CN115414926A - For CO 2 Catalytic conversion CeGaTi catalyst and preparation method thereof - Google Patents
For CO 2 Catalytic conversion CeGaTi catalyst and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of catalysts, and particularly relates to a catalyst for CO 2 A catalyst CeGaTi for catalytic conversion is prepared from the solution of NaOH as precipitant, cerium nitrate, gallium nitrate and titanium sulfate as precursor through hydrothermal synthesis 2 A catalytic conversion CeGaTi catalyst. The catalyst prepared by the invention is used for CO 2 And CH 3 The highest yield of dimethyl carbonate (DMC) can reach 24.643mmol/g. The invention has the characteristics of rich raw materials, no toxicity, no corrosiveness, no flammability and no harm to the environment, and the product dimethyl carbonate is an environment-friendly chemical raw material which meets the requirements of modern clean production, and the reaction can lead the waste gas CO to be converted into the CO 2 To a value-added multi-carbon product with water as the only by-product.
Description
Technical Field
The invention belongs to the technical field of catalysts, and particularly relates to a catalyst for CO 2 Catalytic conversion CeGaTi catalyst and preparation thereofA method.
Background
In recent decades, the ever increasing energy demand has led to an increase in carbon dioxide emissions year by year, and in chemical and petrochemical industrial processes, carbon dioxide can be directly converted by chemical conversion into valuable hydrocarbons, such as urea, salicylic acid, dimethyl carbonate (DMC), cyclic carbonates and polycarbonates, where DMC is considered to be a low-toxicity biodegradable green chemical substance.
Dimethyl carbonate (DMC) is an environment-friendly chemical raw material meeting the requirements of modern clean production. The method is widely applied to lithium ion battery electrolyte, raw materials for producing polycarbonate, pesticides, foods, dyes and the like. DMC is an important precursor for polycarbonate and is also a useful methylating and methoxycarbonylating agent, replacing the toxic phosgene, dimethyl sulfate or methyl iodide. In addition, DMC is a candidate as a gasoline oxygenate additive alternative to MTBE due to its high oxygen content.
Cerium oxide as a superior metal oxide catalyst with Lewis acid and base properties in CO 2 And has higher catalytic activity in synthesizing DMC by methanol. On the basis of this study, various morphologically dispersed cerium oxide nanocrystals, including nanoparticles, polyhedra, nanorods, have been synthesized, and different morphologies of CeO have been found 2 With different acid-base sites, resulting in different DMC yields. Previously studied in CeO 2 The research shows that the Zr doping can increase the oxygen vacancy content of the CeZr catalyst and the Ce 3+ In an amount more favorable to CO activation 2 The yield of DMC was increased, but the DMC yield obtained reached only 14.9mmol/g, and further studies were required to increase the yield of DMC.
Disclosure of Invention
To effectively promote CO 2 And methanol to synthesize dimethyl carbonate (DMC), the invention provides Ga and Ti doped CeO 2 Nanorod application to CO 2 A catalytic conversion CeGaTi catalyst.
The preparation method of the CeGaTi catalyst comprises the following steps:
(1) Weighing Ce (NO) 3 ·6H 2 O、Ga(NO) 3 ·9H 2 O and TiSO 4 Dissolving in deionized water to form solution A, wherein Ce (NO) 3 ·6H 2 O、Ga(NO) 3 ·9H 2 O and TiSO 4 The total mass concentration of the mixed solution is 0.2080-0.2118g/mL.
(2) Weighing NaOH and dissolving the NaOH in deionized water to form a solution B, wherein the concentration of the NaOH is 5-7mol/L.
(3) And (3) slowly dripping the solution B in the step (2) into the solution A in the step (1) to form a mixed solution, continuously stirring for 15-20min, transferring the mixed solution into a hydrothermal reaction kettle for hydrothermal reaction, and then cooling, washing and drying to obtain the CeGaTi precursor.
