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Sediment and deposition preparing method of Pd/Mg(OH)2 catalyst and application of Pd/Mg (OH)2 catalyst

A technology for catalysts and preparation steps, which is applied in the field of preparation of catalysts for the synthesis of dimethyl oxalate by CO gas-phase catalytic coupling, which can solve the problems that are not conducive to the efficient utilization of noble metal Pd, increase catalyst production costs, and high loading capacity, and achieve low pollution , Ease of operation, and improved dispersion

Inactive Publication Date: 2017-08-11
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

Patent CN101791555A discloses a catalyst for the coupling reaction of CO and methyl nitrite to generate dimethyl oxalate. The catalyst uses Pd as an active component, and La and Re as auxiliary agents. Although the catalyst has a selectivity of dimethyl oxalate as high as 99 %, but the loading of noble metal Pd is as high as 1%, and the price of additives La and Re is also relatively expensive, which undoubtedly increases the production cost of the catalyst
Patent CN104190414B reports a method of preparing Pd / α-Al by sodium borohydride reduction 2 o 3 The preparation method of the catalyst, the dispersion degree of the catalyst active component Pd provided by the inventive method is lower than 30%, which is not conducive to the efficient utilization of the precious metal Pd

Method used

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  • Sediment and deposition preparing method of Pd/Mg(OH)2 catalyst and application of Pd/Mg (OH)2 catalyst
  • Sediment and deposition preparing method of Pd/Mg(OH)2 catalyst and application of Pd/Mg (OH)2 catalyst
  • Sediment and deposition preparing method of Pd/Mg(OH)2 catalyst and application of Pd/Mg (OH)2 catalyst

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Experimental program
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Effect test

Embodiment 1

[0021] Take 20mL of the pre-prepared mixed solution of magnesium nitrate and sodium chloropalladate and place it in a 70°C water bath, in which the concentration of magnesium nitrate is 1mol / L, and the concentration of sodium chloropalladate is 0.5mmol / L. Use a dropping funnel to add 1mol / L sodium hydroxide solution to it at a rate of 15 drops / min. When the pH value of the solution at the end of the precipitation reaction is 8.5, stop adding lye and keep it in a 70°C water bath. Stand and age for 12 hours, filter with suction, and wash with deionized water until the filtrate is neutral, dry the obtained solid powder in an oven at 150°C for 12 hours, and then reduce it with pure hydrogen at 150°C for 2 hours to obtain the desired catalyst sample. Using ICP analysis, the mass fraction of noble metal Pd in ​​the carrier is 0.091%. The dispersion of Pd was tested by CO static chemisorption, and the results are shown in Table 1.

Embodiment 2

[0023] Take 20mL of the pre-prepared 2mol / L magnesium acetate and 3.5mmol / L tetraammine palladium nitrate mixed solution and place it in a water bath at 80°C, and then use a dropping funnel to drip at a rate of 20 drops / min under constant stirring. Add 2mol / L sodium hydroxide solution, when the pH value of the solution at the end of the precipitation reaction is 9, stop adding lye, keep it in a water bath at 80°C for 8 hours, and then suction filter the obtained precipitate , and washed with deionized water until the filtrate is neutral, and finally the obtained solid powder was dried in an oven at 120°C for 18 hours, and after drying, it was reduced with pure hydrogen at 150°C for 4 hours to obtain the desired catalyst sample. Using ICP analysis, the mass fraction of noble metal Pd in ​​the carrier is 0.32%. The results of the dispersion test of Pd are shown in Table 1.

Embodiment 3

[0025] Take 20mL of a pre-prepared mixed solution of 3mol / L magnesium chloride and 8mmol / L palladium chloride and place it in a 60°C water bath, then add 2.5mol / L of potassium hydroxide solution, when the pH value of the solution at the end of the precipitation reaction is 10.5, stop adding the lye, keep it in a water bath at 60°C for 20 hours, and then filter the precipitate with suction and use it to remove Wash with ionic water until the filtrate is neutral, and finally place the obtained solid powder in an oven at 150°C for 20 hours, and then reduce it with pure hydrogen at 150°C for 4 hours to obtain the desired catalyst sample. Using ICP analysis, the mass fraction of noble metal Pd in ​​the carrier is 0.47%. The results of the dispersion test of Pd are shown in Table 1.

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Abstract

The invention discloses a preparing method of a Pd / Mg(OH)2 catalyst and application of the Pd / Mg(OH)2 catalyst in a reaction of using CO gas phase catalysis coupling to synthesize dimethyl oxalate. According to the preparing method of the Pd / Mg(OH)2 catalyst and application of the Pd / Mg(OH)2 catalyst in the reaction of using gas phase catalysis coupling to synthesize dimethyl oxalate, a sediment and deposition method is utilized to uniformly fix precious metal Pd onto a carrier Mg(OH)2, thus the dispersity of the precious metal Pd on the carrier is obviously improved, the efficient utilization of the precious metal Pd is achieved, the aggregation and growth of precious metal Pd particles in a reaction process are inhibited, and the problem in the prior art that the dispersity of the precious metal Pd is low and the stability is low is effectively solved. In the obtained Pd / Mg (OH)2 catalyst, Mg(OH)2 is adopted as the carrier, and the precious metal Pd nanometer particles are adopted as an active component, wherein the load capacity of Pd accounts for, by mass, 0.01-1% of the carrier. The Pd / Mg(OH)2 catalyst is mainly used in industrial production of using CO catalysis coupling to synthesize a dimethyl oxalate catalyst.

Description

technical field [0001] The invention belongs to the technical field of preparation of dimethyl oxalate, and in particular relates to a preparation method and application of a catalyst for CO gas-phase catalytic coupling to synthesize dimethyl oxalate. Background technique [0002] Dimethyl oxalate is an important chemical raw material and reaction intermediate, widely used in the fields of pharmacy and organic chemical industry, the most important of which is that dimethyl oxalate can be used as an intermediate to prepare bulk chemical raw material B by low-pressure catalytic hydrogenation Diol, the successful development of this process can effectively alleviate the shortage of oil resources in my country. At present, the traditional production method of dimethyl oxalate is to use oxalic acid and methanol to produce through esterification reaction. Due to the shortcomings of long production cycle, large raw material consumption and serious environmental pollution, this proce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J37/03B01J37/18C07C67/36C07C69/36
CPCB01J23/58B01J37/035B01J37/18C07C67/36C07C69/36
Inventor 姚元根张鑫潘鹏斌黄园园王彦端覃业燕
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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