CN116060014A - Novel hydrocarbon steam conversion catalyst and preparation method and application thereof - Google Patents
Novel hydrocarbon steam conversion catalyst and preparation method and application thereof Download PDFInfo
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- CN116060014A CN116060014A CN202111275016.XA CN202111275016A CN116060014A CN 116060014 A CN116060014 A CN 116060014A CN 202111275016 A CN202111275016 A CN 202111275016A CN 116060014 A CN116060014 A CN 116060014A
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/32—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air
- C01B3/34—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents
- C01B3/38—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using catalysts
- C01B3/40—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using catalysts characterised by the catalyst
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Abstract
The invention belongs to the technical fields of petrochemical industry, natural gasification technology and catalyst manufacturing engineering, and particularly relates to a novel hydrocarbon steam conversion catalyst and a preparation method thereof. The novel hydrocarbon steam conversion catalyst of the invention adopts perovskite type active component, acid calcium cement and alpha-Al 2 O 3 The potassium, magnesium and nickel are prepared into active ingredients with stable perovskite structures, so that the potassium loss in the catalyst can be reduced; and by introducing a structural additive with a heat stabilization effect or loading the perovskite type metal oxide catalyst on a proper carrier, the dispersity of the catalyst can be increased, the heat stability of the catalyst can be improved, and the catalyst has good activity.
Description
Technical Field
The invention belongs to the technical fields of petrochemical industry, natural gasification technology and catalyst manufacturing engineering, and particularly relates to a novel hydrocarbon steam conversion catalyst and a preparation method thereof.
Background
The hydrocarbon steam conversion is a method for producing hydrogen and synthetic gas commonly adopted by the enterprises at home and abroad at present, wherein the light hydrocarbon steam conversion method adopts natural gas, liquefied petroleum gas, refinery gas or naphtha as raw materials. In the hydrocarbon steam conversion process, carbon formation in the hydrocarbon steam conversion process is a thermodynamic process which inevitably occurs under a certain water-carbon ratio, so that in order to prevent carbon deposition on the catalyst in the hydrocarbon steam conversion operation process, the catalyst is required to have strong carbon deposition resistance in addition to good activity, strength and stability.
At present, two main ways for solving the problem of carbon deposit resistance of the conversion catalyst at home and abroad are as follows: firstly, the low-temperature activity of the catalyst is improved as much as possible, and an alkaline carrier is adopted; and secondly, adding potassium salt, and promoting gasification and carbon removal reaction of carbon by means of potassium element. However, although the addition of the common potassium salt can improve the carbon deposit resistance of the catalyst, the potassium salt has the defect of easy loss, the loss of the potassium can reduce the stability of the catalyst to a certain extent, and the potassium is easy to gather in a waste boiler system after loss, corrode and scale to block the waste boiler system.
At present, perovskite type composite metal oxides (structural general formula ABO 3 ) The catalyst is a catalyst with great development potential, is commonly used as a catalytic combustion reaction and a photocatalytic material, and is not widely used as a hydrocarbon steam conversion reaction. However, the perovskite-type metal oxide catalyst has problems such as a low specific surface area and easy sintering at high temperature, although it has a good stability, and thus the perovskite-type catalyst has a certain limit in application.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to provide a hydrocarbon steam conversion catalyst which has the advantages of high carbon deposit resistance, strong potassium fixation capacity, good thermal stability and good activity;
the second technical problem to be solved by the invention is to provide a preparation method of the catalyst, which adopts a sol-gel method for pulping to load active component gel on alumina, and the active component gel is roasted to generate a perovskite structure, so that the active component is uniformly dispersed on an alumina carrier, and the comprehensive performance of the catalyst is effectively improved.
In order to solve the technical problems, the novel hydrocarbon steam conversion catalyst disclosed by the invention comprises the following components in percentage by mass:
35-45wt% of perovskite type active component;
15-25wt% of calcium aluminate cement;
α-Al 2 O 3 the balance;
the perovskite active component has a general formula K x Mg 1-x NiO 3 The structure shown, wherein x=0.1-0.2.
Specifically, the pore volume of the catalyst is 0.30-0.50mL/g, the bulk density is 0.85-0.95Kg/L, and the lateral pressure strength of the catalyst is more than 250N/particle.