Wherein, in the hydrothermal kettle, the volume of the liquid is 40-50% of the total volume of the hydrothermal kettle; the hydrothermal reaction temperature is 343-423K, the reaction time is 12-36h,
(4) And (4) roasting the CeGaTi precursor obtained in the step (3) in a muffle furnace, heating to 400-600 ℃ at the heating rate of 1-3 ℃/min, and keeping the temperature for 3-5h to obtain the CeGaTi catalyst.
The CeGaTi catalyst of the invention is applied to CO 2 And methanol to dimethyl carbonate. With CO 2 And anhydrous methanol as raw material, wherein the volume of the methanol is 60-80% of the total volume of the reaction kettle, and 0.2MPa CO is used 2 After three times of replacement, the pressure of 3MPa is filled, the mass of the CeGaTi catalyst is 0.4-1.1 percent of the total mass of reactants, the reaction temperature is 120-160 ℃, and the reaction time is 2-6h.
After the technical method is adopted, the invention has the beneficial effects that:
by using CO 2 And the methanol is used for synthesizing the dimethyl carbonate, so that the method has the advantages of wide and easily obtained raw materials, green and environment-friendly process and the like.
The CeGaTi catalyst of the invention has more oxygen vacancies and Ce 3+ Is more favorable to CO 2 The yield of the dimethyl carbonate can reach 24.642mmol/g.
Drawings
FIG. 1 is pure CeO prepared in the examples 2 A rod andx-ray diffraction pattern of doped CeGaTi catalyst. Wherein Cat 1 is pure CeO 2 The rod catalysts, cat 2, cat 3, cat 4, cat 5 and Cat 6 are CeGaTi catalysts with different doping ratios respectively.
Detailed Description
The invention will now be further illustrated by reference to specific examples, which are intended to be illustrative of the invention and are not intended to be a further limitation of the invention.
Comparative example 1
(1) Weighing 0.868g Ce (NO) 3 ·6H 2 Dissolving O in 5mL of deionized water to form solution A;
(2) Weighing 8.4g of NaOH and dissolving in 35mL of deionized water to form a solution B;
(3) Slowly dripping the solution B in the step (2) into the solution A in the step (1) to form a mixed solution, continuously stirring for 20min, and transferring the mixed solution into a hydrothermal reaction kettle, wherein the volume of the liquid is 40% of the total volume of the hydrothermal kettle; wherein the hydrothermal reaction temperature is 373K, the reaction time is 24h, and then the Ce (OH) is obtained after cooling, washing and drying 2 A precursor.
(4) The Ce (OH) obtained in the step (3) 2 Roasting the precursor in a muffle furnace, heating to 500 ℃ at the heating rate of 2 ℃/min, and keeping the temperature for 4 hours to obtain the CeO 2 The nanorod catalyst is marked as Cat 1.
The CeO prepared in comparative example 1 was added 2 Application of nanorod catalyst in CO 2 And methanol to dimethyl carbonate. Measuring 35mL CH 3 OH、0.2g CeO 2 Filling 3MPa CO into the batch reactor with the nano-rod catalyst 2 . The reaction temperature was set at 140 ℃, the reaction time was set at 2h, and the rotational speed of the magnetic stirrer was set at 800rpm. After the reaction was completed, the solution was centrifuged and subjected to qualitative and quantitative analysis by gas chromatography to obtain DMC with a yield of 10.608mmol/g.
Comparative example 2
Weighing 0.868g Ce (NO) 3 ·6H 2 O and 0.1670g Ga (NO) 3 ·9H 2 O dissolved in 5mL deionized water to form solution A, remainder procedure and comparative exampleExample 1 is the same.
Application of the CeGa catalyst prepared in comparative example 2 to CO 2 And methanol to dimethyl carbonate. Measuring 35mL CH 3 OH、0.2g CeO 2 Filling 3MPa CO into the batch reactor with the nano-rod catalyst 2 . The reaction temperature was set at 140 ℃, the reaction time was set at 2h, and the rotational speed of the magnetic stirrer was set at 800rpm. After the reaction was completed, the solution was centrifuged and subjected to qualitative and quantitative analysis by gas chromatography to obtain DMC in a yield of 19.628mmol/g.
