CN104178221A - Catalytic coal gasification catalyst dispersion method - Google Patents
Catalytic coal gasification catalyst dispersion method Download PDFInfo
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- CN104178221A CN104178221A CN201310195949.7A CN201310195949A CN104178221A CN 104178221 A CN104178221 A CN 104178221A CN 201310195949 A CN201310195949 A CN 201310195949A CN 104178221 A CN104178221 A CN 104178221A
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- coal
- catalyzer
- catalytic
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Abstract
The invention discloses a preparation process for rapid dispersion of a catalyst on a coal based material, and provides a simple and efficient method for the preparation of a catalytic coal gasification catalyst. According to the method, rapid distribution of the catalytic coal gasification catalyst on the coal based material by ultrasonic assisted technology. The preparation process is applied in a catalytic coal gasification fixed bed reactor, and compared with a routine method for production of the catalytic coal gasification catalyst, the preparation process can not only shorten the time of preparing the catalyst, but also can greatly improve the gasification efficiency of the coal based material and increase the methane production, and can improve the clean and efficient use of the coal based material.
Description
Technical field
The invention belongs to chemical technology field, specifically, proposed a kind of dispersing method of catalytic coal gasifaction catalyzer of simple and efficient.
Background technology
Coal be plant remains in suitable geologic media, pile up gradually and reach certain thickness, and covered by water or silt, passed through very long geological age, experienced physics, chemistry and biological complexing action, and the organic-biological rock forming gradually.The hyle complexity that generates coal is various, the external conditions that generates coal was had nothing in common with each other with the historical age that generates coal, caused coal when thering are some general character, with general mineral facies ratio, at aspects such as mineralogy and petrography, basic Physical and chemical characteristics, have more the diversity of kind and the complicacy of structure.
The energy structure feature of China is that the many gas of coal is few, coal plays an important role to the development of Chinese national economy, but the raising along with expanding economy and living standards of the people, coal is directly as fuel, not only efficiency is low, and the gas of discharge has increased PM2.5 content in air, causes environment to be endangered.Utilize Coal Gasification Technology, it is a kind of important channel that coal clean and effective utilizes that coal is converted into geseous fuel.Utilize Coal Gasification Technology to change coal into synthetic gas, recycling synthetic gas is produced the multiple important Chemicals such as ammonia, methyl alcohol.The Coal Gasification Technology of the Coal Gasification Technology of suitability for industrialized production for not adding catalyzer.Only have when gasification temperature is during at 1100-1700 ℃, gasification reaction speed just can reach suitability for industrialized production demand.But gasification temperature is higher, need to consume more coal and maintain high-temperature gasification state, and the temperature of working off one's feeling vent one's spleen is higher, increased the power loss of temperature-fall period.So relatively traditional gasification, catalytic coal gasifaction has many advantages, and its major cause is, under the effect of catalyzer, can significantly reduce gasification temperature, keep carrying out at a lower temperature, can also regulate gas composition, be referred to as third generation Coal Gasification Technology simultaneously.
Sonochemistry is utilize ultrasonic energy to accelerate and control chemical reaction, improves a frontier branch of science of the new chemical reaction of reaction yield and initiation.Ultrasonication comes from ultrasonic " cavitation ".For solid-liquid nonhomogeneous system, the kern oscillation that cavitation produces, microjet can impact fluids, show as the strong mutual collision of Hydrodynamic turbulence and particle, be conducive to the diffusion of component in micropore (J. Am. Chem. Soc., 1983,60:1494).Ultrasonic wave, for the preparation process of catalyzer, can be increased to the perviousness of active ingredient, make it dispersed, resulting catalyzer has that active specy is uniformly dispersed and active high premium properties (J. Mol. Catal., 1981,1:253).
