CN100506948C - Method for increasing tar yield of coalite pyrolysis with methane as reaction gas - Google Patents

Method for increasing tar yield of coalite pyrolysis with methane as reaction gas Download PDF

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CN100506948C
CN100506948C CNB2005100458538A CN200510045853A CN100506948C CN 100506948 C CN100506948 C CN 100506948C CN B2005100458538 A CNB2005100458538 A CN B2005100458538A CN 200510045853 A CN200510045853 A CN 200510045853A CN 100506948 C CN100506948 C CN 100506948C
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CN1664069A (en
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胡浩权
刘全润
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Dalian University of Technology
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Abstract

The invention belongs to energy technology field and provides a method for increasing coking yield in coal pyrolytic and coking process. The method comprises employing methane as reacting gas and adding adequate oxidant, mixing them and introducing them to the pyrolytic reactor, which comprises two layers, the middle layer is separated by gas grid plate, activating the methane by catalyst, and introducing it to the coal layer, pyrolising and charring the coal. The invention is characterized in that it employs the methane instead of pure hydrogen gas as reacting gas, which can deduce the pyrolising cost; the coking yield is higher than that of employing hydrogen gas in the same condition; the char coal yield is equal to that of in the inert atmosphere but higher than that of employing hydrogen gas; the catalyst and coal do not mix directly, which is suitable for recovering.

Description

A kind of is the method that reaction gas improves the pyrolysis of coal tar yield with methane
Technical field
The invention belongs to energy technology field, relating in particular to a kind of is the method that reaction gas improves pyrolysis of coal and coking tar yield with methane.
Background technology
The pyrolysis of coal is the basis of thermal transition technology such as coal combustion, gasification and liquefaction.In addition, it is the liquid fuel and the industrial chemicals of purpose product that the pyrolysis of coal under inert atmosphere and reducing atmosphere can obtain with tar, and the low-sulfur semicoke of Huo Deing is a kind of clean solid fuel simultaneously.Therefore, the pyrolysis of coal and hydropyrolysis are subjected to more and more investigators' attention as a kind of independent clean coal transformation technology.The pyrolysis transformation efficiency of coal under inert atmosphere is low, and tar yield is low; To obtain tar products to greatest extent is purpose hydropyrolysis technology, is reaction gas with the pure hydrogen, the process for making hydrogen complexity, and the facility investment expense is big, operational condition harshness, running cost height.Therefore, develop new pyrolytic process, improve the pyrolytic tar productive rate and become the new research direction of pyrolysis of coal technology to substitute hydropyrolysis.Be that the pyrolytic process research of purpose mainly contains following a few class at present to improve tar yield:
1, pre-treatment.By various pretreatment technology, can change the physics and the chemical structure of coal to a certain extent, thereby improve the pyrolytic tar productive rate.Cypres etc. utilize H2, He, CO 2, H 2Deng gas coal is carried out pre-treatment, wish to change the pore structure of coal, improve the pyrolytic tar productive rate.Found that, the coal process is at 2～3MPa, temperature is 350～400 ℃ hydrogen pre-treatment, can improve the pyrolytic tar productive rate to a certain extent, but other several gas pre-treatment to improve the not effect of pyrolytic tar productive rate (Cypres et al.Fuel Process.Technol.1988,20:337).Graff etc. are to through 320～360 ℃, the Illinois#6 coal of the subcritical water steam pre-treatment of 5MPa carries out pyrolysis and finds, tar yield improves 30%, they think, the subcritical water steam pre-treatment can fully be destroyed the bridged bond in the coal molecule, but this test-results fails to be repeated by other investigators.The investigator thinks that this pretreatment process is to too strong (the Graff et al.Energy ﹠amp of the selectivity of coal; Fuel, 1987,3: 84).
