CN113441143B - Nickel-cobalt-aluminum ternary metal composite catalyst and preparation method and application thereof - Google Patents
Nickel-cobalt-aluminum ternary metal composite catalyst and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a nickel-cobalt-aluminum ternary metal composite catalyst and a preparation method and application thereof, wherein the Ni-Co-Al composite ternary metal catalyst is formed by urea hydrolysis coprecipitation and then calcination reduction, the catalyst is marked as xNiyCoAl, wherein x represents the molar ratio of nickel element to Al element, x =1.5-2.5, y represents the molar ratio of Co element to Al element, and y =0.25-2. The catalyst can efficiently catalyze levulinic acid to hydrogenate and synthesize gamma-valerolactone in 1,4-dioxane under mild reaction conditions. The catalyst has high catalytic activity at 120-130 deg.C and 3-4MPa H 2 The reaction is carried out for 2 to 3 hours under the catalytic reaction condition, and the yield of the gamma-valerolactone can reach 100 percent; other non-noble metal catalysts reported at present usually need to be at a reaction temperature of 140-200 ℃ to achieve similar catalytic effects.
Description
Technical Field
The invention belongs to the field of catalysts, and particularly relates to a nickel-cobalt-aluminum ternary metal composite catalyst and a preparation method and application thereof.
Background
The biomass is a natural clean renewable carbon resource with wide source, abundant reserves and low price. Biomass can be converted into various important high value-added fuels, chemical products and materials, has great potential for replacing traditional fossil resources, and methods for exploring more effective utilization of biomass resources are receiving wide attention. Among them, converting biomass raw materials into various biomass-based platform compounds and then converting the biomass-based platform compounds to prepare high value-added chemicals is generally considered as an important biomass resource utilization mode. Levulinic acid is an important biomass-based platform molecule, and can be used for preparing gamma-valerolactone through catalytic hydrogenation, and the gamma-valerolactone can be widely applied to aspects of green solvents, organic synthesis, fuel additives and the like.
At present, the solvent system for preparing gamma-valerolactone by directly hydrogenating levulinic acid mainly comprises 1,4-dioxane organic solvents. Since hydrogen has a higher solubility in 1,4-dioxane, 1,4-dioxane is considered a more desirable hydrogenation solvent and enables higher gamma valerolactone yields (ACS Catalysis,2016,6 (8): 5462-5472 chemical Engineering journal,2019,369, 386-393 Catalysis letters,2017,147 (3): 1-7 Catalysis, 2015,6 (1): 6-15.. However, the reaction conditions of 1,4-dioxane systems are more severe at present, especially when non-noble metal catalysts are used, the reaction temperature is much between 140 ℃ and 200 ℃ (Fuel, 2020,259, 116208.1-116208.4 catalysts letters,2017,147 (3): 1-7 catalysts,2015,6 (1): 6-15 catalysts today,2016, 274. Other reported non-noble metal catalysts usually need to be at a reaction temperature of 140-200 ℃ to achieve similar catalytic effects.
The non-noble metal has more application prospect than the noble metal due to the abundant reserves and the relatively lower cost. The development of a non-noble metal catalyst with high-efficiency catalytic activity and the realization of the high-efficiency hydrogenation reduction of levulinic acid in a 1,4-dioxane system under mild conditions have become a great technical difficulty in the industrial production of gamma-valerolactone.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a nickel-cobalt-aluminum ternary metal composite catalyst and a preparation method and application thereof. The nickel-cobalt-aluminum ternary metal composite hydrogenation catalyst provided by the invention can efficiently catalyze levulinic acid to be hydrogenated and synthesized into gamma-valerolactone in a 1,4-dioxane system under mild conditions.
One of the technical schemes of the invention provides the nickel-cobalt-aluminum ternary metal composite catalyst prepared by the preparation method. The catalyst is marked as xNiyCoAl, wherein x represents the molar ratio of Ni element to Al element in the catalyst, x =1.5-2.5, y represents the molar ratio of Co element to Al element in the catalyst, and y =0.25-2.
The second technical scheme of the invention is to provide a preparation method of a nickel-cobalt-aluminum ternary metal composite catalyst, which comprises the following steps: dissolving cobalt nitrate hexahydrate, urea, nickel nitrate hexahydrate and aluminum nitrate nonahydrate in deionized water; reacting at 100-140 deg.C for 3-5h, separating solid and liquid, drying the solid precipitate, and grinding into powder; calcining at 400-600 ℃ for 3-5h, and then reducing at 550-750 ℃ for 4-6h under protective gas to obtain the nickel-cobalt-aluminum ternary metal composite catalyst.
