CN111420697A - Pt/Ce-USY catalyst for oxidative degradation of chlorine-containing VOCs and preparation method thereof - Google Patents

Pt/Ce-USY catalyst for oxidative degradation of chlorine-containing VOCs and preparation method thereof Download PDF

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CN111420697A
CN111420697A CN202010263327.3A CN202010263327A CN111420697A CN 111420697 A CN111420697 A CN 111420697A CN 202010263327 A CN202010263327 A CN 202010263327A CN 111420697 A CN111420697 A CN 111420697A
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usy
catalyst
chlorine
hours
ceo
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周仁贤
李志明
石壹军
王佳露
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Zhejiang University ZJU
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J29/00—Catalysts comprising molecular sieves
    • B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
    • B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
    • B01J29/08—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y
    • B01J29/10—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y containing iron group metals, noble metals or copper
    • B01J29/12—Noble metals
    • B01J29/126—Y-type faujasite
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
    • F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
    • F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
    • F23G7/07—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
    • B01J2229/10—After treatment, characterised by the effect to be obtained
    • B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
    • F23G2209/00—Specific waste
    • F23G2209/14—Gaseous waste or fumes
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
    • F23G2209/00—Specific waste
    • F23G2209/14—Gaseous waste or fumes
    • F23G2209/142—Halogen gases, e.g. silane

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Environmental & Geological Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Catalysts (AREA)
  • Exhaust Gas Treatment By Means Of Catalyst (AREA)

Abstract

The invention discloses a Pt/Ce-USY catalyst for oxidative degradation of chlorine-containing VOCs and a preparation method thereof, and provides a preparation method of the Pt/Ce-USY catalyst for oxidative degradation of chlorine-containing VOCs, which takes platinum II tetramine dichloride, cerous chloride and an ultrastable Y molecular sieve as raw materials and adopts a precipitation-deposition method to load CeO2Pt is loaded by an ion exchange method to prepare a Pt/Ce-USY catalyst, and CeO in the catalyst2And the content of Pt is 3-20% and 0.1-0.45% respectively. The catalyst has the advantages of simple preparation process, low cost, good low-temperature catalytic oxidation activity and stability for chlorine-containing and non-chlorine-containing VOCs, and good application prospect.