2, change reaction atmosphere.Methane hydrogen-to-carbon ratio height has the investigator to propose to utilize methane to substitute hydrogen as reaction gas, but discovers, below 800 ℃, methane and coal-based do not react, be equivalent to rare gas element (Cypres, Fuel, 1982,61:721).Chinese scholars also proposes, utilize coke-oven gas instead of pure hydrogen as the hydropyrolysis reaction gas, result of study shows, coal-coke(oven)gas copyrolysis can obtain with coke-oven gas in the tar yield (Liao Hongqiang etc. of hydropyrolysis under the hydrogen dividing potential drop uniform pressure, the chemistry of fuel journal, 1997,25:104).Li Baoqing etc. (Chinese patent CN1224043A) add fixed-bed reactor sneak into the 0.25g polyethylene in the bituminous coal of 5g Yanzhou after, feeding pressure is 3MPa, flow is the coke-oven gas of 1L/min, temperature rise rate with 10 ℃/min is heated to 650 ℃, constant temperature 10min, the pyrolytic tar yield is compared net increase 7.52% (weight percentage of dry ash-free basis coal) with the former pyrolysis of coal result who does not add plastic waste as a result.Miura etc. carry out fast pyrogenation to the Morwell brown coal in ethylbenzene steam under 800 ℃, find that tar yield has increased by 10% (Miura et al.Energy﹠amp; Fuels 1992,6:179).
3, catalyse pyrolysis.There is investigator's original position in coal to support transition-metal catalyst, coal is carried out fast pyrogenation.Test-results shows, catalyzer is mainly catalytic to be gas-phase reaction, be the macromolecular substance catalysis in the fugitive constituent micromolecular gaseous matter promptly, can not obviously improve productive rate (Takarada, Fuel, 1992 of tar, 71:1087), and original position is catalyst-loaded, can't reclaim the catalyzer in the semicoke.
Summary of the invention
The purpose of this invention is to provide a kind of with methane instead of pure hydrogen as reaction gas, improving a kind of of pyrolysis of coal tar yield is the method that reaction gas improves the pyrolysis of coal tar yield with methane, can reduce the hydropyrolysis cost, the coal-tar middle oil productive rate of product is higher than hydropyrolysis tar yield under the same terms, and catalyzer is easy to reclaim.
The technical solution adopted for the present invention to solve the technical problems is, a kind of is the method that reaction gas improves the pyrolysis of coal tar yield with methane, be to be reaction gas with methane, in methane, add the oxygenant of 0～20% volume, methane and oxygenant mix the back and enter pyrolysis reactor by gas inlet (A), after the activation of load type metal nickel catalyzator, enter pyrolysis of coal responding layer 1, coal is carried out pyrolysis and coking as reaction gas.Pyrolysis and coking condition are: 400 ℃～800 ℃ of temperature, and pressure 0.1～3.0MPa, constant temperature 0～60min, pyrogenous origin product is taken reactor out of by pneumatic outlet (B), collects tar products by gas-liquid separator.Methane can and be rich in any substituting in the mixed gas of methane with Sweet natural gas, coal-seam gas, and oxygenant is O 2, NO, H 2O, CO 2With airborne any, used catalyzer be any catalyzer that can make methane activation.Pyrolysis reactor is made up of gas inlet (A), methane inlet (C), oxidant inlet (D), pneumatic outlet (B), pyrolysis of coal responding layer (1), catalyst layer (2) and gas distribution grid (3), the upper strata is pyrolysis of coal responding layer (1), lower floor is catalyst layer (2), the centre separates with gas distribution grid (3), and catalyzer closely not only contacts but also directly do not mix with the coal seam.The pyrolysis reactor form is fixed bed or fluidized-bed.Gas distribution grid (3) is a porous barrier.When adopting fluidized bed pyrolysis reactor, can adopt the large granular catalyst bed, directly use as gas distribution grid (3).
The invention has the beneficial effects as follows, with methane instead of pure hydrogen as the hydropyrolysis reaction gas, can reduce the hydropyrolysis cost, the coal-tar middle oil productive rate of product is higher than hydropyrolysis tar yield under the same terms, and the pyrolysis char yield is suitable under semi-coke yield and the inert atmosphere, be higher than hydropyrolysis semi-coke yield under the same terms, catalyzer and coal directly do not mix, and are easy to reclaim.
Description of drawings
The present invention is further described below in conjunction with the drawings and specific embodiments.
Fig. 1 is a pyrolysis reactor structural representation of the present invention.
Among the figure, A, gas inlet, B, pneumatic outlet, C, methane inlet, D, oxidant inlet, 1, the coal seam, 2, catalyst layer, 3, gas distribution grid.
Embodiment
Comparative Examples 1
Selected coal is a Yanzhou coal, and its technical analysis and ultimate analysis see Table one.Test coal 5g, catalyst-free, pyrolytical condition are 700 ℃ of temperature, constant temperature time 30min, and pressure 2.0MPa, reaction gas are 500ml/min N 2A enters reactor by the gas inlet.Pyrogenous origin product liquid is taken reactor by reaction gas out of by pneumatic outlet B, collects with cold-trap (20 ℃), according to ASTM D95-83 method separating oil and water.The tar yield that obtains thus is 17.1wt%daf, and semi-coke yield is 67.7wt%daf.