Specifically, the appearance of the catalyst can be in the forms of four-hole columns, seven-hole columns, raschig rings, seven-rib wheels and the like.
The invention also discloses a method for preparing the novel hydrocarbon steam conversion catalyst, which comprises the following steps:
(1) Taking a selected amount of said alpha-Al 2 O 3 Adding citric acid, and adding water, and mixing to form liquid mixture;
(2) Adding potassium nitrate, magnesium nitrate and nickel nitrate according to the proportion of the selected perovskite type active component to prepare a solution for later use;
(3) Dripping the solution obtained in the step (2) into the liquid mixture obtained in the step (1), fully and uniformly mixing and heating to evaporate water so as to gradually change the water into gel;
(4) Drying and roasting the gel obtained in the step (3) to obtain a semi-finished catalyst product for later use;
(5) Pulverizing the obtained catalyst semi-finished product, adding a selected amount of calcium carbonate cement, uniformly mixing, continuously adding water, uniformly mixing, performing compression molding, and curing to obtain the catalyst.
Specifically, the molar ratio of the addition amount of the citric acid in the step (1) to the total amount of the nitrate in the step (2) is 1:2-4.
Specifically, in the step (4), the temperature of the drying step is 80-150 ℃.
Specifically, in the step (4), the temperature of the roasting step is 500-1000 ℃ and the roasting time is 4-8h. Preferably, the roasting temperature is 700-850 ℃, the roasting time is 5-10h, and the formation of perovskite as an active component is influenced by the temperature.
Specifically, in the step (5), the curing step is steam curing, and the curing time is 24-36h.
The invention also discloses application of the catalyst in a hydrocarbon steam conversion process.
In particular, the catalyst is suitable for converting carbon space velocity of 8000h at the inlet temperature of 430-600 ℃ and the outlet temperature of 700-850 ℃ of a reformer －1 The hydrocarbon steam converting process with water-carbon ratio of 1.2-3.5 and pressure of 2.0-4.0MPa is used in preparing hydrogen or synthetic gas. Under the conditions, the potassium loss rate of the catalyst is less than 3%.
The novel hydrocarbon steam conversion catalyst of the invention adopts perovskite type active component, acid calcium cement and alpha-Al 2 O 3 The potassium, magnesium and nickel are prepared into active ingredients with stable perovskite structures, so that the potassium loss in the catalyst can be reduced; and by introducing a structural additive with a heat stabilization effect or loading the perovskite type metal oxide catalyst on a proper carrier, the dispersity of the catalyst can be increased, the heat stability of the catalyst can be improved, and the catalyst has good activity.
The novel hydrocarbon steam conversion catalyst of the invention utilizes the conventional potassium element to prevent carbon deposit, on one hand, the potassium can catalyze C and H 2 The reaction between O accelerates the carbon elimination efficiency; on the other hand, potassium can also neutralize the acid centers of the catalyst, thereby slowing down the formation of char. The catalyst provided by the invention has the advantages that the potassium is alkaline after a proper amount of K content is added, so that the acid center of the catalyst is effectively neutralized, the gasification reaction of water vapor and carbon is effectively promoted, and the situation that the acid center of the catalyst is unfavorable for catalyzing higher hydrocarbon to carry out carbon chain cracking to CH due to the fact that the potassium content is high is effectively avoided x The conversion activity of the catalyst is effectively ensured in the process of free radicals. Meanwhile, the magnesium contained in the catalyst is alkaline and has stronger water absorption, so that the catalyst has a certain carbon precipitation resistance effect, and the addition of the magnesium can reduce the addition amount of the potassium in the catalyst, so that the moderate potassium content and better effect are ensured.
The catalyst of the invention has the advantages of strong potassium fixation capability, high carbon deposition resistance and high activity, and compared with the industrial catalyst, the catalyst can be used for preparing the catalyst with the system pressure of 3.0MPa and the carbon space velocity of 8000h -1 、H 2 The O/C (mol/mol) is 1.5, the temperature of the inlet of the bed layer is 430 ℃, the temperature of the outlet of the bed layer is 720 ℃, and the catalyst has better activity and stability.
