CN111408371A - Efficient and stable Pt/CeO for oxidative degradation of VOCs2-TiO2Process for preparing catalyst - Google Patents
Efficient and stable Pt/CeO for oxidative degradation of VOCs2-TiO2Process for preparing catalyst Download PDFInfo
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- CN111408371A CN111408371A CN202010458552.2A CN202010458552A CN111408371A CN 111408371 A CN111408371 A CN 111408371A CN 202010458552 A CN202010458552 A CN 202010458552A CN 111408371 A CN111408371 A CN 111408371A
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/63—Platinum group metals with rare earths or actinides
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
- B01J37/035—Precipitation on carriers
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- 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
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
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Abstract
The invention provides a high-efficiency stable Pt/CeO for VOCs oxidative degradation2‑TiO2The preparation method of the catalyst adopts a precipitation method to prepare CeO by taking cheap cerous chloride or cerous nitrate, titanium tetrachloride and a small amount of chloroplatinic acid as raw materials2‑TiO2The Pt/CeO is prepared by loading Pt on the composite oxide carrier by adopting an electroless deposition method2‑TiO2Catalyst, CeO in catalyst2/TiO2The optimal molar ratio of (A) is 4:1 to 1: 1. The catalyst has simple preparation process and low cost. The catalyst prepared by the invention is particularly suitable for catalyzing organic waste gas containing chlorine VOCs or coexisting with non-chlorine VOCs containing benzene, normal hexane and the likeThe complete oxidation temperature of the catalyst to dichloroethane and n-hexane is only about 290 ℃ and 140 ℃ respectively, the catalytic activity of the catalyst does not decrease when the dichloroethane and the n-hexane coexist, and the catalyst has excellent low-temperature catalytic oxidation degradation activity and stability and good application prospect.
Description
Technical Field
The invention relates to a method for preparing a catalyst, in particular to a method for preparing a catalystIs high-efficiency and stable Pt/CeO for the oxidative degradation of VOCs2-TiO2A method for preparing the catalyst.
Background
Volatile Organic Compounds (VOCs) are compounds which are extremely harmful to the environment and human health, are widely derived from waste gas emission in industries such as petrochemical production, printing and coating, food and rubber production and the like, and are often complex in components and large in exhaust amount, while a catalytic combustion technology is one of important and effective means for purifying VOCs pollutants, and development of a catalyst which is low in cost, efficient, stable and good in broad spectrum is a key for realizing application of the technology. CeO (CeO)2-TiO2The composite oxide has rich weak and medium strong acid centers, is very favorable for the catalytic degradation of chlorine-Containing VOCs (CVOCs), has good tolerance, but when the waste gas contains other non-chlorine-containing VOCs (such as normal hexane, benzene and the like), the CeO is easy to be caused due to the insufficient oxidizing capability of the catalyst2-TiO2The catalyst deposits carbon to affect the stability of the catalyst. The catalyst has good acidity and oxidizability, can promote deep oxidation of intermediate products while maintaining the environment favorable for CVOCs to absorb broken bonds, and has high oxidation performance on other non-chlorine-containing VOCs. Therefore, the development of a highly stable and highly adaptable catalyst for combustion of organic exhaust gas has become a significant issue for the wide application of catalytic combustion technology.