Salt of basic metal, alkaline-earth metal, transition metal (Fe, Co, Ni) and composition thereof has significant facilitation effect to catalytic coal gasifaction.These catalyzer mostly are solid particulate, accelerate the carrying out of gasification reaction, so the hybrid mode of catalyzer and coal have a significant impact by being distributed in coal grain surface to the effect of catalytic coal gasifaction.Conventional hybrid mode has mechanically mixing and pickling process to mix.Although mechanically mixing operates simple and easy, because the bonding force of mixing between inhomogeneous and catalyzer and coal dust is not strong, result has affected catalytic effect; Although mixing, pickling process can make to a certain extent catalyst component be distributed in preferably on coal-based material, but preparing the consuming time and dispersion effect of catalyst component on coal-based material neither be too desirable, and this has also restricted the raising of catalytic activity to a certain extent.Therefore, the limitation existing in catalyst preparation process for current catalytic coal gasifaction, develop catalyst component has good dispersion effect and preparation process novel process not consuming time on coal-based material, has important theoretical significance and actual application value.
Summary of the invention
The present invention exists catalyst component can not effectively be scattered on coal-based material and prepares the shortcomings such as consuming time according to existing catalytic coal gasifaction catalyst preparation process, provide a kind of utilize ultrasonic technology by catalyst component simple and fast be distributed on coal-based material, greatly accelerate the process of sample preparation, and avoided conventional mechanical method and the pickling process can not be equably by the problem of effectively mixing between catalyzer and coal-based material.At fixed-bed reactor, carry out in catalytic coal gasification, active result shows to utilize catalyst preparation process provided by the present invention, and this catalyzer shows more excellent catalytic effect.
The catalytic coal gasifaction method for preparing catalyst of simple and efficient of the present invention, it is characterized in that the ultrasonic energy that utilizes ultrasonic emitting to go out, act on and contain on catalyzer and coal-based material, the particle diameter of this mixture is 40 order-80 orders, the loading of active ingredient is metal quality and coal-based quality of materials ratio, and loading is 6%-30%.
Usually, preparation method of the present invention is: coal-based material, catalyzer, water are mixed, utilize ultrasonic emitting to go out energy in this mixture, then carry out drying treatment, after compressing tablet, fragmentation is sieved.
Said method comprising the steps of: coal-based material and catalyzer are placed in to distilled water, after being 50 KHz ul-trasonic irradiations, carry out drying treatment by fixed frequency, after compressing tablet, fragmentation is screened to 40 order-80 orders.
Described ultrasonic power is 40 W-120 W preferably.
The described ul-trasonic irradiation time is 40 min-100 min preferably.
Described coal-based material is brown coal, bituminous coal, coke, refinery coke or hard coal.
The loading of described active ingredient is metal quality and coal-based quality of materials ratio, and preferably loading is 10%-25%.
Described catalyzer is K
2cO
3, Na
2cO
3, CaCO
3, Ca (OH)
2, Fe (NO
3)
3.9H
2a kind of, two or more combination in O, KOH, NaOH, NaAc.
A kind of typical laboratory of the present invention preparation process is as follows:
Take 0.2-10 g K
2cO
3be placed in beaker, measure 20-200 ml distilled water, distilled water is added drop-wise to and fills K
2cO
3beaker in, stir it dissolved, then take the accurate eastern coal of 0.5-50 g, joined K
2cO
3the aqueous solution in, then this beaker is placed in to the ultrasonic generator that fixed frequency is 50 kHz, at power, be to act on certain hour under 20 W-200 W, preferred 40 W-120 W.The ul-trasonic irradiation time is at 20 min-120 min, preferably 40 min-100 min.Go in baking oven and carry out drying treatment, after compressing tablet, fragmentation is screened to 40 order-80 orders.
The significant advantage that the present invention presents shows as: the ultrasonic wave dispersion technology that the present invention improves can by catalytic coal gasifaction catalyst activity component simple and fast be distributed on coal-based material, the active ingredient of catalyzer is penetrated in the hole of coal-based material rapidly, and can be uniformly distributed, overcome conventional preparation technology consuming time and disperse the shortcomings such as inhomogeneous, catalyzer and coal-based material have stronger interaction force.The catalyzer that utilizes preparation technology provided by the present invention to prepare applies in the reaction of fixed bed coal catalytic gasification preparing natural gas, result shows the gasification temperature that has effectively reduced coal-based material, increased the gasification efficiency of coal-based material, in addition, within the identical time, utilize technology of preparing provided by the invention, the semi-invariant of methane is higher than the methane content in conventional preparation technology.This is conducive to simplify the SNG process of back segment operation, so this has met the demand that people utilize the clean and effective of coal resources to a certain extent, has accelerated the paces of the industrial application of China's catalytic coal gasifaction preparing natural gas technology.
