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Oxalate hydrogenated Au-Ag bimetallic catalyst and preparation method thereof

A metal catalyst and oxalate technology, which is applied in the preparation of carboxylate, metal/metal oxide/metal hydroxide catalyst, molecular sieve catalyst, etc., can solve the problem of high cost of chromium treatment, increased production links and unsafe products and other problems, to achieve the effect of easy scale-up production, stable performance and simple preparation process

Inactive Publication Date: 2012-08-22
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The earliest relevant U.S. patent U.S.4,112,245, the active components of the catalyst mainly include copper and chromium, and the carrier is alumina and silicon oxide, etc.; the outstanding characteristics of the copper / chromium catalyst are good stability and activity, and the optimal catalytic activity stability period Not less than 1134h (Industrial Catalysis, 1996, April, 24-29), but chromium (especially high-valence chromium) has greater biological toxicity, and the use of chromium-containing catalysts increases the safety of production links and products, and catalyst failure The processing cost of chromium in chromium is high, so the development and use of chromium-free and environmentally friendly catalysts are very active

Method used

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  • Oxalate hydrogenated Au-Ag bimetallic catalyst and preparation method thereof
  • Oxalate hydrogenated Au-Ag bimetallic catalyst and preparation method thereof
  • Oxalate hydrogenated Au-Ag bimetallic catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) The surface area prepared in the laboratory is 833m 2 / g of SBA-15 carrier 3.0g.

[0029] 2) Dissolve 0.5 g of PVA completely in 30 mL of tetrahydrofuran, pour the above-mentioned carrier into the solution, let it stand for 4 hours, filter, wash and dry to obtain the P-SBA-15 product, which is ready for use.

[0030] 3) Add 0.3g of ethylenediamine (ED) and 30ml of deionized water to the above P-SBA-15 product, heat at 90°C for 12h, cool to room temperature, rinse with deionized water, and dry under vacuum at 60°C to obtain functional group ED-P-SBA-15 solid powder A, spare.

[0031] 4) At room temperature, use a pipette to pipette 18.5mL of chloroauric acid solution with a concentration of 0.01g / mL, add 50ml of deionized water to dilute to obtain an orange-yellow solution, and add 1.0g of functionalized ED-P-SBA under stirring -15 solid powder A, after stirring for 10 minutes, add 20 mL of 0.005 g / mL sodium borohydride aqueous solution dropwise while stirring, afte...

Embodiment 2

[0039] The preparation method of the catalyst is the same as in Example 1, changing the 0.01g / mL silver nitrate solution to 0.85mL, and keeping the other compositions unchanged, to prepare the 8%Au-0.5%Ag / ED-P-SBA-15 catalyst.

[0040] ICP-MS quantitative analysis results show that the content of Au and Ag is within the error range of the theoretical loading; after nitrogen adsorption test, the specific surface area is 564m 2 / g, the pore volume is 0.80ml / g, and the average pore diameter is 5.3nm. The performance evaluation and analysis conditions of the catalyst for the hydrogenation of dimethyl oxalate are the same as in Example 1, and the results are shown in Table 1.

Embodiment 3

[0042] The preparation method of the catalyst was the same as in Example 1, changing the 0.01g / mL silver nitrate solution to 2.55mL, and keeping the other compositions unchanged, to prepare the 8%Au-1.5%Ag / ED-P-SBA-15 catalyst.

[0043] ICP-MS quantitative analysis results show that the content of Au and Ag is within the error range of the theoretical load; after nitrogen adsorption test, the specific surface area is 555m 2 / g, the pore volume is 0.76ml / g, and the average pore diameter is 5.4nm. The performance evaluation and analysis conditions of the catalyst for the hydrogenation of dimethyl oxalate are the same as in Example 1, and the results are shown in Table 1.

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Abstract

Disclosed are an oxalate hydrogenation Au-Ag bimetallic catalyst and a preparation method thereof, which relate to catalysts. The oxalate hydrogenated Au-Ag bimetallic catalyst comprises, by mass percentage, 2-12% of Au, 0.5-5% of Ag and the balance being carriers. The formula of the catalyst is x%Au-y%Ag / carriers, wherein the x% is the mass percentage of Au of the catalyst, and the y% is the massage percentage of Ag of the catalyst. The preparation method includes: modifying the carriers with high polymer, preparing a precursor of the catalyst by adding components of Au and Ag, reducing the precursor of the catalyst at an hydrogen-containing atmosphere, and finally obtaining the oxalate hydrogenated loaded Au-Ag bimetallic catalyst. With the preparation method, methyl glycollate or ethylene glycol can be prepared selectively by controlling reaction temperature. The catalyst prepared by the preparation method has the advantages of excellent low-temperature catalytic activity, fine catalytic stability, long service life and the like.

Description

technical field [0001] The invention relates to a catalyst, especially a catalyst for synthesizing methyl glycolate or ethylene glycol. Background technique [0002] Methyl glycolate (MG) is a multipurpose chemical raw material, synthetic intermediate and excellent solvent, and is widely used in the fields of chemical industry, medicine, pesticide, feed, spice and fuel. Its molecular structure contains functional groups such as α-hydrogen, hydroxyl and ester groups at the same time. It has the chemical properties of alcohol and ester. It is an excellent solvent for many cellulose, resin and rubber. It is easily soluble in nitrocellulose, cellulose acetate, In cellulose acetate propionate and polyvinyl acetate, reactions such as carbonylation, hydrolysis, alcoholysis and oxidation can occur. Methyl glycolate is an important intermediate in the synthesis of isoharringtonine and its analogues with anticancer activity, and is also a raw material for anti-carrier additives to im...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/52B01J29/035C07C69/675C07C67/31C07C31/20C07C29/149
CPCY02P20/52
Inventor 袁友珠郑建伟林海强王亚楠段新平
Owner XIAMEN UNIV
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