soil are not evenly distributedAnd contaminants tend to have a relatively high boiling point, requiring a significant amount of heat energy to be consumed during processing. Wherein, the organic matters such as polychlorinated biphenyl and the like have high molecular weight and high boiling point, so that the energy required by thermal desorption is obviously increased. Patent CN103658165a indicates that the high temperature tail gas generated during the repair process is the main part of heat energy loss in the thermal desorption system, and for the conventional rotary kiln heating system, the soil throughput is 25m 3 And/h, the heat loss emitted by the high-temperature flue gas is 30-60%. The high-temperature flue gas can cause heat loss and difficult tail gas treatment, so that the tail gas treatment cost is increased. Therefore, how to optimize the thermal desorption system has important engineering significance for reducing heat loss and pollution soil disposal cost.
Disclosure of Invention
The invention aims to provide an aluminum nitride ceramic-based organic matter polluted soil thermal desorption catalyst aiming at the current situation and problems of the existing soil thermal desorption, and the other aim of the invention is to provide a preparation method and application of the catalyst.
The catalyst uses an aluminum nitride ceramic wafer as a carrier, lanthanum yttrium composite oxide as a catalytic active component and nickel oxide as a cocatalyst. Based on the mass of the carrier, the mass percentage of the catalytic active component is 1% -5%, the mass percentage of the cocatalyst is 0.5% -1%, and the mass ratio of lanthanum oxide to yttrium oxide in the active component is 1: (0.2-1).
The preparation method of the catalyst comprises the following steps:
(1) Preparation of ceramic wafer carrier
Pressurizing aluminum nitride powder in a mould, maintaining the pressure, preparing a ceramic wafer blank, and then placing the ceramic wafer blank in a kiln to calcine the ceramic wafer blank in a nitrogen protective atmosphere to obtain an aluminum nitride ceramic wafer;
(2) Surface modification of ceramic wafer carrier
Placing the aluminum nitride ceramic wafer in a plasma surface treatment instrument, vacuumizing the plasma surface treatment instrument, then filling oxygen, and performing surface treatment to form an oxide layer on the surface of the aluminum nitride ceramic wafer; then placing the modified aluminum nitride ceramic wafer in a dilute hydrochloric acid solution, and soaking and corroding for 6-12 h to obtain a ceramic wafer carrier with a modified surface;
(3) Preparation of active component and cocatalyst precursor Mixed solution
Weighing lanthanum salt, yttrium salt and nickel salt, adding the lanthanum salt, yttrium salt and nickel salt into deionized water, and stirring in a water bath at 50-70 ℃ until the solution is clear and transparent to obtain a mixed solution of an active component and a promoter precursor;
(4) Catalyst preparation
And (3) immersing the ceramic wafer carrier subjected to surface modification prepared in the step (2) in the mixed solution of the active component and the promoter precursor prepared in the step (3), placing the ceramic wafer carrier subjected to surface modification in a blast drying oven for heat preservation and drying after the mixed solution is completely adsorbed, and then placing the ceramic wafer carrier into a muffle furnace for roasting to prepare the aluminum nitride ceramic-based organic matter contaminated soil thermal desorption catalyst.
The preparation method comprises the following steps: the aluminum nitride powder in the step (1) is YB-AlN (Beijing Shangbang new material science and technology Co., ltd.), the pressurizing pressure is 10-15 MPa, the pressure maintaining time is 1-3 min, the gas flow rate of the protective atmosphere nitrogen is 10-30 min/mL, the calcining temperature is 1600-1800 ℃, and the temperature is kept for 6-12 h.
The preparation method comprises the following steps: the Plasma surface treatment instrument in the step (2) is Plasma clean-PL-5010 (environmental protection technology Co., ltd., winko) with an input voltage of 220V, a working distance of 5-12 mm, a Plasma flame scanning rate of 20-100 mm/s and a surface treatment time of 1-3 h.
