CN114225668B - Reaction device, method and application for preparing formic acid by capturing carbon dioxide and hydrogenating - Google Patents
Reaction device, method and application for preparing formic acid by capturing carbon dioxide and hydrogenating Download PDFInfo
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- CN114225668B CN114225668B CN202111420665.4A CN202111420665A CN114225668B CN 114225668 B CN114225668 B CN 114225668B CN 202111420665 A CN202111420665 A CN 202111420665A CN 114225668 B CN114225668 B CN 114225668B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
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- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
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- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
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Abstract
The invention relates to a reaction device for preparing formic acid by capturing carbon dioxide and hydrogenating, a method and application thereof. The reactor is of a cylindrical tubular structure, a gas distributor is arranged at the bottom of the reactor, a reaction medium is filled in the reactor and is positioned above the gas distributor; the bottom of the reactor and the lower part of the gas distributor are provided with a raw material gas inlet. Compared with the traditional kettle type reactor, the reactor has the advantages of high mass transfer efficiency, mild operation conditions, continuity, modularization and the like.
Description
Technical Field
The invention belongs to the technical field of energy chemical industry, and particularly relates to a reaction device and a method for preparing formic acid by carbon dioxide capture and hydrogenation.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
The average concentration of carbon dioxide in the atmosphere exceeds 410ppm, and the prior art carries out carbon dioxide Capture by Direct Air Capture technology (DAC), thereby solving the problem of excessive emission of carbon dioxide. Capturing and further converting carbon dioxide into useful chemicals or fuels reduces the overall cost but still requires harsh reaction conditions such as high temperature and high pressure, mainly because carbon dioxide molecules are stable (Δ G = -396 kJ/mol), and often require harsh reaction conditions (high temperature and high pressure) to be effectively activated.
Existing by CO 2 The carbon dioxide is captured in the process of preparing formic acid by hydrogenation, but the problems of poor reaction continuity, easy loss of catalyst, difficult product separation and the like of a homogeneous catalysis system do not existPotential for large-scale use. And the reaction process is mainly carried out through a kettle type reactor, the mass transfer effect is relatively poor, large-scale amplification is not facilitated, and the carbon dioxide capture process is not coupled.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a reaction device and a method for preparing formic acid by capturing carbon dioxide and hydrogenating the carbon dioxide, and an application of the reaction device.
In order to solve the technical problems, the technical scheme of the invention is as follows:
in a first aspect, a reaction device for preparing formic acid by capturing carbon dioxide and hydrogenating comprises a reactor,
the reactor is of a cylindrical tubular structure, the bottom of the reactor is provided with a gas distributor, the interior of the reactor is filled with a reaction medium, and the reaction medium is positioned above the gas distributor;
the bottom of the reactor and the lower part of the gas distributor are provided with a raw material gas inlet.
The reaction device for preparing the formic acid by capturing the carbon dioxide and hydrogenating the carbon dioxide is used for reacting in a cylindrical tubular structure, a reaction medium is filled in the reaction device, gas moves upwards from the bottom of the reactor, and then the reaction product formic acid is obtained from the reactor. Since the reaction proceeds while the gas moves upward, the carbon dioxide can be continuously absorbed at a constant rate, and a continuous reaction can be performed.
The bottom of the reactor is provided with the gas distributor, so that the raw material gas can be dispersed into tiny small bubbles, the mass transfer efficiency is improved, the reaction medium is arranged above the gas distributor, and the gas medium is not easy to lose.
Compared with the traditional kettle type reactor, the reactor has the advantages of high mass transfer efficiency, mild operation conditions, continuity, modularization and the like. The method is expected to solve the problem of low efficiency of catalytic conversion of carbon dioxide into formic acid by a heterogeneous catalyst under mild conditions, provides a successful example for large-scale capture and conversion of carbon dioxide at normal temperature and normal pressure, and has the advantages of simple structure, low production cost and good practical application value.
In a second aspect, a reaction method for preparing formic acid by capturing carbon dioxide and hydrogenating comprises the following steps:
the raw material gas enters from the bottom of the reactor, then under the action of alkali liquor, carbon dioxide is absorbed by the alkali liquor to obtain a product A, then hydrogen is introduced into the reactor, and the product A is subjected to hydrogenation reaction under the action of a catalyst to obtain formic acid.
