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Glycol catalyst prepared by dimethyl oxalate hydrogenation and preparation method thereof

A technology of dimethyl oxalate and catalyst, which is applied in the field of catalysis, can solve the problem of activity reduction and achieve the effect of avoiding structural damage

Active Publication Date: 2009-12-23
HAISO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] There are many literature reports on the activity improvement effect of additives on catalysts. Foreign Brands and others have studied CuSi catalysts used for ester hydrogenation. The role of additives has a large and small order of Mo>Co>Zn≥Mn>Fe>Y>Ni >Mg, all introduced during the co-precipitation process, but the esters they tested only chose methyl acetate
The applicant used the above method to introduce additives in the research on the hydrogenation of dimethyl oxalate. As a result, the activity was greatly reduced after adding the additives.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Step 1: 16gCu(NO 3 ) 2 ·3H 2 O and 50ml concentrated ammonia water are made into 500ml solution respectively;

[0031] Step 2: Add 50 g of silica sol with a concentration of 30% into a stirred container in parallel with the above-mentioned copper solution and precipitant solution;

[0032] Step 3: raise the temperature to 100°C to evaporate most of the water, and precipitate the precipitate, wash the precipitate with water three times, and finally dry it;

[0033] Step 4: The CuSi catalyst precursor prepared by the above co-precipitation is then impregnated with a solution prepared by 1 g of zinc nitrate;

[0034] Step 5: The catalyst precursor of the above-mentioned impregnation aid is calcined at 400°C for 8 hours, and finally tableted to form a catalyst, the composition of which is calculated as the mass percentage of oxygen compounds: 20% CuO, 3% ZnO, SiO 2 margin.

[0035] Before using the catalyst, 10% H should be used 2 -N 2Gas reduction, the reduction tem...

Embodiment 2

[0037] Step 1: 16.7gCu(Ac) 2 ·H 2 O and 60ml concentrated ammonia water are configured into 500ml solution respectively;

[0038] Step two, step three are the same as embodiment 1;

[0039] Step 4: impregnating the CuSi catalyst precursor prepared by the above co-precipitation with a solution prepared by 1 g of ferric nitrate;

[0040] Step 5: The catalyst precursor of the above-mentioned impregnation aid is calcined at 500°C for 8 hours, and finally tableted to form a catalyst, the composition of which is calculated as the mass percentage of oxygen compounds: 25% CuO, 2.5% Fe 2 o 3 , SiO 2 margin.

[0041] Before using the catalyst, 5% H should be used 2 -N 2 Gas reduction, the reduction temperature is 400°C. The activity of the catalyst was evaluated on a small particle size device, and the evaluation conditions were the same as in Example 1. The results are shown in Table 1.

Embodiment 3

[0043] Step 1: 24gCu(NO 3 ) 2 ·3H 2 O and 80ml concentrated ammonia water are configured into 500ml solution respectively;

[0044] Step two, step three are the same as embodiment 1;

[0045] Step 4: The CuSi catalyst precursor prepared by the above co-precipitation is then impregnated with a solution prepared by 0.2 g of silver nitrate;

[0046] Step 5: The catalyst precursor of the above-mentioned impregnation aid is calcined at 300°C for 8 hours, and finally tableted to form a catalyst, the composition of which is calculated as the mass percentage of oxygen compounds: 30% CuO, 0.7% AgO, SiO 2 margin.

[0047] The catalyst needs 20% H before use 2 -N 2 Gas reduction, the reduction temperature is 300°C. The activity of the catalyst was evaluated on a small particle size device, and the evaluation conditions were the same as in Example 1. The results are shown in Table 1.

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Abstract

The invention discloses a glycol catalyst prepared by dimethyl oxalate hydrogenation and a preparation method thereof, which is characterized in that the catalyst takes copper nitrate or copper acetate as copper source, ludox as silicon source, ammonia, ammonium bicarbonate or urea as precipitant which are coprecipitated to prepare CuSi catalyst forerunner; one or two of Zn, Fe, Ag, and Pd is soaked in the catalyst forerunner and used as additive agent, and then mixture is baked in the temperature of 200 to 500 DEG C, and finally is beaten into pieces and formed to obtain the catalyst. The catalyst comprises 20-50% of Cuo, 0.005%-3% of additive agent and the rest of SiO2 according to mass percent of oxygen compound, wherein additive agent is oxidate of one or two of Zn, Fe, Ag, and Pd. Before using, the catalyst is reduced by hydrogen and nitrogen combination gas containing 1% to 90% of hydrogen; and the reduction temperature is 150 to 500 DEG C.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and relates to a catalyst and a preparation method thereof, in particular to a dimethyl oxalate hydrogenation ethylene glycol catalyst and a preparation method thereof. technical background [0002] Ethylene glycol is an important chemical raw material, mainly used in the production of polyester fibers, antifreeze agents, unsaturated polyester resins, lubricants and other products, and its demand has continued to grow in recent years. [0003] At present, the industrial production of ethylene glycol mainly adopts the route of producing ethylene oxide through gas-phase oxidation of petroleum ethylene, and then through liquid-phase catalytic hydration to produce ethylene glycol. my country's oil resources are insufficient, and the production of ethylene by cracking consumes a lot of oil. Ethylene is also a raw material for many important products. From the perspective of my country's decreasing o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J23/80B01J23/745B01J37/03B01J37/02C07C31/20C07C29/149
Inventor 孔渝华刘华伟钱胜涛胡典明刘应杰肖二飞李仕禄王先厚徐俊鹏
Owner HAISO TECH
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