CN110590488B - Method for preparing low-carbon olefin by hydrogenation of carbon monoxide by using composite hydrogen storage material - Google Patents
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Abstract
The invention relates to a method for preparing low-carbon olefin by hydrogenation of carbon monoxide by using a composite hydrogen storage material, which belongs to the technical field of chemical industry, and the method comprises the steps of firstly placing magnesium-aluminum alloy powder and cerium oxide powder in a ball milling tank, and carrying out ball milling activation under the atmosphere of zirconia grinding medium and argon to reduce the particle size; then opening the ball milling tank, replacing part of zirconia grinding balls with iron balls, and carrying out ball milling activation in a hydrogen atmosphere to obtain a composite hydrogen storage material; and (3) putting the obtained composite hydrogen storage material into a fixed bed reactor, introducing synthesis gas, increasing the pressure and heating the reactor, so that carbon monoxide and hydrogen generate low-carbon olefin under the action of the hydrogen storage material. The composite hydrogen storage material prepared by the hydrogenation method has the advantages of low raw material cost, high reaction activity, mild use conditions and high selectivity of low-carbon olefin.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a method for preparing low-carbon olefin by hydrogenating carbon monoxide by using a composite hydrogen storage material.
Background
Generally, when the carbonaceous material is not completely combusted, toxic and harmful carbon monoxide gas is generated. In the industrial processes of iron making, coking, casting, calcining, garbage disposal and the like, carbon monoxide gas is generated. Carbon monoxide and hydrogen in the coal-based synthesis gas can be used for synthesizing high value-added products such as methanol, ethanol, ethylene glycol, low-carbon olefin, oil products and the like, wherein the low-carbon olefin is an important chemical raw material. Currently, the methanol route is mainly adopted for industrially converting synthesis gas into low-carbon olefins, i.e. carbon monoxide is firstly hydrogenated to prepare methanol, and then the methanol is converted into the low-carbon olefins. The process has high energy consumption, serious pollution and insignificant economic benefit. The one-step method for preparing the low-carbon olefin from the carbon monoxide is beneficial to shortening the process flow, reducing the equipment investment and improving the economic benefit. At present, the preparation of low-carbon olefin from carbon monoxide by a one-step method is still a bottleneck problem in the coal chemical industry. The development and development of new and highly efficient catalysts is an important approach to solving this problem.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a method for preparing low-carbon olefin by hydrogenating carbon monoxide by using a composite hydrogen storage material. The method uses the composite hydrogen storage material to hydrogenate the carbon monoxide, and the composite hydrogen storage material is prepared by a mechanochemical method, so that the preparation method is simple and has strong repeatability. The obtained product low-carbon olefin has high selectivity.
In order to achieve the purpose, the invention adopts the specific scheme that:
the method for preparing the low-carbon olefin by hydrogenating the carbon monoxide by using the composite hydrogen storage material comprises the following steps:
placing magnesium-aluminum alloy powder and cerium oxide powder in a ball milling tank, adding zirconia grinding balls as grinding media, introducing argon, and carrying out ball milling under the argon atmosphere;
step two, opening the ball milling tank after ball milling is finished, replacing part of zirconia grinding balls with iron balls, introducing hydrogen, and performing ball milling activation in hydrogen atmosphere to obtain a composite hydrogen storage material;
and step three, putting the composite hydrogen storage material obtained in the step two into a fixed bed reactor, introducing synthesis gas with a lower hydrogen-carbon ratio, heating for reaction, and generating low-carbon olefin from carbon monoxide and hydrogen under the action of the hydrogen storage material.
As a further optimization of the scheme, in the step one, the mass ratio of the magnesium-aluminum alloy powder to the cerium oxide powder is 8:2, and the ball milling time in the argon atmosphere is 3-5 h.
As a further optimization of the scheme, the diameters of the zirconia grinding balls in the step one are respectively 3mm, 6mm, 10mm and 20mm, and the numbers of the zirconia grinding balls with the diameters of 3mm, 6mm, 10mm and 20mm are respectively 1000, 300, 30 and 2.
As a further optimization of the scheme, in the step two, replacing part of the zirconia grinding balls with the iron balls, 15-30 zirconia grinding balls with the diameter of 10mm are replaced with 15-30 iron balls with the diameter of 10 mm.
And as a further optimization of the scheme, in the step two, ball milling activation is carried out in a hydrogen atmosphere, the pressure of hydrogen in a ball milling tank is 1-2 MPa, and the activation time is 3-5 h.