In a third aspect, the carbon dioxide capturing and hydrogen adding formic acid making reaction device or the carbon dioxide capturing and hydrogen adding formic acid making reaction method is applied to the field of carbon dioxide capturing.
One or more technical schemes of the invention have the following beneficial effects:
1. according to the technical scheme, the reactor and the system for preparing the formic acid by capturing the carbon dioxide and hydrogenating the carbon dioxide can realize the coupling of the capture of the carbon dioxide and the catalytic conversion under the mild condition, and simultaneously realize the capture of the carbon dioxide and the catalytic conversion under the condition of low energy consumption;
2. the reactor related in the technical scheme of the invention can disperse the feed gas into tiny small bubbles to contact with an alkaline medium or a catalyst for capture and hydrogenation reaction, and can maximize the gas-liquid-solid mass transfer efficiency;
3. the reactor and the reaction system disclosed by the technical scheme are composed of one or more reaction tubes, and an array type reaction system can be formed according to requirements, so that the amplification effect caused by the amplification of an industrial reactor is reduced;
4. compared with the traditional kettle type reactor, the reactor provided by the invention has a simple structure, is easy to realize industrial scale-up production, does not need an additional stirring system and the like, and has lower generation cost and lower operation energy consumption. Therefore, it has good practical application value.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are included to explain the illustrative embodiments of the invention and the description of the invention and are not intended to limit the invention.
FIG. 1 is a schematic diagram of a reactor according to the present invention;
FIG. 2 is a schematic diagram of a reaction apparatus for producing formic acid by capturing carbon dioxide and hydrogenating the carbon dioxide under mild conditions according to the present invention;
FIG. 3 is a graph showing the reaction results in example 9 of the present invention;
the device comprises a reactor 1, a reactor 2, a gas distributor 3, a reaction medium 4, an alkali liquor device 5, a product solution device 6, a raw material gas device 7 and a pump.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
As shown in fig. 1 and 2:
in a first aspect, a reaction device for preparing formic acid by capturing carbon dioxide and hydrogenating comprises a reactor,
the reactor 1 is of a cylindrical tubular structure, a gas distributor 2 is arranged at the bottom of the reactor 1, a reaction medium 3 is filled in the reactor, and the reaction medium 3 is positioned above the gas distributor;
the bottom of the reactor 1 and the lower part of the gas distributor 2 are provided with a raw material gas inlet.
In some embodiments of the invention, the cylindrical tubular structure has an aspect ratio of not less than 1. The length is the height and the diameter is the diameter of the cross section.
In some embodiments of the present invention, the tubular structure of the reactor 1 is made of glass, refractory metal or ceramic material. The material of the reactor is high temperature resistant material.
In some embodiments of the invention, the gas distributor 2 is a plate structure with mesh holes or a cylinder structure with honeycomb through holes.
In some embodiments of the invention, reaction medium 3 is a mixture of catalyst particles and a basic solution.
In some embodiments of the present invention, the present invention further comprises a lye unit 4, and a liquid outlet of the lye unit 4 is connected with the reactor.
In some embodiments of the invention, a product solution device 5 is further included, and the product solution device 5 is connected to the reactor 1. The product solution device 5 and the alkali liquor device 4 are respectively connected with the reactor through a product liquid pipeline and an alkali liquor pipeline, and the outlet end of the alkali liquor pipeline is positioned below the liquid suction end of the product liquid pipeline. The arrangement is favorable for the alkali liquor to enter for reaction and the product liquid to be discharged.
The method can be favorable for solving the problem of difficult product separation, and the gas gradually reacts in the upward moving process, so that the reacted formic acid is distributed in the reactor, the formic acid is gradually sucked away from the upper part of the reactor, the formic acid forms gradient concentration, the formic acid moves upward, and then the formic acid is gradually generated below. Is beneficial to continuous operation, and the content of formic acid in the product is higher.
And a product liquid pipeline of the product solution device 5 and an alkali liquor pipeline of the alkali liquor device 4 are respectively provided with a pump for providing liquid flowing power.
In some embodiments of the invention, the top of the reactor 1 is provided with a vent for off-gas. Some unreacted gas is discharged from the off-gas outlet.
In some embodiments of the present invention, a hydrogen plant and a raw material gas plant 6 are further included, and the hydrogen plant and the raw material gas plant 6 are respectively connected with the bottom of the reactor 1.
