CN112794375A - Preparation method of manganese dioxide modified nickel-cobalt spinel catalyst - Google Patents
Preparation method of manganese dioxide modified nickel-cobalt spinel catalyst Download PDFInfo
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- CN112794375A CN112794375A CN202110033652.5A CN202110033652A CN112794375A CN 112794375 A CN112794375 A CN 112794375A CN 202110033652 A CN202110033652 A CN 202110033652A CN 112794375 A CN112794375 A CN 112794375A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
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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
- B01J23/005—Spinels
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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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
Abstract
The invention belongs to the field of biomass recycling, and relates to a preparation method of a manganese dioxide modified nickel-cobalt spinel catalyst, which comprises the following steps: a. preparing the nickel-cobalt spinel. b. And (3) dispersing nickel-cobalt spinel in deionized water to obtain a solution A. c. Dissolving manganese salt and potassium permanganate in deionized water to obtain a solution B. d. And mixing the solution A and the solution B, and stirring for 30min to obtain a mixed solution C. e. And (3) putting the solution C into a hydrothermal kettle with polytetrafluoroethylene as a lining for hydrothermal for 4-10 hours at the temperature of 100-200 ℃, performing suction filtration, and performing vacuum drying. The manganese dioxide modified nickel-cobalt spinel catalyst provided by the invention has the advantages of cheap and easily available raw materials, simple preparation process and wide application range.
Description
Technical Field
The invention belongs to the field of biomass recycling, and particularly relates to a preparation method of a manganese dioxide modified nickel-cobalt spinel catalyst.
Background
As an important platform compound, catalytic oxidation of HMF is a key to the production of high-value chemicals and fuel energy from biomass and its derivatives. In the conventional metering oxidation method, an excessive amount of an oxidizing agent (such as potassium permanganate, potassium dichromate or higher lead compound) is often required, so that the atom utilization rate of the oxidizing agent is low, and a large amount of toxic byproducts are often generated in the oxidation process. When air or oxygen is selected as an oxidant to be used for catalyzing the HMF oxidation reaction, although the atom utilization rate is high and the HMF oxidation reaction is green and environment-friendly, the reaction process is not easy to control, and generally pressurization or high temperature is needed. In addition, although various catalysts have been developed and developed in recent years for oxidizing HMF to produce high-value compounds, the catalysts used for catalytic oxidation of HMF are mainly noble metals and supported catalysts thereof, and the preparation process is complicated, the cost is high, and the catalysts are not suitable for industrial production. And the non-noble metal catalyst has the problems of low activity, poor repeatability and the like. Thus, designing and developing a catalyst for selective oxidation of HMF at low cost and high stability remains a challenging task.
The invention content is as follows:
the invention aims to provide a preparation method of a manganese dioxide modified nickel-cobalt spinel catalyst with high catalytic activity and good stability, which is characterized by comprising the following steps:
a. preparing the nickel-cobalt spinel.
b. And dispersing nickel-cobalt spinel in deionized water, wherein the molar ratio of the nickel-cobalt spinel to the deionized water is 1: 800-1200, so as to obtain a solution A.
c. Dissolving manganous salt and potassium permanganate in deionized water, wherein the molar ratio of the manganous salt to the potassium permanganate to the deionized water is 1:1: 800-1200, and thus obtaining a solution B.
d. And mixing the solution A and the solution B, and stirring for 30min to obtain a mixed solution C.
e. And (3) putting the solution C into a hydrothermal kettle with polytetrafluoroethylene as a lining for hydrothermal for 4-16 h at the temperature of 100-200 ℃, carrying out suction filtration, and carrying out vacuum drying.