Comparative example 3
Weighing 0.868g Ce (NO) 3 ·6H 2 O、0.1670g Ga(NO) 3 ·9H 2 O and 0.0129g ZrOCl 2 ·8H 2 O was dissolved in 5mL of deionized water to form a solution A, and the remaining procedure was the same as in comparative example 1.
Application of the CeGaZr catalyst prepared in comparative example 3 to CO 2 And methanol to dimethyl carbonate. Measuring 35mL CH 3 OH、0.2g CeO 2 Filling 3MPa CO into the batch reactor with the nano-rod catalyst 2 . The reaction temperature was set at 140 ℃, the reaction time was set at 2h, and the rotational speed of the magnetic stirrer was set at 800rpm. After the reaction is finished, the solution is taken out and centrifuged, and qualitative and quantitative analysis is carried out by gas chromatography, so that the yield of DMC is 7.514mmol/g, and the catalytic effect is reduced.
Comparative example 4
Weighing 0.868g Ce (NO) 3 ·6H 2 O、0.1670g Ga(NO) 3 ·9H 2 O and 0.0119gZn (NO) 3 ) 2 ·6H 2 O was dissolved in 5mL of deionized water to form a solution A, and the remaining procedure was the same as in comparative example 1.
Application of the CeGaZn catalyst prepared in comparative example 4 to CO 2 And methanol to dimethyl carbonate. Measuring 35mL CH 3 OH、0.2g CeO 2 Filling 3MPa of CO into a batch reaction kettle by using a nanorod catalyst 2 . The reaction temperature was set at 140 ℃, the reaction time was set at 2h, and the rotational speed of the magnetic stirrer was set at 800rpm. After the reaction, the solution was centrifuged and subjected to gas chromatographyQualitative and quantitative analysis shows that the yield of DMC is 5.945mmol/g, but the catalytic effect is reduced.
Example 1
Weighing 0.868g Ce (NO) 3 ·6H 2 O、0.1670g Ga(NO) 3 ·9H 2 O and 0.0048g TiSO 4 Dissolving in 5mL of deionized water to form solution A;
the rest of the procedure was the same as in comparative example 1, and the catalyst obtained was designated Cat 2.
FIG. 1 is pure CeO prepared in the examples 2 X-ray diffraction patterns of the rods and of the doped CeGaTi catalyst. As can be seen from fig. 1, peaks at 2 θ =28 °, 33 °, 47 °, and 56 ° correspond to the cubic fluorite structure CeO 2 (PDF # 34-0394) (111), (200), (220), and (311). CeO modified with Ga and Ti 2 Nanorods, all of which did not detect Ga 2 O 3 And TiO 2 2 Diffraction phenomena corresponding to the crystalline phase, indicating that gallium oxide species and titanium oxide species are present in highly dispersed or amorphous form in CeO 2 In the nano-rod.
The CeGaTi catalyst prepared in example 1 was applied to CO 2 And methanol to dimethyl carbonate. Measuring 35mL CH 3 OH、0.2g CeO 2 Filling 3MPa CO into the batch reactor with the nano-rod catalyst 2 . The reaction temperature was set at 140 ℃, the reaction time was set at 2h, and the rotational speed of the magnetic stirrer was set at 800rpm. After the reaction was completed, the solution was centrifuged and subjected to qualitative and quantitative analysis by gas chromatography to obtain DMC with a yield of 20.656mmol/g.
Example 2
Weighing 0.868g Ce (NO) 3 ·6H 2 O、0.1670g Ga(NO) 3 ·9H 2 O and 0.0096g TiSO 4 Dissolving in 5mL of deionized water to form solution A;
the rest of the procedure was the same as in comparative example 1, and the catalyst obtained was designated Cat 3.