Disclosure of Invention
The invention aims to provide an efficient and stable organic waste gas combustion catalyst, in particular to Pt/CeO2-TiO2A method for preparing the catalyst. The invention is realized by the following technical scheme:
the invention discloses a high-efficiency stable Pt/CeO for VOCs oxidative degradation2-TiO2Method for preparing catalyst from chloroplatinic acid (H)2PtCl6) Cerium salt, titanium tetrachloride (TiCl)4) Is prepared from CeO by precipitation2-TiO2The Pt/CeO is prepared by loading Pt on the composite oxide carrier by adopting an electroless deposition method2-TiO2Catalyst, CeO in catalyst2/TiO2The molar ratio of (a) to (b) is 4: 1-1: 4, and the preparation method specifically comprises the following steps:
the first step is as follows: as described in CeO2/TiO2Adding inorganic acid into the aqueous solution of cerium salt, stirring uniformly at 0 ℃, and dripping TiCl4Continuously stirring the solution until the solution is transparent, and then dropwise adding ammonia water (NH) with the concentration of 0.5-2.0 mol/L under vigorous stirring3·H2O) until the pH value of the solution reaches 9.5-11.0, standing and aging for 6-12 hours at room temperature, then filtering, washing with deionized water for multiple times until the filtrate is neutral, drying at 80-100 ℃, roasting at 400-550 ℃ for 1-4 hours, and obtaining CeO2-TiO2A composite oxide;
the second step is that: mixing the powder CeO2-TiO2Dispersing the composite oxide in deionized water, adding vitamin C (Vc) after uniformly stirring, washing for a plurality of times by using the deionized water after continuously stirring for 1-2 hours, and then adding H2PtCl6Stirring the aqueous solution for 2-4 hours, filtering, washing with deionized water for multiple times until no Cl is detected in the filtrate-Drying at 60-100 ℃, and roasting at 400-500 ℃ for 1-3 hours to obtain Pt/CeO2-TiO2A catalyst.
As a further improvement, the CeO of the present invention2/TiO2The optimal molar ratio of (A) is 4:1 to 1: 1.
As a further improvement, the cerium salt of the invention is cerous nitrate (Ce (NO)3)3·6H2O) or cerous chloride (CeCl)3·7H2O).
As a further improvement, the inorganic acid of the invention is hydrochloric acid (HCl).
As a further improvement, the Pt loaded by the electroless deposition method of the invention means that CeO is pretreated by Vc solution2-TiO2Composite oxide support, Re-impregnation H2PtCl6Loading Pt; the addition amount of Vc is as follows: CeO (CeO)2The molar ratio to Vc is less than 3.0.
The invention provides Pt/CeO2-TiO2The preparation method of the catalyst has the advantages that:
cheap cerous chloride or cerous nitrate, titanium tetrachloride and small amount of chloroplatinic acid are used as raw materials to prepare CeO by precipitation method2-TiO2The Pt/CeO is prepared by loading Pt on the composite oxide carrier by adopting an electroless deposition method2-TiO2Catalyst, CeO in catalyst2/TiO2The optimal molar ratio of the organic waste gas to the organic waste gas is 4: 1-1: 1, the preparation process is simple, the catalyst cost is low, and the organic waste gas combustion catalyst is efficient and stable. The catalyst prepared by the invention is particularly suitable for catalytic combustion of organic waste gas containing chlorine-containing VOCs or coexisting with non-chlorine-containing VOCs containing benzene, n-hexane and the like, the complete oxidation temperature of the catalyst to dichloroethane and n-hexane is only about 290 ℃ and 140 ℃ respectively, the catalytic activity of the catalyst is not reduced when the dichloroethane and n-hexane coexist, and the catalyst has excellent low-temperature catalytic oxidation degradation activity and stability and good application prospect.
The specific implementation mode is as follows:
the technical solution of the present invention is further illustrated by the following specific examples:
example 1
31.4g cerous nitrate is dissolved in 200ml water, 6.0ml concentrated hydrochloric acid is added, and after even stirring under ice bath condition, 14.0g TiCl is dropped4The solution (concentration: 98%) was stirred until it became clear, and then ammonia (NH) was added dropwise at a concentration of 1.0 mol/L under vigorous stirring3·H2O) until the pH value of the solution reaches 10.0, and the solution is placed and aged for 12 hours at room temperature. Then filtering, washing with deionized water for several times until the filtrate is neutral, drying at 90 deg.C for 12 hr, roasting at 500 deg.C for 2 hr to obtain CeO2/TiO2CeO in a molar ratio of 1:12-TiO2A composite oxide.
