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Ester hydrogenation catalyst and preparation method and application thereof

A technology for hydrogenation of catalysts and esters, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, and the preparation of hydroxyl compounds. Hydrogen-to-ester ratio, reduction of equipment investment and energy consumption

Pending Publication Date: 2020-05-26
PUJING CHEM IND SHA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] One of the technical problems to be solved by the present invention is the technical problems of high hydrogen-ester ratio, large equipment investment and high energy consumption in the prior art, providing a new Catalyst for the hydrogenation of oxalate to ethylene glycol: the ester hydrogenation catalyst, in terms of weight fraction, includes the following components: 5-50 parts of active components, 0-10 parts of amorphous alloy additives, and 50 parts of carrier ~95 servings

Method used

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  • Ester hydrogenation catalyst and preparation method and application thereof
  • Ester hydrogenation catalyst and preparation method and application thereof
  • Ester hydrogenation catalyst and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Take 500mL of a solution containing 0.20mol / L copper nitrate as solution I, add 14 grams of silicon dioxide to solution I under stirring to obtain slurry II, and then add 1.00mol / L sodium carbonate as a precipitating agent to slurry III In the process, the pH at the end point was controlled to be 7, aged at 60°C for 36 hours, and then the slurry was filtered and washed, and the obtained filter cake was dried at 150°C for 10 hours, roasted at 400°C for 5 hours, and 20 mL of 0.005 mol / L PdCl 2 And 0.010mol / L boric acid solution was added to the calcined catalyst and impregnated for 24 hours, then an excess of liquid phase reducing agent KBH was added 4 The solution reduces it, and the end point of the reduction reaction is pH 8. Washing, drying and pressing into tablets is the oxalate hydrogenation catalyst. Its composition is tested by ICP: 31.2 parts of copper, 0.1 part of Pd-B alloy and 68.7 parts of silicon dioxide.

Embodiment 2

[0036] Take 500mL of a solution containing 0.10mol / L copper nitrate as solution I, add 8.00g of silicon dioxide to solution I under stirring to obtain slurry II, and then add 0.50mol / L sodium carbonate as a precipitating agent to slurry III In the process, the pH at the end point is controlled to be 6, aged at 50°C for 48 hours, and then the slurry is filtered and washed, and the obtained filter cake is dried at 120°C for 24 hours, roasted at 500°C for 4 hours, and 50 mL of 0.01mol / L PdCl 2 And 0.03mol / L boric acid solution was added to the calcined catalyst and impregnated for 24 hours, then an excess of liquid phase reducing agent KBH was added 4 The solution reduces it, and the end point of the reduction reaction is pH 7. Washing, drying and pressing into tablets is the oxalate hydrogenation catalyst. Its composition is tested by ICP: 28.1 parts of copper, 1.0 parts of Pd-B alloy and 70.9 parts of silicon dioxide.

Embodiment 3

[0038] Use 1000mL of a solution containing 0.08mol / L copper nitrate as solution I, add 4.8 grams of silicon dioxide to solution I under stirring to obtain slurry II, and then add 0.50mol / L sodium carbonate as a precipitating agent to slurry III In the process, the pH at the end point is controlled to be 6, aged at 120°C for 1 hour, then the slurry is filtered and washed, the obtained filter cake is dried at 100°C for 36 hours, roasted at 600°C for 1 hour, and 30mL of 0.001mol / L PdCl 2 And 0.03mol / L zirconium nitrate solution is added to the calcined catalyst and impregnated for 24 hours, then add excess liquid phase reducing agent KBH 4 The solution reduces it, and the end point of the reduction reaction is pH 5. Washing, drying and pressing into tablets is the oxalate hydrogenation catalyst. Its composition is tested by ICP: 11.5 parts of copper, 2.0 parts of Pd-Zr alloy and 86.5 parts of silicon dioxide.

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Abstract

The invention relates to an ester hydrogenation catalyst and a preparation method and application thereof. The ester hydrogenation catalyst comprises the following components in parts by weight: 5-50parts of an active component, 0-10 parts of an amorphous alloy additive and 50-95 parts of a carrier. According to the method, a solution containing active component copper and auxiliaries is firstlyprecipitated and deposited on the carrier, then a precursor salt solution of amorphous alloy is used for impregnation, and a liquid-phase reduction is carried out, so that the hydrogen adsorption capacity of the catalyst is effectively improved. The problem of high hydrogen-ester ratio is better solved. The method can be used for industrial production of the catalyst for preparing ethylene glycolthrough oxalate hydrogenation. Compared with the prior art, the method has the advantages of low hydrogen-ester ratio, low equipment investment, low energy consumption and the like.

Description

technical field [0001] The invention relates to a catalyst for ester hydrogenation to synthesize alcohol, and also relates to the preparation method and application of the catalyst. Background technique [0002] Ethylene glycol is an important chemical product and basic organic raw material, mainly used in the production of chemical products such as polyester, antifreeze, lubricant and plasticizer, 90% of ethylene glycol is used for terephthalic acid and long-range polyester resin . my country is the world's largest polyester resin producer and ethylene glycol consumer. By the end of 2015, my country's total ethylene glycol production capacity was about 8.5Mt, accounting for about 27% of the global production capacity. At present, the global ethylene glycol production capacity exceeds 30Mt / a, and there is already a risk of excess. However, my country's import dependence is about 70%. Although the growth rate of imports has slowed down in recent years, the quantity is still ...

Claims

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Application Information

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IPC IPC(8): B01J23/72B01J23/75B01J23/755B01J23/80B01J23/89B01J29/03B01J29/89C07C29/149C07C31/20
CPCB01J23/8926B01J23/755B01J23/80B01J23/72B01J23/75B01J29/89B01J29/0333C07C29/149C07C31/202Y02P20/52
Inventor 郑赛男骆念军陈长军计扬吴军闫理宾
Owner PUJING CHEM IND SHA
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