Preparation and reforming methods of catalyst for hydrogen production by reforming light alkane and application of catalyst

A technology for reforming hydrogen and low-carbon alkanes, applied in catalyst activation/preparation, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., can solve environmental pollution and other problems, and achieve simple treatment methods , improve the utilization rate, and have good application prospects

Pending Publication Date: 2021-01-29

KUNMING UNIV OF SCI & TECH

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Problems solved by technology

[0004] The object of the present invention is to address the shortcomings of the prior art described above, to provide a method for preparing a catalyst for hydrogen production by reforming low-carbon alkane; to modify and improve the sulfur resistance of the catalyst from the perspective of resou...

Method used

A kind of catalytic reforming prepares the method for hydrogen and carbon monoxide, the catalyst obtained is used for low-carbon alkane and carbon dioxide catalytic reforming in sulfur-containing gas, and its reaction condition is: total flow velocity is 55cm / min, CH , CO The concentrations of H2S and H2S are respectively 30vol%, 30vol% and 100ppm; under the reaction condition of 700°C, the catalyst dosage is 0.2g. Start the rea...

Abstract

The invention discloses preparation and reforming methods of a catalyst for hydrogen production by reforming light alkane and application of the catalyst. The preparation method comprises the following steps: preparing Ni/SiO2 from Ni (NH3) 6Cl2. 6H2O, and then adding the Ni/SiO2 into an aqueous solution of (NH4) 6Mo7O24. 4H2O to obtain the catalyst. The invention further discloses a method for preparing hydrogen and carbon monoxide through catalytic reforming of light alkane and carbon dioxide. The preparation method has the beneficial effects that the sulfur resistance of the catalyst can beenhanced; the treatment method is simple; important energy and environmental protection significance is realized; and the catalyst is used for hydrogen production by reforming light alkane in a sulfur-containing atmosphere and catalytically reforms the light alkane and carbon dioxide in the sulfur-containing atmosphere, the conversion rate of the light alkane and the carbon dioxide can reach 90%or above, the sulfur resistance can be enhanced by one time or above, and the catalyst has a good application prospect.

Application Domain

HydrogenCarburetting gases +5

Technology Topic

Carbon dioxide lowAlkane +7

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Examples

Experimental program(6)

Example Embodiment

[0033]Example 1

[0034]A method for preparing a catalyst for reforming low-carbon alkane to hydrogen, which comprises the following steps:

[0035](1) Use a 40-mesh sieve to screen the microsphere silica gel to make its particle size uniform; put the selected microsphere silica gel into a 34% nitric acid solution and soak for 9 hours; the obtained microsphere silica gel is washed with deionized water Put it in an oven at 110℃ to dry for 12h, roast in a muffle furnace at 550℃ for 3h, and cool to room temperature to get SiO2Carrier

[0036](2) Add 0.91g Ni(NH3)6Cl2·6H2Dissolve O in 3.5ml deionized water, adjust the pH to 11 with ammonia, then add 2g SiO2The carrier is stirred for 5 minutes and then sonicated at 41kHz for 10 minutes, then placed in a 110°C oven for 12 hours after standing for 9 hours, and then placed in a muffle furnace at 550°C for 3 hours and cooled to room temperature to obtain the catalyst Ni/SiO2;

[0037](3) 0.46g (NH4)6Mo7O24·4H2O is dissolved in 3.5ml deionized water, and then added to Ni/SiO obtained in (2)2, After stirring for 5 minutes, ultrasonic at 41kHz for 10 minutes, then let it stand for 10 hours and put it in a 110 ℃ oven for 12 hours, then put it in a 550 ℃ muffle furnace and roast for 3 hours and cool to room temperature to obtain the catalyst NiMo/SiO2；And the catalyst NiMo/SiO2Perform XRD characterization and see the resultsfigure 1 (Fresh), the XRD pattern of the sample shows that the main components in the sample are NiO and MoO3.

[0038]A method for preparing hydrogen and carbon monoxide by catalytic reforming. The catalyst obtained in (3) is used for the catalytic reforming of low-carbon alkanes and carbon dioxide in sulfur-containing gas. The reaction conditions included are as follows: the total flow rate is 50 cm3/min, CH4, CO2And H2The concentration of S is 30 vol%, 30 vol% and 100 ppm, respectively; under the reaction conditions of 700° C., the amount of catalyst is 0.4 g. The reaction starts after the gas is evenly mixed, and samples are taken every 20 minutes (total reaction time is 240 minutes). Measure CH with gas chromatography instruments FID, TCD, FPD4, CO2, H2S, H2And the concentration of CO and calculate its conversion rate, etc., the results are asFigure 2-4(Fresh) shows that compared with the catalysts in other examples, the initial catalytic reaction activity of this sample is 81%, and the activity drops to half within 80 minutes, which is poor in stability and poor in effect.