Description

Pt/Ce-USY catalyst for oxidative degradation of chlorine-containing VOCs and preparation method thereof
Technical Field
The invention relates to a preparation method of a catalyst for low-temperature oxidative degradation of chlorine-containing VOCs, in particular to a Pt/Ce-USY catalyst for oxidative degradation of chlorine-containing VOCs and a preparation method thereof.
Background
chlorine-Containing Volatile Organic Compounds (CVOCs) are compounds which are extremely harmful to the environment and human health, and common compounds include Dichloromethane (DCM), trichloromethane (CF), Dichloroethane (DCE), Trichloroethylene (TCE), Carbon Tetrachloride (CT), chlorobenzene (PhCl), and the like, and because of their good chemical stability, they are generally widely used as organic solvents and semi-finished products in chemical production processes. The catalytic combustion technology is one of important and effective means for purifying CVOCs pollutants, and the development of a low-cost and high-performance catalyst is the key for realizing the application of the technology. Solid acid (such as molecular sieve) is compounded with cerium-based oxide, so that the catalyst has good acidity and oxidizability, and can promote deep oxidation of intermediate products while maintaining the environment beneficial to adsorption and bond breaking of CVOCs, thereby attracting much attention in recent years. However, the chlorine-containing organic waste gas discharged from the actual industry often contains non-chlorine-containing hydrocarbon organic compounds (such as benzene, alkane, etc.), but the non-noble metal catalyst has low oxidation activity on such VOCs, and in addition, due to competitive adsorption, the catalyst is not favorable for adsorbing and activating CVOCs, and is easy to be deactivated by carbon deposition. Therefore, the development of the high-efficiency, broad-spectrum and stable chlorine-containing organic waste gas combustion catalyst has important significance for the wide application of the catalytic combustion technology.
Disclosure of Invention
The invention aims to provide a high-efficiency broad-spectrum chlorine-containing organic waste gas combustion catalyst, in particular to a Pt/Ce-USY catalyst for the oxidative degradation of chlorine-containing VOCs and a preparation method thereof, and the invention is realized by the following technical scheme:
the invention discloses a Pt/Ce-USY catalyst for oxidative degradation of chlorine-containing VOCs (volatile organic compounds), which is prepared by taking platinum (II) (Pt (NH) tetraammine chloride3)4Cl2·H2O), cerous chloride (CeCl)3·7H2O), ammonium ultrastable Y molecular sieve (NH)4-USY) as main raw material, and carrying CeO by precipitation-deposition method2Pt is loaded by an ion exchange method to prepare a Pt/Ce-USY catalyst, and CeO in the catalyst2The content is 3-20%, and the content of Pt is 0.1-0.45%.
The invention also discloses a preparation method of the Pt/Ce-USY catalyst for oxidative degradation of the chlorine-containing VOCs, which comprises the following specific preparation steps:
1) as described in CeO2CeCl with a content of 0.012-0.12 mol/L3Adding a set amount of powdered NH to the aqueous solution4-USY, adding ammonia (NH) with concentration of 1.0 mol/L dropwise under vigorous stirring after stirring uniformly3·H2O), dropwise adding the mixture until the pH value of the mixed solution reaches 9-11, standing at room temperature for aging for 12 hours, then filtering, washing with deionized water for multiple times until the filtrate is neutral, drying at 60 ℃ for 12 hours, and roasting at 550 ℃ for 2 hours to obtain Ce-USY;
2) pt (NH) at a set concentration according to the Pt content3)4Cl2Adding a certain amount of powder Ce-USY into the aqueous solution, refluxing at 100 deg.C for 3 hr, cooling to room temperature, adding excessive formaldehyde solution (CH)2O) is placed for 4 hours, then filtered and washed by deionized water for a plurality of times until no Cl is detected in the filtrate-Drying at 60 ℃ for 12 hours, and roasting at 500 ℃ for 2 hours to prepare the Pt/Ce-USY catalyst.
As a further improvement, the CeO of the present invention2The optimum content of the Pt is 6-12%, and the optimum content of the Pt is 0.3-0.45%.
As a further improvement, in the step 2) of the invention, CH2The molar ratio of O to Pt is greater than 5.0.
The preparation method of the Pt/Ce-USY catalyst provided by the invention has the advantages that: the Pt/Ce-USY catalyst is prepared by adopting cheap cerous chloride, an industrially produced USY molecular sieve and a small amount of Pt (platinum II dichlorotetramine) as raw materials and adopting a precipitation-deposition combined ion exchange method, has simple preparation process, low cost and high low-temperature oxidation activity, and is a high-efficiency broad-spectrum chlorine-containing organic waste gas combustion catalyst. The catalyst has good low-temperature catalytic degradation activity and stability for chlorine-containing VOCs such as dichloroethane and the like and non-chlorine-containing VOCs such as benzene and the like, and has important significance for wide application of catalytic combustion technology.
