Catalyst for preparing alcohol from acetate through hydrogenation as well as preparation method and application thereof

A technology for hydrogenating acetate and producing ethanol, which is used in metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, preparation of hydroxyl compounds, etc., and achieves good industrial application prospects, good selectivity, and high activity. Effect

Inactive Publication Date: 2013-03-13
JIANGSU SOPO GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ethanol can be obtained by hydrogenation of acetic acid under the action of noble metal catalysts such as Pt and Pd, but the cost of the catalyst is high and there is acetic acid corrosion

Method used

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  • Catalyst for preparing alcohol from acetate through hydrogenation as well as preparation method and application thereof
  • Catalyst for preparing alcohol from acetate through hydrogenation as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The composition of catalyst A is: 40CuO-7ZnO / SiO 2

[0024] The preparation steps are as follows: weigh 26.1g Cu(NO 3 ) 2 .3H 2 O, 5.2g Zn(NO 3 ) 2 .6H 2 O, 38.1g TEOS and 36.3g ethanol, 40.1g water in a 500ml beaker, stirred at room temperature for 6h, gelled in air for 24h, slowly heated to 80~120 o C evaporates the solvent, then slowly raises the temperature to 500 o C is calcined for 1 hour to obtain catalyst A.

[0025] The hydrogenation reaction of methyl acetate was carried out in a fixed-bed stainless steel reactor (id=10mm), and the catalyst dosage was 5.0ml. Catalyst before reaction at 310 o C uses 5NL / h of pure H 2 Reduction 48h. Then reduce the reactor to 250 o C, boost the pressure to 8.0Mpa, then inject the acetate into the reactor with a micro metering pump, adjust LHSV=2.0 h -1 , while adjusting H 2 flow such that H 2 / Ester = 50(mol). After reacting for about 80 hours, take samples for analysis, and at the same time analyze the compositi...

Embodiment 2

[0029] The composition of catalyst B is: 34CuO-7ZnO / SiO 2

[0030] Its preparation steps are as follows: weigh 24.1g Cu(NO 3 ) 2 .3H 2 O, 5.0g Zn(NO 3 ) 2 .6H 2 O, 49.5 g TEOS, 44.6 g ethanol, and 47.5 g water were mixed in a 500ml beaker, stirred at room temperature for 2 hours, poured into a plastic bottle and sealed, left to stand at room temperature for about 4 days to form a gel, cut into thin slices and used pH=11 soaked in ammonia water, and then at 75 o Evaporate to dryness on a C water bath, then slowly raise the temperature to 100 o C to dry for 24h, take it out and wash with water until the filtrate is colorless, then slowly rise to 120 o C dry for 12h, then slowly rise to 300 oC is calcined for 1 hour to obtain catalyst B.

[0031] Catalyst evaluation is the same as embodiment 1, and reduction temperature is 400 o C, reduction time 2h, reduction atmosphere 10%H 2 -N 2 ; The reaction condition is 230 o C, 2.0MPa, LHSV=0.5h -1 , H 2 / ester=10 (mol), ...

Embodiment 3

[0033] The composition of catalyst C is: 34CuO-6ZnO / SiO 2

[0034] The preparation steps are basically the same as catalyst B, except that 3.6g of pore-forming agent PEG400 is added before the sealing gel step to obtain catalyst C. The details are as follows: Weigh 24.1 g Cu(NO 3 ) 2 .3H 2 O, 5.0g Zn(NO 3 ) 2 .6H 2 O, 49.9 g TEOS and 44.8 g ethanol, 47.9 g water, and 3.6 g PEG400 were mixed in a beaker, stirred at room temperature for 2 h, poured into a plastic bottle and sealed, and formed a gel after about 4 days, cut into thin slices and measured with pH = Soak in ammonia water at about 11, and then at 75 o Evaporate to dryness on a C water bath, then slowly raise the temperature to 100 o C to dry for 24h, take it out and wash with water until the filtrate is colorless, then slowly rise to 120 o C dried for 12h, then slowly increased to 500 o C is calcined for 1 hour to obtain catalyst C. Catalyst evaluation is the same as embodiment 1, and reduction temperat...

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Abstract

The invention discloses a catalyst for preparing alcohol from acetate through hydrogenation as well as a preparation method and an application thereof. The active component of the catalyst is Cu element; the assistant is selected from one or the mixture of several of Zn, Co, Ni and Fe; the carrier is silicon oxide, aluminum oxide or SiO2-TiO2 composite oxide; and the content of Cu element is 5-50wt% based on CuO, and the content of the assistant is 1-25wt%. The preparation method comprises the following steps of: weighing the precursor of each component and adding water to prepare a solution, and stirring for 1-10 hours at a temperature from the room temperature to 60 DEG C; hermetically standing at the room temperature or standing in the air at a temperature from the room temperature to 100 DEG C to form gel; and drying the gel and then roasting the gel for 1-10 hours at a temperature of 200-700 DEG C to obtain the catalyst. The prepared catalyst has the advantages of excellent performance, high activity, good selectivity and no reduction of the performance after the catalyst is used for 1200 hours and has very good industrial application prospects.

Description

technical field [0001] The invention relates to a catalyst for preparing ethanol by hydrogenation of acetate and its preparation method and application thereof, in particular to a sol-gel method for preparing a Cu-based catalyst supported by an inorganic oxide carrier, which has high activity, ethanol selectivity and stability sex. technical background [0002] Ethanol is an important bulk chemical. With the depletion of petroleum resources and the increasingly tight food supply, ethanol production from coal, natural gas or biomass through synthesis gas has become a focus of attention. In the 1970s, the homogeneous carbonylation of non-petroleum-based methanol developed by Monsanto gradually became the most important method for the production of acetic acid. In the late 1990s, British company BP successfully commercialized the Cativa catalytic method, which is greener and more efficient than the Monsanto method. Ethanol can be obtained by hydrogenation of acetic acid unde...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/80B01J23/75B01J23/755B01J23/745C07C31/08C07C29/149
Inventor 宋勤华邵守言凌晨朱桂生朱怀松丁云杰陈维苗吕元王涛
Owner JIANGSU SOPO GRP
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