Further, the preparation method of the nickel-cobalt spinel in the step a comprises the following steps: and dissolving nickel salt and cobalt salt into deionized water, wherein the molar ratio of the nickel salt to the cobalt salt to the water is 1:2: 20-100, and thus obtaining a solution D. And adding an ethanol solution, concentrated ammonia water and 1mol/L sodium carbonate into the solution D, wherein the volume ratio of the solution D to the ethanol solution to the concentrated ammonia water to the 1mol/L sodium carbonate is 1: 2-8: 2-6: 1-3, so as to obtain a solution E. And (3) putting the solution E into a hydrothermal kettle with a polytetrafluoroethylene lining for hydrothermal for 8-16 h at the temperature of 100-200 ℃, performing suction filtration, performing vacuum drying, and roasting in a muffle furnace at the temperature of 250-380 ℃ for 2-5 h.
Further, the nickel salt in the preparation process of the nickel-cobalt spinel is one or more of nickel nitrate hexahydrate, nickel sulfate hexahydrate and nickel dichloride hexahydrate. The cobalt salt is one or more of cobalt nitrate hexahydrate, cobalt sulfate heptahydrate and cobalt chloride hexahydrate.
Further, the manganese salt in the step b is one or more of manganese sulfate monohydrate and manganese chloride tetrahydrate.
Further, the molar amount of the deionized water in the step b and the step c is the same.
Detailed Description
The present invention is further described in the following examples, but the technical content described in the examples is illustrative and not restrictive, and the scope of the present invention should not be limited thereby.
Example 1
a. Dissolving 2.9g of nickel nitrate hexahydrate and 5.8g of cobalt nitrate hexahydrate in deionized water, wherein the molar ratio of the nickel nitrate hexahydrate to the cobalt nitrate hexahydrate to the water is 1:2:56, and obtaining a solution A. Adding an ethanol solution, concentrated ammonia water and 1mol/L sodium carbonate into the solution A, wherein the volume ratio of the solution A to the ethanol solution to the concentrated ammonia water to the 1mol/L sodium carbonate is 1:8:6:3, so as to obtain a solution B. Putting the solution B into a hydrothermal kettle with a polytetrafluoroethylene lining for hydrothermal for 11 hours at the temperature of 170 ℃, performing suction filtration, performing vacuum drying, and roasting in a muffle furnace at the temperature of 300 ℃ for 3.3 hours to obtain the nickel-cobalt spinel.
b. 0.193g of nickel cobalt spinel was dispersed in deionized water at a molar ratio of nickel cobalt spinel to deionized water of 1:1042 to obtain solution C.
c. Dissolving 0.135g of manganese sulfate monohydrate and 0.126g of potassium permanganate in deionized water, wherein the molar ratio of the manganese sulfate monohydrate to the potassium permanganate to the deionized water is 1:1:1042, and obtaining a solution D.
d. And mixing the solution A and the solution B, and stirring for 30min to obtain a mixed solution E.
e. And putting the solution F into a hydrothermal kettle with a polytetrafluoroethylene lining for hydrothermal for 6 hours at the temperature of 160 ℃, carrying out suction filtration, and carrying out vacuum drying.
The performance of the manganese dioxide modified nickel-cobalt spinel catalyst is evaluated by adopting a Yangyi brand YZ-MR high-temperature high-pressure reactor, 2ml of 2000 mg/L5-hydroxymethylfurfural is used as a substrate, a solvent is dimethyl sulfoxide, 10mg of the prepared catalyst is taken, the oxygen pressure is controlled to be 2Mpa, the temperature is 120 ℃, the reaction time is 6 hours, and the yield of furan dicarbaldehyde is 75%.
