CN114425277B - Reactor and application thereof in preparation of carbon dioxide by oxidative coupling of methane - Google Patents
Reactor and application thereof in preparation of carbon dioxide by oxidative coupling of methane Download PDFInfo
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- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/06—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
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- C07C2/76—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms by condensation of hydrocarbons with partial elimination of hydrogen
- C07C2/82—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms by condensation of hydrocarbons with partial elimination of hydrogen oxidative coupling
- C07C2/84—Preparation of hydrocarbons from hydrocarbons containing a smaller number of carbon atoms by condensation of hydrocarbons with partial elimination of hydrogen oxidative coupling catalytic
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Abstract
The invention relates to the field of catalysis, and discloses a reactor and application thereof in preparing carbon dioxide by oxidative coupling of methane, wherein the reactor comprises a reaction cavity and a catalyst filled in the reaction cavity, the reaction cavity is made of alumina, and the roughness of the inner surface of the reaction cavity is 0.5-1 micron; the catalyst comprises a carrier and an active component loaded on the carrier, wherein the carrier is at least one of CaO, mgO and BaO; the active component is an oxide of an alkali metal. The reactor has high mechanical strength, high temperature resistance, falling resistance and good stability, is used for methane oxidative coupling reaction, has high raw material conversion rate, less side reaction, high selectivity and yield of the carbon dioxide and is easy for mass production and application.
Description
Technical Field
The invention relates to the field of catalysis, in particular to a reactor and application thereof in preparing carbon dioxide by oxidative coupling of methane.
Background
At present, in the world industry, ethylene is still mainly obtained in two ways, namely, crude oil is directly obtained through pyrolysis, and naphtha obtained through refining crude oil is further cracked to obtain ethylene, so that the raw materials of ethylene are petroleum at present, however, in recent years, as shale gas, combustible ice and other natural gas exploration technologies continuously obtain important breakthrough, a lot of large and medium-sized gas fields continuously emerge, the ascertained reserves and the ascertained yields are rapidly increased, the proportion of natural gas in primary energy is gradually increased, and a natural gasification process gradually becomes one of the development directions of petrochemical industry. Natural gas is one of three energy sources (coal, petroleum and natural gas) in modern industry, has the advantages of high quality, cleanness and rich reserves, and plays a very important role. Therefore, the substitution of natural gas for petroleum to ethylene has become an important point of research in various countries.
The main component of natural gas is methane. The technology for preparing ethylene by oxidative coupling of methane is the most direct and effective way for methane chemical utilization, and although the technology has been studied for more than 30 years, the technology level of economic operation is not reached, and industrial production is not formed yet. Particularly the form and material of the reactor are a difficulty in the art. Because of the large side reactions generated by the stainless steel reactor wall, the reported methane oxidative coupling is carried out on a quartz reactor, but the reported methane oxidative coupling has certain defects in the aspect of mechanical strength.
Thus, the existing reactors for oxidative coupling of methane are in need of further improvement.
Disclosure of Invention
The invention aims to solve the technical problems of more side reactions and poor mechanical strength of the existing reactor for performing the oxidative coupling reaction of methane, and provides the reactor and application thereof in preparing carbon dioxide by oxidative coupling of methane.
In order to achieve the above object, according to one aspect of the present invention, there is provided a reactor comprising a reaction chamber and a catalyst filled in the reaction chamber, wherein the reaction chamber is made of alumina, and the roughness of the inner surface of the reaction chamber is 0.5-1 μm;
the catalyst comprises a carrier and an active component loaded on the carrier, wherein the carrier is at least one of CaO, mgO and BaO; the active component is an oxide of an alkali metal.
The reactor provided by the invention has high mechanical strength, high temperature resistance, falling resistance and good stability, is used for methane oxidative coupling reaction, has high raw material conversion rate, less side reaction, high selectivity and yield of the carbon dioxide, and is easy for mass production and application.
In a second aspect, the present invention provides a method for preparing a carbon dioxide by oxidative coupling of methane, the method comprising:
(1) Filling a reaction cavity of a reactor with a catalyst, wherein the reaction cavity is made of alumina, and the roughness of the inner surface of the reaction cavity is 0.5-1 micron;
the catalyst comprises a carrier and an active component loaded on the carrier, wherein the carrier is at least one of CaO, mgO and BaO; the active component is an oxide of alkali metal;
(2) Methane and oxygen are introduced into the alumina reaction cavity to contact with the catalyst for catalytic reaction.
