CN110586103A - Preparation method of alkali-modified cobalt-based catalyst for low-temperature catalytic degradation of vinyl chloride, product and application thereof - Google Patents
Preparation method of alkali-modified cobalt-based catalyst for low-temperature catalytic degradation of vinyl chloride, product and application thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of an alkali-modified cobalt-based catalyst for low-temperature catalytic degradation of vinyl chloride, and a product and application thereof. The catalyst is Co modified by Mg, Ca, Sr or Ba alkali metal M3O4Wherein the molar ratio of M to Co is 1: (9-24). The catalyst is prepared by a step precipitation-adsorption method, and the precipitator is sodium carbonate (Na)2CO3). The catalyst has simple preparation method, can effectively improve the catalytic oxidation activity of the cobalt-based catalyst on chloroethylene by alkali modification, and is particularly suitable for eliminating chlorinated volatile organic compounds by low-temperature catalytic combustion.
Description
Technical Field
The invention belongs to the technical field of catalytic environmental protection, and particularly relates to a preparation method of an alkali-modified cobalt-based catalyst for low-temperature catalytic degradation of vinyl chloride, and a product and application thereof.
Background
Vinyl Chloride (VC) is listed as a first class carcinogenic substance by the International agency for research on cancers 10 and 27 months in 2017 and also is listed as a first class carcinogenic substance by the United states environmental protection agency at the same time due to high toxicity and high carcinogenicity. It has great harm to natural living things and human body. Therefore, countries in the world set stricter environmental regulations for discharge of the VC, and increasingly higher requirements are put on control and discharge of the VC in the countries in the world. VC is an important industrial intermediate, widely used in various industrial processes, and thus it is difficult to achieve complete control from the source. Therefore, how to effectively eliminate the emission of VC pollutants in the industrial production process is an important concern of environmental researchers. However, due to its high toxicity and strict regulations, there is currently very little worldwide research on the catalytic combustion of vinyl chloride.
Co3O4The catalyst is one of transition metals with highest removal activity for VOCs at present, and has higher catalytic oxidation activity for removing CVOCs. But still less active compared to noble metals (Pt, Pd, Ru, Rh), and Co3O4Polychlorinated byproducts are easily generated on the surface of the catalyst by catalytic oxidation. The catalyst with better activity applied to the catalytic combustion of chloroethylene at present is Ru/Co3O4Catalyst, Guo et al (CN 201710446994, RSC adv., 2016, 6, 99577) studied the catalytic combustion performance of vinyl chloride on noble metal ruthenium catalysts supported on different carriers, and the research results show that Ru/Co3O4The catalyst shows higher activity and stability to low-temperature catalytic combustion of vinyl chloride, and the activity of the catalyst depends on Ru and Co3O4The mutual synergy between the two components.
However, the noble metal catalyst is still relatively high in cost and relatively poor in stability. There are many methods for increasing the activity of cobalt-based catalysts, among which Co is added3O4Other metals are introduced or subjected to surface modification, so that the catalytic performance of the cobalt-based catalyst can be effectively improved. The invention takes into account that the chlorine-containing volatile organic compounds generate acidic species in the catalytic oxidation reaction process3O4Alkali metal M (Mg, Ca, Sr or Ba) is introduced to perform alkaline modification on the surface of the material, so that the activation of chloroethylene on the surface of the chloroethylene is promoted on one hand, and the catalytic oxidation activity is improved; on the other hand, the catalytic oxygen of the chloroethylene is effectively transferred through proper amount of alkaline modificationAcidic species generated in the reaction process are oxidized, so that the stability of the catalyst is improved.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of an alkali modified cobalt-based catalyst for low-temperature catalytic degradation of vinyl chloride.
Yet another object of the present invention is to: provides an alkali modified cobalt-based catalyst product for low-temperature catalytic degradation of vinyl chloride, which is prepared by the method.
Yet another object of the present invention is to: provides an application of the product.