Example 2
a. 1.83g of nickel nitrate hexahydrate and 3.66g of cobalt nitrate hexahydrate are dissolved in deionized water, and the molar ratio of the nickel nitrate hexahydrate, the cobalt nitrate hexahydrate and the water is 1:2:20, so that a solution A is obtained. Adding an ethanol solution, concentrated ammonia water and 1mol/L sodium carbonate into the solution A, wherein the volume ratio of the solution A to the ethanol solution to the concentrated ammonia water to the 1mol/L sodium carbonate is 1:2:2:1, so as to obtain a solution B. Putting the solution B into a hydrothermal kettle with polytetrafluoroethylene as a lining for hydrothermal for 8 hours at the temperature of 100 ℃, performing suction filtration, performing vacuum drying, and roasting in a muffle furnace at the temperature of 380 ℃ for 2 hours to obtain the nickel-cobalt spinel.
b. 0.50g of nickel-cobalt spinel is dispersed in deionized water, and the molar ratio of the nickel-cobalt spinel to the deionized water is 1:800, so as to obtain a solution C.
c. Dissolving 0.35g of manganese sulfate monohydrate and 0.33g of potassium permanganate in deionized water, wherein the molar ratio of the manganese sulfate monohydrate to the potassium permanganate to the deionized water is 1:1:800, and thus obtaining a solution D.
d. And mixing the solution A and the solution B, and stirring for 30min to obtain a mixed solution E.
e. And putting the solution F into a hydrothermal kettle with a polytetrafluoroethylene lining for hydrothermal for 4 hours at the temperature of 100 ℃, carrying out suction filtration, and carrying out vacuum drying.
The performance of the manganese dioxide modified nickel-cobalt spinel catalyst is evaluated by adopting a rock sign YZMR high-temperature high-pressure reactor, 2ml of 2000 mg/L5-hydroxymethylfurfural is used as a substrate, dimethyl sulfoxide is used as a solvent, 10mg of the prepared catalyst is taken, the oxygen pressure is controlled to be 2Mpa, the temperature is 120 ℃, the reaction time is 6 hours, and the yield of furan dicarbaldehyde is 42%.
Example 3
a. Dissolving 2.63g of nickel sulfate hexahydrate and 5.62g of cobalt sulfate heptahydrate into deionized water, wherein the molar ratio of the nickel sulfate hexahydrate and the cobalt sulfate heptahydrate to the water is 1:2:40, and obtaining a solution A. Adding an ethanol solution, concentrated ammonia water and 1mol/L sodium carbonate into the solution A, wherein the volume ratio of the solution A to the ethanol solution to the concentrated ammonia water to the 1mol/L sodium carbonate is 1:5:4:3, so as to obtain a solution B. And putting the solution B into a hydrothermal kettle with polytetrafluoroethylene as an inner lining, performing hydrothermal treatment for 9 hours at the temperature of 130 ℃, performing suction filtration, performing vacuum drying, and roasting in a muffle furnace at the temperature of 250 ℃ for 3 hours to obtain the nickel-cobalt spinel.
b. 0.24g of nickel-cobalt spinel is dispersed in deionized water, and the molar ratio of the nickel-cobalt spinel to the deionized water is 1:900, so as to obtain a solution C.
c. Dissolving 0.17g of manganese sulfate monohydrate and 0.16g of potassium permanganate in deionized water, wherein the molar ratio of the manganese sulfate monohydrate to the potassium permanganate to the deionized water is 1:1:900, and thus obtaining a solution D.
d. And mixing the solution A and the solution B, and stirring for 30min to obtain a mixed solution E.
e. Putting the solution E into a hydrothermal kettle with a polytetrafluoroethylene lining for hydrothermal for 8 hours at the temperature of 140 ℃, carrying out suction filtration, and carrying out vacuum drying.
The performance of the manganese dioxide modified nickel-cobalt spinel catalyst is evaluated by adopting a rock sign YZMR high-temperature high-pressure reactor, 2ml of 2000 mg/L5-hydroxymethylfurfural is used as a substrate, a solvent is dimethyl sulfoxide, 10mg of the prepared catalyst is taken, the oxygen pressure is controlled to be 2Mpa, the temperature is 120 ℃, the reaction time is 6 hours, and the yield of furan dicarbaldehyde is 52%.
