CN101979475B - Process for synthesizing natural gas by performing methanation on coke oven gas - Google Patents
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- CN101979475B CN101979475B CN201010524311XA CN201010524311A CN101979475B CN 101979475 B CN101979475 B CN 101979475B CN 201010524311X A CN201010524311X A CN 201010524311XA CN 201010524311 A CN201010524311 A CN 201010524311A CN 101979475 B CN101979475 B CN 101979475B
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- Y02P20/584—Recycling of catalysts
Abstract
The invention relates to a process for synthesizing natural gas by performing methanation on coke oven gas. The process comprises the following steps of: dispersing a fresh methanation catalyst into an inert liquid-phase medium and putting the mixture into a slurry bed methanation reactor for reducing; performing a methanation reaction on the reduced coke oven gas, introducing tail gas into a gas-liquid separator I, discharging a slurry liquid-phase component in the tail gas and the catalyst from the bottom of the gas-liquid separator I and exhausting a gas phase in the tail gas from the top of the gas-liquid separator I; introducing a part of catalyst-containing inert liquid-phase media into a gas-liquid separator II, exhausting a gas phase from the top of the gas-liquid separator II, combining the gas phase with the gas phase exhausted from the top of the gas-liquid separator I, cooling and performing pressure swing adsorption so as to obtain H2 and synthetic natural gas; and discharging a methanation catalyst-containing inert liquid-phase medium from the bottom, combining the methanation catalyst-containing inert liquid-phase medium with the slurry liquid-phase component and the catalyst which are discharged from the bottom of the gas-liquid separator I, filtering a large-particle catalyst of less than 300 meshes out, separating a fine catalyst of more than 300 meshes from the inert liquid-phase medium and discharging, mixing the separated inert liquid-phase medium and the large-particle catalyst, exchanging heat between the mixture and raw material gas, cooling, and introducing the mixture into the slurry bed methanation reactor together with the methanation catalyst which is newly dispersed into the inert liquid-phase medium for the methanation reaction. The process has the advantages that: the process has low energy consumption and small equipment investment, is easy to operate and can replace the catalyst on line.
Description
Technical field
The invention belongs to a kind of synthetic natural gas technique, be specifically related to a kind of technique to synthesizing natural gas by performing methanation on coke oven gas.
Background technology
Coke-oven gas is as a kind of industrial discharged waste gas, and output is (about 1,430 hundred million m of national coke oven ultimate production in 2008 greatly
3), it is carried out methanation recycle the policy requirements that had both met energy-saving and emission-reduction, can produce certain economic benefit again, be a technology with market outlook.
Coke(oven)gas (COG) composition is comparatively complicated, and variation range is larger, depends on character, coking process and the operational circumstances etc. of used coking coal.Its chief component (Vol) is: H
254-59%, CH
423-28%, N
23-5%, O
20.3-0.7%, CO 5.5-7%, CO
21.2-2.5%, C
mH
m1.5-3%.H in the coke(oven)gas
2, CO, CO
2Carry out methanation reaction and can produce Artificial Natural Gas, reaction formula is as follows:
CO+3H
2＝CH
4+H
2O+206KJ/mol (1)
CO
2+4H
2＝CH
4+2H
2O+165KJ/mol (2)
Methanation reaction is the strong exothermal reaction under catalyst action, and temperature rise ratio is larger.In common gaseous fraction, per 1 percentage point CO methanation can produce 74 ℃ thermal insulation warming; Per 1 percentage point CO
2Methanation can produce 60 ℃ thermal insulation warming.So need the temperature in the methanator in the control synthetic gas methanation, sintering of catalyst and damage equipment that cause are most important to prevent the overheated of catalyst reactor.Therefore how effectively to control the temperature of reaction of gas employing methanation of coke oven, a large amount of heat energy that high efficiente callback utilizes strong exothermal reaction to emit become the focus of research and development.