In a preferred embodiment of the invention, the catalyst is labeled xNiyCoAl, where x represents the molar ratio of Ni element to Al element and y represents the molar ratio of Co element to Al element in the catalyst.
In a preferred embodiment of the present invention, the molar ratio of the nickel element to the aluminum element is 1.5-2.5.
In the preferred embodiment of the invention, the molar ratio of the cobalt element to the aluminum element is 0.25-2:1.
In the preferred embodiment of the invention, the molar ratio of the urea to the total of the three elements of nickel, cobalt and aluminum is 13-14.
In a preferred embodiment of the invention, in the aqueous solution containing nickel nitrate, cobalt nitrate, aluminum nitrate and urea, the concentration of urea is 3-5mol/L, and the concentration of cobalt nitrate is 0.015-0.15mol/L.
In a preferred embodiment of the invention, the calcination is carried out in an air atmosphere.
In a preferred embodiment of the invention, the protective gas is 10% vol% hydrogen +90% vol% nitrogen.
The third technical scheme of the invention is to provide an application of a nickel-cobalt-aluminum ternary metal composite catalyst in preparation of gamma-valerolactone.
The fourth technical scheme of the invention is to provide a method for preparing gamma-valerolactone by using a nickel-cobalt-aluminum ternary metal composite catalyst, which comprises the following steps: mixing levulinic acid and a solvent 1,4-dioxane, placing the mixture into a reaction container, adding a nickel-cobalt-aluminum ternary metal composite catalyst, sealing the reactor, and filling hydrogen, wherein the hydrogen pressure is 1-4MPa, the temperature of the reactor is 100-130 ℃, and the reaction time is 1-3h. Preferably, the hydrogen pressure is 2-4MPa, the reaction temperature is 120-130 ℃, and the reaction time is 2-3h. Under the above conditions, the yield of gamma-valerolactone is about 90.7-100%.
The equipment, reagents, processes, parameters and the like related to the invention are conventional equipment, reagents, processes, parameters and the like except for special description, and no embodiment is needed.
All ranges recited herein include all point values within the range.
As used herein, "about" or "about" and the like refer to a range or value within plus or minus 20 percent of the stated range or value.
In the present invention, the "room temperature", i.e., the normal ambient temperature, may be 10 to 30 ℃.
Compared with the background technology, the technical scheme has the following advantages:
(1) The invention forms the Ni-Co-Al composite ternary metal catalyst by urea hydrolysis coprecipitation method and then calcining and reducing;
(2) The catalyst prepared by the invention has high-efficiency catalytic activity, and efficiently catalyzes levulinic acid to synthesize gamma-valerolactone by hydrogenation in 1,4-dioxane under mild reaction conditions;
(3) The catalyst prepared by the invention has the H of 3-4MPa at the temperature of 120-130 DEG C 2 The reaction is carried out for 2 to 3 hours under the catalytic reaction condition, and the yield of the gamma-valerolactone can reach 100 percent; the catalytic reaction temperature is lower than the reaction temperature of 140-200 ℃ of the non-noble metal catalyst in the prior art, and the similar catalytic effect can be achieved.
Detailed Description
The invention provides a preparation method of a nickel-cobalt-aluminum ternary metal composite catalyst, which specifically comprises the following steps: dissolving cobalt nitrate hexahydrate, urea, nickel nitrate hexahydrate and aluminum nitrate nonahydrate in deionized water, wherein the concentration of the urea is 3-5mol/L, the concentration of the cobalt nitrate is 0.015-0.15mol/L, the molar ratio of a nickel element to an aluminum element is 1.5-2.5; reacting at 100-140 deg.C for 3-5h, separating solid and liquid, drying the solid precipitate, and grinding into powder; calcining at 400-600 deg.C for 3-5h in air atmosphere, and reducing at 550-750 deg.C for 4-6h in 10% vol% hydrogen +90% vol% nitrogen atmosphere to obtain the final product. The catalyst is labeled xNiyCoAl, where x represents the molar ratio of Ni element to Al element, x =1.5-2.5, y represents the molar ratio of Co element to Al element in the catalyst, and y =0.25-2.
The invention provides a method for preparing gamma-valerolactone by using a nickel-cobalt-aluminum ternary metal composite catalyst, which comprises the following steps: mixing levulinic acid and a solvent 1,4-dioxane, placing the mixture into a reaction container, adding a nickel-cobalt-aluminum ternary metal composite catalyst, sealing the reactor, and filling hydrogen, wherein the hydrogen pressure is 1-4MPa, the temperature of the reactor is 100-130 ℃, and the reaction time is 1-3h. Preferably, the hydrogen pressure is 2-3MPa, the reaction temperature is 120-130 ℃, and the reaction time is 2-3h.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following will describe the contents of the present invention in more detail by way of examples, but the scope of the present invention is not limited to these examples.
