Catalyst for synthesizing oxalic ester through oxidative coupling of CO gas phase as well as preparation and application method thereof

A catalyst and oxidation couple technology, applied in the field of oxalate ester preparation, can solve the problems of poor catalytic performance, high price, limited reserves, etc., achieve good catalytic activity and reduce costs

Inactive Publication Date: 2013-04-24
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

Pd is a noble metal with high price and limited reserves. The high loading leads to high catalyst cost and affects its use in industry.
[0005] 2. The space-time yield of oxalate is low, such as Pd-Ti / Al reported in US4507494 2 o 3 When the catalyst is applied to CO and methyl nitrite to synthesize dimethyl oxalate, the space-time yield is 429-462g·L -1 h -1 , Pd-Mo / Al reported in US4384433 2 o 3 and Pd-Ni / Al 2 o 3 The space-time yield of dimethyl oxalate was 400g·L when the catalyst was applied to CO and methyl nitrite to synthesize dimethyl oxalate -1 h -1
[0006] 3. Most of the existing catalysts use α-alumina as the carrier, while silica and activated carbon as the carrier show poor catalytic performance

Method used

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  • Catalyst for synthesizing oxalic ester through oxidative coupling of CO gas phase as well as preparation and application method thereof
  • Catalyst for synthesizing oxalic ester through oxidative coupling of CO gas phase as well as preparation and application method thereof
  • Catalyst for synthesizing oxalic ester through oxidative coupling of CO gas phase as well as preparation and application method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Will K 2 PdCl 4 Dissolve in deionized water to prepare a Pd ion concentration of 0.01M solution, then add 1.06g of nano-magnesium oxide to the above 5ml solution and stir for 2 hours, and ultrasonically disperse in a water bath at 50℃ with 200W energy until the solvent evaporates to dryness to obtain a solid Things. Dry the solid at 100°C for 8 hours, then roast it in an air atmosphere at 400°C for 4 hours, and then reduce it with reducing gas (hydrogen-nitrogen mixed gas) at a temperature of 300°C for 3 hours. The reducing gas space velocity is 3000 h -1 , And then lower the temperature to room temperature in a reducing atmosphere to obtain the desired catalyst. The loading of Pd is 0.5% of the carrier mass.

[0034] Catalyst evaluation: The catalyst in the example of the present invention is applied to the CO gas phase oxidative coupling synthesis of oxalate. The amount of catalyst is 1 mL, the flow ratio of feed gas CO and methyl nitrite is 1.4, and the gas space veloci...

Embodiment 2

[0040] Pd(OAc) 2 Dissolve in acetone to prepare a solution with a Pd ion concentration of 0.005M, then add 1.06g of nano-magnesium oxide to the above 10ml solution and stir for 0.5 hours, and ultrasonically disperse in a water bath at 25°C with 200W energy until the solvent evaporates to dryness to obtain a solid. . The solid was dried at 100°C for 8 hours, and then calcined in an air atmosphere at 400°C for 4 hours, and then reduced with pure hydrogen at a temperature of 300°C for 3 hours. The reducing gas space velocity was 3000 h -1 , And then lower the temperature to room temperature in a reducing atmosphere to obtain the desired catalyst. The loading of Pd is 0.5% of the carrier mass.

Embodiment 3

[0042] Pd(acac) 2 Dissolve in acetone to prepare a solution with a Pd ion concentration of 0.005M, then add 1.06g of nano-magnesium oxide to the above 10ml solution and stir for 0.5 hours, and ultrasonically disperse in a water bath at 25°C with 200W energy until the solvent evaporates to dryness to obtain a solid. . The solid was dried at 100°C for 8 hours, and then calcined in an air atmosphere at 400°C for 4 hours, and then reduced with pure hydrogen at a temperature of 300°C for 3 hours. The reducing gas space velocity was 3000 h -1 , And then lower the temperature to room temperature in a reducing atmosphere to obtain the desired catalyst. The loading of Pd is 0.5% of the carrier mass.

[0043] The catalysts of Comparative Example 1, Example 2 and Example 3 were evaluated in the same manner as in Example 1. The reaction temperature was 140°C. The chromatographic analysis chart is shown in figure 2 , image 3 with Figure 4 , The reaction results are shown in Table 2.

[004...

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Abstract

The invention discloses a catalyst for synthesizing oxalic ester through oxidative coupling of CO gas phase as well as a preparation and application method thereof, belonging to the technical field of oxalic ester preparation. Nanometer magnesia is used as a carrier of the catalyst, and the active component of the catalyst is noble metal palladium; and the content of the active component palladium is 0.01-2 percent by the mass of the carrier of the catalyst. The catalyst is prepared by adopting an improved steeping method which is beneficial to realization of large-scale production of the catalyst. The catalyst disclosed by the invention is characterized in that the commercial nanometer magnesia is used as the carrier of the catalyst while alpha-alumina is used as the carrier of a conventional catalyst. Experiments show that compared with a catalyst taking alpha-aluminum oxide as a carrier, which is prepared under same conditions, the catalyst disclosed by the invention shows better catalytic activity in reaction of synthesizing oxalic ester through oxidative coupling of CO gas phase. The per-pass conversion of CO is up to 65 percent, the selectivity of the oxalic ester is higher than 95 percent, and the space time yield of the oxalic ester is greater than 1200g.L<-1>.h<-1> (airspeed is 3000h<-1>).

Description

Technical field [0001] The invention belongs to the technical field of oxalate preparation, and relates to a catalyst for synthesizing oxalate by CO gas phase oxidative coupling in coal-to-ethylene glycol, and preparation and application methods thereof. Background technique [0002] Oxalate is an important organic chemical raw material, which can be used to prepare oxalic acid, oxalyl chloride, oxalic acid amine, and can also be used for fine chemical production of various dyes, medicines, important solvents, extractants and various intermediates. In addition, oxalate hydrogenation can also prepare extremely important chemical basic raw material ethylene glycol. [0003] At present, oxalic acid and alcohol are still used in the country to produce oxalate by esterification and dehydration with toluene or benzene as dehydrating agent. The method has high production process cost, large energy consumption, serious pollution, and unreasonable utilization of raw materials. In the 1960...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J21/10C07C69/36C07C67/36
Inventor 彭思艳郭国聪徐忠宁陈青松王志巧王明盛姚元根
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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