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Catalyst for synthesizing dimethyl oxalate from CO and ultrasonic dispersion preparation method of catalyst

A technology of dimethyl oxalate and catalyst, which is applied in the field of catalyst and its preparation, can solve the problems of changing the dispersion of noble metal active components, and achieve the effects of ensuring stability, improving utilization rate, and high space-time yield

Inactive Publication Date: 2014-11-19
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

[0005] The purpose of the present invention is to provide a catalyst for the synthesis of dimethyl oxalate from CO prepared by an ultrasonic impregnation method in view of the various problems existing in the current catalyst. The catalyst prepared by this method significantly changes the dispersion of the noble metal active component, and the catalyst activity is remarkable. improve

Method used

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  • Catalyst for synthesizing dimethyl oxalate from CO and ultrasonic dispersion preparation method of catalyst
  • Catalyst for synthesizing dimethyl oxalate from CO and ultrasonic dispersion preparation method of catalyst
  • Catalyst for synthesizing dimethyl oxalate from CO and ultrasonic dispersion preparation method of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Preparation of catalyst

[0025] Dissolve 0.075g palladium chloride and 0.40g auxiliary ferric nitrate in 15ml hydrochloric acid buffer with pH=1.1 volume, and add 15g alumina balls (diameter 2mm, obtained by rotating disc rolling ball method) that have been roasted at 1300℃ In the buffer solution, under the ultrasonic condition of 25Hz frequency, ultrasonic for 2min, place it at room temperature for 12h, then put it in a drying oven at 100℃ for 12h, then at 150℃ for 12h; use 5 times the volume at 60℃ Wash with deionized water 10 times with an interval of 2 to 3 hours. After the last time the soaked solution is poured out, put it in a 100 ℃ oven and continue to dry for 12 hours. The obtained palladium-loaded alumina ball is passed into CO:N 2 1:4 gas is reduced at 150~400℃ for 4h to obtain Pd-Fe / Al 2 O 3 Finished catalyst. The Pd content is 0.3% of the carrier mass, and the auxiliary iron content is 0.60% of the carrier mass.

[0026] (2) Application performance evaluat...

Embodiment 2

[0030] (1) Preparation of catalyst

[0031] Dissolve 0.075g palladium chloride and 0.20g auxiliary ferric nitrate in a 15ml hydrochloric acid buffer with pH=1.1 volume, add 15g of roasted alumina balls into the buffer, and sonicate under 25Hz ultrasonic conditions. After 3 minutes, place it at room temperature for 12 hours, then put it in a drying oven at 100°C for 12 hours and then at 150°C for 12 hours; wash 10 times with 5 times volume of deionized water at 60°C, with an interval of 2 to 3 hours After the immersed solution was poured out for the last time, put it in an oven at 100℃ and continue to dry for 12 hours, and pass the resulting palladium-loaded alumina ball into CO:N 2 1:4 gas is reduced at 150~400℃ for 4h to obtain Pd-Fe / Al 2 O 3 Finished catalyst. The Pd content is 0.3% of the carrier mass, and the auxiliary iron content is 0.30% of the carrier mass.

[0032] (2) Application performance evaluation

[0033] The same conditions as in Example 1 were used for evaluation,...

Embodiment 3

[0035] (1) Preparation of catalyst

[0036] Dissolve 0.075g palladium chloride and 0.27g auxiliary copper nitrate in 15ml hydrochloric acid buffer solution with pH=1.1 volume, add 15g alumina balls after roasting treatment into the buffer solution, under the ultrasonic condition of frequency 25Hz, ultrasonic After 2 minutes, place it at room temperature for 12 hours, then put it in a drying oven at 100°C for 12 hours, and then dry at 150°C for 12 hours; wash 10 times with 5 times volume of deionized water at 60°C, with an interval of 2 to 3 hours. After the immersed solution was poured out for the last time, put it in an oven at 100℃ and continue to dry for 12 hours, and pass the resulting palladium-loaded alumina ball into CO:N 2 1:4 gas is reduced at 150~400℃ for 4h to obtain Pd-Cu / Al 2 O 3 Finished catalyst. The Pd content is 0.3% of the carrier mass, and the auxiliary copper content is 0.60% of the carrier mass.

[0037] (2) Application performance evaluation

[0038] The same ...

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Abstract

The invention discloses a catalyst for synthesizing dimethyl oxalate from CO and an ultrasonic dispersion preparation method of the catalyst. A chemical general formula of the catalyst provided by the invention is Pd-M / Al2O3, wherein the mass percent of palladium serving as an active component is 0.1 to 1%, M is one of Fe, Cu or Zn, and the specific surface area of the catalyst is 1 to 10 m<2> / g; an adopted carrier is a-type spherical aluminum oxide with the particle diameter of 1 to 5 mm; the dispersion degree of the active component of the catalyst is 20 to 27%. The preparation method of the catalyst provided by the invention has the characteristic that the catalyst is prepared by soaking in an ultrasonic condition; according to the catalyst prepared by using the method, the dispersion degree of precious metal as the active component is obviously changed, and the precious metal in the catalyst is low in using amount; in the process of synthesizing dimethyl oxalate, at low bed temperature, the stability of the active component of the catalyst is guaranteed, in addition, the high catalytic activity and the space-time yield of dimethyl oxalate are guaranteed, and the utilization ratio of the precious metal is increased.

Description

Technical field [0001] The present invention relates to a catalyst for the oxidative coupling of carbon monoxide to synthesize dimethyl oxalate and a preparation method thereof, which mainly include Pd-M / Al prepared by the ultrasonic impregnation-precipitation method 2 O 3 Related technologies of supported catalysts, where M is an auxiliary agent. technical background [0002] Dimethyl oxalate is an important chemical raw material. Because of its unique structure and wide range of uses, as well as various organic synthesis intermediates, it has received extensive attention and research. At present, the esterification reaction of oxalic acid and alcohol is still used in China, which has disadvantages such as high cost, serious pollution and low raw material utilization rate. Japanese Ube Industries patent JP8242.656 published a patent report on a supported palladium catalyst, using CO and methyl nitrite to synthesize dimethyl oxalate at atmospheric pressure. The process has the a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J37/34C07C69/36C07C67/36
Inventor 姚元根黄园园潘鹏斌张鑫覃业燕陈建姗
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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