Comparative Examples 2
Selected coal is a Yanzhou coal, and its technical analysis and ultimate analysis see Table one.Test coal 5g, catalyst-free, pyrolytical condition are 700 ℃ of temperature, constant temperature time 30min, and pressure 2.0MPa, reaction gas are 500ml/min H 2A enters reactor by the gas inlet.Pyrogenous origin product liquid is taken reactor by reaction gas out of by pneumatic outlet B, collects with cold-trap (20 ℃), according to ASTM D95-83 method separating oil and water.The tar yield that obtains thus is 24.4wt%daf, and semi-coke yield is 56.4wt%daf.
Comparative Examples 3
Selected coal is a Yanzhou coal, and its technical analysis and ultimate analysis see Table one.Test coal 5g, catalyst-free, pyrolytical condition are 700 ℃ of temperature, constant temperature time 30min, and pressure 2.0MPa, reaction gas are 500ml/min CH 4A enters reactor by the gas inlet.Pyrogenous origin product liquid is taken reactor by reaction gas out of by pneumatic outlet B, collects with cold-trap (20 ℃), according to ASTM D95-83 method separating oil and water.The tar yield that obtains thus is 18.8wt%daf, and semi-coke yield is 68.2wt%daf.
Comparative Examples 4
Selecting catalyzer for use is Ni/Al 2O 3Catalyzer, its preparation method is: at 20-60 purpose Al 2O 3Last dipping 10% (weight percentage) Ni (NO 3) 26H 2O, 100 ℃ of dryings 5 hours, 800 ℃ of roastings 8 hours, 700 ℃ of following H 2Reduction 10min;
Selected coal is a Yanzhou coal, and its technical analysis and ultimate analysis see Table one.Test coal 5g, catalyzer 1g, pyrolytical condition are 700 ℃ of temperature, constant temperature time 30min, and pressure 2.0MPa, reaction gas are 500ml/min CH 4A enters reactor by the gas inlet.Pyrogenous origin product liquid is taken reactor by reaction gas out of by pneumatic outlet B, collects with cold-trap (20 ℃), according to ASTM D95-83 method separating oil and water.The tar yield that obtains thus is 23.8wt%daf, and semi-coke yield is 68.7wt%daf.
Embodiment 1
Selecting catalyzer for use is Ni/Al 2O 3Catalyzer, its preparation method is: at 20-60 purpose Al 2O 3Last dipping 10% (weight percentage) Ni (NO 3) 26H 2O, 100 ℃ of dryings 5 hours, 800 ℃ of roastings 8 hours, 700 ℃ of following H 2Reduction 10min;
Selected coal is a Yanzhou coal, and its technical analysis and ultimate analysis see Table one.Test coal 5g, catalyzer 1g, pyrolytical condition are 700 ℃ of temperature, constant temperature time 30min, and pressure 2.0MPa, reaction gas are 400ml/min CH 4Enter reactor by gas inlet A through methane inlet C and oxidant inlet D after mixing respectively with the 100ml/min air, gas mixture enters pyrolysis of coal responding layer 1 through catalyst layer 2 priming reactions and by gas distribution grid 3.Coal and reactant gases be copyrolysis in pressurization static bed reactor.Pyrogenous origin product liquid is taken reactor by reaction gas out of by pneumatic outlet B, collects with cold-trap (20 ℃), according to ASTM D95-83 method separating oil and water.The tar yield that obtains thus is 26.4wt%daf, and semi-coke yield is 69.1wt%daf.
Embodiment 2
Selecting catalyzer for use is Ni/Al 2O 3Catalyzer, its preparation method is: at 20-60 purpose Al 2O 3Last dipping 10% (weight percentage) Ni (NO 3) 26H 2O, 100 ℃ of dryings 5 hours, 800 ℃ of roastings 8 hours, 700 ℃ of following H 2Reduction 10min;
Selected coal is a Yanzhou coal, and its technical analysis and ultimate analysis see Table one.Test coal 5g, catalyzer 1g, pyrolytical condition are 700 ℃ of temperature, constant temperature time 30min, and pressure 2.0MPa, reaction gas are 400ml/min CH 4Enter reactor by gas inlet A through methane inlet C and oxidant inlet D after mixing respectively with 100ml/min oxygen, gas mixture enters pyrolysis of coal responding layer 1 through catalyst layer 2 priming reactions and by gas distribution grid 3.Coal and reactant gases be copyrolysis in pressurization static bed reactor.Pyrogenous origin product liquid is taken reactor by reaction gas out of by pneumatic outlet B, collects with cold-trap (20 ℃), according to ASTM D95-83 method separating oil and water.The tar yield that obtains thus is 41.5wt%daf, and semi-coke yield is 68.7wt%daf.