The preparation method comprises the following steps: the volume/mass ratio of the oxygen-filled aluminum nitride ceramic in the step (2) is (1-2) mL:1g, the mass ratio of the aluminum nitride ceramic wafer to the dilute hydrochloric acid solution is 1: 15-20 mass percent of dilute hydrochloric acid with the mass concentration of 10-15 percent.
The preparation method comprises the following steps: the lanthanum salt in the step (3) is lanthanum nitrate hexahydrate or lanthanum chloride heptahydrate, the yttrium salt is yttrium nitrate hexahydrate or yttrium chloride hexahydrate, the nickel salt is nickel nitrate hexahydrate or nickel chloride hexahydrate, and the mass ratio of the lanthanum salt to deionized water is 1: (2-5).
The preparation method comprises the following steps: the drying temperature in the step (4) is 80-100 ℃ and the drying time is 4-6 h; the roasting temperature is 400-500 ℃, and the heat preservation is carried out for 1.5-3 hours.
The technical scheme of the invention is as follows: the application of the catalyst in degrading organic pollutant in soil.
Further: the organic pollutant is 3-chlorobiphenyl.
The technical scheme of the invention is as follows: the aluminum nitride ceramic wafer is obtained by roasting aluminum nitride powder at high temperature to form a ceramic wafer, modifying the surface of the aluminum nitride ceramic by using a plasma surface treatment instrument, and then carrying out acid pickling corrosion on activated carbon by using dilute hydrochloric acid to further improve the hydroxyl concentration on the surface of the aluminum nitride ceramic.
Thermal desorption experimental conditions and results of the invention: 50g of soil containing 1% of 3-chlorobiphenyl is taken and put into a catalyst performance evaluation reaction device, the inner diameter of a quartz tube in the reaction device is evaluated to be 20mm, and hot air at 190-230 ℃ is introduced to perform performance evaluation. The soil heating temperature was 190 to 230℃and the catalyst amount was 3 pieces (15 g total). The desorption effect of 3-chlorobiphenyl can reach 100% when the thermal desorption is carried out at 230 ℃ for 20min, and the activity of the catalyst is still stable and unchanged after 10 times of catalyst circulation.
The beneficial effects are that:
the catalyst prepared by the invention has the following advantages:
(1) The aluminum nitride ceramic carrier not only has high thermal conductivity, can promote the catalyst to form a local high-temperature zone under the same circulating hot air and time conditions, shortens the gasification time of organic pollutants, reduces the environmental temperature required by the surface activation of the organic pollutants on the catalyst, but also has higher mechanical strength, can easily separate soil from the catalyst after thermal desorption is finished, and simultaneously ensures that the catalyst is not damaged in the soil extraction process;
(2) The active components lanthanum yttrium composite oxide and the promoter nickel oxide have excellent oxidation-reduction performance, and can be used for catalytically decomposing 3-chlorobiphenyl into small molecules at low temperature, so that the thermal desorption temperature of the 3-chlorobiphenyl is greatly reduced;
(3) After the aluminum nitride ceramic carrier in the catalyst is subjected to surface modification, a thin aluminum oxide layer is formed, and the aluminum oxide layer, the active components and the cocatalyst have synergistic catalysis, so that the catalytic thermal desorption effect is improved;
therefore, the catalyst prepared by the invention not only can greatly reduce the energy consumption of soil thermal desorption and the industrial thermal desorption cost, but also has the advantages of environment-friendly catalyst components, simple preparation process, lower cost, high cost performance and stronger application and popularization value.
Drawings
FIG. 1 is a graph of the performance of the catalyst prepared in example 1;
FIG. 2 is a graph of the performance of the catalyst prepared in example 2;
FIG. 3 is a graph of the performance of the catalyst prepared in example 3;
Detailed Description
The invention is further illustrated below with reference to examples, but the scope of the invention is not limited thereto:
the aluminum nitride powder is YB-AlN, and the manufacturer is: beijing Ming bang New Material technologies Co.
