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Cobalt-manganese double metal catalyst for cyclohexane selective oxidation, preparation method and application

A technology of bimetallic catalyst and cyclohexane, which is applied in the direction of oxidation reaction preparation, organic compound preparation, hydrocarbon oxidation preparation of oxygen-containing compounds, etc., to achieve good stability

Inactive Publication Date: 2018-05-04
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its shortcoming is mainly manifested in that the single-pass conversion rate of cyclohexane is only 4% to 5%, and the selectivity of cyclohexanol and cyclohexanone is about 85%.

Method used

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  • Cobalt-manganese double metal catalyst for cyclohexane selective oxidation, preparation method and application
  • Cobalt-manganese double metal catalyst for cyclohexane selective oxidation, preparation method and application
  • Cobalt-manganese double metal catalyst for cyclohexane selective oxidation, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Weigh 0.05g of cobalt nitrate and 0.05g of manganese nitrate, dissolve in 5ml of 50% ethanol aqueous solution containing 5% pyridine, and stir until the solid is completely dissolved;

[0026] (2) Dissolve 4g of P123 in 84.85g of hydrochloric acid (120ml, 2M) solution, stir at 40°C for 2h at high speed, when the solution becomes transparent, add 8.5g of tetraethylorthosilicate (TEOS), stir at 40°C for 24h. Then the solution was transferred to a hydrothermal reactor and reacted at 100°C for 48h. After the reaction, cool naturally, filter and wash with absolute ethanol, dry at 100°C for 3 hours, and bake at 550°C for 6 hours. After natural cooling, it is mesoporous silica SBA-15 with a BET specific surface area of ​​625m 2 / g. Weigh 1g of mesoporous material SBA-15, slowly add SBA-15 into the above-mentioned solution dissolved with cobalt nitrate and manganese nitrate; keep stirring for 5h, then dry overnight at 80°C to obtain intermediate sample A;

[0027] (3) Cal...

Embodiment 2

[0034] (1) Take by weighing theoretically calculated cobalt nitrate 0.05g and manganese nitrate 0.03g, then dissolve the weighed sample in 5ml of 50% ethanol aqueous solution containing 5% pyridine, and stir until the solid is completely dissolved;

[0035] (2) Weigh 1g of mesoporous material SBA-15, slowly add SBA-15 into the above-mentioned solution dissolved with cobalt nitrate and manganese nitrate; keep stirring for 5h, then dry at 80°C overnight to obtain intermediate sample A;

[0036] (3) Calcining A at 350°C for 5 hours to obtain a catalyst;

[0037] (4) Take by weighing 50 mg of the catalyst prepared above, place 100 ml in a stainless steel reaction kettle with a polytetrafluoro liner, then add 20 ml of cyclohexane, and replace the gas with oxygen three times, and the reaction conditions are oxygen pressure 1 MPa, and the reaction The temperature was 150° C. and the stirring speed was 800 rpm for 70 minutes.

[0038] (5) After the reaction, the mixed solution after ...

Embodiment 3

[0043] (1) Take by weighing theoretically calculated cobalt nitrate 0.05g and manganese nitrate 0.02g, dissolve in 5ml of 50% ethanol aqueous solution containing 5% pyridine, and stir until the solid is completely dissolved;

[0044] (2) Weigh 1 g of mesoporous material SBA-15, slowly add SBA-15 into the solution dissolved with cobalt nitrate and manganese nitrate; keep stirring for 5 hours, then dry at 80°C overnight to obtain intermediate sample A;

[0045] (3) Calcining the intermediate sample A at 350° C. for 3 hours to obtain a catalyst;

[0046] (4) Take by weighing 50 mg of the catalyst prepared above, place 100 ml in a stainless steel reaction kettle with a polytetrafluoro liner, then add 20 ml of cyclohexane, and replace the gas with oxygen three times, and the reaction conditions are oxygen pressure 1 MPa, and the reaction The temperature was 150° C. and the stirring speed was 800 rpm for 70 minutes.

[0047] (5) After the reaction finishes, analyze with GC-9790 gas...

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Abstract

The invention discloses a cobalt-manganese double metal catalyst for cyclohexane selective oxidation, a preparation method and an application. The catalyst is a loaded catalyst, wherein the carrier which is a mesoporous material loads manganese nitrate and cobalt nitrate, the loading amount of cobalt nitrate is 1.0-6.0wt% and that of the manganese nitrate is 0.5-5.0wt%. The preparation method comprises the following steps: dissolving manganese nitrate and cobalt nitrate in a mixed solution of water and ethanol containing pyridine and adding the mesoporous material in a stirring condition; andthen drying the mixture overnight and calcining the same to obtain the cobalt-manganese double metal catalyst. The cobalt and manganese mixed catalyst is applied to a multiphase catalytic reaction forpreparing cyclohexanol and cyclohexanone by cyclohexane selective oxidization for the first time. The catalyst shows excellent activity and high selectivity, and has good stability.

Description

technical field [0001] The invention belongs to the technical field of organic catalysis, and specifically relates to a cobalt-manganese bimetallic catalyst for the selective oxidation of cyclohexane, a preparation method and an application. Background technique [0002] Cyclohexanol and cyclohexanone are important raw materials for the synthesis of chemical products such as caprolactam (CPL) and adipic acid (AA). They can be used as solvents for paint shellac and varnish, and are also used to prepare spices (such as civet ketone) and fruit antifungal agent phenyl An important raw material for phenol rubber anti-aging agents, etc. Among them, the most important use of the downstream products of cyclohexanone and cyclohexanol is to synthesize adipic acid, followed by the monomer caprolactam of synthetic fiber nylon-6 and nylon-66. The development of the industry for preparing cyclohexanol and cyclohexanone relies on the development of the caprolactam and adipic acid industri...

Claims

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Application Information

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IPC IPC(8): B01J29/04C07C29/50C07C35/08C07C45/33C07C49/403C07C27/12
CPCB01J29/045B01J2229/18C07C29/50C07C45/33C07C35/08C07C49/403
Inventor 李俊段小刚岳鲁敏付伟代士维
Owner SHANGHAI INST OF TECH
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