Embodiment 3
Selecting catalyzer for use is Ni/Al 2O 3Catalyzer, its preparation method is: at 20-60 purpose Al 2O 3Last dipping 10% (weight percentage) Ni (NO 3) 26H 2O, 100 ℃ of dryings 5 hours, 800 ℃ of roastings 8 hours, 700 ℃ of following H 2Reduction 10min;
Pyrolysis: pyrolysis reactor as shown in drawings, this reactor is divided into two-layer up and down, gas inlet one end is a catalyst layer 2, the other end is coal seam 1, middlely separates with gas distribution grid 3.
Selected coal is a Yanzhou coal, and its technical analysis and ultimate analysis see Table one.Test coal 5g, catalyzer 1g, pyrolytical condition are 600 ℃ of temperature, constant temperature time 30min, and pressure 2.0MPa, reaction gas are 400ml/min CH 4Enter reactor by gas inlet A through methane inlet C and oxidant inlet D after mixing respectively with 100ml/min oxygen, gas mixture enters pyrolysis of coal responding layer 1 through catalyst layer 2 priming reactions and by gas distribution 3 plates.Coal and reactant gases be copyrolysis in pressurization static bed reactor.Pyrogenous origin product liquid is taken reactor by reaction gas out of by pneumatic outlet B, collects with cold-trap (20 ℃), according to ASTM D95-83 method separating oil and water.The tar yield that obtains thus is 35.9wt%daf, and semi-coke yield is 71.7wt%daf.
Embodiment 4
Selecting catalyzer for use is Ni/Al 2O 3Catalyzer, its preparation method is: at 20-60 purpose Al 2O 3Last dipping 10% (weight percentage) Ni (NO 3) 26H 2O, 100 ℃ of dryings 5 hours, 800 ℃ of roastings 8 hours, 700 ℃ of following H 2Reduction 10min;
Selected coal is a Yanzhou coal, and its technical analysis and ultimate analysis see Table one.Test coal 5g, catalyzer 1g, pyrolytical condition are 700 ℃ of temperature, constant temperature time 30min, and pressure 0.1MPa, reaction gas are 400ml/min CH 4Enter reactor by gas inlet A through methane inlet C and oxidant inlet D after mixing respectively with 100ml/min oxygen, gas mixture enters pyrolysis of coal responding layer 1 through catalyst layer 2 priming reactions and by gas distribution grid 3.Coal and reactant gases be copyrolysis in pressurization static bed reactor.Pyrogenous origin product liquid is taken reactor by reaction gas out of by pneumatic outlet B, collects with cold-trap (20 ℃), according to ASTM D95-83 method separating oil and water.The tar yield that obtains thus is 25.2wt%daf, and semi-coke yield is 66.1wt%daf.
Comparative Examples 5
Selected coal is Datong District's coal, and its technical analysis and ultimate analysis see Table one.Test coal 5g, catalyst-free, pyrolytical condition are 650 ℃ of temperature, constant temperature time 30min, and pressure 2.0MPa, reaction gas are 500ml/min H 2A enters reactor by the gas inlet.Pyrogenous origin product liquid is taken reactor by reaction gas out of by pneumatic outlet B, collects with cold-trap (20 ℃), according to ASTM D95-83 method separating oil and water.The tar yield that obtains thus is 14.1wt%daf, and semi-coke yield is 64.1wt%daf.