Prior art adopts many fixed bed methanator series connection to carry out adiabatic reaction mostly, and in the methanation reaction process, usually control temperature with the complex appts of a plurality of heat exchangers and gas circulator, and employing is diluted to the CO in the producing synthesis gas from coal about 2%～4% by about 25% up to the circulation gas more than 5 times, with the heat that produces in the control methanation reaction process, this has not only increased facility investment, has also significantly increased the circulation gas power consumption.
Patent CN200610021836.5 discloses a kind of method of utilizing coke-oven gas to prepare synthetic natural gas, after now coke-oven gas being removed benzene, naphthalene, heavy hydrocarbons, sulfide by purification, under catalyst action, carry out again methanation reaction, make hydrogen and carbon monoxide and carbon dioxide reaction generation methane among the COG, obtain take methane as main gas mixture; Then by PSA Technology, obtain the gas product of methane concentration more than 90%.But this technique needs multistage methanator, and needs a large amount of circulation gas with CO+CO in the raw material
2Total concn be controlled at below 4%, greatly increased facility investment and energy consumption.
Patent CN200910058611.1 discloses a kind of methanation reaction process that utilizes coke-oven gas to prepare synthetic natural gas, adopts multistage methanator, controls CO+CO in the gasinlet temperature of every one-level methanator and the inlet gas
2Total content≤3.5%, make methanation after, every one-level methanator work off one's feeling vent one's spleen temperature all≤450 ℃.By this technique, although can reduce to a certain extent for dilution raw coke oven gas CO+CO
2Product tolerance greatly reduce, and can control the Outlet Gas Temperature of methanator, but still need many methanators, increased facility investment.
Patent CN200910018047.X discloses a kind of technique of gas employing methanation of coke oven synthetic natural gas, introduces water steam, need not to adopt gas segmentation circulation technology, and technical process is simpler, and energy consumption is lower.But be the control temperature in this technique methanation, introduce a large amount of recirculated water steams in unstripped gas, increased energy consumption, it adopts the multistage insulation reactor, has also greatly increased equipment.
Summary of the invention
It is low to the purpose of this invention is to provide a kind of energy consumption, easy to operate, and facility investment is low, is applicable to CO/CO on a large scale
2Concentration range, and can be online the technique of the synthesizing natural gas by methanation of coal synthesis gas of catalyst changeout more.
The present invention to achieve the above object of the invention, in the methanation reaction process, introduce the inert liquid phase component that thermal conductivity is large, thermal capacitance is large, be dispersed in uniformly methanation catalyst in the inert liq, improved heat transfer efficiency, make bed near isothermal operation, make (CO+CO in the gas employing methanation of coke oven process
2) transformation efficiency is up to more than 95%, need not the exhaust gas recirculation reaction, and can avoid the phenomenon of the sintering of catalyst that occurs in the conventional fixed bed methanation method.
The technical solution used in the present invention and concrete technology are:
(1) fresh methanation catalyst is dispersed in the inert liquid phase medium, enter the slurry attitude bed methanator from slurry attitude bed methanator bottom, then reducing gas is passed into from slurry attitude bed methanator bottom, be warming up to reduction temperature after normal pressure methanation catalyst is reduced;
(2) after reduction finishes, reducing gas is switched to coke-oven gas after the purification, and with the recycling catalyst heat exchange, boost to simultaneously reaction pressure, temperature is adjusted into temperature of reaction, carries out methanation reaction in slurry attitude bed methanator, and tail gas enters gas-liquid separator I, the slurry attitude liquid phase component of carrying secretly in the tail gas and catalyzer are discharged by gas-liquid separator I bottom, and the gas phase in the tail gas is discharged by gas-liquid separator I top;
(3) in the methanation reaction process, the inert liquid phase medium that part contains catalyzer enters into gas-liquid separator II, wherein gas phase is discharged by gas-liquid separator II top, and merge with the gas phase of being discharged by gas-liquid separator I top in the tail gas, remove water in the tail gas by cooling afterwards, then get purity through pressure-variable adsorption and be higher than 99% H
2And synthetic natural gas; And the inert liquid phase medium that contains methanation catalyst is discharged by gas-liquid separator II bottom, and with discharge slurry attitude liquid phase component by gas-liquid separator I bottom and methanation catalyst merges, then after filtration the large granular catalyst below 300 orders is leached, and the above thin catalyzer of 300 orders separates with the inert liquid phase medium after separating and discharges, isolated inert liquid phase medium is mixed with large granular catalyst, through with the unstripped gas heat exchange after cool off, and jointly enter in the slurry attitude bed methanator with the fresh methanation catalyst that is dispersed in the inert liquid phase medium and to carry out methanation reaction.