2g of powdered CeO2-TiO2The composite oxide is dispersed in 200ml of deionized water, 1.76g of vitamin C is added after uniform stirring, and the mixture is washed for a plurality of times by the deionized water after being continuously stirred for 1 hour. Then 1ml of H was added2PtCl6The aqueous solution (the concentration is 10mgPt/ml), the pH value of the mixed solution is 6.0, the mixture is stirred for 3 hours, filtered and washed by deionized water for multiple times until no Cl is detected in the filtrate-And dried at 70 ℃ for 12 hoursRoasting at 400 deg.c for 2 hr to obtain Pt/CeO with Pt loading of 0.5%2-TiO2A catalyst.
Example 2
The same procedure as in example 1 was used, except that: the dosage of cerous nitrate is changed to 7.85g, and CeO is contained in the catalyst2/TiO2The molar ratio is 1: 4.
Example 3
The same procedure as in example 1 was used, except that: the dosage of cerous nitrate is changed to 15.7g, and CeO is contained in the catalyst2/TiO2The molar ratio is 1: 2.
Example 4
The same procedure as in example 1 was used, except that: the dosage of cerous nitrate is changed to 31.4g, TiCl4The amount of the solution was changed to 7.0g, and CeO was contained in the catalyst2/TiO2The molar ratio was 2: 1.
Example 5
The same procedure as in example 1 was used, except that: the dosage of cerous nitrate is changed to 31.4g, TiCl4The amount of the solution was changed to 3.5g, and CeO was contained in the catalyst2/TiO2The molar ratio was 4: 1.
Example 6
The same procedure as in example 1 was used, except that: the dosage of cerous nitrate is changed to 31.4g, TiCl4The amount of the solution was changed to 1.75g, and CeO was contained in the catalyst2/TiO2The molar ratio was 8: 1.
Example 7
The same procedure as in example 1 was used, except that: the amount of cerous nitrate was changed to 0g, TiCl4The amount of the solution was changed to 14.0g, and CeO was contained in the catalyst2/TiO2The molar ratio was 0: 1.
Example 8
The same procedure as in example 1 was used, except that: the dosage of the cerous nitrate is changed to cerous chloride, and the dosage is changed to 26.94g, TiCl4The amount of the solution was changed to 14.0g, and CeO was contained in the catalyst2/TiO2The molar ratio is 1: 1.
The catalytic degradation activity of the catalyst on VOCs in the examples 1-8 is shown in the following table:
note: 0.3ml of catalyst with the particle size of 40-60 meshes and the space velocity of 15000h－1。
The above table lists the various CeO2/TiO2Ratio 0.5% Pt/CeO2-TiO2Catalytic Oxidation Activity of catalyst (examples 1-8) on n-Hexane, complete conversion of n-Hexane (conversion)>90%) of temperature (T)90) Lower means higher oxidation activity of the catalyst; CeO (CeO)2/TiO2The catalyst has a complete oxidation temperature of about 140 ℃ for n-hexane at an optimum molar ratio of 4:1 to 1: 1. The oxidation activity of the catalyst on other various VOCs (benzene, ethyl acetate, acetonitrile and dichloroethane) is evaluated by taking the catalyst prepared in example 4 as a representative, and the various VOCs can be completely oxidized and converted at the temperature of below 290 ℃, which shows that the catalyst has good broad-spectrum adaptability.