Embodiment 5
Selecting catalyzer for use is Ni/Al 2O 3Catalyzer, its preparation method is: at 20-60 purpose Al 2O 3Last dipping 10% (weight percentage) Ni (NO 3) 26H 2O, 100 ℃ of dryings 5 hours, 800 ℃ of roastings 8 hours, 700 ℃ of following H 2Reduction 10min;
Selected coal is Datong District's coal, and its technical analysis and ultimate analysis see Table one.Test coal 5g, catalyzer 1g, pyrolytical condition are 650 ℃ of temperature, constant temperature time 30min, and pressure 2.0MPa, reaction gas are 400ml/min CH 4Enter reactor by gas inlet A through methane inlet C and oxidant inlet D after mixing respectively with 100ml/min oxygen, gas mixture enters pyrolysis of coal responding layer 1 through catalyst layer 2 priming reactions and by gas distribution grid 3.Coal and reactant gases be copyrolysis in pressurization static bed reactor.Pyrogenous origin product liquid is taken reactor by reaction gas out of by pneumatic outlet B, collects with cold-trap (20 ℃), according to ASTM D95-83 method separating oil and water.The tar yield that obtains thus is 31.8wt%daf, and semi-coke yield is 77.6wt%daf.
Table one coal analysis data
Figure C200510045853D00071

Claims (7)

1, a kind of is the method that reaction gas improves the pyrolysis of coal tar yield with methane, it is characterized in that, be to be reaction gas with methane, in methane, add the oxygenant of 0～20% volume, methane and oxygenant mix the back and enter pyrolysis reactor by gas inlet (A), after the activation of load type metal nickel catalyzator, enter pyrolysis of coal responding layer (1) as reaction gas, coal is carried out pyrolysis and coking, pyrolysis and coking condition are: 400 ℃～800 ℃ of temperature, pressure 0.1～3.0MPa, constant temperature 0～60min, pyrogenous origin product is taken reactor out of by pneumatic outlet (B), collects tar products by gas-liquid separator.
2, according to claim 1 a kind of be the method that reaction gas improves the pyrolysis of coal tar yield with methane, it is characterized in that described methane can and be rich in any substituting in the mixed gas of methane with Sweet natural gas, coal-seam gas.
3, according to claim 1 a kind of be the method that reaction gas improves the pyrolysis of coal tar yield with methane, it is characterized in that described oxygenant is O 2, NO, H 2O, CO 2With airborne any.
4, according to claim 1 a kind of be the method that reaction gas improves the pyrolysis of coal tar yield with methane, it is characterized in that, described pyrolysis reactor is made up of gas inlet (A), methane inlet (C), oxidant inlet (D), pneumatic outlet (B), pyrolysis of coal responding layer (1), catalyst layer (2) and gas distribution grid (3), the upper strata is pyrolysis of coal responding layer (1), lower floor is catalyst layer (2), and the centre separates with gas distribution grid (3).
5, according to claim 1 a kind of be the method that reaction gas improves the pyrolysis of coal tar yield with methane, it is characterized in that described pyrolysis reactor form is a fixed bed.
6, according to claim 1 a kind of be the method that reaction gas improves the pyrolysis of coal tar yield with methane, it is characterized in that described pyrolysis reactor form is a fluidized-bed.
7, according to claim 4 a kind of be the method that reaction gas improves the pyrolysis of coal tar yield with methane, it is characterized in that described gas distribution grid (3) is a porous barrier.
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CN101747922A (en) * 2010-01-05 2010-06-23 大连理工大学 Method for increasing yield of coal-pyrolysis-based tar in reaction atmosphere of methane-rich gas mixture in fluidized bed
CN102175710B (en) * 2011-02-25 2012-08-01 首钢总公司 Method for predicting yield of coal tar
CN102161904B (en) * 2011-03-10 2013-12-25 大连理工大学 Method for increasing tar yield by coupling aromatization of hydrocarbons with coal pyrolysis
CN102391879A (en) * 2011-09-23 2012-03-28 北京华福工程有限公司 Rotary bed dry distillation furnace and method for improving yield of coal dry distillation tar by activating pyrolysis gas
CN102559226A (en) * 2012-02-13 2012-07-11 北京神雾环境能源科技集团股份有限公司 Coal pyrolysis system and pyrolysis method
CN103571541B (en) * 2012-07-30 2016-08-10 新奥科技发展有限公司 A kind of co-production of methane and the catalysis gasification method of tar
CN102942948A (en) * 2012-11-15 2013-02-27 太原理工大学 Method for applying loaded nickel-based catalyst to direct coal liquefaction in presence of methane
CN104293363A (en) * 2014-10-24 2015-01-21 新疆大学 Method and device for improving quality of coal pyrolytic tar by taking simulated pyrolysis gas as reaction atmosphere
CN105925317A (en) * 2016-07-11 2016-09-07 河南理工大学 Method for improving yield of coal microwave pyrolysis tar by using methane and carbon dioxide as reactant gases

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