Preparation method for synthesizing copper-based catalyst by sol-gel ammonia still process

A copper-based catalyst, sol-gel technology, applied in the field of catalysis, to achieve the effects of industrial scale-up, high catalytic activity, and easy operation

Inactive Publication Date: 2012-10-10
河南能源化工集团研究总院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using orthosilicate as a silicon source, under the condition of ethanol as a co-solvent, a copper-based catalyst wa

Method used

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  • Preparation method for synthesizing copper-based catalyst by sol-gel ammonia still process

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Catalyst preparation: 12.3g Cu (NO 3 ) 2 ·3H 2 O was dissolved in 25.0g distilled water, fully dissolved and then added to the mixed solution formed by 42.0g ethanol and 46.5g tetraethyl orthosilicate, mechanically stirred the above mixed solution and placed in a water bath at 40°C for 2 hours to form a sol-gel. After aging at room temperature for 36 hours, the gel was cut into thin slices, soaked in ammonia water with pH = 13 for 12 hours, then placed in a 90°C water bath to evaporate the liquid, and then transferred to an oven to dry at 120°C for 24 hours. The obtained solid particles were calcined and dried for 5 hours at ℃. After calcined, the solid particles were pressed into tablets, crushed and sieved, and 40-80 mesh particles were sieved.

[0029] (2) Performance evaluation: Weigh a certain amount of 40-80 mesh catalyst precursor particles and reduce them in a hydrogen atmosphere at 150°C for 24 hours, with a hydrogen air velocity of 5000 hours -1 , the r...

Embodiment 2

[0031] (1) Catalyst preparation: 16.4g Cu (NO 3 ) 2 ·3H 2 O hydrated copper nitrate was dissolved in 50.0g of distilled water, fully dissolved and then added to the mixed solution formed by 42.0g of ethanol and 46.5g of ethyl orthosilicate, mechanically stirred the above mixed solution and placed in a water bath at 80°C for 0.5h to form a sol Gel, after aging the gel at room temperature for 48 hours, cut it into thin slices, add ammonia water with pH=11 to soak, then put it in a water bath at 80 ℃ to evaporate the liquid, then transfer it to an oven and dry it at 100 ℃ for 24 hours, and then dry it in a muffle The obtained solid particles were calcined and dried at 450°C in a furnace for 3 hours. After calcined, the solid particles were pressed into tablets, crushed and sieved, and 40-80 mesh particles were sieved.

[0032] (2) Performance evaluation: Weigh a certain amount of 40-80 mesh catalyst precursor particles and reduce them in a hydrogen atmosphere at 200°C for 12 ho...

Embodiment 3

[0034] (1) Catalyst preparation: 21.1g Cu (NO 3 ) 2 ·3H 2O hydrated copper nitrate was dissolved in 100.0g of distilled water, fully dissolved and then added to the mixed solution formed by 75.0g of ethanol and 46.5g of ethyl orthosilicate, mechanically stirred the above mixed solution and placed in a water bath at 40°C for 1 hour to form a sol gel After aging the gel at room temperature for 48 hours, cut the gel into thin slices, add ammonia water with pH=13 to soak, then put it in a water bath at 80 ℃ to evaporate the liquid, and then transfer it to an oven to dry at 120 ℃ for 24 hours. The obtained solid particles were calcined and dried at 350° C. for 5 hours. After calcined, the solid particles were compressed into tablets, crushed and sieved, and 40-80 mesh particles were sieved.

[0035] (2) Performance evaluation: Weigh a certain amount of 40-80 mesh catalyst precursor particles and reduce them in a hydrogen atmosphere at 250°C for 8 hours with a hydrogen air velocit...

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PUM

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Abstract

The invention relates to a method for synthesizing a copper-based catalyst by a sol-gel ammonia still process. Metallic copper is an active component of the catalyst, ortho-silicic acid ester serves as a silicon source, the copper-silicon catalyst prepared by the sol-gel process is treated after the ammonia still process by using alcohol as a cosolvent, and reactivity of dimethyl oxalate and selectivity of glycol are effectively improved. Compared with the sol-gel process, the method has the advantages that at a low reaction temperature (190-200 DEG C), the conversion rate of the dimethyl oxalate can be close to 100%, and the selectivity of the glycol is higher than 96%. The stability of the catalyst can be reduced by reducing the optimal active temperature of the catalyst, the preparation process of the catalyst is simple, and industrial amplification is facilitated.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and in particular relates to a preparation method for synthesizing a copper-based catalyst by adopting a sol-gel ammonia distillation method and its application in ester hydrogenation reaction. technical background [0002] Ethylene glycol, also known as glycol, is an important chemical raw material, mainly used in the production of polyester fibers, antifreeze, unsaturated polyester resins, lubricants and other products. With the rapid development of my country's polyester industry, the demand for ethylene glycol continues to grow. The overall supply of ethylene glycol in my country is in short supply, and a large amount of imports are needed to meet downstream demand. The glycol approach has been severely tested due to resource constraints. my country is rich in coal resources, which account for more than 90% of fossil resource reserves. From the perspective of my country's declining oil reso...

Claims

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Application Information

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IPC IPC(8): B01J23/72C07C31/20C07C29/149
CPCY02P20/52
Inventor 穆仕芳蒋元力尚如静魏灵朝王占修张秀全闫捷李丰
Owner 河南能源化工集团研究总院有限公司
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