Drawings
In order that the invention may be more readily understood, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings, in which,
FIG. 1 is an XRD pattern of a catalyst prepared in example 1 of the present invention;
FIG. 2 is a schematic flow chart of a small pressurized activity evaluation device for evaluating catalyst activity;
the reference numerals in the drawings are as follows: 1-oil metering pump, 2-water metering pump, 3-vaporizer, 4-mixer, 5-tube reactor, 6-condenser, 7-separator, 8-voltage stabilizer, 9-wet flowmeter.
Detailed Description
In order to enable those skilled in the art to more clearly understand the technical scheme of the present invention, the technical scheme of the present invention will be described in detail with reference to specific embodiments.
Example 1
The preparation method of the hydrocarbon steam reforming catalyst in the embodiment comprises the following steps:
(1) 192g of citric acid and 142.5g of alumina are weighed and added into 500mL of deionized water, and the mixture is uniformly mixed for standby; .
(2) Weighing 20.2g of potassium nitrate, 205.1g of magnesium nitrate and 290.7g of nickel nitrate, adding into 1000mL of deionized water, and fully and uniformly mixing to prepare a solution for later use;
(3) Dropwise adding the solution obtained in the step (2) into the liquid mixture obtained in the step (1) under stirring, and fully and uniformly mixing; then heating the obtained liquid mixture to raise the temperature to evaporate water so as to gradually change the liquid mixture into gel;
(4) Placing the formed gel into a drying oven, drying at 120 ℃, and then continuously placing into an electric furnace to bake for 6 hours at 750 ℃ to obtain a semi-finished catalyst;
(5) Crushing the semi-finished product obtained by roasting, adding 69.1g of calcium aluminate cement and a proper amount of water, uniformly mixing, performing compression molding, and performing steam curing for 24 hours to obtain the finished catalyst cat-1.
The active component of the catalyst is K 0.2 Mg 0.8 NiO 3 The XRD pattern is shown in figure 1.
Example 2
The preparation method of the hydrocarbon steam reforming catalyst in the embodiment comprises the following steps:
(1) Weighing 96g of citric acid and 102.5 g of aluminum oxide, adding into 500mL of deionized water, and uniformly mixing for later use;
(2) 10.1g of potassium nitrate, 230.8g of magnesium nitrate and 290.7g of nickel nitrate are weighed and added into 1000mL of deionized water to prepare a solution for later use;
(3) Dropwise adding the solution formed in the step (2) into the liquid mixture obtained in the step (1) under stirring, and fully and uniformly mixing; then heating the obtained liquid mixture to raise the temperature to evaporate water so as to gradually change the liquid mixture into gel;
(4) Placing the obtained gel into a drying oven, drying at 120 ℃, then placing into an electric furnace, and roasting at 800 ℃ for 8 hours to obtain a semi-finished catalyst;
(5) Pulverizing the above semi-finished catalyst, adding 58.6g calcium aluminate cement and appropriate amount of water, mixing, press molding, steam curing for 24 hr to obtain final catalyst cat-2, wherein the active component of the catalyst is K 0.1 Mg 0.9 NiO 3 。
Example 3
The preparation method of the hydrocarbon steam reforming catalyst in the embodiment comprises the following steps:
(1) 150g of citric acid and 169.5g of alumina are weighed and added into 500mL of deionized water, and the mixture is uniformly mixed for standby;
(2) 10.1g of potassium nitrate, 230.8g of magnesium nitrate and 290.7g of nickel nitrate are weighed and added into 1000mL of deionized water to prepare a solution for later use;
(3) Dropwise adding the solution obtained in the step (2) into the liquid mixture obtained in the step (1) under stirring, and fully and uniformly mixing; heating the obtained liquid mixture to raise the temperature and evaporate water so as to gradually change the liquid mixture into gel;
(4) Placing the obtained gel into a drying oven, drying at 120 ℃, then placing into an electric furnace, and roasting at 800 ℃ for 8 hours to obtain a semi-finished catalyst;
(5) Pulverizing the above semi-finished catalyst, adding 75.3g calcium aluminate cement and appropriate amount of water, mixing, press molding, steam curing for 24 hr to obtain final catalyst cat-3, wherein the active component of the catalyst is K 0.1 Mg 0.9 NiO 3 。
Example 4
The preparation method of the hydrocarbon steam reforming catalyst in the embodiment comprises the following steps:
(1) 135g of citric acid and 133g of alumina are weighed and added into 500mL of deionized water, and the mixture is uniformly mixed for standby;
(2) 15.2g of potassium nitrate, 217.9g of magnesium nitrate and 290.7g of nickel nitrate are weighed and added into 1000mL of deionized water to prepare a solution for later use;
(3) Dropwise adding the solution obtained in the step (2) into the liquid mixture obtained in the step (1) under stirring, and fully and uniformly mixing; then heating the obtained liquid mixture to raise the temperature to evaporate water so as to gradually change the liquid mixture into gel;
(4) Drying the gel in a drying oven at 120 ℃, and then roasting the gel in an electric furnace at 850 ℃ for 6 hours to obtain a semi-finished catalyst;
(5) Pulverizing the semi-finished catalyst obtained by roasting, adding 66.5g of calcium aluminate cement and a proper amount of water, uniformly mixing, pressing and forming, and curing for 24 hours by steam to obtain the finished catalyst cat-4, wherein the active component of the catalyst is K 0.15 Mg 0.85 NiO 3 。
Comparative example 1
The preparation method of the catalyst in the comparative example comprises the following steps:
(1) Weighing 192g of citric acid, and adding the citric acid into 500mL of deionized water for dissolution to obtain a citric acid solution for later use;
(2) Weighing 20.2g of potassium nitrate, 205.1g of magnesium nitrate and 290.7g of nickel nitrate, and adding into 1000mL of deionized water to prepare a solution for later use;
(3) Dropwise adding the solution obtained in the step (2) into the citric acid solution obtained in the step (1) under the stirring state, and fully and uniformly mixing; then heating the obtained solution to raise the temperature to evaporate water so as to gradually change the water into gel;
(4) Drying the obtained gel in a drying oven at 120 ℃, and then roasting the dried gel in an electric furnace at 750 ℃ for 6 hours to obtain a semi-finished catalyst;
(5) Pulverizing the semi-finished product of the catalyst obtained by roasting, adding 69.1g of calcium aluminate cement, 142.5g of alumina and a proper amount of water, uniformly mixing, pressing and forming, and curing for 24 hours by steam to obtain a comparative catalyst cat-5, wherein the active component of the catalyst is K 0.2 Mg 0.8 NiO 3 。
Comparative example 2
The comparative example compares the carbon conversion rate and the potassium loss rate of the industrial catalyst A, the chemical component NiO% (m/m) of the catalyst is more than or equal to 16, and the carbon deposition resistance of the catalyst is improved by directly adding kalioplast double salt.
Comparative example 3
The preparation method of the hydrocarbon steam conversion catalyst in the comparative example comprises the following steps:
(1) 192g of citric acid and 142.5g of alumina are weighed and added into 500mL of deionized water, and the mixture is uniformly mixed for standby; .
(2) 30.3g of potassium nitrate, 179.5g of magnesium nitrate and 290.7g of nickel nitrate are weighed and added into 1000mL of deionized water, and the mixture is fully and uniformly mixed to prepare a solution for standby;
(3) Dropwise adding the solution obtained in the step (2) into the liquid mixture obtained in the step (1) under stirring, and fully and uniformly mixing; then heating the obtained liquid mixture to raise the temperature to evaporate water so as to gradually change the liquid mixture into gel;
(4) Placing the formed gel into a drying oven, drying at 120 ℃, and then continuously placing into an electric furnace to bake for 6 hours at 750 ℃ to obtain a semi-finished catalyst;
(5) Crushing the semi-finished product obtained by roasting, adding 69.1g of calcium aluminate cement and a proper amount of water, uniformly mixing, performing compression molding, and performing steam curing for 24 hours to obtain the comparative catalyst cat-6.
The active component of the catalyst is K 0.3 Mg 0.7 NiO 3 。
Experimental example
In view of the complex characterization of the pressurizing activity of the hydrocarbon steam conversion catalyst and the balance of a plurality of data indexes, the invention adopts normal hexane as a raw material, selects the carbon conversion rate as a catalyst activity reference index, adopts a conventional device in the field for evaluating the catalyst activity, has a specific structure schematic diagram shown in figure 2, and uses the steps which are well known to the person skilled in the art.
