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A kind of method utilizing waste and old palladium catalyst to synthesize dimethyl oxalate catalyst

A dimethyl oxalate and palladium catalyst technology, which is applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve environmental pollution, waste of resources, and no mention of carrier alumina ball treatment methods, etc. problem, to achieve the effects of less environmental pollution, lower production costs, and curb the loss of precious metal palladium

Active Publication Date: 2020-09-04
河南能源集团研究总院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the process still does not mention the treatment method of the carrier alumina balls, causing environmental pollution and waste of resources

Method used

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  • A kind of method utilizing waste and old palladium catalyst to synthesize dimethyl oxalate catalyst

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Effect test

Embodiment 1

[0031] The method of utilizing the waste palladium catalyst of the present embodiment to synthesize dimethyl oxalate catalyst, the steps are as follows:

[0032] (1) Dilute concentrated hydrochloric acid in deionized water to obtain a solution with a concentration of 0.01~5mol / L, which is recorded as solution A, and weigh a certain amount of NaClO 3 , dissolved in deionized water to obtain a solution with a concentration of 0.01~5mol / L, which is designated as solution B;

[0033] (2) Weigh 100 g of spent palladium catalyst, gradually add 1500 mL of solution A to the weighed spent catalyst, then drop into 150 mL of solution B, soak for 24 hours, and then filter out the liquid to obtain carrier alumina pellets;

[0034] (3) Repeated washing with water until the pH value of the water is between 6.5 and 7.5;

[0035](4) Then the carrier alumina pellets were dried at 110 °C for 24 hours, then heated to 550 °C in a muffle furnace at a heating rate of 5 °C / min, roasted for 5 hours, ...

Embodiment 2

[0043] The method of utilizing the waste palladium catalyst of the present embodiment to synthesize dimethyl oxalate catalyst, the steps are as follows:

[0044] (1) Dilute concentrated hydrochloric acid in deionized water to obtain a solution with a concentration of 0.01mol / L, which is recorded as solution A, and weigh a certain amount of H 2 o 2 , denoted as solution B;

[0045] (2) Weigh 100 g of spent palladium catalyst, gradually add 2000 mL of solution A to the weighed spent catalyst, then drop into 150 mL of solution B, soak for 24 hours, and then filter out the liquid to obtain carrier alumina pellets;

[0046] (3) Repeated washing with water until the pH value of the water is between 6.5 and 7.5;

[0047] (4) Then, the carrier alumina pellets were dried at 60°C for 24 hours, then heated to 600°C in a muffle furnace at a heating rate of 5°C / min, roasted for 1 hour, and naturally cooled to room temperature;

[0048] (5) PdCl 2 Dissolved in deionized water to obtain ...

Embodiment 3

[0055] The method of utilizing the waste palladium catalyst of the present embodiment to synthesize dimethyl oxalate catalyst, the steps are as follows:

[0056] (1) Dilute concentrated hydrochloric acid in deionized water to obtain a solution with a concentration of 1mol / L, which is recorded as solution A, and weigh a certain amount of NaClO 3 , was dissolved in deionized water to obtain a solution with a concentration of 1mol / L, which was designated as solution B;

[0057] (2) Weigh 100 g of spent palladium catalyst, gradually add solution A to the weighed spent catalyst, then drop into solution B, soak for 24 hours, and then filter out the liquid to obtain carrier alumina pellets;

[0058] (3) Repeated washing with water until the pH value of the water is between 6.5 and 7.5;

[0059] (4) Then the carrier alumina pellets were dried at 110 °C for 24 hours, then heated to 550 °C in a muffle furnace at a heating rate of 5 °C / min, roasted for 5 hours, and naturally cooled to r...

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Abstract

The invention discloses a method for synthesizing a dimethyl oxalate catalyst by using a waste palladium catalyst. The leaching method is used to recover the metal palladium in the waste palladium-alumina catalyst. The remaining alumina pellets are washed, dried and roasted, and then reused. Load palladium and additives to prepare a catalyst for the reaction between methyl nitrite and CO to generate dimethyl oxalate. The extracted alumina balls are reused as catalyst carriers. The catalyst activity is good, the conversion rate of methyl nitrite and the selectivity of the product dimethyl oxalate are very good, the service life is long, and the adhesion of the carrier beads to palladium is significantly enhanced. The loss of precious metal palladium in the catalyst palladium-alumina is greatly suppressed.

Description

technical field [0001] The invention belongs to the field of recovery and utilization of catalyst secondary resources, and in particular relates to a method for synthesizing a dimethyl oxalate catalyst by using a waste palladium catalyst. Background technique [0002] Palladium is a catalyst often used in chemical and chemical reactions. There are many types of palladium-containing catalysts. Most of them are used in catalytic hydrogenation and catalytic oxidation in petrochemical industry. They have the advantages of high catalytic activity and good selectivity. , making many difficult-to-realize reaction processes possible, palladium is compounded with other metals or co-catalysts, and has better catalytic performance, such as palladium-based catalysts used in hydrogenation reactions, and supported platinum-rhodium-palladium triple-effect catalysts used in automobile exhaust purification Catalyst, Pd-Cu catalyst for ethylene oxidation to acetaldehyde, palladium-rhodium-pla...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/89B01J23/96B01J35/08B01J37/02C07C67/36C07C69/36C22B11/00
CPCC22B11/048C07C67/36B01J23/8926B01J23/96B01J37/0203B01J37/0205B01J37/0207B01J37/0236B01J35/51C07C69/36Y02P20/584Y02P10/20
Inventor 张鲁湘穆仕芳宋军超张磊蒋元力魏灵朝徐柳
Owner 河南能源集团研究总院有限公司
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