In some embodiments of the invention, the reactors 1 are provided in several numbers, several reactors 1 being connected in series.
In a second aspect, a reaction method for preparing formic acid by capturing carbon dioxide and hydrogenating comprises the following steps:
the raw material gas enters from the bottom of the reactor, then under the action of alkali liquor, carbon dioxide is absorbed by the alkali liquor to obtain a product A, then hydrogen is introduced into the reactor, and the product A is subjected to hydrogenation reaction under the action of a catalyst to obtain formic acid.
In some embodiments of the present invention, the feed gas and hydrogen are simultaneously introduced into the reactor, and the hydrogenation reaction is carried out in the presence of an alkali solution to obtain formic acid.
In some embodiments of the invention, the catalyst is a particulate Pd-based or Pd-based bimetallic catalyst, the active metal is Pd, the second metal is any one of Fe, co, ni, cu, zn, and the support is a nitrogen-containing carbon-based material with a nitrogen content of 0-30wt.%.
In some embodiments of the present invention, the solute of the alkali solution is an inorganic base or an organic base, including organic amine, carbonate, etc., preferably organic amine, and further preferably C 1 -C 6 Corresponding primary, secondary and tertiary amines and their corresponding alcohol amines.
In some embodiments of the invention, the feed gas is air, flue gas, or pure carbon dioxide gas.
In some embodiments of the invention, the reaction temperature in the reactor is 20-80 ℃; reaction pressure: 0.1-2MPa. The reaction temperature is mild, and the processes of carbon dioxide capture and hydrogenation for preparing formic acid under mild conditions can be realized.
In a third aspect, the carbon dioxide capturing and hydrogen adding formic acid making reaction device or the carbon dioxide capturing and hydrogen adding formic acid making reaction method is applied to the field of carbon dioxide capturing.
Examples 1 to 6
Examples 1 to 6 show the reactor shown in fig. 1, in which the carbon dioxide capturing and hydrogenation reaction apparatus provided by the present invention is used to capture and hydrogenate carbon dioxide in a discontinuous manner, and the capturing and hydrogenation performance of different types of organic amine solutions on carbon dioxide is examined. The specific parameters of the reactor are that the diameter of the reaction tube is 1cm, the length is 20cm, the aperture of the gas distributor is 15 μm, and the reactor is made of glass materials. The specific operation flow is as follows: weighing a certain mass of catalyst, placing the catalyst in a reaction tube, then adding 5mL of 2mol/L organic amine aqueous solution, reacting at room temperature under 1 atm, introducing air from the bottom end of the reactor for capturing carbon dioxide, introducing pure hydrogen for hydrogenation after adsorption saturation, and detecting the concentration of formic acid in the product by using high performance liquid chromatography after reacting for half an hour, wherein the concentration is shown in Table 1.
Table 1 examples 1-6 high performance liquid chromatography test results
Examples 7 to 8
Examples 7 to 8 are the reaction apparatus for producing formic acid by capturing carbon dioxide and hydrogenating it according to the present invention, and the performance of the carbon dioxide capturing and hydrogenating reaction at different concentrations was examined by performing the reaction in a non-continuous manner, and the reactor is shown in fig. 1. The specific parameters of the reactor are that the diameter of the reaction tube is 1cm, the length is 20cm, the aperture of the gas distributor is 15 μm, and the reactor is made of glass materials. The specific operation flow is as follows: weighing a certain mass of catalyst, placing the catalyst in a reaction tube, then adding 5mL of organic amine aqueous solution with the concentration of 2mol/L, controlling the reaction temperature to be room temperature and the reaction pressure to be 1 atmosphere, then introducing carbon dioxide gas with a certain concentration from the bottom end of the reactor for carbon dioxide capture, introducing pure hydrogen for hydrogenation reaction after adsorption saturation, and detecting the concentration of formic acid in the product by using high performance liquid chromatography after the reaction is carried out for half an hour, wherein the concentration is shown in the following table. .
