Catalyst, preparation method thereof and application in preparation of oxalate

A catalyst and oxalate technology, which is applied in the direction of catalyst activation/preparation, carbon monoxide or formate reaction preparation, chemical instruments and methods, etc., can solve the problems of high loading capacity and increased catalyst cost, and achieve improved performance and small size. , cost reduction effect

Active Publication Date: 2017-04-26
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Catalyst Pd / α-A1 used in industry 2 o 3 The high loading of Pd in ​​the medium (about 2wt%) makes the cost of the catalyst for the production of ethylene glycol increase significantly

Method used

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  • Catalyst, preparation method thereof and application in preparation of oxalate
  • Catalyst, preparation method thereof and application in preparation of oxalate
  • Catalyst, preparation method thereof and application in preparation of oxalate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Embodiment 1 Catalyst sample preparation

[0051] Preparation of graphene nanosheets

[0052] A two-electrode system is adopted, with high-purity graphite paper as the anode and cathode, followed by cleaning with 0.1mol / L hydrochloric acid, acetone, ethanol, and ultrapure water; 1mol / L ammonium sulfate solution as the electrolyte. Using the square wave potentiometric method, the upper limit is 9V, the lower limit is -9V, and the frequency is 10 Hz, the graphite electrode is electrolyzed, and the graphene nanosheet suspension is obtained through sulfate radical intercalation expansion and stripping, and the graphene nanosheet suspension is ultrasonically filtered, washed, After vacuum drying, graphene nanosheets are obtained, which are denoted as GNPs.

[0053] Preparation of nitrogen-doped graphene nanosheets

[0054] The above-mentioned graphene nanosheet GNP obtained is placed in a tube furnace, and at nitrogen doping temperature, feeds ammonia gas for a period ...

Embodiment 2

[0066] Example 2 Sample Characterization

[0067] The nitrogen doping amount in the nitrogen-doped graphene nanosheet samples N-GNP-1-N-GNP-3 was measured by XPS, and the results are shown in Table 1.

[0068] The loading capacity of palladium in the catalyst samples CAT-1 to CAT-7 was measured by ICP, and the results are shown in Table 2.

[0069] Scanning electron micrographs of graphene nanosheets GNPs such as figure 1 As can be seen from the figure, GNP is a nanosheet with a thickness of 0.8-30 nm and a size of 1-15 μm.

[0070] Catalyst samples CAT-1~CAT-7 were characterized by transmission electron microscopy. The results showed that nitrogen doping greatly improved the dispersion of active component palladium. Taking sample CAT-1 as a typical representative, its transmission electron microscope pictures are as follows figure 2 shown by figure 2 It can be seen that palladium nanoparticles are highly dispersed on the surface of nitrogen-doped graphene nanosheets, an...

Embodiment 3

[0072] Embodiment 3 catalyst sample is used for the reaction evaluation of preparing oxalic acid ester

[0073] The catalyst samples CAT-1~CAT-7 and the comparative sample Pd / GNP were respectively placed in a fixed-bed reactor and applied to the gas-phase oxidative coupling of CO to prepare oxalate. The raw material gas included CO and methyl nitrite. The flow volume ratio of CO and methyl nitrite is 1.4, and the gas phase space velocity of the feed gas is 3L g -1 h -1 , the reaction temperature was 130°C, and the reaction pressure was 0.1Mpa. The feed gas and products were monitored and analyzed by on-line gas chromatography. The reaction results are shown in Table 3.

[0074] table 3

[0075]

[0076] As can be seen from the data in Table 3, compared with the catalyst sample provided by the technical solution of the present application, when the palladium loading is similar (compared with CAT-4), the comparative example sample has a single-pass conversion rate of CO far...

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Abstract

The invention discloses a catalyst, a preparation method thereof and application in preparation of oxalate. The catalyst comprises a carrier and an active ingredient, and is characterized in that the carrier comprises nitrogen doped graphene nano-sheets, and the active ingredient comprises nano-palladium. The content of the active ingredient palladium in the catalyst is 0.03-2wt%, and the defects of high loading capacity of precious metals, low space time yield of oxalate and the like in production of an oxalate catalyst through CO coupling in the prior art are overcome when the catalyst is used in a CO coupling oxalate production technology.

Description

technical field [0001] The application relates to a catalyst, its preparation method and its application in the preparation of oxalate, belonging to the field of chemistry and chemical engineering. Background technique [0002] Oxalate is an important organic chemical raw material and is widely used in the preparation of various important chemical products, such as hydrolysis of oxalate to obtain oxalic acid, ammoniation to obtain oxamide, and hydrogenation to prepare ethylene glycol. CO gas-phase oxidative coupling to oxalate (2CO+2RONO→(COOR)2+2NO) is a key step in "coal to ethylene glycol" and has important industrial application value. In addition, this process also has important application prospects in industrial tail gas treatment. Many industrial tail gases contain a large amount of CO, which is currently mainly treated by combustion. If the CO in the tail gas is collected and converted into oxalate with high added value, it can not only achieve energy saving and em...

Claims

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Application Information

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IPC IPC(8): B01J27/24C07C67/36C07C69/36
CPCC07C67/36B01J27/24B01J37/02B01J37/08B01J37/18B01J35/396B01J35/393C07C69/36
Inventor 陈青松郭国聪唐敬筱徐忠宁陈毓敏王志巧谭洪梓
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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