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Preparation method for catalyst for synthesizing oxalic ester by gas-phase

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 price, high catalyst cost, and influence on use, and achieve low cost Effect

Active Publication Date: 2009-09-30
HAISO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 1. The space-time yield of the catalyst is not high, such as Pd-Ti / Al reported in US4507494 2 o 3 When the catalyst is used to synthesize dimethyl oxalate from CO and methyl nitrite, the space-time yield is 429-462g / L.h
[0007] 2. The use temperature of the catalyst is high
Pd is a noble metal, which is expensive, and the high loading makes the catalyst cost high, which affects its use in industry

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Dissolve 10 grams of ferric nitrate and 5 grams of manganese nitrate in 35 g of water, then pour it into a beaker with 100 grams of spherical α-alumina carrier with a diameter of 4 mm, dry it after impregnation, and roast it at 450 ° C for 2 hours, then roast The final carrier was put into 35 g of solution made with 0.5 gram of palladium chloride to impregnate and adsorb palladium to obtain the catalyst.

[0029] The catalyst uses H 2 The hydrogen-nitrogen mixture with a content of 90% was reduced at 250°C for 8 hours, then cooled to 105°C, and the H 2 After purging, the volume composition of the feed is 15% CH 3 ONO+30%CO+55%N 2 Air source, air speed 6000h -1 , to synthesize dimethyl oxalate, the space-time yield of the catalyst is 1050g / L.h, and the selectivity of dimethyl oxalate is 99.75%.

Embodiment 2

[0031] 15 grams of ammonium molybdate and 10 grams of ammonium paratungstate were dissolved in 40 grams of ammonia water with a mass concentration of 17%, and then poured into a beaker with 100 grams of 3mm in diameter and 8mm in length strip-shaped α-alumina carrier, dried after immersion, and Calcined at 550° C. for 2 hours, then put the calcined carrier into 36 g solution prepared with 0.9 g palladium acetate to impregnate and adsorb palladium to obtain the catalyst.

[0032] The catalyst uses H 2 The hydrogen-nitrogen mixed gas with a content of 50% was reduced at 350°C for 8 hours, and then the temperature was lowered to 120°C, and the H 2 After purging, the volume composition of the feed is 10% CH 3 ONO+20%CO+70%N 2 Air source, air speed 4000h -1 , to synthesize dimethyl oxalate, the space-time yield of the catalyst is 780g / L.h, and the selectivity of dimethyl oxalate is 99.85%.

Embodiment 3

[0034] Dissolve 25 grams of ferric nitrate and 12 grams of nickel nitrate in 45 grams of water, then pour it into a beaker with 100 grams of clover-shaped α-alumina carrier, dry it after impregnation, and roast it at 750 ° C for 2 hours, then put the roasted The carrier was put into 0.15 g of palladium chloride and mixed with 35 g of solution to impregnate and adsorb palladium to obtain an oxygen catalyst.

[0035] The catalyst uses H 2 The hydrogen-nitrogen mixed gas with a content of 10% was reduced at 450°C for 8 hours, and then cooled to 100°C, and the H 2 After purging, the volume composition of the feed is 15% CH 3 ONO+30%CO+55%N 2 Air source, air speed 4500h -1 , to synthesize dimethyl oxalate, the space-time yield of the catalyst is 1050g / L.h, and the selectivity of dimethyl oxalate is 99.85%. Example 4

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Abstract

The invention discloses a preparation method for a catalyst for synthesizing oxalic ester by gas-phase. The catalyst takes alpha-alumina as a carrier, palladium as an active component and 2 MOxes as an additive, M is magnesium, titanium, zirconium, vanadium, manganese, iron, nickel, copper, zinc, molybdenum or tungsten, and components of the catalyst (calculated by carrier mass) are: 0.01 to 0.75 percent of the palladium and 0.1 to 20 percent of MOxes. The preparation method comprises the following steps that: firstly, an additive metal salt solution is used to impregnate the carrier, and a palladium salt solution is used to impregnate the carrier to obtain the catalyst after the carrier is dried and roasted. Before the use, pure hydrogen or H2-N2 mixed gas is activated by the catalyst at a temperature of between 150 and 450 DEG C. The catalyst can be used for synthesizing oxalic ester by the carbonylation of CO and nitrous acid ester, the using reaction temperature of the catalyst is between 70 and 150 DEG C, and the reaction space velocity is between 500 and 9,000h<-1>. The catalyst has higher reaction activity and selectivity; and the catalyst has low cost.

Description

technical field [0001] The invention relates to a preparation method of a gas phase synthesis oxalate ester catalyst. Specifically, it is a preparation method suitable for the carbonylation of CO and nitrite to synthesize oxalate. technical background [0002] Oxalate is an important organic chemical raw material, which can be used to prepare intermediates of oxalic acid, oxalyl chloride, oxamide, ethylene glycol, certain drugs, dyes and solvents. In the mid-1960s, Fenton of the Union Oil Company in the United States discovered that under the catalysis of platinum group metals, CO and methanol can directly synthesize oxalate in an oxidizing atmosphere, opening up the C 1 An important way to chemically synthesize oxalate. Since the 1980s, C 1 New progress in chemical synthesis of oxalate esters. JP8242.656 open patent bulletin has reported a kind of adopting platinum group metal supported catalyst, utilizes CO and methyl nitrite to synthesize the technological process of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J23/652B01J23/44B01J23/60B01J37/02C07C69/36C07C67/36
Inventor 孔渝华胡典明钱胜涛刘华伟肖二飞刘应杰雷军李仕禄王先厚
Owner HAISO TECH
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