Application of the CeGaTi catalyst prepared in example 2 to CO 2 And methanol to dimethyl carbonate. Measuring 35mL CH 3 OH、0.2g CeO 2 Nanorod catalyst in batchThe reaction kettle is filled with 3MPa of CO 2 . The reaction temperature was set at 140 ℃, the reaction time was set at 2h, and the rotational speed of the magnetic stirrer was set at 800rpm. After the reaction was completed, the solution was centrifuged and subjected to qualitative and quantitative analysis by gas chromatography to obtain DMC with a yield of 24.643mmol/g.
Example 3
Weighing 0.868g Ce (NO) 3 ·6H 2 O、0.1670g Ga(NO) 3 ·9H 2 O and 0.0144g TiSO 4 Dissolving in 5mL of deionized water to form solution A;
the rest of the procedure was the same as in comparative example 1 and the catalyst obtained was designated Cat 4.
Application of the CeGaTi catalyst prepared in example 3 to CO 2 And methanol to dimethyl carbonate. Measuring 35mL CH 3 OH、0.2g CeO 2 Filling 3MPa CO into the batch reactor with the nano-rod catalyst 2 . The reaction temperature was set at 140 ℃, the reaction time was set at 2h, and the rotational speed of the magnetic stirrer was set at 800rpm. After the reaction was completed, the solution was centrifuged and subjected to qualitative and quantitative analysis by gas chromatography to obtain DMC with a yield of 18.275mmol/g.
Example 4
Weighing 0.868g Ce (NO) 3 ·6H 2 O、0.1670g Ga(NO) 3 ·9H 2 O and 0.0192g TiSO 4 Dissolving in 5mL of deionized water to form solution A;
the rest of the procedure was the same as in comparative example 1, and the catalyst obtained was designated Cat 5.
Application of the CeGaTi catalyst prepared in example 4 to CO 2 And methanol to dimethyl carbonate. Measuring 35mL CH 3 OH、0.2g CeO 2 Filling 3MPa of CO into a batch reaction kettle by using a nanorod catalyst 2 . The reaction temperature was set at 140 ℃, the reaction time was set at 2h, and the rotational speed of the magnetic stirrer was set at 800rpm. After the reaction was completed, the solution was centrifuged and subjected to qualitative and quantitative analysis by gas chromatography to obtain DMC with a yield of 17.996mmol/g.
Example 5
Weighing 0.868g Ce (NO) 3 ·6H 2 O、0.1670g Ga(NO) 3 ·9H 2 O and 0.0240g TiSO 4 Dissolving in 5mL of deionized water to form solution A;
the rest of the procedure was the same as in comparative example 1, and the catalyst obtained was designated Cat 6.
The CeGaTi catalyst prepared in example 5 was applied to CO 2 And methanol to dimethyl carbonate. Measuring 35mL CH 3 OH、0.2g CeO 2 Filling 3MPa CO into the batch reactor with the nano-rod catalyst 2 . The reaction temperature was set at 140 ℃, the reaction time was set at 2h, and the rotational speed of the magnetic stirrer was set at 800rpm. After the reaction was completed, the solution was centrifuged and subjected to qualitative and quantitative analysis by gas chromatography to obtain DMC with a yield of 12.608mmol/g.
Example 6
Measuring 35mL CH 3 OH and 0.1g Cat 3 catalyst are filled in a batch reactor with 3MPa of CO 2 . The reaction temperature was set at 140 ℃, the reaction time was set at 2h, and the rotational speed of the magnetic stirrer was set at 800rpm. After the reaction was completed, the solution was centrifuged and subjected to qualitative and quantitative analysis by gas chromatography to obtain DMC with a yield of 16.932mmol/g.
Example 7
Measuring 35mL CH 3 OH and 0.4g Cat 3 catalyst are filled in an intermittent reaction kettle with 3MPa of CO 2 . The reaction temperature was set at 140 ℃, the reaction time was set at 2h, and the rotational speed of the magnetic stirrer was set at 800rpm. After the reaction was completed, the solution was centrifuged and subjected to qualitative and quantitative analysis by gas chromatography to obtain DMC with a yield of 23.215mmol/g.