Example 4
a. Dissolving 2.38g of nickel dichloride hexahydrate and 4.76g of cobalt chloride hexahydrate in deionized water, wherein the molar ratio of the nickel dichloride hexahydrate, the cobalt chloride hexahydrate and the water is 1:2:80, and obtaining a solution A. Adding an ethanol solution, concentrated ammonia water and 1mol/L sodium carbonate into the solution A, wherein the volume ratio of the solution A to the ethanol solution to the concentrated ammonia water to the 1mol/L sodium carbonate is 1:5:6:2, so as to obtain a solution B. Putting the solution B into a hydrothermal kettle with polytetrafluoroethylene as a lining for hydrothermal for 14 hours at the temperature of 140 ℃, performing suction filtration, performing vacuum drying, and putting into a muffle furnace for roasting at the temperature of 320 ℃ for 4 hours to obtain the nickel-cobalt spinel.
b. 0.480g of nickel-cobalt spinel is dispersed in deionized water, and the molar ratio of the nickel-cobalt spinel to the deionized water is 1:1100, so as to obtain a solution C.
c. 0.394g of manganese chloride tetrahydrate and 0.336g of potassium permanganate are dissolved in deionized water, and the molar ratio of the manganese chloride tetrahydrate to the potassium permanganate to the deionized water is 1:1:1100, so that a solution D is obtained.
d. And mixing the solution A and the solution B, and stirring for 30min to obtain a mixed solution E.
e. And (3) putting the solution E into a hydrothermal kettle with a polytetrafluoroethylene lining for hydrothermal for 9 hours at the temperature of 180 ℃, carrying out suction filtration, and carrying out vacuum drying.
The performance of the manganese dioxide modified nickel-cobalt spinel catalyst is evaluated by adopting a rock sign YZMR high-temperature high-pressure reactor, 2ml of 2000 mg/L5-hydroxymethylfurfural is used as a substrate, a solvent is dimethyl sulfoxide, 10mg of the prepared catalyst is taken, the oxygen pressure is controlled to be 2Mpa, the temperature is 120 ℃, the reaction time is 6 hours, and the yield of furan dimethyl aldehyde is 50%.
Claims (5)
1. A preparation method of manganese dioxide modified nickel-cobalt spinel catalyst is characterized by comprising the following steps:
a. preparing the nickel-cobalt spinel.
b. And dispersing nickel-cobalt spinel in deionized water, wherein the molar ratio of the nickel-cobalt spinel to the deionized water is 1: 800-1200, so as to obtain a solution A.
c. Dissolving manganous salt and potassium permanganate in deionized water, wherein the molar ratio of the manganous salt to the potassium permanganate to the deionized water is 1:1: 800-1200, and thus obtaining a solution B.
d. And mixing the solution A and the solution B, and stirring for 30min to obtain a mixed solution C.
e. And (3) putting the solution C into a hydrothermal kettle with polytetrafluoroethylene as a lining for hydrothermal for 4-10 hours at the temperature of 100-200 ℃, performing suction filtration, and performing vacuum drying.
2. The method for preparing manganese dioxide modified nickel cobalt spinel catalyst according to claim 1, characterized in that: the preparation method of the nickel-cobalt spinel in the step a comprises the following steps: and dissolving nickel salt and cobalt salt into deionized water, wherein the molar ratio of the nickel salt to the cobalt salt to the water is 1:2: 20-100, and thus obtaining a solution D. And adding an ethanol solution, concentrated ammonia water and 1mol/L sodium carbonate into the solution D, wherein the volume ratio of the solution D to the ethanol solution to the concentrated ammonia water to the 1mol/L sodium carbonate is 1: 2-8: 2-6: 1-3, so as to obtain a solution E. And (3) putting the solution E into a hydrothermal kettle with a polytetrafluoroethylene lining for hydrothermal for 8-16 h at the temperature of 100-200 ℃, performing suction filtration, performing vacuum drying, and roasting in a muffle furnace at the temperature of 250-380 ℃ for 2-5 h.