The Plasma surface treatment instrument is of a Plasma clean-PL-5010 type, and the manufacturers are: environmental protection technology Co.Ltd.
Example 1
(1) Preparation of ceramic wafer carrier
Weighing 5g of aluminum nitride powder, adding the aluminum nitride powder into a die, pressurizing to 10MPa, keeping the pressure for 1min, taking out a sample, repeating the blank molding for 10 times to obtain 10 aluminum nitride ceramic blanks, placing the 10 aluminum nitride ceramic blanks in a kiln, and calcining the 10 aluminum nitride ceramic blanks at 1600 ℃ under the protection atmosphere of nitrogen (the gas flow rate is 10 min/mL) to obtain aluminum nitride ceramic wafers;
(2) Surface modification of ceramic wafer carrier
Placing 1 piece of aluminum nitride ceramic wafer obtained in the step (1) in a plasma surface treatment instrument, vacuumizing the plasma surface treatment instrument, then filling 5mL of oxygen, carrying out surface treatment for 1h, and forming a thin aluminum oxide layer on the surface of the aluminum nitride ceramic wafer, wherein the input voltage is 220V, the working distance is 5mm, and the plasma flame scanning speed is 20 mm/s; repeating plasma surface modification for 10 times to obtain 10 aluminum nitride ceramic wafers subjected to plasma surface modification, and then placing the modified aluminum nitride ceramic wafers in 750g of dilute hydrochloric acid solution with the mass concentration of 10%, and soaking for 6 hours to obtain a ceramic wafer carrier subjected to surface modification;
(3) Preparation of active component and cocatalyst precursor Mixed solution
1.1075g of lanthanum nitrate hexahydrate, 0.2827g of yttrium nitrate hexahydrate and 0.9731g of nickel nitrate hexahydrate are weighed, added into 5.5375g of deionized water and stirred in a water bath at 50 ℃ until the solution is clear and transparent, so as to obtain a mixed solution of an active component and a promoter precursor;
(4) Preparation of the catalyst
Based on the mass of the carrier, the mass percentage of the active component to the mass of the carrier is 1%, the mass percentage of the cocatalyst to the mass of the carrier is 0.5%, and the mass ratio of lanthanum oxide to yttrium oxide in the active component is 1:0.2, weighing 50g of the surface-modified aluminum nitride ceramic wafer carrier prepared in the step (2), immersing the surface-modified aluminum nitride ceramic wafer carrier in the mixed solution of the active component and the promoter precursor prepared in the step (3), placing the ceramic wafer carrier in a blast drying oven after the mixed solution is completely adsorbed, preserving heat for 4 hours at 80 ℃ for drying, and placing the ceramic wafer carrier in a muffle furnace for roasting at 400 ℃ for 1.5 hours to prepare the aluminum nitride ceramic-based organic matter contaminated soil thermal desorption catalyst;
(4) Catalytic Activity test
As shown in FIG. 1, 50g of a soil containing 1% of 3-chlorobiphenyl was charged into a catalyst performance evaluation reaction apparatus, the inside diameter of a quartz tube in the reaction apparatus was evaluated to be 20mm, and hot air at 190 to 230℃was introduced to evaluate the performance. The soil heating temperature was 190 to 230℃and the catalyst amount was 3 pieces (15 g total). The desorption effect of 3-chlorobiphenyl can reach 100% when the thermal desorption is carried out at 230 ℃ for 20min, and the activity of the catalyst is still stable and unchanged after 10 times of catalyst circulation.
