Method for preparing low-carbon olefin catalyst through carbon dioxide hydrogenation

A low-carbon olefin and carbon dioxide technology, which is applied in the production of hydrocarbons from carbon oxides, organic chemistry, and bulk chemical production, etc. Controllable particle size, stable catalyst and high selectivity

Inactive Publication Date: 2015-05-20
NINGXIA UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the preparation of related catalysts and its application in the reaction of carbon dioxide hydrogenation to light olefins have problems such as poor preparation repeatability, many by-products, low conversion of carbon dioxide, and low selectivity of light olefins.

Method used

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  • Method for preparing low-carbon olefin catalyst through carbon dioxide hydrogenation
  • Method for preparing low-carbon olefin catalyst through carbon dioxide hydrogenation

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Weigh 40.4g Fe(NO 3 ) 3 9H 2 O and 54.0g urea are mixed into 200mL homogeneously mixed solution, wherein urea / Fe molar ratio is 9, transfer to sample dissolving cup, in microwave 2450MHz, power 500W, 1.6MPa, heat 2 hours, drop to room temperature, filter, wash and precipitate to Neutral, dry at 120°C for 12 hours, and bake at 400°C for 4 hours. Weigh 0.60g K 2 CO 3 , dissolved in 4mL of deionized water, impregnated into 7g of the above sample, dried at 120°C for 12 hours, and granulated at 20-40 mesh to obtain catalyst sample 1, in which zirconium / iron was 0. At a temperature of 400°C and normal pressure, the space velocity is 1000h -1 30% H 2 The catalyst samples were reduced for 8 hours. Then switch to carbon dioxide hydrogenation feed gas (H 2 / CO 2 =3、Airspeed=1000h -1 ), reacted for 100 hours at a temperature of 320° C. and a pressure of 2 MPa. The results are shown in Table 1.

Embodiment 2

[0028] Weigh 40.4g Fe(NO 3 ) 3 9H 2 O, 3.82g ZrO(NO 3 ) 2 2H 2 O and 54.8g urea are mixed with 200mL homogeneous mixed solution, wherein urea / (Fe+Zr) molar ratio is 8, in microwave 2450MHz, power 500W, 1.6MPa conditions heating 2 hours, down to room temperature, filter, wash and precipitate to medium properties, dry at 120°C for 12 hours, and bake at 500°C for 4 hours. Weigh 0.49g K 2 CO 3 , dissolved in 4mL of deionized water, impregnated into 7g of the above sample, dried at 120°C for 12 hours, and granulated at 20-40 mesh to obtain catalyst sample 2, wherein the zirconium / iron ratio was 1:7. At a temperature of 400°C and normal pressure, the space velocity is 1000h -1 30% H 2 The catalyst samples were reduced for 8 hours. Then switch to carbon dioxide hydrogenation feed gas (H 2 / CO 2 =3、Airspeed=1000h -1 ), reacted for 100 hours at a temperature of 320° C. and a pressure of 2 MPa. The results are shown in Table 1.

Embodiment 3

[0030] Weigh 40.4g Fe(NO 3 ) 3 9H 2 O, 5.34g ZrO(NO 3 ) 2 2H 2 O and 43.7g urea are mixed with 200mL homogeneously mixed solution, wherein urea / (Fe+Zr) mol ratio is 6, transfers to the sample dissolving cup, in microwave 2450MHz, power 500W, 1.6MPa condition heating 2 hours, down to room temperature, Filter and wash the precipitate until neutral, dry at 120°C for 12 hours, and bake at 500°C for 4h. Weigh 0.46g K 2 CO 3 , dissolved in 4mL of deionized water, impregnated into 7g of the above sample, dried at 120°C for 12 hours, and granulated at 20-40 mesh to obtain catalyst sample 3, wherein the zirconium / iron ratio was 1:5. At a temperature of 400°C and normal pressure, the space velocity is 1000h -1 30% H 2 The catalyst samples were reduced for 8 hours. Then switch to carbon dioxide hydrogenation feed gas (H 2 / CO 2 =3、Airspeed=1000h -1 ), reacted for 100 hours at a temperature of 320° C. and a pressure of 2 MPa. The results are shown in Table 1.

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Abstract

The invention relates to a method for preparing a low-carbon olefin catalyst through carbon dioxide hydrogenation. The low-carbon olefin catalyst comprises the following element components: iron, zirconium, potassium and oxygen, the atomic molar ratio of zirconium to iron is (0-1):1, and the atomic molar ratio of iron to potassium is 10:1. The method for preparing the low-carbon olefin catalyst through carbon dioxide hydrogenation comprises the following steps: (1) weighing an iron source and a zirconium sourse, preparing aqueous solution, and marking the prepared aqueous solution as solution A; (2) adding a precipitator into the solution A, stirring, and marking the obtained solution as solution B; (3) carrying out microwave induction on the solution B; (4) centrifuging, filtering and washing reaction products, drying and roasting the obtained sample, and marking the roasted sample as a sample C; (5) weighing a potassium source, dissolving the potassium source in deionized water, impregnating the sample C, drying, and marking the dried sample as a sample D; and (6) carrying out tabletting, pelletizing and hydrogen gas reduction on the sample D, so that a catalyst sample is obtained. The method for preparing the low-carbon olefin catalyst through the carbon dioxide hydrogenation has the advantages that conversion ratio of carbon dioxide raw material is high, selectivity of low-carbon olefin is high, few CH4 and CO byproducts are produced, the catalyst is stable, and powder particles of the obtained catalyst are small and uniform.

Description

technical field [0001] The invention relates to the field of catalyst preparation, in particular to a method for preparing a catalyst for carbon dioxide hydrogenation to produce low-carbon olefins. Background technique [0002] Low-carbon olefins (ethylene, propylene, butene) are important chemical basic raw materials, which can be used to produce polyethylene, polypropylene, ethylene oxide and other products. With the increasing scarcity of petroleum resources, the non-petroleum route of low-carbon olefins has been paid more attention. Molecular Catalysis (1995, Volume 9, Issue 1, Pages 78-80) reported that Fe 3 (CO) 12 The metal cluster catalyst is used for hydrogenation reaction of carbon dioxide, the conversion rate of carbon dioxide is 43.5%, and the selectivity of low carbon olefins is 98.4%. However, the catalytic preparation conditions are harsh. Journal of Fuel Chemistry (1999, Vol. 27, No. 2, Pages 145-149) reported the catalytic performance of Fe-Co bimetallic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/78C07C11/04C07C11/06C07C11/08C07C1/12
CPCY02P20/52
Inventor 赵天生苏晓娟张建利范素兵马清祥
Owner NINGXIA UNIVERSITY
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