The method for preparing the carbon dioxide by oxidative coupling of methane has the advantages of high conversion rate of raw materials of catalytic reaction, less side reaction, high selectivity and yield of the carbon dioxide and easiness in large-scale production and application.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The invention provides a reactor, which comprises a reaction cavity and a catalyst filled in the reaction cavity, wherein the reaction cavity is made of alumina, and the roughness of the inner surface of the reaction cavity is 0.5-1 micron;
the catalyst comprises a carrier and an active component loaded on the carrier, wherein the carrier is at least one of CaO, mgO and BaO; the active component is an oxide of an alkali metal.
In some embodiments of the invention, the roughness of the inner surface of the reaction chamber is preferably 0.6-0.8 microns. Roughness refers to the small pitch and the unevenness of the minute peaks and valleys of the machined surface as measured by the needle drawing method. In particular, the roughness of the inner surface of the cavity is large, and the wall of the cavity can generate more side reactions.
In some embodiments of the invention, the ratio of the thickness of the reaction chamber to the inner diameter of the reaction chamber is preferably 0.2-0.3:1.
in some embodiments of the invention, the reactor is made of a commercially available common alumina product, preferably α -Al 2 O 3 。
In some embodiments of the invention, the reactor further comprises a stainless steel support sleeve disposed around the reaction chamber along an outer wall of the reaction chamber. In the invention, a gap is not reserved between the stainless steel support sleeve and the alumina reaction cavity, and the stainless steel support sleeve and the alumina reaction cavity are tightly attached.
In some embodiments of the present invention, preferably, the catalyst further comprises an auxiliary agent, preferably at least one selected from the group consisting of oxides of Sr, la, Y and Sm. More preferably, the content of the auxiliary agent is 1 to 8g, still more preferably 2 to 4g, based on 100g of the carrier.
In some embodiments of the invention, the active component is preferably at least one of an oxide of Li, an oxide of Na, an oxide of K, and an oxide of Rb.
In some embodiments of the invention, the active ingredient is present in an amount of 1 to 25g, preferably 3 to 20g, based on 100g of the carrier.
In some embodiments of the invention, the catalysts used are prepared by methods commercially available or using prior art techniques.
According to a preferred embodiment of the invention, the preparation method of the catalyst without auxiliary agent comprises the following steps: adding the precursor of the active component into deionized water, adding a carrier, stirring for 1-3 hours, then drying at 100-120 ℃ for 20-24 hours, and roasting at 700-750 ℃ for 4-6 hours to obtain the catalyst.
According to another preferred embodiment of the present invention, the method for preparing the catalyst with auxiliary agent comprises the following steps: adding the precursor of the active component into deionized water, adding a carrier, stirring for 1-3 hours, and then drying at 100-120 ℃ for 20-24 hours to obtain a solid A; then dissolving the precursor of the auxiliary agent in deionized water, adding the solid A, stirring for 1-3 hours, then drying for 20-24 hours at 100-120 ℃, and roasting for 4-6 hours at 700-750 ℃ to obtain the catalyst.
In a second aspect, the present invention provides a method for preparing a carbon dioxide by oxidative coupling of methane, the method comprising:
(1) Filling a reaction cavity of a reactor with a catalyst, wherein the reaction cavity is made of alumina, and the roughness of the inner surface of the reaction cavity is 0.5-1 micron;
the catalyst comprises a carrier and an active component loaded on the carrier, wherein the carrier is at least one of CaO, mgO and BaO; the active component is an oxide of alkali metal;
(2) Methane and oxygen are introduced into the alumina reaction cavity to contact with the catalyst for catalytic reaction.
In some embodiments of the invention, the roughness of the inner surface of the reaction chamber is preferably 0.6-0.8 microns.
In the present invention, the description of the structure of the reactor is not repeated here as described above.
In some embodiments of the present invention, preferably, the catalyst further comprises an auxiliary agent, preferably at least one selected from the group consisting of oxides of Sr, la, Y and Sm. More preferably, the content of the auxiliary agent is 1 to 8g, still more preferably 2 to 4g, based on 100g of the carrier.