Example 2:
(1) Preparation of ceramic wafer carrier
Weighing 5g of aluminum nitride powder, adding the aluminum nitride powder into a die, pressurizing to 15MPa, keeping the pressure for 3min, taking out a sample, repeating the blank molding for 10 times to obtain 10 aluminum nitride ceramic blanks, placing the 10 aluminum nitride ceramic blanks in a kiln, and calcining the 10 aluminum nitride ceramic blanks at 1800 ℃ under the protection atmosphere of nitrogen (the gas flow rate is 30 min/mL) to obtain aluminum nitride ceramic wafers;
(2) Surface modification of ceramic wafer carrier
Placing 1 piece of aluminum nitride ceramic wafer obtained in the step (1) in a plasma surface treatment instrument, vacuumizing the plasma surface treatment instrument, then filling 10mL of oxygen, carrying out surface treatment for 2 hours, and forming a thin aluminum oxide layer on the surface of the aluminum nitride ceramic wafer, wherein the input voltage is 220V, the working distance is 12mm, and the plasma flame scanning speed is 100 mm/s; repeating plasma surface modification for 10 times to obtain 10 aluminum nitride ceramic wafers subjected to plasma surface modification, and then placing the modified aluminum nitride ceramic wafers in 1000g of dilute hydrochloric acid solution with the mass concentration of 15%, and soaking for 12 hours to obtain a ceramic wafer carrier subjected to surface modification;
(3) Preparation of active component and cocatalyst precursor Mixed solution
2.8495g of lanthanum chloride heptahydrate, 3.3585g of yttrium chloride hexahydrate and 2.0249g of nickel chloride hexahydrate are weighed, added into 5.6990g of deionized water and stirred in a water bath at 70 ℃ until the solution is clear and transparent, so as to obtain a mixed solution of an active component and a promoter precursor;
(4) Preparation of the catalyst
Based on the mass of the carrier, the mass percentage of the active component to the mass of the carrier is 5%, the mass percentage of the cocatalyst to the mass of the carrier is 1%, and the mass ratio of lanthanum oxide to yttrium oxide in the active component is 1:1, weighing 50g of the surface-modified aluminum nitride ceramic wafer carrier prepared in the step (2), immersing the surface-modified aluminum nitride ceramic wafer carrier in the mixed solution of the active component and the promoter precursor prepared in the step (3), placing the ceramic wafer carrier in a blast drying oven after the mixed solution is completely adsorbed, preserving heat for 6 hours at 100 ℃ for drying, and placing the ceramic wafer carrier in a muffle furnace for roasting for 3 hours at 500 ℃ to prepare the thermal desorption catalyst for the organic matter contaminated soil of the aluminum nitride ceramic matrix;
(4) Catalytic Activity test
As shown in FIG. 2, 50g of a soil containing 1% of 3-chlorobiphenyl was charged into a catalyst performance evaluation reaction apparatus, the inside diameter of a quartz tube in the reaction apparatus was evaluated to be 20mm, and hot air at 190 to 230℃was introduced to evaluate the performance. The soil heating temperature was 190 to 230℃and the catalyst amount was 3 pieces (15 g total). The desorption effect of the 3-chlorobiphenyl can reach 100% when the thermal desorption is carried out for 30min at 190 ℃, and the activity of the catalyst is still stable and unchanged after 10 times of catalyst circulation.