Example 8
Measuring 35mL CH 3 OH and 0.2g Cat 3 catalyst are filled into a batch reactor with 3MPa of CO 2 . The reaction temperature was set at 130 ℃, the reaction time was set at 2h, and the rotational speed of the magnetic stirrer was set at 800rpm. After the reaction was completed, the solution was centrifuged and subjected to qualitative and quantitative analysis by gas chromatography to obtain DMC with a yield of 22.844mmol/g.
Example 9
Measuring 35mL CH 3 OH and 0.2g Cat 3 catalyst are filled into a batch reaction kettle and is filled with 3MPa of CO 2 . The reaction temperature was set at 150 ℃, the reaction time was set at 2h, and the rotational speed of the magnetic stirrer was set at 800rpm. After the reaction was completed, the solution was centrifuged and subjected to qualitative and quantitative analysis by gas chromatography to obtain DMC with a yield of 24.016mmol/g.
Example 10
Measuring 35mL CH 3 OH and 0.2g Cat 3 catalyst are filled into a batch reactor with 2.5MPa of CO 2 . The reaction temperature was set at 140 ℃, the reaction time was set at 2h, and the rotational speed of the magnetic stirrer was set at 800rpm. After the reaction was completed, the solution was centrifuged and subjected to qualitative and quantitative analysis by gas chromatography to obtain DMC with a yield of 15.375mmol/g.
Example 11
Measuring 35mL CH 3 OH and 0.2g Cat 3 catalyst are filled into a batch reaction kettle and is filled with 4MPa of CO 2 . The reaction temperature was set at 140 ℃, the reaction time was set at 2h, and the rotational speed of the magnetic stirrer was set at 800rpm. After the reaction was completed, the solution was centrifuged and subjected to qualitative and quantitative analysis by gas chromatography to obtain DMC with a yield of 23.781mmol/g.
Example 12
Measuring 35mL CH 3 OH and 0.2g Cat 3 catalyst are filled into a batch reactor with 3MPa of CO 2 . The reaction temperature was set at 140 ℃, the reaction time was set at 1h, and the rotational speed of the magnetic stirrer was set at 800rpm. After the reaction was completed, the solution was centrifuged and subjected to qualitative and quantitative analysis by gas chromatography to obtain DMC with a yield of 13.307mmol/g.
Example 13
Measuring 35mL CH 3 OH and 0.2g Cat 3 catalyst are filled into a batch reactor with 3MPa of CO 2 . The reaction temperature was set at 140 ℃, the reaction time was set at 6h, and the rotational speed of the magnetic stirrer was set at 800rpm. After the reaction was completed, the solution was centrifuged and subjected to qualitative and quantitative analysis by gas chromatography to obtain DMC in a yield of 15.645mmol/g.
TABLE 1 operating conditions and reaction results for examples 1-13
As can be seen from the results in Table 1, the CeGaTi catalyst prepared by the present invention has a high CO content 2 And CH 3 The dimethyl carbonate synthesized by OH has good reaction catalytic performance, the catalyst Cat 3 in the example 2 is used for the reaction, and the yield of DMC reaches 24.643mmol/g.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the contents of the specification, and must be determined according to the scope of the claims.
Claims (6)
1. For CO 2 A catalytically converted CeGaTi catalyst characterized by: the CeGaTi catalyst is CeO doped with Ga and Ti 2 The dosage of elements of the nano-rod is Ce>Ga>Ti。
2. The method of claim 1 for CO 2 The preparation method of the catalytic conversion CeGaTi catalyst is characterized by comprising the following steps:
(1) Weighing Ce (NO) 3 ·6H 2 O、Ga(NO) 3 ·9H 2 O and TiSO 4 Dissolving in deionized water to form solution A, wherein the total mass concentration of the solution A is 0.2080-0.2118g/mL;
(2) Weighing NaOH and dissolving the NaOH in deionized water to form a solution B, wherein the concentration of the NaOH is 5-7mol/L;
(3) Slowly dripping the solution B in the step (2) into the solution A in the step (1) to form a mixed solution, continuously stirring for 15-20min, transferring the mixed solution into a hydrothermal reaction kettle for hydrothermal reaction, and then cooling, washing and drying to obtain a CeGaTi precursor;
(4) And (4) roasting the CeGaTi precursor obtained in the step (3) in a muffle furnace, heating to 400-600 ℃ at the heating rate of 1-3 ℃/min, and keeping the temperature for 3-5h to obtain the CeGaTi catalyst.