Example 1
Preparing a nickel-cobalt-aluminum ternary metal composite catalyst:
2.907g (0.01 mol) nickel nitrate hexahydrate, 1.88g (0.005 mol) aluminum nitrate nonahydrate, 0.364g cobalt nitrate hexahydrate (0.00125 mol) and 13.5g urea were dissolved in 70mL deionized water; reacting the solution at 120 ℃ for 4 hours, and separating to obtain solid precipitate; grinding the dried solid into powder, calcining the powder at 500 ℃ for 4 hours in an air atmosphere, and then calcining and reducing the calcined solid for 5 hours in a 10-vol% hydrogen + 90-vol% nitrogen atmosphere at 650 ℃ to obtain the nickel-cobalt-aluminum ternary metal composite catalyst. The catalyst is labeled 2Ni0.25CoAl.
The nickel-cobalt-aluminum ternary metal composite catalyst prepared by the method is used for preparing the following gamma-valerolactone:
0.125g of levulinic acid and 5mL of 1, 4-dioxane are added into a 25mL autoclave, 0.075g of 2Ni0.25CoAl is added as a catalyst, the reaction kettle is sealed, 3MPa of hydrogen is introduced, the mixture is magnetically stirred, the mixture is heated to 100 ℃ and kept for 2 hours, the reaction is finished, the mixture is cooled to room temperature and sampled for detection, and the detection result is shown as the serial number 1 in Table 1.
Example 2
Preparing a nickel-cobalt-aluminum ternary metal composite catalyst:
2.907g (0.01 mol) nickel nitrate hexahydrate and 1.88g (0.005 mol) aluminum nitrate nonahydrate, 0.7275g cobalt nitrate hexahydrate (0.0025 mol) and 14.4g urea were dissolved in 70mL deionized water; reacting the solution at 120 ℃ for 4 hours, and separating to obtain solid precipitate; grinding the dried solid into powder, calcining the powder at 500 ℃ for 4 hours in an air atmosphere, and then calcining and reducing the calcined solid for 5 hours in a 10-vol% hydrogen + 90-vol% nitrogen atmosphere at 650 ℃ to obtain the nickel-cobalt-aluminum ternary metal composite catalyst. The catalyst was labeled 2Ni0.5CoAl.
The nickel-cobalt-aluminum ternary metal composite catalyst prepared by the method is used for preparing the following gamma-valerolactone:
0.125g of levulinic acid and 5mL of 1, 4-dioxane are added into a 25mL autoclave, 0.075g of 2Ni0.5CoAl is added as a catalyst, the reaction kettle is sealed, 3MPa hydrogen is introduced, the mixture is magnetically stirred, the mixture is heated to 100 ℃ and kept for 2 hours, the reaction is finished, the mixture is cooled to room temperature, sampling detection is carried out, and the detection result is shown as the serial number 2 in the table 1.
Example 3
Preparing a nickel-cobalt-aluminum ternary metal composite catalyst:
2.907g (0.01 mol) nickel nitrate hexahydrate and 1.88g (0.005 mol) aluminum nitrate nonahydrate, 1.455g cobalt nitrate hexahydrate (0.005 mol) and 16.2g urea were dissolved in 70mL deionized water; reacting the solution at 120 ℃ for 4 hours, and separating to obtain solid precipitate; grinding the dried solid into powder, calcining the powder at 500 ℃ for 4 hours in an air atmosphere, and then calcining and reducing the calcined solid for 5 hours in a 10-vol% hydrogen + 90-vol% nitrogen atmosphere at 650 ℃ to obtain the nickel-cobalt-aluminum ternary metal composite catalyst. The catalyst is labeled 2Ni1CoAl.
The nickel-cobalt-aluminum ternary metal composite catalyst prepared by the method is used for preparing the following gamma-valerolactone:
0.125g of levulinic acid and 5mL of 1, 4-dioxane are added into a 25mL autoclave, 0.075g of 2Ni1CoAl is added as a catalyst, the reaction kettle is sealed, 3MPa of hydrogen is introduced, the mixture is magnetically stirred, the mixture is heated to 100 ℃ and kept for 2 hours, the reaction is finished, the mixture is cooled to room temperature, and sampling detection is carried out, wherein the detection result is shown as the serial number 3 in the table 1.