Embodiment
Below in conjunction with specific embodiment, the present invention is set forth.But, should be understood that these embodiment only do not form limitation of the scope of the invention for the present invention is described.
embodiment 1: CS-K
2cO
3the catalytic performance of accurate eastern catalytic coal gasifaction on catalyzer
Take 0.177 g K
2cO
3, be transferred in beaker, then with graduated cylinder, measure 20 ml distilled water, and measured distilled water is added drop-wise in above-mentioned beaker, with glass stick, stir it is fully dissolved, then take the accurate eastern coal of 0.5 g, then added in beaker, then this beaker is placed in to the ultrasonic generator that fixed frequency is 50 kHz, power is 60 W, and be 50 min action time, finally this beaker is gone to and in baking oven, carries out drying treatment, after compressing tablet, fragmentation is screened to 40 order-80 orders, and catalyzer is labeled as CS-K
2cO
3.
Catalytic coal gasification condition: distilled water flow 1.0 ml/min, temperature of reaction 973 K, reaction system pressure 3.4 MPa.Efficiency of carbon conversion curve and CH over time on this catalyzer
4the accumulation amount of separating out sees attached list 1.
embodiment 2: K
2cO
3the catalytic performance of accurate eastern catalytic coal gasifaction on catalyzer
Take 0.177 g K
2cO
3be transferred in beaker, then with graduated cylinder, measure 20 ml distilled water, and measured distilled water is added drop-wise in above-mentioned beaker, with glass stick, stir it is fully dissolved, take again the accurate eastern coal of 0.5 g, then added in beaker, be then placed on magnetic stirring apparatus and stir, churning time is 6 h, finally this beaker is gone in baking oven and carry out drying treatment, after compressing tablet, fragmentation is screened to 40 order-80 orders, and catalyzer is labeled as K
2cO
3.
Catalytic coal gasification condition: distilled water flow 1.0 ml/min, temperature of reaction 973 K, reaction system pressure 3.4 MPa.Efficiency of carbon conversion curve and CH over time on this catalyzer
4the accumulation amount of separating out is respectively in Table 1.
embodiment 3: CS-Ca (OH)
2the catalytic performance of accurate eastern catalytic coal gasifaction on catalyzer
Take 0.185 g Ca (OH)
2, be transferred in beaker, then with graduated cylinder, measure 40 ml distilled water, and measured distilled water is added drop-wise in above-mentioned beaker, with glass stick, stir for some time, then take the accurate eastern coal of 0.5 g, then added in beaker, then this beaker is placed in to the ultrasonic generator that fixed frequency is 50 kHz, power is 80 W, and be 40 min action time, finally this beaker is gone to and in baking oven, carries out drying treatment, after compressing tablet, fragmentation is screened to 40 order-80 orders, and catalyzer is labeled as CS-Ca (OH)
2.
Catalytic coal gasification condition: distilled water flow 1.0 ml/min, temperature of reaction 973 K, reaction system pressure 3.4 MPa.Efficiency of carbon conversion curve and CH over time on this catalyzer
4the accumulation amount of separating out is respectively in Table 2.
embodiment 4: Ca (OH)
2the catalytic performance of accurate eastern catalytic coal gasifaction on catalyzer
Take 0.185 g Ca (OH)
2be transferred in beaker, then with graduated cylinder, measure 40 ml distilled water, and measured distilled water is added drop-wise in above-mentioned beaker, with glass stick, stir for some time, take again the accurate eastern coal of 0.5 g, then added in beaker, be then placed on magnetic stirring apparatus and stir, churning time is 6 h, finally this beaker is gone in baking oven and carry out drying treatment, after compressing tablet, fragmentation is screened to 40 order-80 orders, and catalyzer is labeled as Ca (OH)
2.