As a further optimization of the scheme, the hydrogen-carbon ratio of the synthesis gas in the third step is 1: 4-1: 10; the reaction pressure is 1-2 MPa, and the reaction temperature is 280-350 ℃.
The method for preparing the low-carbon olefin by hydrogenating the carbon monoxide by using the composite hydrogen storage material adopts a mechanochemical method to cause material particles to generate a large amount of defects and reduce reaction potential barrier, thereby compounding the cerium oxide and the hydrogen storage material and doping iron elements on the surface of the hydrogen storage material. During the hydrogenation of carbon monoxide, the hydrogen storage components (magnesium, aluminum and iron) in the composite hydrogen storage material can activate hydrogen to be hydrogen ions with negative valence, and the cerium oxide component activates the hydrogen to be hydrogen ions with positive valence. The negative hydrogen ions attack the carbon sites of carbon monoxide and the positive hydrogen ions attack the oxygen sites of carbon monoxide. Under the condition of low hydrogen partial pressure, the carbon chain is increased to generate low-carbon olefin.
The invention has the beneficial effects that:
1. the method for preparing the low-carbon olefin by hydrogenating the carbon monoxide by using the composite hydrogen storage material is simple in preparation method and strong in repeatability, and the composite hydrogen storage material is prepared by adopting a mechanochemical method. The used raw materials are cheap and easy to obtain, and have strong market competitiveness;
2. according to the method for preparing the low-carbon olefin by hydrogenating the carbon monoxide by using the composite hydrogen storage material, the hydrogenation method is a one-step hydrogenation method, the obtained product low-carbon olefin has high economic value, the process flow is simple, the reaction conditions are mild, the low-carbon olefin selectivity is high, and the economic benefit is obvious.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.
Example 1
And placing the magnesium-aluminum alloy powder and the cerium oxide powder in a ball milling tank, wherein the mass percentages of the magnesium-aluminum alloy powder and the cerium oxide powder are respectively 80% and 20%, and carrying out ball milling activation for 3 hours in the atmosphere of a zirconium oxide grinding medium and argon gas to reduce the particle size. The zirconia grinding medium is formed by adding zirconia grinding balls with four different diameters into a ball milling tank, wherein the four different diameters of the zirconia grinding balls are respectively 3mm, 6mm, 10mm and 20mm, and the number of the zirconia grinding balls with the diameters of 3mm, 6mm, 10mm and 20mm is respectively 1000, 300, 30 and 2.
Replacing the zirconium oxide grinding balls with the same diameter by 15 iron balls with the diameter of 10mm, and carrying out ball milling for 3 hours under the hydrogen pressure of 1MPa to obtain the composite hydrogen storage material. 0.5g of the composite hydrogen storage material was placed in a fixed bed reactor having an inner diameter of 8mm, and a synthesis gas having a hydrogen-carbon ratio of 1/4 was introduced. The reaction conditions are that the temperature is 300 ℃, and the space velocity is 2400h-1. The reaction product was analyzed by an on-line gas chromatograph, with a carbon monoxide conversion of 23% and a low-carbon olefin selectivity of 56%.
Example 2
And placing the magnesium-aluminum alloy powder and the cerium oxide powder in a ball milling tank, wherein the mass percentages of the magnesium-aluminum alloy powder and the cerium oxide powder are respectively 80% and 20%, and carrying out ball milling activation for 4 hours in the atmosphere of a zirconium oxide grinding medium and argon gas. The zirconia grinding medium is formed by adding zirconia grinding balls with four different diameters into a ball milling tank, wherein the four different diameters of the zirconia grinding balls are respectively 3mm, 6mm, 10mm and 20mm, and the number of the zirconia grinding balls with the diameters of 3mm, 6mm, 10mm and 20mm is respectively 1000, 300, 30 and 2.
Replacing zirconium oxide grinding balls with the same diameter by 20 iron balls with the diameter of 10mm, and carrying out ball milling for 4 hours under the hydrogen pressure of 2MPa to obtain the composite hydrogen storage material. 0.5g of the composite hydrogen storage material was placed in a fixed bed reactor having an inner diameter of 8mm, and a synthesis gas having a hydrogen-carbon ratio of 1/4 was introduced. The reaction conditions are that the temperature is 300 ℃, and the space velocity is 2400h-1. And (3) analyzing the reaction product by adopting an online gas chromatograph, wherein the conversion rate of the carbon monoxide is 25%, and the selectivity of the low-carbon olefin is 58%.