Example 3:
(1) Preparation of ceramic wafer carrier
Weighing 5g of aluminum nitride powder, adding the aluminum nitride powder into a die, pressurizing to 15MPa, keeping the pressure for 1min, taking out a sample, repeating the blank molding for 10 times to obtain 10 aluminum nitride ceramic blanks, placing the 10 aluminum nitride ceramic blanks in a kiln, and calcining the 10 aluminum nitride ceramic blanks at 1700 ℃ for 8 hours under the protection atmosphere of nitrogen (the gas flow rate is 20 min/mL) to obtain aluminum nitride ceramic wafers;
(2) Surface modification of ceramic wafer carrier
Placing 1 piece of aluminum nitride ceramic wafer obtained in the step (1) in a plasma surface treatment instrument, vacuumizing the plasma surface treatment instrument, then filling 7mL of oxygen, carrying out surface treatment for 3 hours, and forming a thin aluminum oxide layer on the surface of the aluminum nitride ceramic wafer, wherein the input voltage is 220V, the working distance is 8mm, and the plasma flame scanning speed is 60 mm/s; repeating plasma surface modification for 10 times to obtain 10 aluminum nitride ceramic wafers subjected to plasma surface modification, and then placing the modified aluminum nitride ceramic wafers in 900g of 17% dilute hydrochloric acid solution, and soaking for 10 hours to obtain a ceramic wafer carrier subjected to surface modification;
(3) Preparation of active component and cocatalyst precursor Mixed solution
2.8495g of lanthanum chloride heptahydrate, 3.3585g of yttrium chloride hexahydrate and 0.9731g of nickel nitrate hexahydrate are weighed, added into 5.6990g of deionized water and stirred in a water bath at 70 ℃ until the solution is clear and transparent, so as to obtain a mixed solution of an active component and a promoter precursor;
(4) Preparation of the catalyst
Based on the mass of the carrier, the mass percentage of the active component to the mass of the carrier is 5 percent, the mass percentage of the cocatalyst to the mass of the carrier is 0.5 percent, and the mass ratio of lanthanum oxide to yttrium oxide in the active component is 1:1, weighing 50g of the surface-modified aluminum nitride ceramic wafer carrier prepared in the step (2), immersing the surface-modified aluminum nitride ceramic wafer carrier in the mixed solution of the active component and the promoter precursor prepared in the step (3), placing the ceramic wafer carrier in a blast drying oven after the mixed solution is completely adsorbed, preserving heat for 6 hours at 90 ℃ for drying, and placing the ceramic wafer carrier in a muffle furnace for roasting for 2 hours at 450 ℃ to prepare the thermal desorption catalyst for the organic matter contaminated soil of the aluminum nitride ceramic matrix;
(4) Catalytic Activity test
As shown in FIG. 3, 50g of a soil containing 1% of 3-chlorobiphenyl was charged into a catalyst performance evaluation reaction apparatus, the inside diameter of a quartz tube in the reaction apparatus was evaluated to be 20mm, and hot air at 190 to 230℃was introduced to evaluate the performance. The soil heating temperature was 190 to 230℃and the catalyst amount was 3 pieces (15 g total). The desorption effect of the 3-chlorobiphenyl can reach 100% when the catalyst is thermally desorbed for 30min at 210 ℃, and the activity of the catalyst is still stable and unchanged after 10 times of catalyst circulation.
Comparative example 1
(1) Preparation of the catalyst
The conditions were the same as in example 1 except that the surface modification in step (2) was not performed on the aluminum nitride ceramic wafer carrier during catalyst preparation;
(2) Contrast effect
Compared with the example 1, the surface modification in the step (2) is not carried out when the catalyst is prepared, and the mixed solution of the active component and the promoter precursor is difficult to adsorb in the ceramic carrier, so that the aluminum nitride-based ceramic thermal desorption catalyst is difficult to prepare.
Comparative example 2
(1) Preparation of the catalyst
The conditions were the same as in example 2 except that lanthanum yttrium composite oxide was not added as a catalytically active component in the preparation of the catalyst;
(2) Catalytic Activity test
50g of soil containing 1% of 3-chlorobiphenyl is taken and put into a catalyst performance evaluation reaction device, the inner diameter of a quartz tube in the reaction device is evaluated to be 20mm, and hot air at 190-230 ℃ is introduced to perform performance evaluation. The soil heating temperature was 190 to 230℃and the catalyst amount was 3 pieces (15 g total). The desorption effect of the 3-chlorobiphenyl is 54% when the thermal desorption is carried out at 230 ℃ for 30 min.