Example 4
Preparing a nickel-cobalt-aluminum ternary metal composite catalyst:
2.907g (0.01 mol) nickel nitrate hexahydrate and 1.88g (0.005 mol) aluminum nitrate nonahydrate, 2.91g cobalt nitrate hexahydrate (0.01 mol) and 19.8g urea were dissolved in 70mL deionized water; reacting the solution at 120 ℃ for 4 hours, and separating to obtain solid precipitate; grinding the dried solid into powder, calcining the powder at 500 ℃ for 4 hours in an air atmosphere, and then calcining and reducing the calcined solid for 5 hours in a 10-vol% hydrogen + 90-vol% nitrogen atmosphere at 650 ℃ to obtain the nickel-cobalt-aluminum ternary metal composite catalyst. The catalyst is labeled 2Ni2CoAl.
The nickel-cobalt-aluminum ternary metal composite catalyst prepared by the method is used for preparing the following gamma-valerolactone:
0.125g of levulinic acid and 5mL of 1, 4-dioxane are added into a 25mL autoclave, 0.075g of 2Ni2CoAl is added as a catalyst, the reaction kettle is sealed, 3MPa of hydrogen is introduced, the mixture is magnetically stirred, the mixture is heated to 100 ℃ and kept for 2 hours, the reaction is finished, the mixture is cooled to room temperature, and sampling detection is carried out, wherein the detection result is shown as the serial number 4 in the table 1.
Examples 5 to 8
Preparing a nickel-cobalt-aluminum ternary metal composite catalyst:
2.907g (0.01 mol) nickel nitrate hexahydrate and 1.88g (0.005 mol) aluminum nitrate nonahydrate, 0.7275g cobalt nitrate hexahydrate (0.0025 mol) and 14.4g urea were dissolved in 70mL deionized water; reacting the solution at 120 ℃ for 4 hours, and separating to obtain solid precipitate; grinding the dried solid into powder, calcining the powder at 500 ℃ for 4 hours in an air atmosphere, and then calcining and reducing the calcined solid for 5 hours in 10% vol% of hydrogen +90% vol% of nitrogen atmosphere at 650 ℃ to obtain the nickel-cobalt-aluminum ternary metal composite catalyst. The catalyst was labeled 2Ni0.5CoAl.
The nickel-cobalt-aluminum ternary metal composite catalyst prepared by the method is used for preparing the following gamma-valerolactone:
0.125g of levulinic acid and 5mL of 1, 4-dioxane were added into a 25mL autoclave, 0.075g of 2Ni0.5CoAl was added as a catalyst, the reaction vessel was sealed, 3MPa of hydrogen was introduced, magnetic stirring was carried out, the temperature was increased to 100 ℃, 110 ℃, 120 ℃ and 130 ℃ and held for 2 hours, the reaction was terminated, the temperature was cooled to room temperature, sampling was carried out, and the results of detection are shown in Table 1 as numbers 5 to 8.
Examples 9 to 12
Preparing a nickel-cobalt-aluminum ternary metal composite catalyst:
2.907g (0.01 mol) nickel nitrate hexahydrate and 1.88g (0.005 mol) aluminum nitrate nonahydrate, 0.7275g cobalt nitrate hexahydrate (0.0025 mol) and 14.4g urea were dissolved in 70mL deionized water; reacting the solution at 120 ℃ for 4 hours, and separating to obtain solid precipitate; grinding the dried solid into powder, calcining the powder at 500 ℃ for 4 hours in an air atmosphere, and then calcining and reducing the calcined solid for 5 hours in 10% vol% of hydrogen +90% vol% of nitrogen atmosphere at 650 ℃ to obtain the nickel-cobalt-aluminum ternary metal composite catalyst. The catalyst was labeled 2Ni0.5CoAl.
The nickel-cobalt-aluminum ternary metal composite catalyst prepared by the method is used for preparing the following gamma-valerolactone:
adding 0.125g of levulinic acid and 5mL of 1, 4-dioxane into a 25mL autoclave, adding 0.075g of 2Ni0.5CoAl serving as a catalyst, sealing the reaction kettle, introducing 1MPa, 2MPa, 3MPa and 4MPa of hydrogen, magnetically stirring, heating to 120 ℃ and keeping for 2 hours, cooling to room temperature after the reaction is finished, sampling and detecting, wherein the detection result is listed as the serial number 9-12 in the table 1.