Example 3
And placing the magnesium-aluminum alloy powder and the cerium oxide powder in a ball milling tank, wherein the mass percentages of the magnesium-aluminum alloy powder and the cerium oxide powder are respectively 80% and 20%, and carrying out ball milling activation for 5 hours in the atmosphere of a zirconium oxide grinding medium and argon gas. The zirconia grinding medium is formed by adding zirconia grinding balls with four different diameters into a ball milling tank, wherein the four different diameters of the zirconia grinding balls are respectively 3mm, 6mm, 10mm and 20mm, and the number of the zirconia grinding balls with the diameters of 3mm, 6mm, 10mm and 20mm is respectively 1000, 300, 30 and 2.
Replacing the zirconium oxide grinding balls with the same diameter by 30 iron balls with the diameter of 10mm, and carrying out ball milling for 5 hours under the hydrogen pressure of 2MPa to obtain the composite hydrogen storage material. 0.5g of the composite hydrogen storage material was placed in a fixed bed reactor having an inner diameter of 8mm, and a synthesis gas having a hydrogen-carbon ratio of 1/4 was introduced. The reaction conditions are that the temperature is 300 ℃, and the space velocity is 2400h-1. The reaction product was analyzed by an on-line gas chromatograph, and the conversion of carbon monoxide was 27% and the selectivity of low-carbon olefin was 60%.
Example 4
And placing the magnesium-aluminum alloy powder and the cerium oxide powder in a ball milling tank, wherein the mass percentages of the magnesium-aluminum alloy powder and the cerium oxide powder are respectively 80% and 20%, and carrying out ball milling activation for 3h in the atmosphere of a zirconium oxide grinding medium and argon. The zirconia grinding medium is formed by adding zirconia grinding balls with four different diameters into a ball milling tank, wherein the four different diameters of the zirconia grinding balls are respectively 3mm, 6mm, 10mm and 20mm, and the number of the zirconia grinding balls with the diameters of 3mm, 6mm, 10mm and 20mm is respectively 1000, 300, 30 and 2.
Replacing the zirconium oxide grinding balls with the same diameter by 15 iron balls with the diameter of 10mm, and carrying out ball milling for 3 hours under the hydrogen pressure of 1MPa to obtain the composite hydrogen storage material. 0.5g of the composite hydrogen storage material was placed in a fixed bed reactor having an inner diameter of 8mm, and a synthesis gas having a hydrogen-carbon ratio of 1/8 was introduced. The reaction conditions are that the temperature is 320 ℃, and the space velocity is 2400h-1. And (3) analyzing the reaction product by using an online gas chromatograph, wherein the conversion rate of carbon monoxide is 24%, and the selectivity of low-carbon olefin is 58%.
Example 5
And placing the magnesium-aluminum alloy powder and the cerium oxide powder in a ball milling tank, wherein the mass percentages of the magnesium-aluminum alloy powder and the cerium oxide powder are respectively 80% and 20%, and carrying out ball milling activation for 3h in the atmosphere of a zirconium oxide grinding medium and argon. The zirconia grinding medium is formed by adding zirconia grinding balls with four different diameters into a ball milling tank, wherein the four different diameters of the zirconia grinding balls are respectively 3mm, 6mm, 10mm and 20mm, and the number of the zirconia grinding balls with the diameters of 3mm, 6mm, 10mm and 20mm is respectively 1000, 300, 30 and 2.
Replacing the zirconium oxide grinding balls with the same diameter by 15 iron balls with the diameter of 10mm, and carrying out ball milling for 3 hours under the hydrogen pressure of 1MPa to obtain the composite hydrogen storage material. 0.5g of the composite hydrogen storage material was placed in a fixed bed reactor having an inner diameter of 8mm, and a synthesis gas having a hydrogen-carbon ratio of 1/10 was introduced. The reaction conditions are that the temperature is 350 ℃, and the space velocity is 2400h-1. The reaction product was analyzed by an on-line gas chromatograph, and the conversion of carbon monoxide was 28% and the selectivity of low-carbon olefins was 59%.
Example 6
And placing the magnesium-aluminum alloy powder and the cerium oxide powder in a ball milling tank, wherein the mass percentages of the magnesium-aluminum alloy powder and the cerium oxide powder are respectively 80% and 20%, and carrying out ball milling activation for 5 hours in the atmosphere of a zirconium oxide grinding medium and argon gas. The zirconia grinding medium is formed by adding zirconia grinding balls with four different diameters into a ball milling tank, wherein the four different diameters of the zirconia grinding balls are respectively 3mm, 6mm, 10mm and 20mm, and the number of the zirconia grinding balls with the diameters of 3mm, 6mm, 10mm and 20mm is respectively 1000, 300, 30 and 2.