The purpose of the invention is realized by the following scheme: a process for preparing the alkali modified Co-based catalyst used for low-temp catalytic degradation of chloroethylene by fractional precipitation-adsorption method features that the sodium carbonate (Na) is used as precipitant2CO3) The catalyst is obtained by step precipitation-adsorption under the stirring of water bath, and the method comprises the following steps:
(1) preparing a sodium carbonate aqueous solution with the concentration of 0.5 ~ 1.0.0 mol/L;
(2) preparing a cobalt nitrate solution with the concentration of 0.1 ~ 0.2.2 mol/L;
(3) preparing a nitrate solution of Mg, Ca, Sr or Ba alkali metal (M) with the same concentration as that in the step (2);
(4) according to the molar concentration ratio of M to Co of 1: (9-24) cobalt nitrate solution and alkali metal nitrate solution are respectively taken and respectively marked as V1And V2；
(5) Taking sodium carbonate solution and recording as V3Making the molar amount thereof 3 times the total molar amount of the cobalt nitrate and the alkali metal taken out in the step (4);
(6) the V taken out in the step (4) is hydrothermally processed at 40 ~ 60 ℃ and 60 DEG C1Adding V taken out in the step (5)3Stirring for 20min to obtain precipitate;
(7) v taken out in the step (4)2Adding the precipitate obtained in the step (6) into the mixture, and continuously stirring the mixture for 20min to obtain a precipitate;
(8) continuing to remove the rest of V2/2 addition step(7) Stirring the obtained precipitate for 20min to obtain precipitate;
(9) precipitating for overnight aging to obtain a precursor;
(8) washing the obtained precursor with deionized water for 3-5 times, and then washing with ethanol for 2-3 times;
(9) the obtained precursor was dried at 40 ~ 60 ℃ overnight;
(10) and uniformly grinding the dried precursor, and roasting at 400 ~ 500 ℃ for 2-4h to obtain the catalyst.
The invention further improves the activity and stability of the cobalt-based catalyst on the catalytic combustion of the chlorohydrocarbon by carrying out surface alkaline modification on the cobalt-based catalyst on the basis of the existing research, and reduces the generation of polychlorinated byproducts on the catalyst.
The invention also provides an alkali-modified cobalt-based catalyst for low-temperature catalytic degradation of vinyl chloride, which is prepared by the method and is an alkali metal-modified cobalt-based catalyst, wherein the alkali metal is one of M (Mg, Ca, Sr or Ba), and the molar ratio of M to Co is 1: 9-1: 24.
the invention also provides an application of the alkali modified cobalt-based catalyst in low-temperature catalytic degradation of vinyl chloride.
The activity evaluation of the catalyst used for the catalytic combustion of vinyl chloride is carried out in a fixed bed microreactor (a quartz tube with an inner diameter of 3 mm), the dosage of the catalyst is 200mg, and the temperature is automatically controlled by a K-type thermocouple. The chloroethylene standard gas is mixed with air and enters a reactor for combustion. The total flow is controlled by a mass flow meter, the concentration of chloroethylene is 0.05 vol%, air is used as carrier gas, the concentration of oxygen is 10%, the reaction temperature is 140-. The relationship between the conversion of vinyl chloride and the reaction temperature is shown in Table 1, wherein T50%、T90%The reaction temperatures required for 50% and 90% conversion, respectively. The reaction tail gas is subjected to chromatographic on-line tracking, and the main reaction products are HCl, carbon dioxide, water and a very small amount of trichloroethylene.
Compared with the existing catalyst, the catalyst and the preparation method thereof have the characteristics that: (1) the activity and stability of the cobalt-based catalyst are improved through surface alkali modification; (2) reduces the polychlorinated byproducts.
Detailed Description
Example 1
A cobalt-based catalyst for low-temperature catalytic degradation of vinyl chloride is prepared by the following steps:
(1) na with the concentration of 0.5mol/L is prepared2CO3An aqueous solution;
(2) preparing a cobalt nitrate aqueous solution with the concentration of 0.2 mol/L;
(3) taking 25ml of the cobalt nitrate solution prepared in the step (2), and recording the solution as V1；
(4) Taking 30ml of the sodium carbonate solution prepared in the step (1), and recording the solution as a solution V2；
(5) V taken out in the step (3) is subjected to hydrothermal condition at 40 DEG C1Adding V taken out in the step (4)2Stirring for 20min to obtain precipitate;
(6) the obtained precipitate was aged overnight;
(7) washing the obtained precursor with deionized water for 5 times, and then continuing washing with ethanol for 3 times;
(8) drying the obtained precursor at 60 ℃ overnight;
(9) grinding the dried precursor uniformly, and roasting at 500 ℃ for 4h to obtain the catalyst of the invention, which is recorded as Co3O4(ii) a The catalytic oxidation activity of vinyl chloride on different catalysts is shown in table 1.