Examples 13 to 15
Preparing a nickel-cobalt-aluminum ternary metal composite catalyst:
2.907g (0.01 mol) nickel nitrate hexahydrate and 1.88g (0.005 mol) aluminum nitrate nonahydrate, 0.7275g cobalt nitrate hexahydrate (0.0025 mol) and 14.4g urea were dissolved in 70mL deionized water; reacting the solution at 120 ℃ for 4 hours, and separating to obtain solid precipitate; grinding the dried solid into powder, calcining the powder at 500 ℃ for 4 hours in an air atmosphere, and then calcining and reducing the calcined solid for 5 hours in a 10-vol% hydrogen + 90-vol% nitrogen atmosphere at 650 ℃ to obtain the nickel-cobalt-aluminum ternary metal composite catalyst. The catalyst was labeled 2Ni0.5CoAl.
The nickel-cobalt-aluminum ternary metal composite catalyst prepared by the method is used for preparing the following gamma-valerolactone:
0.125g of levulinic acid and 5mL of 1, 4-dioxane were added into a 25mL autoclave, 0.075g of 2Ni0.5CoAl was added as a catalyst, the reaction vessel was sealed, 3MPa of hydrogen was introduced, magnetic stirring was carried out, the temperature was increased to 120 ℃ and held for 1 hour, 2 hours and 3 hours, the reaction was terminated, the temperature was cooled to room temperature, sampling was carried out, and the results of detection are shown in Table 1 as numbers 13 to 15.
TABLE 1 test results in examples
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims and their equivalents.
Claims (5)
1. The nickel-cobalt-aluminum ternary metal composite catalyst is characterized in that the catalyst is marked as xNiyCoAl, wherein x represents the molar ratio of Ni element to Al element, x =2,y represents the molar ratio of Co element to Al element, and y =0.5;
the catalyst is prepared by the following method: dissolving cobalt nitrate hexahydrate, urea, nickel nitrate hexahydrate and aluminum nitrate nonahydrate in deionized water; reacting at 110-140 deg.C for 3-5h, separating solid and liquid, drying the solid precipitate, and grinding into powder; calcining at 400-600 ℃ for 3-4h, and then reducing at 550-750 ℃ for 4-6h under protective gas to obtain the nickel-cobalt-aluminum ternary metal composite catalyst;
the catalyst is applied to the preparation of gamma-valerolactone, and the preparation method comprises the following steps: mixing levulinic acid and a solvent 1,4-dioxane, placing the mixture into a reaction container, adding a nickel-cobalt-aluminum ternary metal composite catalyst, sealing the reactor, and filling hydrogen, wherein the hydrogen pressure is 3-4MPa, the temperature of the reactor is 120-130 ℃, and the reaction time is 2-3h.
2. The Ni-Co-Al ternary metal composite catalyst according to claim 1, wherein the molar ratio of urea to the total of the three elements of Ni, co and Al is 12.5-14.5.
3. The nickel-cobalt-aluminum ternary metal composite catalyst according to claim 1, wherein in the aqueous solution containing nickel nitrate, cobalt nitrate, aluminum nitrate and urea, the concentration of urea is 3 to 5mol/L, and the concentration of cobalt nitrate is 0.015 to 0.15mol/L.
4. The Ni-Co-Al ternary metal composite catalyst according to claim 1, wherein the calcination is performed in an air atmosphere.
5. The Ni-Co-Al ternary metal composite catalyst according to claim 1, wherein the protective gas is 10% vol% H +90% vol% N.
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| CN112371150A (en) * | 2020-10-26 | 2021-02-19 | 厦门大学 | Nickel-aluminum bimetal nitrogen-carbon doped catalyst, preparation method thereof and application thereof in catalyzing levulinic acid hydrogenation to prepare gamma-valerolactone |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105056954B (en) * | 2015-08-27 | 2018-05-18 | 厦门大学 | A kind of hydrogenation catalyst and preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102407121A (en) * | 2011-10-18 | 2012-04-11 | 华南理工大学 | Preparation method of hydrogenation catalyst with X/Ni/A1 hydrotalcite as precursor |
| CN103193736A (en) * | 2013-03-30 | 2013-07-10 | 浙江工业大学 | Method for synthesizing gamma-valerolactone based on catalytic hydrogenation |
| WO2016056030A1 (en) * | 2014-10-08 | 2016-04-14 | Council Of Scientific & Industrial Research | A process for the preparation of gamma-valerolactone by catalytic hydrogenation of levulinic acid using ru-based catalysts |
| CN106558695A (en) * | 2016-10-25 | 2017-04-05 | 荆门市格林美新材料有限公司 | A kind of nickel cobalt aluminum complex hydroxide, nickel cobalt aluminium composite oxide and preparation method thereof |
| CN112371150A (en) * | 2020-10-26 | 2021-02-19 | 厦门大学 | Nickel-aluminum bimetal nitrogen-carbon doped catalyst, preparation method thereof and application thereof in catalyzing levulinic acid hydrogenation to prepare gamma-valerolactone |
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