Aforesaid inert liquid phase medium is paraffinic hydrocarbon, and thermal oil is (such as THERMINOL
The VP-1 type) and the inert liquid phase component that the thermal conductivity such as hydrogenated terphenyl (such as SHHG-340) is large, thermal capacitance is large, boiling point is high.
Aforesaid methanation catalyst is with Al
2O
3Or SiO
2Be carrier, Ni content is at the domestic and international industrialization nickel catalyst of 5～60wt%, between catalyst grain size 100～300 orders.
The concentration of aforesaid methanation catalyst in the inert liquid phase medium is 1～40wt%.
The inert liquid phase medium that contains as mentioned above catalyzer recycles after heat exchange is cooled to below 50 ℃, and speed of circulation is the 1～10wt%/min that contains the inert media of catalyzer in the reactor.
Aforesaid reduction temperature is 300 ℃～450 ℃, and reducing gas forms and is comprised of nitrogen and hydrogen, and wherein hydrogen volume concentration is between 10%～30%, and the reducing gas air speed is 1000～5000L/ (hkg).
The temperature of aforesaid methanation reaction is 250 ℃～500 ℃, and more excellent is 300 ℃～450 ℃, and reaction pressure is 1～6MPa, and the unstripped gas air speed is 1000～12000L/ (hkg).
The present invention compared with prior art, has substantive distinguishing features and marked improvement is: the isothermal of (1) bed, the inertia liquid phase thermal barrier that thermal conductivity is large, thermal capacitance is large causes reaction heat to disperse rapidly and passes to heat-eliminating medium, make bed near isothermal, the unreasonable distribution of conventional methanation catalyst layer temperature can not appear, local superheating can not occur, can not work the mischief to catalyzer and equipment.(2) adaptability of raw material is owing to starch the good heat transfer of attitude bed so that the unstripped gas adaptability of slurry attitude bed methanation is stronger, CO/CO in the reaction gas
2Component can be regulated in 2%～30% large concentration range, still can keep the constant of bed temperature, thereby need not to dilute CO/CO in the unstripped gas
2Concentration, greatly reduces the usage quantity of inert component and circulation gas, thereby save heat energy, and this is impossible for the fixed bed methanation process.(3) high efficiency of reaction, slurry attitude bed methanation reaction uses finely grained catalyst, has greatly improved catalyst utilization, high density reactive component (CO/CO
2) employing be conducive to positive reaction speed, therefore, can obtain larger unstripped gas transformation efficiency and principal product selectivity, thermo-efficiency is high.Thereby synthesis procedure can save energy about 25%～30%.(4) can be online catalyst changeout more, guaranteed the continuity of producing.
Description of drawings
Fig. 1 is schema of the present invention
As shown in the figure, the 1st, live catalyst storage tank, the 2nd, slurry attitude bed methanator, the 3rd, interchanger, the 4th, gas-liquid separator I, the 5th, gas-liquid separator II, the 6th, water cooler, the 7th, recycle pump; P1, p2, p3, p4, p5, p6, p7, p8 and p9 are pipelines.
Embodiment
Below by specific embodiment the specific embodiment of the present invention is made further detailed description.