Example 2
An alkali-modified cobalt-based catalyst for low-temperature catalytic degradation of vinyl chloride is prepared by a fractional precipitation-adsorption method, wherein a precipitator is obtained by fractional precipitation-adsorption under water bath stirring, and the catalyst is prepared by the following steps:
(1) na with the concentration of 0.5mol/L is prepared2CO3An aqueous solution;
(2) preparing a cobalt nitrate solution with the concentration of 0.2 mol/L;
(3) preparing a barium nitrate solution with the concentration of 0.2 mol/L;
(4) get24ml of the cobalt nitrate solution prepared in step (2) are designated V1Taking 1ml of the barium nitrate solution prepared in the step (3) and recording the solution as V2；
(5) Taking 30ml of Na prepared in the step (1)2CO3Solution, denoted solution V3；
(6) V taken out in the step (4) is subjected to hydrothermal condition at 50 DEG C1Adding V taken out in the step (5)3Stirring for 20min to obtain precipitate;
(7) v taken out in the step (4)2Adding the precipitate obtained in the step (6) into the mixture, and continuously stirring the mixture for 20min to obtain a precipitate;
(8) continuing to remove the rest of V2Adding the precipitate obtained in the step (7) into the solution, and continuously stirring the solution for 20min to obtain a precipitate;
(9) the obtained precipitate is aged overnight to obtain a precursor;
(8) washing the obtained precursor with deionized water for 5 times, and then continuing washing with ethanol for 3 times;
(9) drying the obtained precursor at 60 ℃ overnight;
(10) uniformly grinding the dried precursor, and roasting at 500 ℃ for 4h to obtain the catalyst, which is recorded as Co24Ba 1; the catalytic oxidation activity of vinyl chloride on different catalysts is shown in table 1.
Example 3
An alkali modified cobalt-based catalyst for low-temperature catalytic degradation of vinyl chloride is prepared by the following steps:
(1) preparing a sodium carbonate aqueous solution with the concentration of 0.5 mol/L;
(2) preparing a cobalt nitrate solution with the concentration of 0.1 mol/L;
(3) preparing a strontium nitrate solution with the concentration of 0.1 mol/L;
(4) taking 28ml of the cobalt nitrate solution prepared in the step (2), and recording the solution as V1Taking 2ml of the barium nitrate solution prepared in the step (3) and recording the solution as V2；
(5) Taking 24ml of the sodium carbonate solution prepared in the step (1), and recording the solution as a solution V3；
(6) V taken out in the step (4) is subjected to hydrothermal condition at 50 DEG C1Adding V taken out in the step (5)3Stirring for 20min to obtain precipitate;
(7) v taken out in the step (4)2Adding the precipitate obtained in the step (6) into the mixture, and continuously stirring the mixture for 20min to obtain a precipitate;
(8) continuing to remove the rest of V2Adding the precipitate obtained in the step (7) into the solution, and continuously stirring the solution for 20min to obtain a precipitate;
(9) the obtained precipitate is aged overnight to obtain a precursor;
(8) washing the obtained precursor with deionized water for 5 times, and then continuing washing with ethanol for 3 times;
(9) drying the obtained precursor at 60 ℃ overnight;
(10) uniformly grinding the dried precursor, and roasting at 500 ℃ for 4h to obtain the catalyst, which is marked as Co19Sr 1; the catalytic oxidation activity of vinyl chloride on different catalysts is shown in table 1.
