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Preparation method and application for low carbon olefin zirconium-based catalyst through synthesis gas

A technology of low-carbon olefins and catalysts, applied in the field of modified zirconia catalysts, can solve the problems of low yield of total olefins, poor product selectivity, and reduced utilization efficiency of synthesis gas, etc., and achieve high reaction activity, short cycle, and improved product distribution Effect

Inactive Publication Date: 2015-07-01
NINGXIA UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The above catalytic systems have made good progress in the direct production of low-carbon olefins from syngas. Although the traditional modified Fischer-Tropsch synthesis catalysts have high activity, they are limited by the distribution of products A-S-F, resulting in poor product selectivity and low yield of total olefins; In addition, large amounts of CO 2 The generation reduces the utilization efficiency of syngas

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Weigh ZrO(NO 3 ) 2 2H 2 O 20.0g, measure NH 4 40mL of OH (25wt%) solution was prepared into 100mL solutions respectively, and precipitated in parallel flow, and the flow rate was adjusted to control pH=11. The cake was dried at 120°C for 12h, calcined at 500°C for 2h, and ground to obtain a dry powder; weigh 5.0g of the dry powder, and weigh K 2 CO 3 0.10g, made into a solution, the 5.0g dry powder is impregnated in the prepared K 2 CO 3 In the solution, dry at 120°C for 8 hours, roast at 500°C for 1 hour, grind and granulate, and sieve to 20-40 mesh to obtain the Zr / K catalyst. Catalyst loading volume 2.0mL, reaction condition: H 2 / CO=2, 1.5MPa, 360°C, space velocity 1000h -1 . CO conversion 56.3%, C 2 =-C 4 = 48.7% by weight of total hydrocarbons, CO 2 The selectivity is 5.3%.

Embodiment 2

[0028] Weigh ZrO(NO 3 ) 2 2H 2 O 10.0g, measure NH 4 OH (25wt%) solution 40mL, respectively prepared into 100mL solution, co-current precipitation, by adjusting the flow rate to control pH = 12, dropwise, continue to stir for 0.5h, stand for aging for 12h, wash, suction filter, filter cake at 120 ℃, dried at 500℃ for 2.5h; ground the roasted powder evenly, impregnated equal volume in 5wt% Fe(NO 3 )·9H 2 O and 2wt%K 2 CO 3 The mixed solution was dried at 120°C, calcined at 500°C for 2 hours, and the calcined powder was ground and granulated to 20-40 mesh to obtain the Zr / Fe-K catalyst. Catalyst loading 2.0mL, reduction condition: H 2 / CO=1:1, 0.1MPa, 300℃ / 12h, space velocity 500h -1 ; Reaction conditions: H2 / CO=2, 2MPa, 400℃, space velocity 1000h -1 . CO conversion 65.1%, C 2 =-C 4 = 50.2% by weight of total hydrocarbons, CO 2 The selectivity is 9.5%.

Embodiment 3

[0030] Weigh ZrO(NO 3 ) 2 2H 2 O 5.0g, Fe(NO 3 ) 3 9H 2 O 7.55g; measure NH 4 10mL of OH (25wt%) solution was formulated into 100mL solutions respectively, co-precipitated by co-precipitation, and the flow rate was adjusted to control pH=11. ℃, dry at 500℃ for 2h; grind the powder evenly after calcination, impregnate 2wt% K in equal volume 2 CO 3 and 2%Mn(NO 3 ) 2 (50wt%) mixed solution, dried at 120°C, calcined at 500°C for 2h, and the calcined powder was ground and granulated to 20-40 mesh to obtain the Zr / Fe-Mn-K catalyst. Catalyst loading 2.0mL, reduction condition: H 2 / CO=1:1, 0.1MPa, 300℃ / 12h, space velocity 500h -1 . Reaction condition: H 2 / CO=2, 0.5MPa, 360℃, space velocity 500h -1 . CO conversion rate 78.3%, C 2 =-C 4 = 58.6% by weight of total hydrocarbons, CO 2 The selectivity was 13.5%.

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Abstract

The invention discloses a preparation method and application for low carbon olefin zirconium-based catalyst through synthesis gas. By employing a coprecipitation method and an impregnation method, the base catalyst takes ZrO2 as a principle active ingredient, the solution of one or two or more aids M is impregnated for modification, M is nitrate or oxalate or carbonate of Fe, Mn, La, Ce and K, the aid content accounts for 0.5-50 percent of the base catalyst, and the weight of the aids and the base catalyst is calculated based on oxides. The catalyst is simple in preparation process and short in period. The catalyst is used for directly preparing low carbon olefin through synthesis gas, the reaction activity is high, the conversion per pass is more than 55 percent, the C2-4 olefin accounts for more than 50 weight percent of the total olefin distribution, and the CO2 selectivity is lower than 15 percent. The catalyst can be used for effectively improving the product distribution in a high-temperature Fischer-Tropsch reaction, and the generation of components with more than 5 carbon atoms is suppressed.

Description

technical field [0001] The invention provides a kind of by synthesis gas (H 2 and CO) to directly produce low carbon olefins (ethylene, propylene and butylene) modified zirconia (ZrO 2 )catalyst. Background technique [0002] Low-carbon olefins include ethylene, propylene and butene, which are the basic organic chemical raw materials for synthetic plastics, fibers and other chemical products. Currently, they are mainly obtained through by-products in the cracking process of light oil. With the increasing demand for low-carbon olefins and the depletion of global petroleum resources, it is imperative to develop a technology for obtaining low-carbon olefins from non-petroleum resources. Along with the industrial application of methanol-to-olefins processes such as MTO and MTP processes, the development of the olefins synthesis industry has been greatly promoted. The direct catalytic conversion of synthesis gas to produce light olefins has a simple process route, low investme...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/04B01J23/78B01J23/889B01J23/83C07C1/04C07C11/04C07C11/06C07C11/08
CPCY02P20/52
Inventor 张建利赵天生马利海范素兵
Owner NINGXIA UNIVERSITY