(3) Contrast effect
Compared with the embodiment 2, the catalyst is prepared without adding lanthanum yttrium composite oxide as a catalytic active component, and the catalyst promoter nickel oxide has certain oxidation-reduction performance, so that 3-chlorobiphenyl is catalytically degraded into small molecules, and the catalyst has certain thermal desorption activity at the temperature lower than the boiling point of 3-chlorobiphenyl, but the thermal desorption activity is obviously lower than that of an aluminum nitride ceramic-based catalyst with lanthanum yttrium composite oxide as the catalytic active component.
Comparative example 3
(1) Preparation of the catalyst
The conditions were the same as in example 3 except that alumina powder was replaced with aluminum nitride powder at the time of catalyst preparation;
(2) Catalytic Activity test
50g of soil containing 1% of 3-chlorobiphenyl is taken and put into a catalyst performance evaluation reaction device, the inner diameter of a quartz tube in the reaction device is evaluated to be 20mm, and hot air at 190-230 ℃ is introduced to perform performance evaluation. The soil heating temperature was 190 to 230℃and the catalyst amount was 3 pieces (15 g total). The desorption effect of the 3-chlorobiphenyl can reach 61% when the thermal desorption is carried out at 230 ℃ for 30 min.
(3) Contrast effect
Compared with example 3, the aluminum nitride powder is replaced by the aluminum oxide powder, the thermal conductivity of the catalyst is obviously reduced, and the catalyst cannot form a local high-temperature zone under the same circulating hot air and time conditions, so that the gasification time of organic pollutants is prolonged, and the activity is obviously reduced.
Claims (8)
1. An aluminum nitride ceramic-based organic matter contaminated soil thermal desorption catalyst is characterized in that: the catalyst takes an aluminum nitride ceramic wafer as a carrier, lanthanum yttrium composite oxide as a catalytic active component and nickel oxide as a cocatalyst, the mass percentage of the catalytic active component is 1% -5% based on the mass of the carrier, the mass percentage of the cocatalyst is 0.5% -1%, and the mass ratio of lanthanum oxide to yttrium oxide in the active component is 1: (0.2-1);
the preparation method of the catalyst comprises the following steps:
(1) Preparation of ceramic wafer carrier
Pressurizing aluminum nitride powder in a mould, maintaining the pressure, preparing a ceramic wafer blank, and then placing the ceramic wafer blank in a kiln to calcine the ceramic wafer blank in a nitrogen protective atmosphere to obtain an aluminum nitride ceramic wafer;
(2) Surface modification of ceramic wafer carrier
Placing the aluminum nitride ceramic wafer in a plasma surface treatment instrument, vacuumizing the plasma surface treatment instrument, then filling oxygen, and performing surface treatment to form an oxide layer on the surface of the aluminum nitride ceramic wafer; then placing the modified aluminum nitride ceramic wafer in a dilute hydrochloric acid solution, and soaking and corroding for 6-12 hours to obtain a ceramic wafer carrier with a modified surface;
(3) Preparation of active component and cocatalyst precursor Mixed solution
Weighing lanthanum salt, yttrium salt and nickel salt, adding the lanthanum salt, yttrium salt and nickel salt into deionized water, and stirring in a water bath at 50-70 ℃ until the solution is clear and transparent to obtain a mixed solution of an active component and a promoter precursor;
(4) Catalyst preparation
And (3) immersing the ceramic wafer carrier subjected to surface modification prepared in the step (2) in the mixed solution of the active component and the promoter precursor prepared in the step (3), placing the ceramic wafer carrier subjected to surface modification in a blast drying oven for heat preservation and drying after the mixed solution is completely adsorbed, and then placing the ceramic wafer carrier into a muffle furnace for roasting to prepare the aluminum nitride ceramic-based organic matter contaminated soil thermal desorption catalyst.