Example 4
An alkali modified cobalt-based catalyst for low-temperature catalytic degradation of vinyl chloride is prepared by the following steps:
(1) preparing a sodium carbonate aqueous solution with the concentration of 0.5 mol/L;
(2) preparing a cobalt nitrate solution with the concentration of 0.1 mol/L;
(3) preparing a calcium nitrate solution with the concentration of 0.1 mol/L;
(4) taking 24ml of the cobalt nitrate solution prepared in the step (2), and recording the solution as V1Taking 2ml of the barium nitrate solution prepared in the step (3) and recording the solution as V2；
(5) Taking 18ml of the sodium carbonate solution prepared in the step (1), and recording the solution as a solution V3；
(6) V taken out in the step (4) is subjected to hydrothermal condition at 40 DEG C1Adding V taken out in the step (5)3Stirring for 20min to obtain precipitate;
(7) v taken out in the step (4)2Adding the precipitate obtained in the step (6) into the mixture, and continuously stirring the mixture for 20min to obtain a precipitate;
(8) continuing to remove the rest of V2Adding the precipitate obtained in the step (7) into the solution, and continuously stirring the solution for 20min to obtain a precipitate;
(9) the obtained precipitate is aged overnight to obtain a precursor;
(8) washing the obtained precursor with deionized water for 5 times, and then continuing washing with ethanol for 3 times;
(9) drying the obtained precursor overnight at 50 ℃;
(10) grinding the dried precursor uniformly, and roasting at 400 ℃ for 4h to obtain the catalyst, which is recorded as Co14Ca 1; the catalytic oxidation activity of vinyl chloride on different catalysts is shown in table 1.
Example 5
An alkali modified cobalt-based catalyst for low-temperature catalytic degradation of vinyl chloride is prepared by the following steps:
(1) preparing a sodium carbonate aqueous solution with the concentration of 1.0 mol/L;
(2) preparing a cobalt nitrate solution with the concentration of 0.2 mol/L;
(3) preparing a magnesium nitrate solution with the concentration of 0.2 mol/L;
(4) taking 36ml of the cobalt nitrate solution prepared in the step (2), and recording the solution as V1Taking 4ml of the barium nitrate solution prepared in the step (3) and recording the solution as V2；
(5) Taking 24ml of the sodium carbonate solution prepared in the step (1), and recording the solution as a solution V3；
(6) V taken out in the step (4) is subjected to hydrothermal condition at 40 DEG C1Adding V taken out in the step (5)3Stirring for 20min to obtain precipitate;
(7) v taken out in the step (4)2Adding the precipitate obtained in the step (6) into the mixture, and continuously stirring the mixture for 20min to obtain a precipitate;
(8) continuing to remove the rest of V2Adding the precipitate obtained in the step (7) into the solution, and continuously stirring the solution for 20min to obtain a precipitate;
(9) the obtained precipitate is aged overnight to obtain a precursor;
(8) washing the obtained precursor with deionized water for 5 times, and then continuing washing with ethanol for 3 times;
(9) drying the obtained precursor overnight at 50 ℃;
(10) uniformly grinding the dried precursor, and roasting at 400 ℃ for 4h to obtain the catalyst, which is recorded as Co9Mg 1; the catalytic oxidation activity of vinyl chloride on different catalysts is shown in table 1.
Catalyst Activity test
The catalysts of examples 1 to 5 were used for the catalytic combustion of vinyl chloride, the evaluation of the activity of the catalyst used for the catalytic combustion of vinyl chloride was carried out in a fixed-bed microreactor (quartz tube 3mm in internal diameter), the amount of the catalyst used was 200mg, and the temperature was automatically controlled using a type K thermocouple. The chloroethylene standard gas is mixed with air and enters a reactor for combustion. The total flow is controlled by a mass flow meter, the concentration of chloroethylene is 0.05 vol%, air is used as carrier gas, the concentration of oxygen is 10%, the reaction temperature is 140-. The relationship between the conversion of vinyl chloride and the reaction temperature is shown in Table 1, wherein T50%、T90%The reaction temperatures required for 50% and 90% conversion, respectively. The reaction tail gas is subjected to chromatographic on-line tracking, and the main reaction products are HCl, carbon dioxide, water and a very small amount of trichloroethylene.
As can be seen from the above results of catalytic oxidation activity of vinyl chloride, the catalyst of example 2 ~ 5 was used at a high reaction space velocity (30,000 ml. g)–1·h–1) Low and wide reaction temperature range, and Co ratio3O4High catalytic combustion activity of vinyl chloride. Further confirmation of Co3O4The surface of the cobalt-based catalyst is modified by alkali, so that the activity of the cobalt-based catalyst for catalytic oxidation of chlorinated hydrocarbon can be improved.