The specific implementation mode is as follows:
the invention discloses a Pt/Ce-USY catalyst for oxidative degradation of chlorine-containing VOCs and a preparation method thereof, wherein the catalyst is prepared by taking platinum-IV-diammine-dichloride II (Pt (NH)3)4Cl2·H2O), cerous chloride (CeCl)3·7H2O), ammonium ultrastable Y molecular sieve (NH)4-USY) as main raw material and adopting precipitation-deposition method to prepare negativeCarried CeO2Pt is loaded by an ion exchange method to prepare a Pt/Ce-USY catalyst, and CeO in the catalyst2The content of the Pt is 3-20%, the content of the Pt is 0.1-0.45%, and the specific preparation steps are as follows:
1) as described in CeO2CeCl with a content of 0.012-0.12 mol/L3Adding a set amount of powdered NH to the aqueous solution4-USY, adding ammonia (NH) with concentration of 1.0 mol/L dropwise under vigorous stirring after stirring uniformly3·H2O), dropwise adding the mixture until the pH value of the mixed solution reaches 9-11, standing at room temperature for aging for 12 hours, then filtering, washing with deionized water for multiple times until the filtrate is neutral, drying at 60 ℃ for 12 hours, and roasting at 550 ℃ for 2 hours to obtain Ce-USY;
2) pt (NH) at a set concentration according to the Pt content3)4Cl2Adding a certain amount of powder Ce-USY into the aqueous solution, refluxing at 100 deg.C for 3 hr, cooling to room temperature, adding excessive formaldehyde solution (CH)2O) is placed for 4 hours, then filtered and washed by deionized water for a plurality of times until no Cl is detected in the filtrate-Drying at 60 ℃ for 12 hours, and roasting at 500 ℃ for 2 hours to prepare the Pt/Ce-USY catalyst.
CeO2The optimal content of (2) is 6-12%, the optimal content of Pt is 0.3-0.45%, and in the step 2), CH2The molar ratio of O to Pt is greater than 5.0.
The technical solution of the present invention is further illustrated by the following specific examples:
example 1
1.3g of cerous chloride was dissolved in 100ml of water, and 10g of powdered NH was added4-USY, adding ammonia (NH) with concentration of 1.0 mol/L dropwise under vigorous stirring after stirring uniformly3·H2O) is added to the mixed solution in a dropwise manner until the pH value of the mixed solution reaches 10.0, then the mixed solution is placed at room temperature for aging for 12 hours, then the mixed solution is filtered and washed by deionized water for multiple times until the filtrate is neutral, the mixed solution is dried for 12 hours at the temperature of 60 ℃, and is roasted for 2 hours at the temperature of 550 ℃ to obtain CeO2Ce-USY with the content of 6 percent.
Dissolving 0.081g of tetraammineplatinum dichloride II in 100ml of water, adding the powder Ce-USY, carrying out reflux reaction at 100 ℃ for 3 hours, cooling to room temperature, addingPlacing the formaldehyde solution for 4 hours, filtering, washing with deionized water for many times until no Cl is detected in the filtrate-Drying at 60 ℃ for 12 hours, and roasting at 500 ℃ for 2 hours to prepare the Pt/Ce-USY catalyst. CeO in the catalyst2And Pt contents of 6% and 0.45%, respectively.
Example 2
The same procedure as in example 1 was used, except that: the dosage of the platinum II tetrammine dichloride is changed to 0.054g, and CeO in the catalyst2And Pt contents of 6% and 0.3%, respectively.
Example 3
The same procedure as in example 1 was used, except that: the dosage of the tetraammineplatinum dichloride II is changed to 0.018g, and CeO is contained in the catalyst2And Pt contents of 6% and 0.1%, respectively.
Example 4
The same procedure as in example 1 was used, except that: the dosage of the cerous chloride is changed to 2.6g, and CeO is contained in the catalyst2And Pt contents of 12% and 0.45%, respectively.
Example 5
The same procedure as in example 1 was used, except that: the dosage of the cerous chloride is changed to 4.3g, and CeO is contained in the catalyst2And Pt contents of 20% and 0.45%, respectively.
Example 6
The same procedure as in example 1 was used, except that: the dosage of the cerous chloride is changed to 0.65g, and CeO is contained in the catalyst2And Pt contents of 3% and 0.45%, respectively.
Example 7
The same procedure as in example 1 was used, except that: the obtained Ce-USY does not further load Pt, and CeO in the catalyst2And Pt contents of 6% and 0%, respectively.
Example 8
The same procedure as in example 1 was used, except that: will not contain CeO2The USY of (1) directly supports Pt, and CeO in the catalyst2And Pt contents of 0% and 0.45%, respectively.
The catalytic degradation activity of the catalyst on chlorinated organic compounds in examples 1-4 is shown in the following table:
Figure BDA0002440228120000041
note: 0.3ml of catalyst with the particle size of 40-60 meshes and the space velocity of 15000h－1。T90The smaller the value, the higher the low-temperature oxidation activity of the catalyst.
The foregoing description is not intended to limit the present invention, and it should be noted that various changes, modifications, additions and substitutions may be made by those skilled in the art without departing from the spirit and scope of the present invention, and such changes and modifications should be construed as within the scope of the present invention.

