High-efficiency nano Pd catalyst used in the process of preparing oxalate through CO carbonylation and prepared by dipping-controllable reduction method

A catalyst and reducing agent technology, applied in the field of high-efficiency nano-Pd catalysts, can solve the problems of active component crystallite coalescence, catalytic activity reduction, and high dispersion of active groups, and achieve simple preparation process, low cost, and industrialization Effect

Active Publication Date: 2012-07-04
贵州鑫醇科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the influence of the solvation effect of the impregnation solvent and the cluster effect of the active components, the traditional impregnation method is not easy to highly disperse the active groups, and the active components may crystallite coalesce during the subsequent calcination and high-temperature reduction process, resulting in catalytic Reduced activity

Method used

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  • High-efficiency nano Pd catalyst used in the process of preparing oxalate through CO carbonylation and prepared by dipping-controllable reduction method
  • High-efficiency nano Pd catalyst used in the process of preparing oxalate through CO carbonylation and prepared by dipping-controllable reduction method
  • High-efficiency nano Pd catalyst used in the process of preparing oxalate through CO carbonylation and prepared by dipping-controllable reduction method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Weigh 1g of α-alumina and impregnate it into 1.25mL of 37.6mmol / L K 2 PdCl 4- Add 4 mL of ethanol to the aqueous solution, stir for 3 hours, ultrasonically disperse in a 40°C water bath with 200W energy for 4 hours, dry at 110°C for 4 hours, and roast at 400°C for 4 hours, add 0.070g ascorbic acid, 0.353g KBr, and 0.444g PVP , reduced at 100°C for 30 minutes, and dried in vacuum at 60°C for 10 hours. TEM photo see figure 1 , it can be seen from the figure that Pd is evenly dispersed on the surface of the carrier, and the particles are mainly spherical, with a small amount of irregular polyhedron, and the average size is 6–7nm.

[0045] Catalyst evaluation: The catalyst in the examples of the present invention was applied to the gas-phase carbonylation of CO to produce oxalate, the catalyst dosage was 1 mL, and the N in the raw gas 2 : CO: RONO = 48: 28: 20 (volume ratio), gas phase space velocity is 3000h -1 , the reaction temperature is 130°C, the reaction pressure...

Embodiment 2

[0047] Weigh 1g of α-alumina and impregnate it into 1.25mL of 37.6mmol / L Pd(NO 3 ) 2- Add 4 mL of acetone to the aqueous solution, stir for 3 hours, ultrasonically disperse in a 35°C water bath with 200W energy for 3 hours, dry at 110°C for 4 hours, and roast at 400°C for 4 hours, add 0.105g citric acid, 0.353g KBr, 0.444g PVP was reduced at 90°C for 15 hours, then 0.018g of ascorbic acid was added to continue the reduction at 90°C for 30 minutes, and then dried in vacuum at 60°C for 10 hours. TEM photo see figure 2 , it can be seen from the figure that Pd is evenly dispersed on the surface of the carrier, and the particles are mainly spherical, with a small amount of irregular polyhedrons, and the average size is 4–6 nm. For chromatographic analysis see Figure 6 , and the reaction results are shown in Table 1.

Embodiment 3

[0049] Weigh 1g of α-alumina and impregnate it into 1.25mL of 37.6mmol / L Pd(OAc) 2- Add 4 mL of acetone to the acetone solution, stir for 3 hours, ultrasonically disperse in a 35°C water bath with 200W energy for 3 hours, dry at 110°C for 4 hours, bake at 400°C for 2 hours, add 0.070g of ascorbic acid, 0.353g of KBr, 0.444g For PVP, reduce at 100°C for 30 minutes, and dry at 60°C for 10 hours under vacuum. TEM photo see image 3 , it can be seen from the figure that Pd is evenly dispersed on the surface of the carrier, and the particles are mainly spherical, with a small amount of irregular polyhedrons, and the average size is 4–6 nm. For chromatographic analysis see Figure 7 , and the reaction results are shown in Table 1.

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Abstract

The invention discloses a high-efficiency nano Pd catalyst used in the process of preparing oxalate through CO carbonylation. The catalyst comprises alpha-aluminum oxide serving as a carrier and 0.05 to 2 weight percent of noble metal Pd nanoparticles serving as active ingredients. The catalyst is prepared by a dipping-alkali-free liquid phase controllable reduction method. The catalyst is high in metal dispersion degree and narrow in dimensional distribution and can efficiently catalyze CO gas phase carbonylation to prepare the oxalate under the conditions of low temperature and low noble metal load, wherein the single-pass conversion ratio of the CO is 48 percent; the selectivity of the oxalate is over 99 percent; and the space time yield of the oxalate is more than 1,000 g.L<-1>.h<-1> (space velocity is 3,000 h<-1>).

Description

technical field [0001] The invention relates to a high-efficiency nano-Pd catalyst, in particular to a high-efficiency nano-Pd catalyst for producing oxalate by CO gas-phase carbonylation in a two-step coal-to-ethylene glycol process. technical background [0002] Ethylene glycol is an extremely important and strategic bulk chemical raw material. At present, the world's annual demand is more than 20 million tons, of which one-third of the market demand is in China. The total output of ethylene glycol in the world exceeds 18 million tons, while my country's production capacity is about 1.5 million tons, with a gap of about 5 million tons. The contradiction between supply and demand is very prominent, and a large amount of reliance is placed on imports. At present, ethylene glycol is mainly synthesized from petroleum ethylene, and my country is a country rich in coal and low in oil. Therefore, the development of coal-based ethylene glycol can not only effectively alleviate the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J37/16C07C69/36C07C67/36
Inventor 徐忠宁郭国聪王明盛姚元根
Owner 贵州鑫醇科技发展有限公司
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