In some embodiments of the invention, the active component is preferably at least one of an oxide of Li, an oxide of Na, an oxide of K, and an oxide of Rb.
In some embodiments of the invention, the active ingredient is present in an amount of 1 to 25g, preferably 3 to 20g, based on 100g of the carrier.
In some embodiments of the invention, the volume ratio of methane to oxygen is preferably 2-10:1, more preferably 2.2-4:1.
in some embodiments of the invention, the conditions of the catalytic reaction include: the reaction temperature is preferably 700 to 780 ℃, more preferably 700 to 750 ℃. The reaction pressure of the catalytic reaction is preferably 0.001-0.02MPa, and the reaction time of the catalytic reaction is preferably 0.5-20h. The reaction gas hourly space velocity in terms of methane and oxygen is preferably 5000 to 35000 mL/(g.h).
In the invention, the fillers at the two ends of the catalyst are inert materials, and the inert materials only play a role of supporting the catalyst and do not participate in the reaction. Preferably, the inert material is silica and/or alumina, the silica being derived from quartz sand.
In the present invention, the unit "mL/(g.h)" is the amount of the total gas of methane and oxygen (mL) used for 1 hour with respect to 1g of the catalyst.
In the present invention, the pressures refer to gauge pressure.
In the present invention, the carbon dioxide may be ethane and/or ethylene.
Will be hereinafter describedThe present invention will be described in detail with reference to examples. In both examples and comparative examples, the reagents used were commercially available analytically pure reagents. SiO (SiO) 2 From quartz sand, which was purchased from Qingdao ocean chemical Co. Alumina is purchased from world chemical filler limited. The method for measuring the element composition of the catalyst is an X-ray fluorescence method, and specific detection is referred to GB/T30905-2014.
Preparation example 1
The preparation method of the catalyst without the auxiliary agent comprises the following steps: the precursor of the active component was added to 50℃and 25g of deionized water, the carrier was added, stirred for 2 hours, dried at 120℃for 24 hours, and then calcined at 750℃for 6 hours, to obtain the catalyst used in the examples.
Preparation example 2
The preparation method of the catalyst with the auxiliary agent comprises the following steps: adding the precursor of the active component into deionized water with the temperature of 50 ℃ and the weight of 25g, adding a carrier, stirring for 2 hours, and drying at the temperature of 120 ℃ for 24 hours to obtain a solid A; then, the precursor of the auxiliary agent was dissolved in 50℃and 25g of deionized water, and solid A was added thereto, stirred for 2 hours, dried at 120℃for 24 hours, and then calcined at 750℃for 6 hours to obtain the catalyst used in the examples or comparative examples.
The precursors of the active components and the precursors of the auxiliary agents in the preparation examples are nitrate, and the use amount of each component is such that the content of the active components and the auxiliary agents in the catalyst is shown in table 1:
TABLE 1
Note that: the content of each component in the catalyst is the relative content calculated by taking 100g of carrier as a reference;
"/" indicates that no promoter is present in the catalyst.
Example 1
The reactor is alpha-Al with the inner diameter of 10mm and the length of 530mm 2 O 3 The catalyst loading of the reaction tube is 0.2g, the thickness of the reaction tube is 2mm, the roughness of the inner surface of the reaction tube is 0.6 micrometers, the reaction pressure is the pressure generated by the raw materials, namely 0.014MPa, and the reaction is carried outThe temperature was 750 ℃, and the volume ratio of methane to oxygen was 2.2:1, the reaction gas hourly space velocity in terms of methane and oxygen was 12000 mL/(g.h), and the reaction product was collected after 1 hour of reaction.
Example 2
The reactor is alpha-Al with the inner diameter of 12mm and the length of 530mm 2 O 3 The catalyst loading of the reaction tube is 0.2g, the thickness of the reaction tube is 3.5mm, the roughness of the inner surface of the reaction tube is 0.7 micron, the reaction pressure is the pressure generated by the raw materials, namely 0.006MPa, the reaction temperature is 700 ℃, and the volume ratio of methane to oxygen is 3:1, the reaction gas hourly space velocity based on methane and oxygen was 5000 mL/(g.h), and the reaction product was collected after 1 hour of reaction.