3. A process for CO according to claim 1 2 Use of a catalyst CeGaTi for catalytic conversion, characterized in that the catalyst CeGaTi is used for catalyzing CO 2 And methanol to dimethyl carbonate.
4. The use of cegai catalyst according to claim 3, wherein the reaction method for the synthesis of dimethyl carbonate is: in a 50mL batch reactor with CO 2 And anhydrous methanol as raw material, wherein the volume of the methanol is 60-80% of the total volume of the reaction kettle, and 0.2MPa CO is used 2 After the three times of replacement, the pressure of 3MPa is filled, and CeGaTi catalyst is added, and the rotating speed is 800rpm for reaction.
5. Use of a CeGaTi catalyst according to claim 4, wherein the CeGaTi catalyst has a mass of 0.4-1.1% of the total mass of the reactants.
6. The use of a CeGaTi catalyst according to claim 4, wherein the reaction temperature is 120-160 ℃ and the reaction time is 2-6h.
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Citations (4)
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|---|---|---|---|---|
| WO2014072802A2 (en) * | 2012-11-09 | 2014-05-15 | Council Of Scientific & Industrial Research | Synthesis of dimethyl carbonate and related compounds |
| CN110683951A (en) * | 2019-10-23 | 2020-01-14 | 熊飞龙 | Method for directly preparing dimethyl carbonate by low-temperature high-efficiency catalysis of reaction of urea and methanol |
| CN111153801A (en) * | 2018-11-07 | 2020-05-15 | 中国科学院大连化学物理研究所 | Preparation method of aromatic carboxylic ester compound |
| CN112823879A (en) * | 2019-11-21 | 2021-05-21 | 中国科学院大连化学物理研究所 | Application of cerium-based catalyst in preparation of dimethyl carbonate through direct conversion of carbon dioxide and methanol |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014072802A2 (en) * | 2012-11-09 | 2014-05-15 | Council Of Scientific & Industrial Research | Synthesis of dimethyl carbonate and related compounds |
| CN111153801A (en) * | 2018-11-07 | 2020-05-15 | 中国科学院大连化学物理研究所 | Preparation method of aromatic carboxylic ester compound |
| CN110683951A (en) * | 2019-10-23 | 2020-01-14 | 熊飞龙 | Method for directly preparing dimethyl carbonate by low-temperature high-efficiency catalysis of reaction of urea and methanol |
| CN112823879A (en) * | 2019-11-21 | 2021-05-21 | 中国科学院大连化学物理研究所 | Application of cerium-based catalyst in preparation of dimethyl carbonate through direct conversion of carbon dioxide and methanol |
Non-Patent Citations (2)
| Title |
|---|
| HYE JIN LEE ET AL.: ""Direct synthesis of dimethyl carbonate from methanol and carbon dioxide over Ga2O3-CeO2-ZrO2 catalysts prepared by a single-step sol-gel method: Effect of acidity and basicity of the catalysts"", 《KOREAN J. CHEM. ENG.》, vol. 29, pages 1019 - 1024, XP035093277, DOI: 10.1007/s11814-012-0017-0 * |
| ZHONGWEI FU ET AL.: ""TiO2‑Doped CeO2 Nanorod Catalyst for Direct Conversion of CO2 and CH3OH to Dimethyl Carbonate: Catalytic Performance and Kinetic Study"", 《ACS OMEGA》, vol. 3, pages 198 - 207 * |
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