Claims (4)

1. A Pt/Ce-USY catalyst for the oxidative degradation of chlorine-containing VOCs is characterized in that platinum II (Pt (NH) tetraammine chloride is used3)4Cl2·H2O), cerous chloride (CeCl)3·7H2O), ammonium ultrastable Y molecular sieve (NH)4-USY) as main raw material, and carrying CeO by precipitation-deposition method2And loading Pt by an ion exchange method to prepare a Pt/Ce-USY catalyst, wherein CeO in the catalyst2The content is 3-20%, and the content of Pt is 0.1-0.45%.
2. A preparation method of a Pt/Ce-USY catalyst for oxidative degradation of chlorine-containing VOCs comprises the following specific preparation steps:
1) as described in CeO2CeCl with a content of 0.012-0.12 mol/L3Adding a set amount of powdered NH to the aqueous solution4-USY, adding ammonia (NH) with concentration of 1.0 mol/L dropwise under vigorous stirring after stirring uniformly3·H2O), dropwise adding the mixture until the pH value of the mixed solution reaches 9-11, standing at room temperature for aging for 12 hours, then filtering, washing with deionized water for multiple times until the filtrate is neutral, drying at 60 ℃ for 12 hours, and roasting at 550 ℃ for 2 hours to obtain Ce-USY;
2) pt (NH) at a set concentration according to the Pt content3)4Cl2Dissolving in waterAdding a certain amount of powder Ce-USY into the solution, refluxing at 100 deg.C for 3 hr, cooling to room temperature, adding excessive formaldehyde solution (CH)2O) is placed for 4 hours, then filtered and washed by deionized water for a plurality of times until no Cl is detected in the filtrate-Drying at 60 ℃ for 12 hours, and roasting at 500 ℃ for 2 hours to prepare the Pt/Ce-USY catalyst.
3. The method for preparing Pt/Ce-USY catalyst for oxidative degradation of VOCs containing chlorine as claimed in claim 2, wherein said CeO2The optimum content of the Pt is 6-12%, and the optimum content of the Pt is 0.3-0.45%.
4. The method for preparing the Pt/Ce-USY catalyst for oxidative degradation of VOCs containing chlorine according to claim 3, wherein in the step 2), CH is added2The molar ratio of O to Pt is greater than 5.0.
CN202010263327.3A 2020-04-07 2020-04-07 Pt/Ce-USY catalyst for oxidative degradation of chlorine-containing VOCs and preparation method thereof Pending CN111420697A (en)

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CN112058217A (en) * 2020-09-04 2020-12-11 山东大学 Silicon-based adsorption material capable of being rapidly regenerated and method for microwave in-situ degradation of organic pollutants
CN112588289A (en) * 2020-12-01 2021-04-02 光大环境修复(江苏)有限公司 High CO2Selective CVOCs removal catalyst and preparation method thereof
CN113145161A (en) * 2020-12-31 2021-07-23 南京大学 Catalyst for catalytic oxidation of volatile organic compounds by ozone and preparation method thereof
CN114471682A (en) * 2022-01-18 2022-05-13 安庆市长三角未来产业研究院 Catalyst suitable for CVOCs catalytic combustion and preparation method and application thereof
CN115518673A (en) * 2022-10-25 2022-12-27 浙江大学 Preparation method of Pt-CeTi composite molecular sieve catalyst for efficiently degrading VOCs (volatile organic compounds)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112058217A (en) * 2020-09-04 2020-12-11 山东大学 Silicon-based adsorption material capable of being rapidly regenerated and method for microwave in-situ degradation of organic pollutants
CN112588289A (en) * 2020-12-01 2021-04-02 光大环境修复(江苏)有限公司 High CO2Selective CVOCs removal catalyst and preparation method thereof
CN113145161A (en) * 2020-12-31 2021-07-23 南京大学 Catalyst for catalytic oxidation of volatile organic compounds by ozone and preparation method thereof
CN114471682A (en) * 2022-01-18 2022-05-13 安庆市长三角未来产业研究院 Catalyst suitable for CVOCs catalytic combustion and preparation method and application thereof
CN114471682B (en) * 2022-01-18 2023-07-07 安庆市长三角未来产业研究院 Catalyst applicable to CVOCs catalytic combustion as well as preparation method and application thereof
CN115518673A (en) * 2022-10-25 2022-12-27 浙江大学 Preparation method of Pt-CeTi composite molecular sieve catalyst for efficiently degrading VOCs (volatile organic compounds)

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