By 20 straightReplacing zirconium oxide grinding balls with the same diameter with iron balls with the diameter of 10mm, and carrying out ball milling for 3 hours under the hydrogen pressure of 1MPa to obtain the composite hydrogen storage material. 0.5g of the composite hydrogen storage material was placed in a fixed bed reactor having an inner diameter of 8mm, and a synthesis gas having a hydrogen-carbon ratio of 1/10 was introduced. The reaction conditions are that the temperature is 350 ℃, and the space velocity is 2400h-1. The reaction product is analyzed by an online gas chromatograph, the conversion rate of carbon monoxide is 30%, and the selectivity of low-carbon olefin is 60%.
Example 7
And placing the magnesium-aluminum alloy powder and the cerium oxide powder in a ball milling tank, wherein the mass percentages of the magnesium-aluminum alloy powder and the cerium oxide powder are respectively 80% and 20%, and carrying out ball milling activation for 5 hours in the atmosphere of a zirconium oxide grinding medium and argon gas. The zirconia grinding medium is formed by adding zirconia grinding balls with four different diameters into a ball milling tank, wherein the four different diameters of the zirconia grinding balls are respectively 3mm, 6mm, 10mm and 20mm, and the number of the zirconia grinding balls with the diameters of 3mm, 6mm, 10mm and 20mm is respectively 1000, 300, 30 and 2.
Replacing the zirconium oxide grinding balls with the same diameter by 30 iron balls with the diameter of 10mm, and carrying out ball milling for 5 hours under the hydrogen pressure of 2MPa to obtain the composite hydrogen storage material. 0.5g of the composite hydrogen storage material was placed in a fixed bed reactor having an inner diameter of 8mm, and a synthesis gas having a hydrogen-carbon ratio of 1/10 was introduced. The reaction conditions are that the temperature is 350 ℃, and the space velocity is 2400h-1. And (3) analyzing the reaction product by using an online gas chromatograph, wherein the conversion rate of the carbon monoxide is 32%, and the selectivity of the low-carbon olefin is 62%.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (4)
1. The method for preparing the low-carbon olefin by hydrogenating the carbon monoxide by using the composite hydrogen storage material is characterized by comprising the following steps of: the method comprises the following steps:
placing magnesium-aluminum alloy powder and cerium oxide powder in a ball milling tank, adding zirconia grinding balls as grinding media, introducing argon, and carrying out ball milling under the argon atmosphere; the mass ratio of the magnesium-aluminum alloy powder to the cerium oxide powder is 8:2, and the ball milling time in the argon atmosphere is 3-5 h;
step two, opening the ball milling tank after ball milling is finished, replacing part of zirconia grinding balls with iron balls, introducing hydrogen, and performing ball milling activation in hydrogen atmosphere to obtain a composite hydrogen storage material;
and step three, putting the composite hydrogen storage material obtained in the step two into a fixed bed reactor, introducing synthesis gas with a hydrogen-carbon ratio of 1: 4-1: 10, heating for reaction, wherein the reaction pressure is 1-2 MPa, the reaction temperature is 280-350 ℃, and carbon monoxide and hydrogen generate low-carbon olefin under the action of the hydrogen storage material.
2. The method for preparing the low-carbon olefin by hydrogenating the carbon monoxide by using the composite hydrogen storage material according to claim 1, wherein the method comprises the following steps: the diameters of the zirconia grinding balls in the step one are respectively 3mm, 6mm, 10mm and 20mm, and the number of the zirconia grinding balls with the diameters of 3mm, 6mm, 10mm and 20mm is respectively 1000, 300, 30 and 2.
3. The method for preparing the low-carbon olefin by hydrogenating the carbon monoxide by using the composite hydrogen storage material according to claim 1, wherein the method comprises the following steps: and replacing part of the zirconia grinding balls with iron balls in the second step, namely replacing 15-30 zirconia grinding balls with the diameter of 10mm with 15-30 iron balls with the diameter of 10 mm.
4. The method for preparing the low-carbon olefin by hydrogenating the carbon monoxide by using the composite hydrogen storage material according to claim 1, wherein the method comprises the following steps: and step two, ball milling activation is carried out in a hydrogen atmosphere, the pressure of hydrogen in a ball milling tank is 1-2 MPa, and the activation time is 3-5 h.
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