TABLE 2 detection results of examples 7 to 8 by HPLC
Example 9
Embodiment 9 is a reaction apparatus for preparing formic acid by capturing carbon dioxide and hydrogenating, which is provided by the present invention, and directly reacts a mixed gas of carbon dioxide and hydrogen at normal temperature and normal pressure to generate formic acid by using a continuous method of fluidizing a reaction medium, wherein the reactor is enlarged by 100 times compared with embodiments 1-8, and the reaction apparatus for preparing formic acid by capturing carbon dioxide and hydrogenating is shown in fig. 2. The specific parameters of the reactor are that the diameter of the reaction tube is 5cm, the length is 1m, and the aperture of the gas distributor is 30 μm. The reaction medium is circulated, a certain amount of fresh alkali solution is added into the reaction system in real time to the lower end of the reaction tube by using a peristaltic pump, and the solution after reaction is extracted from the top end of the reaction tube. The following operating conditions were used: the reaction was continued for 24 hours at room temperature under normal pressure using 40g of catalyst, a mixed gas of carbon dioxide and hydrogen at 1:1, and 1L of a 2mol/L aqueous solution of organic amine (example 9) as a reaction medium at a flow rate of 12mL/min, and after the reaction was completed, the concentration of formic acid in the product was measured by high performance liquid chromatography, as shown in the following table. The reaction results are shown in FIG. 3.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A reaction method for preparing formic acid by capturing carbon dioxide and hydrogenating is characterized in that: a reaction device for preparing formic acid by capturing carbon dioxide and hydrogenating comprises a reactor, wherein the reactor is of a cylindrical tubular structure, a gas distributor is arranged at the bottom of the reactor, a reaction medium is filled in the reactor, and the reaction medium is positioned above the gas distributor; the reaction medium is the mixture of catalyst particles and alkali liquor; a raw material gas inlet is arranged at the bottom of the reactor and below the gas distributor; the device also comprises an alkali liquor device, wherein a liquor outlet of the alkali liquor device is connected with the reactor; the device also comprises a product solution device, and the product solution device is connected with the reactor; the product solution device and the alkali liquor device are respectively connected with the reactor through a product liquid pipeline and an alkali liquor pipeline, and the outlet end of the alkali liquor pipeline is positioned below the liquid absorption end of the product liquid pipeline;
the method comprises the following steps:
raw material gas enters from the bottom of the reactor, then under the action of alkali liquor, carbon dioxide is absorbed by the alkali liquor to obtain a product A, then hydrogen is introduced into the reactor, and the product A is subjected to hydrogenation reaction under the action of a catalyst to obtain formic acid;
the catalyst is a granular Pd-based or Pd-based bimetallic catalyst, the active metal is Pd, the second metal is any one of Fe, co, ni, cu and Zn, and the carrier is a nitrogen-containing carbon-based material, wherein the nitrogen content is 0-30 wt%;
the solute of the alkali liquor is inorganic alkali or organic alkali, and the organic alkali comprises organic amine and carbonate;
the raw material gas is air, flue gas or pure carbon dioxide gas.
2. The carbon dioxide capture and hydrogenation formic acid production reaction process of claim 1, which is characterized in that: the length-diameter ratio of the cylindrical tubular structure is not less than 1.
3. The carbon dioxide capture and hydrogenation formic acid production reaction process of claim 1, which is characterized in that: the tubular structure of the reactor is made of glass, high-temperature-resistant metal or ceramic material.
4. The carbon dioxide capture and hydrogenation formic acid production reaction process of claim 1, which is characterized in that: the gas distributor is a plate body structure with meshes or a cylinder body structure with honeycomb through holes.
5. The carbon dioxide capture and hydrogenation formic acid production reaction process of claim 1, which is characterized in that: the reactor also comprises a hydrogen device and a raw material gas device, wherein the hydrogen device and the raw material gas device are respectively connected with the bottom of the reactor.
6. The carbon dioxide capture and hydrogenation formic acid production reaction process of claim 1, which is characterized in that: the organic base is organic amine.
7. The carbon dioxide capture and hydrogenation formic acid production reaction process of claim 1, which is characterized in that: the reaction temperature in the reactor is 20-80 ℃; reaction pressure: 0.1-2MPa.
8. Use of the carbon dioxide capture and hydrogen formic acid production reaction process of any of claims 1-7 in the field of carbon dioxide capture.
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| US8791297B2 (en) * | 2010-06-29 | 2014-07-29 | Basf Se | Process for preparing formic acid by reaction of carbon dioxide with hydrogen |
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