At first the domestic J101 type methanation catalyst of (catalyst concn in the liquid phase is 30wt%) in the inert liquid phase medium will be dispersed in the live catalyst storage tank 1, be pressed into from the bottom by recycle pump 7 the slurry attitude bed methanator 2 through pipeline p1, then will consist of H
2-10mol% and N
2The reducing gas of-90mol% passes into from slurry attitude bed methanator 2 bottoms through pipeline p2, with the temperature rise rate of 1 ℃/min temperature is warming up to 400 ℃ after, normal pressure reduces to catalyzer, after reduction finishes reducing gas is switched to (V%): H
257.6%, CH
426%, N
24%, O
20.4%, CO 8%, CO
22%, the coke-oven gas of CmHn 2%, and with pipeline p8 in recycling catalyst in interchanger 3 heat exchange, simultaneously pressure is risen to 3Mpa, temperature is adjusted into temperature of reaction, 2 carry out methanation reaction in slurry attitude bed methanator, tail gas enters among the gas-liquid separator I 4 through pipeline p3, the liquid phase component of carrying secretly in the tail gas and catalyzer are discharged by separator I bottom, and through pipeline p5 and pipeline p8 merging, tail gas is discharged from gas-liquid separator I4 top by cooling and is removed water the tail gas, then gets purity through pressure-variable adsorption and is higher than 99% and synthetic natural gas.In the methanation reaction process, speed with the 3wt%/min that accounts for the inert liquid phase medium that contains catalyzer in the reactor passes among the gas-liquid separator II 5 through pipeline p6, wherein gas phase is discharged by gas-liquid separator II 5 tops and is merged through pipeline p7 and exhaust pipe p4, and the inert media that contains catalyzer is discharged from gas-liquid separator II 5 bottoms through pipeline p8, and merge with catalyzer from pipe p5, then after filtration the large granular catalyst below 300 orders is leached, and the above thin catalyzer of 300 orders separates with the inert liquid phase medium after separating and discharges, and isolated inert liquid phase medium mixes with large granular catalyst, through with the unstripped gas heat exchange by water cooler 6 cooling, and jointly enter in the slurry attitude bed methanator 2 with the fresh methanation catalyst that is dispersed in the inert liquid phase medium and to carry out methanation reaction.
On the basis of embodiment 1,2～11 pairs of catalyst type of embodiment, the concentration of catalyzer in slurry attitude bed methanator, inert liquid phase medium kind, reducing gas forms, the reducing gas air speed, reduction temperature, reaction gas air speed, temperature of reaction, the reaction pressure factor is adjusted, concrete data and the results are shown in subordinate list 1, and unstripped gas and gas product form sees attached list 2.
Claims (4)
1. the technique of a synthesizing natural gas by performing methanation on coke oven gas is characterized in that comprising the steps:
(1) fresh methanation catalyst is dispersed in the inert liquid phase medium, enter the slurry attitude bed methanator from slurry attitude bed methanator bottom, then reducing gas is passed into from slurry attitude bed methanator bottom, be warming up to reduction temperature after normal pressure methanation catalyst is reduced;
(2) after reduction finishes, reducing gas is switched to coke-oven gas after the purification, and with the recycling catalyst heat exchange, boost to simultaneously reaction pressure, temperature is adjusted into temperature of reaction, carries out methanation reaction in slurry attitude bed methanator, and tail gas enters gas-liquid separator I, the slurry attitude liquid phase component of carrying secretly in the tail gas and catalyzer are discharged by gas-liquid separator I bottom, and the gas phase in the tail gas is discharged by gas-liquid separator I top;
(3) in the methanation reaction process, the inert liquid phase medium that part contains catalyzer enters into gas-liquid separator II, wherein gas phase is discharged by gas-liquid separator II top, and merge with the gas phase of being discharged by gas-liquid separator I top in the tail gas, remove water in the tail gas by cooling afterwards, then get purity through pressure-variable adsorption and be higher than 99% H2 and synthetic natural gas; And the inert liquid phase medium that contains methanation catalyst is discharged by gas-liquid separator II bottom, and with discharge slurry attitude liquid phase component by gas-liquid separator I bottom and methanation catalyst merges, then after filtration the large granular catalyst below 300 orders is leached, and the above thin catalyzer of 300 orders separates with the inert liquid phase medium after separating and discharges, isolated inert liquid phase medium is mixed with large granular catalyst, through with the unstripped gas heat exchange after cool off, and jointly enter in the slurry attitude bed methanator with the fresh methanation catalyst that is dispersed in the inert liquid phase medium and to carry out methanation reaction;
Described inert liquid phase medium is thermal oil;
Described methanation catalyst is with Al
2O
3Or SiO
2Be carrier, Ni content is at the nickel catalyst of 5～60wt%, and between catalyst grain size 100～300 orders, the concentration of methanation catalyst in the inert liquid phase medium is 1～40wt%;
Described reduction temperature is 300 ℃～450 ℃, and reducing gas forms and is comprised of nitrogen and hydrogen, and wherein hydrogen volume concentration is between 10%～30%, and the reducing gas air speed is 1000～5000L/hkg;
The temperature of described methanation reaction is 250 ℃～500 ℃, and reaction pressure is 1～6MPa, and the unstripped gas air speed is 1000～12000L/hkg.