Claims (3)
1. Be used for chloroethylene low temperature catalysis to fallThe preparation method of the decomposed alkali modified cobalt-based catalyst is characterized in that the catalyst is prepared by a step precipitation-adsorption method, and the precipitator is sodium carbonate (Na)2CO3) The catalyst is obtained by step precipitation-adsorption under the stirring of water bath, and the method comprises the following steps:
(1) preparing a sodium carbonate aqueous solution with the concentration of 0.5 ~ 1.0.0 mol/L;
(2) preparing a cobalt nitrate solution with the concentration of 0.1 ~ 0.2.2 mol/L;
(3) preparing a nitrate solution of Mg, Ca, Sr or Ba alkali metal (M) with the same concentration as that in the step (2);
(4) according to the molar concentration ratio of M to Co of 1: (9-24) cobalt nitrate solution and alkali metal nitrate solution are respectively taken and respectively marked as V1And V2；
(5) Taking sodium carbonate solution and recording as V3Making the molar amount thereof 3 times the total molar amount of the cobalt nitrate and the alkali metal taken out in the step (4);
(6) the V taken out in the step (4) is hydrothermally processed at 40 ~ 60 ℃ and 60 DEG C1Adding V taken out in the step (5)3Stirring for 20min to obtain precipitate;
(7) v taken out in the step (4)2Adding the precipitate obtained in the step (6) into the mixture, and continuously stirring the mixture for 20min to obtain a precipitate;
(8) continuing to remove the rest of V2Adding the precipitate obtained in the step (7) into the solution, and continuously stirring the solution for 20min to obtain a precipitate;
(9) precipitating for overnight aging to obtain a precursor;
(8) washing the obtained precursor with deionized water for 3-5 times, and then washing with ethanol for 2-3 times;
(9) the obtained precursor was dried at 40 ~ 60 ℃ overnight;
(10) and uniformly grinding the dried precursor, and roasting at 400 ~ 500 ℃ for 2-4h to obtain the catalyst.
2. An alkali-modified cobalt-based catalyst for the low temperature catalytic degradation of vinyl chloride, characterized in that it is an alkali metal-modified cobalt-based catalyst prepared according to the method of claim 1.
3. Use of the base-modified cobalt-based catalyst according to claim 2 for the low temperature catalytic degradation of vinyl chloride.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111167458A (en) * | 2020-03-18 | 2020-05-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Barium carbonate-promoted cobaltosic oxide catalyst for vinyl chloride low-temperature catalytic combustion degradation |
| CN113244924A (en) * | 2021-05-25 | 2021-08-13 | 南昌航空大学 | Alkali metal modified metal oxide catalyst and preparation method and application thereof |
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| CN106994348A (en) * | 2017-03-22 | 2017-08-01 | 华东理工大学 | It is a kind of for catalyst of chlorination aromatic hydrocarbon low-temperature catalytic burning and its preparation method and application |
| CN109126798A (en) * | 2018-07-18 | 2019-01-04 | 上海纳米技术及应用国家工程研究中心有限公司 | Supported cobalt-base catalyst and its preparation method and application for vinyl chloride low-temperature catalytic oxidation |
| CN109395730A (en) * | 2018-11-15 | 2019-03-01 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for vinyl chloride low-temperature catalytic burning ruthenium cerium codope tin-based catalyst and products thereof and application |
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| CN101767011A (en) * | 2008-12-30 | 2010-07-07 | 华东理工大学 | Low-temperature catalytic combustion eliminating method of volatile chloro aryl hydrocarbons |
| CN106994348A (en) * | 2017-03-22 | 2017-08-01 | 华东理工大学 | It is a kind of for catalyst of chlorination aromatic hydrocarbon low-temperature catalytic burning and its preparation method and application |
| CN109126798A (en) * | 2018-07-18 | 2019-01-04 | 上海纳米技术及应用国家工程研究中心有限公司 | Supported cobalt-base catalyst and its preparation method and application for vinyl chloride low-temperature catalytic oxidation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111167458A (en) * | 2020-03-18 | 2020-05-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Barium carbonate-promoted cobaltosic oxide catalyst for vinyl chloride low-temperature catalytic combustion degradation |
| CN113244924A (en) * | 2021-05-25 | 2021-08-13 | 南昌航空大学 | Alkali metal modified metal oxide catalyst and preparation method and application thereof |
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Application publication date: 20191220 |