2. The aluminum nitride ceramic matrix organic matter contaminated soil thermal desorption catalyst according to claim 1, wherein: the aluminum nitride powder in the step (1) has the pressurization pressure of 10-15 MPa, the dwell time of 1-3 min, the gas flow rate of the protective atmosphere nitrogen of 10-30 min/mL, the calcination temperature of 1600-1800 ℃ and the heat preservation time of 6-12 h.
3. The aluminum nitride ceramic matrix organic matter contaminated soil thermal desorption catalyst according to claim 1, wherein: the Plasma surface treatment instrument in the step (2) is of a Plasma clean-PL-5010 type, the input voltage during surface treatment is 220V, the working distance is 5-12 mm, the Plasma flame scanning speed is 20-100 mm/s, and the surface treatment time is 1-3 h.
4. The aluminum nitride ceramic matrix organic matter contaminated soil thermal desorption catalyst according to claim 1, wherein: the volume/mass ratio of the oxygen filled ceramic to the aluminum nitride ceramic in the step (2) is (1-2) mL:1g, the mass ratio of the aluminum nitride ceramic wafer to the dilute hydrochloric acid solution is 1: 15-20% of diluted hydrochloric acid, and the mass concentration of the diluted hydrochloric acid is 10-15%.
5. The aluminum nitride ceramic matrix organic matter contaminated soil thermal desorption catalyst according to claim 1, wherein: the lanthanum salt in the step (3) is lanthanum nitrate hexahydrate or lanthanum chloride heptahydrate, the yttrium salt is yttrium nitrate hexahydrate or yttrium chloride hexahydrate, and the nickel salt is nickel nitrate hexahydrate or nickel chloride hexahydrate.
6. The aluminum nitride ceramic matrix organic matter contaminated soil thermal desorption catalyst according to claim 1, wherein: the drying temperature in the step (4) is 80-100 ℃ and the drying time is 4-6 h; the roasting temperature is 400-500 ℃, and the heat preservation is carried out for 1.5-3 hours.
7. Use of the catalyst of claim 1 for degrading organic contaminants in soil.
8. The use according to claim 7, characterized in that: the organic pollutant is 3-chlorobiphenyl.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110756213A (en) * | 2019-11-07 | 2020-02-07 | 中国科学院上海高等研究院 | Aluminum nitride-based catalyst, preparation method and application |
| CN113019412A (en) * | 2021-03-08 | 2021-06-25 | 大连理工大学 | Catalyst for preparing olefin by light alkane dehydrogenation, preparation method and application thereof |
| CN113731409A (en) * | 2021-09-28 | 2021-12-03 | 昆明理工大学 | Catalytic oxidation purification catalyst for thermal desorption waste gas of organic contaminated soil and preparation method and application thereof |
| CN113877597A (en) * | 2021-08-06 | 2022-01-04 | 南京工业大学 | Thermal desorption monatomic catalyst for organic matter contaminated soil and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10651080B2 (en) * | 2016-04-26 | 2020-05-12 | Lam Research Corporation | Oxidizing treatment of aluminum nitride films in semiconductor device manufacturing |
-
2022
- 2022-03-24 CN CN202210294751.3A patent/CN114602525B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110756213A (en) * | 2019-11-07 | 2020-02-07 | 中国科学院上海高等研究院 | Aluminum nitride-based catalyst, preparation method and application |
| CN113019412A (en) * | 2021-03-08 | 2021-06-25 | 大连理工大学 | Catalyst for preparing olefin by light alkane dehydrogenation, preparation method and application thereof |
| CN113877597A (en) * | 2021-08-06 | 2022-01-04 | 南京工业大学 | Thermal desorption monatomic catalyst for organic matter contaminated soil and preparation method thereof |
| CN113731409A (en) * | 2021-09-28 | 2021-12-03 | 昆明理工大学 | Catalytic oxidation purification catalyst for thermal desorption waste gas of organic contaminated soil and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 上海半导体器件研究所.《半导体器件新工艺技术译文集》.上海半导体器件研究所,1980,第61-62页. * |
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