3. The preparation method of manganese dioxide modified nickel cobalt spinel catalyst according to claims 1 and 2, characterized by comprising the following steps: the nickel salt in the preparation process of the nickel-cobalt spinel is one or more of nickel nitrate hexahydrate, nickel sulfate hexahydrate and nickel dichloride hexahydrate. The cobalt salt is one or more of cobalt nitrate hexahydrate, cobalt sulfate heptahydrate and cobalt chloride hexahydrate.
4. The method for preparing manganese dioxide modified nickel cobalt spinel catalyst according to claim 1, characterized in that: and the manganese salt in the step b is one or more of manganese sulfate monohydrate and manganese chloride tetrahydrate.
5. The method for preparing manganese dioxide modified nickel cobalt spinel catalyst according to claim 1, characterized in that: the molar amount of the deionized water in the step b and the step c is the same.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113546640A (en) * | 2021-07-13 | 2021-10-26 | 常州大学 | NiO-CoMn2O4Preparation method of catalyst and application of catalyst in catalytic oxidation degradation of toluene |
| CN115582120A (en) * | 2022-09-16 | 2023-01-10 | 福州大学 | Preparation method of assistant modified supported Ru and/or Ni-based catalyst |
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| US5061675A (en) * | 1989-08-08 | 1991-10-29 | Mitsubishi Gas Chemical Company, Inc. | Process for producing a denaturated manganese dioxide catalyst for the hydration reaction of cyanohydrins |
| WO2018223054A1 (en) * | 2017-06-01 | 2018-12-06 | University Of Connecticut | Manganese-cobalt spinel oxide nanowire arrays |
| CN111001414A (en) * | 2019-12-06 | 2020-04-14 | 浙江工业大学 | Structure-controllable hollow nickel cobaltate nanowire/flaky manganese oxide core-shell array material and preparation method thereof |
| CN111054391A (en) * | 2019-12-15 | 2020-04-24 | 南京星宁环保科技有限公司 | Novel Pd-type NiCo loaded with noble metal2O4Preparation method of spinel catalyst |
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2021
- 2021-01-12 CN CN202110033652.5A patent/CN112794375B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US5061675A (en) * | 1989-08-08 | 1991-10-29 | Mitsubishi Gas Chemical Company, Inc. | Process for producing a denaturated manganese dioxide catalyst for the hydration reaction of cyanohydrins |
| WO2018223054A1 (en) * | 2017-06-01 | 2018-12-06 | University Of Connecticut | Manganese-cobalt spinel oxide nanowire arrays |
| CN111001414A (en) * | 2019-12-06 | 2020-04-14 | 浙江工业大学 | Structure-controllable hollow nickel cobaltate nanowire/flaky manganese oxide core-shell array material and preparation method thereof |
| CN111054391A (en) * | 2019-12-15 | 2020-04-24 | 南京星宁环保科技有限公司 | Novel Pd-type NiCo loaded with noble metal2O4Preparation method of spinel catalyst |
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| Title |
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| SI-WEN ZHANG等: "《Self-assembling hierarchical NiCo2O4/MnO2 nanosheets and MoO3/PPy core-shell heterostructured nanobelts for supercapacitor》", 《CHEMICAL ENGINEERING JOURNAL》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113546640A (en) * | 2021-07-13 | 2021-10-26 | 常州大学 | NiO-CoMn2O4Preparation method of catalyst and application of catalyst in catalytic oxidation degradation of toluene |
| CN113546640B (en) * | 2021-07-13 | 2023-10-20 | 常州大学 | NiO-CoMn 2 O 4 Preparation method of catalyst and application of catalyst in catalytic oxidative degradation of toluene |
| CN115582120A (en) * | 2022-09-16 | 2023-01-10 | 福州大学 | Preparation method of assistant modified supported Ru and/or Ni-based catalyst |
| CN115582120B (en) * | 2022-09-16 | 2023-12-19 | 福州大学 | Preparation method of auxiliary agent modified supported Ru and/or Ni-based catalyst |
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