Preparation method of catalyst used for synthesizing ethyl alcohol through hydrogenation on dimethyl oxalate, catalyst obtained by adopting preparation method and application thereof

A dimethyl oxalate and catalyst technology, applied in the field of catalyst preparation, can solve the problems of restricting large-scale application, easy sintering, and accelerated catalyst deactivation

Active Publication Date: 2018-07-03
HIGHCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For exothermic catalytic reactions, as the reaction process proceeds, the continuously released heat of reaction will inevitably accelerate the deactivation of the catalyst and affect the stability of the catalyst.
Copper-based catalysts, due to the low melting point of copper, the main active component, are easy to sinter in the hydrogenation of dimethyl oxalate to ethanol, which limits the large-scale application of this route

Method used

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  • Preparation method of catalyst used for synthesizing ethyl alcohol through hydrogenation on dimethyl oxalate, catalyst obtained by adopting preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] Catalyst preparation

[0072] Weigh 1.37g of copper nitrate trihydrate and dissolve in 50ml of deionized water to form solution I, weigh 0.28g of boric acid and dissolve in 50ml of deionized water to obtain solution II, and mix solutions I and II to obtain solution III. 2.4 g of urea was added to solution III, and after mixing and stirring for 30 min, 2 g of carbon nanotube carrier was added into the obtained solution, and stirring was continued for 60 min. Then the obtained mixture was put into a hydrothermal synthesis tank, and hydrothermally synthesized at 100° C. for 24 h at a rotational speed of 2 r / min. The obtained hydrothermal synthesis product was filtered, washed with deionized water, placed in a closed autoclave, and continuously fed with supercritical CO 2 , Dry at 40°C and 10MPa for 20h. Then it was calcined at 500° C. for 3 h in a nitrogen atmosphere in a tube furnace to obtain catalyst A, which contained 15% Cu and 2% B in terms of elements.

[0073] C...

Embodiment 2

[0076] Weigh 0.80g of ferric nitrate nonahydrate and dissolve in 50ml of deionized water to form solution I, weigh 0.17g of silver nitrate and dissolve in 50ml of deionized water to obtain solution II, and mix solutions I and II to obtain solution III. Add 6.3g of urea to the solution III, mix and stir for 30min, then add 5g of 40wt% silica sol dropwise, and continue stirring for 120min. Then the obtained mixture was put into a hydrothermal synthesis tank, and hydrothermally synthesized at 120° C. for 10 h at a rotation speed of 2 r / min. The obtained hydrothermal synthesis product was filtered, washed with deionization, placed in a closed autoclave, and continuously fed with supercritical CO 2 , Dry at 40°C and 10MPa for 24h. Then it was calcined at 350° C. for 3 h in an air atmosphere in a tube furnace to obtain catalyst B, which contained 5% Fe and 5% Ag in terms of elements.

[0077] The catalyst reduction and hydrogenation reaction steps in Example 1 were repeated, excep...

Embodiment 3

[0079] Weigh 0.58g of silver nitrate and dissolve it in 50ml of deionized water to form solution I, weigh 0.23g of lanthanum nitrate hexahydrate and dissolve it in 50ml of deionized water to obtain solution II, and mix solutions I and II to obtain solution III. Add 1.6 g of urea to solution III, mix and stir for 30 min, then add 2 g of graphene carrier into the obtained solution, and continue stirring for 60 min. Then the obtained mixture was put into a hydrothermal synthesis tank, and hydrothermally synthesized at 180° C. for 24 hours at a rotational speed of 2 r / min. The obtained hydrothermal synthesis product was filtered, washed with deionized water, placed in a closed autoclave, and continuously fed with supercritical CO 2 , Dry at 40°C and 10MPa for 48h. Then it was calcined at 500° C. for 3 h in a nitrogen atmosphere in a tube furnace to obtain catalyst C, which contained 15% Ag and 3% La in terms of elements.

[0080] The catalyst reduction and hydrogenation reaction...

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Abstract

The invention relates to a method for preparing a catalyst used for synthesizing ethyl alcohol through hydrogenation on dimethyl oxalate. The catalyst contains a carrier, a catalytic active componentloaded on the carrier, and an optional catalytic promoter, concretely the catalyst contains: (A) based on element, 1-50wt% of elements which are selected from Cu, Fe, Ni, Co, Ag and Au and taken as the catalytic active component; (B) based on element, 0-10wt% of elements which are selected from third main group elements, transition elements and lanthanide elements and taken as the catalytic promoter; and (C) the carrier. The catalyst is prepared by adopting a urea-assisted hydrothermal synthesis method, and CO2 supercritical drying is adopted, so that high ethyl alcohol selectivity can be obtained, and high dimethyl oxalate conversion rate also can be obtained when the prepared catalyst is used for producing ethyl alcohol through hydrogenation on dimethyl oxalate. The invention also relates to the catalyst prepared by adopting the method provided by the invention and application of the catalyst in production of ethyl alcohol through hydrogenation on dimethyl oxalate.

Description

technical field [0001] The invention relates to a preparation method of a catalyst used for hydrogenation of dimethyl oxalate to synthesize ethanol, and also relates to the catalyst obtained by the method and the application of the catalyst. Background technique [0002] Ethanol, commonly known as alcohol, is an important chemical raw material. It can not only be used as a raw material for the synthesis of a series of small molecule chemical products and polymers, but also a potential liquid fuel resource, which has attracted extensive attention from all over the world. At present, ethanol production is mainly through the following two ways: (1) grain fermentation; (2) ethylene hydration obtained from petroleum cracking. The ethylene hydration method not only relies heavily on the increasingly depleted petroleum resources, but also requires high equipment materials, which is not suitable for large-scale ethanol production. Although most of the ethanol currently on the mark...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72B01J23/89B01J23/66B01J23/75B01J29/46B01J23/745B01J29/03C07C29/149C07C31/08
CPCB01J23/66B01J23/72B01J23/745B01J23/75B01J23/8906B01J23/8926B01J29/03B01J29/46C07C29/149C07C31/08B01J23/755B01J23/83B01J23/89B01J37/03C07C31/20
Inventor 柴剑宇椿范立杨国辉李永烨
Owner HIGHCHEM
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