2. the technique of a kind of synthesizing natural gas by performing methanation on coke oven gas as claimed in claim 1 is characterized in that described thermal oil is paraffinic hydrocarbon or hydrogenated terphenyl.
3. the technique of a kind of synthesizing natural gas by performing methanation on coke oven gas as claimed in claim 1, the temperature that it is characterized in that described methanation reaction is 300 ℃～450 ℃.
4. the technique of a kind of synthesizing natural gas by performing methanation on coke oven gas as claimed in claim 1, it is characterized in that the described inert liquid phase medium that contains catalyzer is cooled to below 50 ℃ through heat exchange recycles, and speed of circulation is the 1～10wt%/min that contains the inert liquid phase medium of catalyzer in the reactor.
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| CN102755864B (en) * | 2012-07-25 | 2014-10-29 | 华北电力大学 | Reversed flow cycle operation reaction device for methanation of synthesis gas and application thereof |
| CN102872874B (en) * | 2012-09-19 | 2015-01-07 | 太原理工大学 | Loaded type nickel-based catalyst used for slurry bed methanation, and preparation method and application thereof |
| CN102942971B (en) * | 2012-09-19 | 2014-01-15 | 太原理工大学 | Application of raney nickel as slurry reactor to synthesize methane catalyst |
| CN102952596B (en) * | 2012-09-19 | 2014-07-02 | 赛鼎工程有限公司 | Process and device for synthesizing natural gas through methanation based on slurry bed |
| CN110903870B (en) * | 2018-09-18 | 2021-08-20 | 中国石油化工股份有限公司 | Process for preparing methane by single pass of coal-based synthesis gas in slurry bed |
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| CN1593740A (en) * | 2004-06-25 | 2005-03-16 | 太原理工大学 | Highly effective slurry phase bed reactor |
| CN101733104A (en) * | 2009-12-07 | 2010-06-16 | 中国科学院山西煤炭化学研究所 | Catalyst for methanation of carbon dioxide-containing synthesis gas, preparation method and application |
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Patent Citations (2)
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|---|---|---|---|---|
| CN1593740A (en) * | 2004-06-25 | 2005-03-16 | 太原理工大学 | Highly effective slurry phase bed reactor |
| CN101733104A (en) * | 2009-12-07 | 2010-06-16 | 中国科学院山西煤炭化学研究所 | Catalyst for methanation of carbon dioxide-containing synthesis gas, preparation method and application |
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Effective date of registration: 20180809 Address after: 056302 Handan City, Handan City, Hebei, Wuan City, the city of the city of two street Patentee after: Hebei Huafeng energy science and Technology Development Co., Ltd. Address before: 030024 No. 79 West Main Street, Taiyuan, Shanxi, Yingze Co-patentee before: Sedin Engineering Co., Ltd. Patentee before: Taiyuan University of Technology |