Catalytic coal gasification condition: distilled water flow 1.0 ml/min, temperature of reaction 973 K, reaction system pressure 3.4 MPa.Efficiency of carbon conversion curve and CH over time on this catalyzer
4the accumulation amount of separating out is respectively in Table 2.
embodiment 5: CS-Na
2cO
3the catalytic performance of Shengli coal catalytic gasification on catalyzer
Take 0.4 g Na
2cO
3, be transferred in beaker, then with graduated cylinder, measure 30 ml distilled water, and measured distilled water is added drop-wise in above-mentioned beaker, with glass stick, stir it is fully dissolved, then take 2.5 g Shengli coals, then added in beaker, then this beaker is placed in to the ultrasonic generator that fixed frequency is 50 kHz, power is 80 W, and be 30 min action time, finally this beaker is gone to and in baking oven, carries out drying treatment, after compressing tablet, fragmentation is screened to 40 order-80 orders, and catalyzer is labeled as CS-Na
2cO
3.
Catalytic coal gasification condition: distilled water flow 1.0 ml/min, temperature of reaction 973 K, reaction system pressure 3.4 MPa.
embodiment 6: Na
2cO
3the catalytic performance of Shengli coal catalytic gasification on catalyzer
Take 0.4 g Na
2cO
3be transferred in beaker, then with graduated cylinder, measure 40 ml distilled water, and measured distilled water is added drop-wise in above-mentioned beaker, with glass stick, stir for some time, take again 2.5 g Shengli coals, then added in beaker, be then placed on magnetic stirring apparatus and stir, churning time is 6 h, finally this beaker is gone in baking oven and carry out drying treatment, after compressing tablet, fragmentation is screened to 40 order-80 orders, and catalyzer is labeled as Na
2cO
3.
Catalytic coal gasification condition: distilled water flow 1.0 ml/min, temperature of reaction 973 K, reaction system pressure 3.4 MPa.
embodiment 7: CS-Fe (NO
3)
3the catalytic performance of Shengli coal catalytic gasification on catalyzer
Take 0.8 g Fe (NO
3)
3.9H
2o, is transferred in beaker, then with graduated cylinder, measures 30 ml distilled water, and measured distilled water is added drop-wise in above-mentioned beaker, with glass stick, stir it is fully dissolved, then take 2.5 g Shengli coals, then added in beaker, then this beaker is placed in to the ultrasonic generator that fixed frequency is 50 kHz, power is 20 W, and be 30 min action time, finally this beaker is gone to and in baking oven, carries out drying treatment, after compressing tablet, fragmentation is screened to 40 order-80 orders, and catalyzer is labeled as CS-Fe (NO
3)
3.
Catalytic coal gasification condition: distilled water flow 1.0 ml/min, temperature of reaction 973 K, reaction system pressure 3.4 MPa.
embodiment 8: Fe (NO
3)
3the catalytic performance of Shengli coal catalytic gasification on catalyzer
Take 0.8 g Fe (NO
3)
3.9H
2o, be transferred in beaker, then with graduated cylinder, measure 40 ml distilled water, and measured distilled water is added drop-wise in above-mentioned beaker, with glass stick, stir for some time, take again 2.5 g Shengli coals, then added in beaker, be then placed on magnetic stirring apparatus and stir, churning time is 6 h, finally this beaker is gone in baking oven and carry out drying treatment, after compressing tablet, fragmentation is screened to 40 order-80 orders, and catalyzer is labeled as Fe (NO
3)
3.
Catalytic coal gasification condition: distilled water flow 1.0 ml/min, temperature of reaction 973 K, reaction system pressure 3.4 MPa.
Table 1, CS-K
2cO
3and K
2cO
3on catalyzer, the interior carbon of different time changes transformation efficiency and the methane accumulation growing amount of gas-phase product into
Table 2, CS-Ca (OH)
2and Ca (OH)
2on catalyzer, the interior carbon of different time changes transformation efficiency and the methane accumulation growing amount of gas-phase product into
From table 1, CS-K
2cO
3on catalyzer, when reaction proceeds to 50 minutes, the transformation efficiency that the carbon on this catalyzer changes gas-phase product into is 12.4%, and within the same reaction times, K
2cO
3the transformation efficiency that carbon on catalyzer changes gas-phase product into is only 3.1%, along with reaction passing in time, CS-K in the time of 200 minutes
2cO
3the transformation efficiency that on catalyzer, carbon changes gas-phase product into has reached 45%, and within the same time K
2cO
3the transformation efficiency that carbon on catalyzer changes gas-phase product into is only 13.2%; According to the methane content shown in table 1, CS-K in 200 minutes
2cO
3cumulative methane amount on catalyzer has reached 2.0 mmol g (C)
-1, this result is K under the same time
2cO
33.8 times of catalyzer.