Example 3
The reactor is alpha-Al with the inner diameter of 10mm and the length of 530mm 2 O 3 The catalyst loading of the reaction tube is 0.2g, the thickness of the reaction tube is 2.5mm, the roughness of the inner surface of the reaction tube is 0.8 micron, the reaction pressure is the pressure generated by the raw materials, namely 0.018MPa, the reaction temperature is 780 ℃, and the volume ratio of methane to oxygen is 4:1, the reaction gas hourly space velocity in terms of methane and oxygen was 35000 mL/(g.h), and the reaction product was collected after 1 hour of reaction.
Example 4
The reactor is alpha-Al with the inner diameter of 10mm and the length of 530mm 2 O 3 The catalyst loading of the reaction tube is 0.2g, the thickness of the reaction tube is 2mm, the roughness of the inner surface of the reaction tube is 1 micron, the reaction pressure is the pressure generated by the raw materials, namely 0.009MPa, the reaction temperature is 780 ℃, and the volume ratio of methane to oxygen is 6:1, the reaction gas hourly space velocity based on methane and oxygen is 8000 mL/(g.h), and the reaction product is collected after 1 hour of reaction.
Example 5
The reactor is alpha-Al with the inner diameter of 10mm and the length of 530mm 2 O 3 The catalyst loading of the reaction tube is 0.2g, the thickness of the reaction tube is 2mm, the roughness of the inner surface of the reaction tube is 0.5 micron, the reaction pressure is the pressure generated by the raw material, namely 0.015MPa, the reaction temperature is 730 ℃, and the volume ratio of methane to oxygen is 10:1, the reaction gas hourly space velocity in terms of methane and oxygen was 15000 mL/(g.cndot.)h) The reaction product was collected after 1 hour of reaction.
Comparative example 1
The reaction for producing a carbon dioxide by oxidative coupling of methane was carried out in the same manner as in example 1, except that the material of the reactor was 314L stainless steel.
Comparative example 2
The oxidative coupling of methane to make carbon dioxide was performed as in example 1, except that the material of the reactor was quartz.
Comparative example 3
The oxidative coupling of methane to make carbon dioxide was performed as in example 1, except that the catalyst was replaced with the catalyst shown in comparative example 3 in table 1.
Comparative example 4
The oxidative coupling of methane to make carbon dioxide was performed as in example 1, except that the roughness of the inner surface of the reactor was 2.5 microns.
Comparative example 5
The reaction for producing a carbon dioxide by oxidative coupling of methane was carried out in the same manner as in comparative example 1, except that the catalyst of comparative example 3 was used.
Test example 1
The reaction product components obtained in the examples and comparative examples were tested on a gas chromatograph available from Agilent company under the model number 7890A. The product was assayed using a double detection channel three-valve four column system in which the FID detector was attached to an alumina column for CH analysis 4 、C 2 H 6 、C 2 H 4 、C 3 H 8 、C 3 H 6 、C 4 H 10 、C 4 H 8 、C n H m Isocompositions, TCD detector is mainly used for detecting CO and CO 2 、N 2 、O 2 、CH 4 。
The calculation method of methane conversion rate and the like is as follows:
methane conversion = amount of methane consumed by the reaction/initial amount of methane x 100%
Ethylene selectivity = amount of methane consumed by ethylene produced/total amount of methane consumed x 100%
Ethane selectivity = amount of methane consumed by ethane produced/total amount of methane consumed x 100%
Carbon dioxane selectivity = ethane selectivity + ethylene selectivity
CO x (CO+CO 2 ) Selectivity = CO and CO produced 2 Total methane consumption x 100% of total methane consumption
Yield of carbon diolefms = methane conversion x (ethane selectivity + ethylene selectivity)
The results obtained are shown in Table 2.