Finally, it is also noted that the above-mentioned list is only a few specific embodiments of the present invention. It is obvious that the invention is not limited to the above embodiments, but that many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (5)
1. Efficient and stable Pt/CeO for oxidative degradation of VOCs2-TiO2The preparation method of the catalyst is characterized in that chloroplatinic acid (H) is used2PtCl6) Cerium salt, titanium tetrachloride (TiCl)4) Is prepared from CeO by precipitation2-TiO2The Pt/CeO is prepared by loading Pt on the composite oxide carrier by adopting an electroless deposition method2-TiO2Catalyst, CeO in catalyst2/TiO2The molar ratio of (a) to (b) is 4: 1-1: 4, and the preparation method specifically comprises the following steps:
the first step is as follows: as described in CeO2/TiO2Adding inorganic acid into the aqueous solution of cerium salt, stirring uniformly at 0 ℃, and dripping TiCl4Continuously stirring the solution until the solution is transparent, and then dropwise adding ammonia water (NH) with the concentration of 0.5-2.0 mol/L under vigorous stirring3·H2O) until the pH value of the solution reaches 9.5-11.0, standing and aging for 6-12 hours at room temperature, then filtering, washing with deionized water for multiple times until the filtrate is neutral, drying at 80-100 ℃, roasting at 400-550 ℃ for 1-4 hours, and obtaining CeO2-TiO2A composite oxide;
the second step is that: mixing the powder CeO2-TiO2Dispersing the composite oxide in deionized water, adding vitamin C (Vc) after uniformly stirring, washing for a plurality of times by using the deionized water after continuously stirring for 1-2 hours, and then adding H2PtCl6Stirring the aqueous solution for 2-4 hours, filtering, washing with deionized water for multiple times until no Cl is detected in the filtrate-Drying at 60-100 ℃, and roasting at 400-500 ℃ for 1-3 hours to obtain Pt/CeO2-TiO2A catalyst.
2. Pt/CeO according to claim 12-TiO2The preparation method of the catalyst is characterized in that the CeO2/TiO2The optimal molar ratio of (A) is 4:1 to 1: 1.
3. Pt/CeO according to claim 12-TiO2The preparation method of the catalyst is characterized in that the cerium salt is cerous nitrate (Ce (NO)3)3·6H2O) or cerous chloride (CeCl)3·7H2O).
4. Pt/CeO according to claim 12-TiO2The preparation method of the catalyst is characterized in that the inorganic acid is hydrochloric acid (HCl).
5. According to claim1 said Pt/CeO2-TiO2The preparation method of the catalyst is characterized in that the Pt loaded by the electroless deposition method is to pretreat CeO by using Vc solution2-TiO2Composite oxide support, Re-impregnation H2PtCl6Loading Pt; the addition amount of Vc is as follows: CeO (CeO)2The molar ratio to Vc is less than 3.0.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112169788A (en) * | 2020-10-15 | 2021-01-05 | 南京工业大学 | Organic mixed waste gas rare earth-based catalytic combustion catalyst and preparation method and application thereof |
| 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 |
| CN113996292A (en) * | 2021-10-20 | 2022-02-01 | 北京动力机械研究所 | Preparation and application of integral torch combustion catalyst |
| 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) |
| CN116328753A (en) * | 2023-02-16 | 2023-06-27 | 五邑大学 | TiO (titanium dioxide) 2 -CeO 2 Composite nano material and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112169788A (en) * | 2020-10-15 | 2021-01-05 | 南京工业大学 | Organic mixed waste gas rare earth-based catalytic combustion catalyst and preparation method and application thereof |
| CN112169788B (en) * | 2020-10-15 | 2023-10-27 | 南京工业大学 | Organic mixed waste gas rare earth-based catalytic combustion catalyst and preparation method and application thereof |
| 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 |
| CN113996292A (en) * | 2021-10-20 | 2022-02-01 | 北京动力机械研究所 | Preparation and application of integral torch combustion catalyst |
| CN113996292B (en) * | 2021-10-20 | 2023-12-19 | 北京动力机械研究所 | Preparation and application of integral torch burning catalyst |
| 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) |
| CN116328753A (en) * | 2023-02-16 | 2023-06-27 | 五邑大学 | TiO (titanium dioxide) 2 -CeO 2 Composite nano material and preparation method and application thereof |
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