Equally according to shown in table 2, the CS-Ca being prepared by ultrasonic technique (OH)
2catalyzer is when carrying out 100 minutes gasification reactions, and on this catalyzer, to change the transformation efficiency of gas-phase product into be 14.1% to carbon, and this result is Ca (OH) prepared by conventional method
21.8 times of catalyzer, when proceeding to 250 minutes, CS-Ca (OH)
2the transformation efficiency that on catalyzer, carbon changes gas-phase product into has reached 41.7%, far above Ca (OH)
2on catalyzer 19.7%; Growing amount based on methane compares in addition, at 100 minutes in 250 minutes, CS-Ca (OH)
2on catalyzer, the semi-invariant of methane is by 1.1 mmol g
-1be increased to 2.22 mmol g
-1, increased by 1.12 mmol g
-1, and Ca (OH)
2on catalyzer, the semi-invariant of methane is only by 0.62 mmol g
-1be increased to 1.23 mmol g
-1, only increased by 0.61 mmol g
-1.
By the above results, show, in catalytic coal gasifaction field, utilize the technology of the present invention not only can reach the gasification efficiency that improves carbon, but also can obtain preferably methane content, the present invention simultaneously can also effectively shorten catalyzer preparation time, demonstrates good using value.
Claims (9)
1. the dispersing method of a catalytic coal gasifaction catalyzer, it is characterized in that the ultrasonic energy that utilizes ultrasonic emitting to go out, catalyzer is incorporated on coal-based material, and the particle diameter of the coal-based material after processing is 40 order-80 orders, and metal quality is 6%-30% with coal-based quality of materials ratio.
2. dispersing method according to claim 1, is characterized in that said method comprising the steps of: coal-based material, catalyzer, water are mixed, utilize ultrasonic emitting to go out energy in this mixture, then carry out drying treatment, after compressing tablet, fragmentation is sieved.
3. dispersing method according to claim 1 and 2, is characterized in that ultrasonic power is at 20 W-200 W.
4. preparation method according to claim 3, is characterized in that ultrasonic power is at 40 W-120 W.
5. dispersing method according to claim 1 and 2, is characterized in that the ul-trasonic irradiation time is at 20 min-120 min.
6. according to right, want the dispersing method described in 5, it is characterized in that the ul-trasonic irradiation time is at 40 min-100 min.
7. dispersing method according to claim 1 and 2, is characterized in that coal-based material is brown coal, bituminous coal, coke, refinery coke or hard coal.
8. dispersing method according to claim 1, is characterized in that metal quality and coal-based quality of materials than being 10%-25%.
9. dispersing method according to claim 1 and 2, is characterized in that catalyzer is K
2cO
3, Na
2cO
3, CaCO
3, Ca (OH)
2, Fe (NO
3)
3.9H
2one or more in O, KOH, NaOH, NaAc.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106311339A (en) * | 2015-06-19 | 2017-01-11 | 中国石油化工股份有限公司 | Catalyst used for coal hydrogenation catalytic gasification, and preparation method and use thereof |
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| CN102272267A (en) * | 2008-12-30 | 2011-12-07 | 格雷特波因特能源公司 | Processes for preparing a catalyzed carbonaceous particulate |
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2013
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Patent Citations (5)
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| US4200439A (en) * | 1977-12-19 | 1980-04-29 | Exxon Research & Engineering Co. | Gasification process using ion-exchanged coal |
| US4848983A (en) * | 1986-10-09 | 1989-07-18 | Tohoku University | Catalytic coal gasification by utilizing chlorides |
| CN101795761A (en) * | 2007-08-02 | 2010-08-04 | 格雷特波因特能源公司 | Catalyst-loaded coal compositions, methods of making and use |
| CN102272267A (en) * | 2008-12-30 | 2011-12-07 | 格雷特波因特能源公司 | Processes for preparing a catalyzed carbonaceous particulate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106311339A (en) * | 2015-06-19 | 2017-01-11 | 中国石油化工股份有限公司 | Catalyst used for coal hydrogenation catalytic gasification, and preparation method and use thereof |
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Application publication date: 20141203 |