TABLE 2
| Numbering device | Methane conversion/% | Carbon Dihydrocarbon Selectivity/% | CO x Selectivity/% | Yield of carbon diolefms/% |
| Example 1 | 23.5 | 70.6 | 27.3 | 16.6 |
| Example 2 | 23.3 | 70.1 | 27.8 | 16.3 |
| Example 3 | 23 | 69.5 | 28.1 | 16 |
| Example 4 | 22.6 | 69.1 | 28.5 | 15.6 |
| Example 5 | 22.2 | 69 | 28.8 | 15.3 |
| Comparative example 1 | 12.4 | 43.5 | 52.5 | 5.4 |
| Comparative example 2 | 22.9 | 70 | 27.4 | 16 |
| Comparative example 3 | 17.8 | 51.8 | 45.2 | 9.2 |
| Comparative example 4 | 20.1 | 55.7 | 41.3 | 11.2 |
| Comparative example 5 | 16.9 | 41.2 | 54.6 | 7 |
As can be seen from the test results in Table 2, the selectivity of the carbon dioxide is higher, the yield of the carbon dioxide is higher, and the CO is higher in examples 1 to 5, compared with comparative example 1 x The selectivity is relatively low, which means that the deep oxidation of methane is inhibited and the occurrence of side reaction is reduced when methane oxidative coupling is carried out to prepare carbon dioxide by adopting the reactor of the invention. In example 1, the quartz tube used in comparative example 2 had a maximum temperature of about 1400℃in a short period of time, whereas the alumina tube of example 1 had a maximum use temperature of 1700 ℃. The methane oxidative coupling is a high-temperature strong exothermic reaction, the reaction temperature is generally higher than 750 ℃, the reaction heat is as high as 83kcal/mol, a significant hot zone exists in the reactor, and the bed temperature can be even increased to 1200 ℃, which is not bearable by a quartz reactor. In addition, compared with a quartz tube, the alumina reaction tube has high strength, high drop resistance, good stability and high temperature resistance. Thus, the alumina reaction tube is more suitable for large-scale use for the high-temperature strong exothermic reaction of methane oxidative coupling. The higher selectivity and higher yield of the carbon dioles of examples 1-5 relative to comparative examples 3-5 indicates that superior catalytic performance can be achieved only with this method for the particular catalyst.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (9)
1. A method for preparing a carbon dioxide by oxidative coupling of methane, the method comprising:
(1) Filling a reaction cavity of a reactor with a catalyst, wherein the reaction cavity is made of alumina, and the roughness of the inner surface of the reaction cavity is 0.5-1 micron;
the catalyst comprises a carrier and an active component loaded on the carrier, wherein the carrier is at least one of CaO, mgO and BaO; the active component is an oxide of alkali metal; the catalyst also contains an auxiliary agent, wherein the auxiliary agent is at least one selected from oxides of Sr, la, Y and Sm; the content of the auxiliary agent is 1-8g based on 100g of the carrier, and the content of the active component is 1-25g;
(2) Methane and oxygen are introduced into the alumina reaction cavity to contact with the catalyst for catalytic reaction.
2. The method of claim 1, wherein the roughness of the interior surface of the reaction chamber is 0.6-0.8 microns;
and/or the ratio of the thickness of the reaction cavity to the inner diameter of the reaction cavity is 0.2-0.3:1, a step of;
and/or the material of the reaction cavity is alpha-Al 2 O 3 ；
And/or the reactor further comprises a stainless steel support sleeve which is fixedly arranged along the outer wall of the reaction cavity in a surrounding manner.
3. The process according to claim 1, wherein the auxiliary is present in an amount of 2-4g based on 100g of the carrier.
4. The method of claim 1, wherein the active component is at least one of an oxide of Li, an oxide of Na, an oxide of K, and an oxide of Rb.
5. The method according to claim 1, wherein the active ingredient is contained in an amount of 3 to 20g based on 100g of the carrier.
6. The method of any of claims 1-5, wherein the volume ratio of methane to oxygen is from 2 to 10:1.
7. the method of any of claims 1-5, wherein the volume ratio of methane to oxygen is from 2.2 to 4:1.
8. the method of claim 1, wherein the conditions of the catalytic reaction comprise: the reaction temperature is 700-780 ℃, the reaction pressure is 0.001-0.02MPa, the reaction time is 0.5-20h, and the hourly space velocity of the reaction gas calculated by methane and oxygen is 5000-35000 mL/(g.h).
9. The method of claim 1, wherein the conditions of the catalytic reaction comprise: the reaction temperature is 700-750 ℃.
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