Example Embodiment

[0039]Example 2

[0040]A method for preparing a catalyst for reforming low-carbon alkane to hydrogen, which comprises the following steps:

[0041](1) Use a 60-mesh sieve to screen the microsphere silica gel to make it uniform in particle size; put the screened microsphere silica gel into a 34% nitric acid solution and soak for 9 hours; the obtained microsphere silica gel is washed with deionized water Put it in an oven at 180℃ to dry for 12h, roast in a muffle furnace at 500℃ for 3h, and cool to room temperature to get SiO2Carrier

[0042](2) Add 0.91g Ni(NH3)6Cl2·6H2Dissolve O in 3.5ml deionized water, adjust the PH to 10 with ammonia, then add 2g SiO2The carrier is stirred for 5 minutes and then sonicated at 50kHz for 8 minutes, then placed in an oven at 120°C for 10 hours after standing for 9 hours, and then baked in a muffle furnace at 500°C for 2 hours and cooled to room temperature to obtain the catalyst Ni/SiO2;

[0043](3) 0.46g (NH4)6Mo7O24·4H2O is dissolved in 3.5ml deionized water, and then added to Ni/SiO obtained in (2)2After stirring for 5min, ultrasonic for 10min, then let it stand for 8h, then put it in a 130℃ oven to dry for 12h, then put it in a 500℃ muffle furnace and roast it for 3h and cool to room temperature to get the catalyst NiMo/SiO2.

[0044]The newly prepared catalyst NiMo/SiO2Carry out activation treatment, the steps involved in activation treatment are as follows: The catalyst NiMo/SiO2Placed in a fixed-bed reactor, continuously pass 10% H2Under /Ar condition, the temperature is raised from 30°C to 700°C and stays for 1h (the temperature rise is 10°C/min) for reduction. The reduced material was characterized by XRD, and the results are shown in the attachmentfigure 1 (30-700), the XRD pattern of the sample shows that the main components in the sample are Ni and Ni3Mo, with a small amount of Ni3Mo exists, but compared with the catalysts in Examples 3 and 4, its Ni3Mo and Ni3The crystal phase difference of Mo is not obvious.

[0045]A method for preparing hydrogen and carbon monoxide by catalytic reforming. The obtained catalyst is used for the catalytic reforming of low-carbon alkanes and carbon dioxide in sulfur-containing gas. The reaction conditions are: the total flow rate is 50 cm3/min, CH4, CO2And H2The concentration of S is 30 vol%, 30 vol% and 100 ppm, respectively; under the reaction conditions of 700° C., the amount of catalyst is 0.2 g. The reaction starts after the gas is evenly mixed, and samples are taken every 20 minutes (total reaction time is 240 minutes). Measure CH with gas chromatography instruments FID, TCD, FPD4, CO2, H2S, H2And the concentration of CO and calculate its conversion rate, etc. The results are asFigure 2-4As shown (30-700), compared with Example 1, the initial activity of the catalytic reaction is 85%, and it takes more than 100 minutes to reduce the activity to half, and the stability is improved.

Example Embodiment

[0046]Example 3

[0047]A method for preparing a catalyst for reforming low-carbon alkane to hydrogen, which comprises the following steps:

[0048](1) Use a 50-mesh sieve to screen the microsphere silica gel to make it uniform in particle size; put the selected microsphere silica gel into a 34% nitric acid solution and soak for 9 hours; the obtained microsphere silica gel is washed with deionized water Put it in an oven at 110℃ to dry for 12h, roast in a muffle furnace at 550℃ for 3h, and cool to room temperature to get SiO2Carrier

[0049](2) Add 0.91g Ni(NH3)6Cl2·6H2Dissolve O in 3.5ml deionized water, adjust the pH to 11 with ammonia, then add 2g SiO2The carrier is stirred for 5 minutes and then sonicated at 50kHz for 10 minutes, then placed in a 110°C oven for 12 hours after standing for 9 hours, and then placed in a 550°C muffle furnace for roasting for 3 hours and cooling to room temperature to obtain the catalyst Ni/SiO2;

[0050](3) 0.46g (NH4)6Mo7O24·4H2O is dissolved in 3.5ml deionized water, and then added to Ni/SiO obtained in (2)2After stirring for 5min, 40kHz ultrasonic for 10min, then standing for 8h, drying in 110℃ oven for 12h, then roasting in 550℃ muffle furnace for 3h and cooling to room temperature to obtain the catalyst NiMo/SiO2.

[0051]The newly prepared catalyst NiMo/SiO2Carry out activation treatment, the steps involved in activation treatment are as follows: NiMo/SiO2Placed in a fixed-bed reactor, continuously pass 10% H2Under /Ar conditions, the temperature is increased from 30°C to 400°C for 30 minutes for deep steady-state reduction, and then the temperature is increased to 700°C for 1 hour (10°C/min) for final reduction, and the material is characterized by XRD. The results are shown in the attachmentfigure 1 (30-400-700), the XRD pattern of the sample shows that the main components in the sample are Ni and Ni3Mo, with a small amount of Ni3Mo exists, compared with the catalysts in Example 2 and Example 4, its Ni3Mo and Ni3Mo has the best crystal phase, which is very obvious.

[0052]A method for preparing hydrogen and carbon monoxide by catalytic reforming. The obtained catalyst is used in the catalytic reforming of low-carbon alkanes and carbon dioxide in a sulfur-containing gas. The reaction conditions are as follows: a total flow rate of 55 cm3/min, CH4, CO2And H2The concentration of S is 30 vol%, 30 vol% and 100 ppm, respectively; under the reaction conditions of 700° C., the amount of catalyst is 0.2 g. The reaction starts after the gas is evenly mixed, and samples are taken every 20 minutes (total reaction time is 240 minutes). Use gas chromatograph FID, TCD, FPD to measure CH4, CO2, H2S, H2And the concentration of CO and calculate its conversion rate, etc. The results are asFigure 2-4As shown ((30-400-700), the initial catalytic reaction activity of the catalyst is 90%, and the stability is the best.

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Classification and recommendation of technical efficacy words

increase profit
Improve sulfur resistance

Preparation and reforming methods of catalyst for hydrogen production by reforming light alkane and application of catalyst

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Method used

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