The specific catalyst pressurization activity conditions are as follows:
catalyst particle size: 40-60 meshes;
catalyst loading: 45mL;
pressure: 3.0MPa;
carbon space velocity: 10000h -1 ；
H 2 O/C(mol/mol)：2.0；
Bed temperature: the inlet temperature is 480 ℃, and the outlet temperature is 700 ℃;
operating time: 100h;
carbon conversion= (conversion process gas CO content (%) + conversion process gas CO 2 Content (%))/total carbon of conversion process gas (%);
determination of potassium loss rate: weighing 40-50 mesh sample quantitatively, immersing with 200mL of water, heating and refluxing for boiling for 6h, and measuring the potassium content in the water by using a flame photometer.
The carbon content in the sample unloading at the outlet section of the catalyst bed layer is measured by a carbon-sulfur analyzer.
The results of the evaluation data of the catalysts are shown in Table 1 below.
Table 1 after 100h of pressure evaluation, evaluation and analysis data
As can be seen from the data in Table 1, the carbon conversion rate of the catalyst prepared by the method is equivalent to that of the industrial catalyst A, and after 100h evaluation, the potassium loss rate and the carbon content in sample unloading of the catalyst prepared by the method are both superior to those of the industrial catalyst A. The catalyst prepared by the invention has good carbon deposition resistance, potassium fixation and good activity, and can be used for industrial production.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (10)
1. A novel hydrocarbon steam reforming catalyst, characterized in that the catalyst comprises the following components in mass content, based on the total amount thereof:
35-45wt% of perovskite type active component;
15-25wt% of calcium aluminate cement;
α-Al 2 O 3 the balance;
the perovskite active component has a general formula K x Mg 1-x NiO 3 The structure shown, wherein x=0.1-0.2.
2. The novel hydrocarbon steam reforming catalyst of claim 1, wherein the catalyst has a pore volume of 0.30-0.50mL/g, a bulk density of 0.85-0.95Kg/L, and a catalyst side pressure strength of greater than 250N/particle.
3. The novel hydrocarbon steam reforming catalyst of claim 1 or 2, wherein the catalyst comprises a four-hole column, a seven-hole column, a raschig ring, a seven-tendon wheel.
4. A process for preparing the novel hydrocarbon steam reforming catalyst of any one of claims 1 to 3, comprising the steps of:
(1) Taking a selected amount of said alpha-Al 2 O 3 Adding citric acid, and adding water, and mixing to form liquid mixture;
(2) Adding potassium nitrate, magnesium nitrate and nickel nitrate according to the proportion of the selected perovskite type active component to prepare a solution for later use;
(3) Dripping the solution obtained in the step (2) into the liquid mixture obtained in the step (1), fully and uniformly mixing and heating to evaporate water so as to gradually change the water into gel;
(4) Drying and roasting the gel obtained in the step (3) to obtain a semi-finished catalyst product for later use;
(5) Pulverizing the obtained catalyst semi-finished product, adding a selected amount of calcium carbonate cement, uniformly mixing, continuously adding water, uniformly mixing, performing compression molding, and curing to obtain the catalyst.
5. The method for preparing a novel hydrocarbon vapor conversion catalyst according to claim 4, wherein the molar ratio of the amount of citric acid added in the step (1) to the total amount of nitrate in the step (2) is 1:2-4.
6. The method for producing a novel hydrocarbon vapor conversion catalyst according to claim 4 or 5, wherein in said step (4), the temperature of said drying step is 80 to 150 ℃.
7. The method for preparing a novel hydrocarbon steam reforming catalyst according to any one of claims 4 to 6, wherein in the step (4), the temperature of the calcination step is 500 to 1000 ℃ and the calcination time is 4 to 8 hours.
8. The method for preparing a novel hydrocarbon steam reforming catalyst according to any one of claims 4 to 7, wherein in the step (5), the curing step is steam curing, and the curing time is 24 to 36 hours.
9. Use of the catalyst of any one of claims 1-3 in a hydrocarbon steam reforming process.
10. The use according to claim 9, wherein the catalyst is suitable for converting carbon space velocity 8000h at a temperature of 430-600 ℃ at the inlet of the converter and 700-850 ℃ at the outlet －1 The hydrocarbon steam converting process with water-carbon ratio of 1.2-3.5 and pressure of 2.0-4.0MPa is used in preparing hydrogen or synthetic gas.
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