CN104418703B - Serial methanol and methane synthesis process taking coke-oven gas as raw material - Google Patents

Serial methanol and methane synthesis process taking coke-oven gas as raw material Download PDF

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CN104418703B
CN104418703B CN201310396839.7A CN201310396839A CN104418703B CN 104418703 B CN104418703 B CN 104418703B CN 201310396839 A CN201310396839 A CN 201310396839A CN 104418703 B CN104418703 B CN 104418703B
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gas
synthesis
methane
methanol
reactor
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CN104418703A (en
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魏士新
祝东红
张�杰
蔡进
黄先亮
陈长新
蔡成伟
吴学其
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China Petroleum and Chemical Corp
Research Institute of Sinopec Nanjing Chemical Industry Co Ltd
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China Petroleum and Chemical Corp
Research Institute of Nanjing Chemical Industry Group Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/15—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively
    • C07C29/151—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively with hydrogen or hydrogen-containing gases
    • C07C29/1516—Multisteps
    • C07C29/1518—Multisteps one step being the formation of initial mixture of carbon oxides and hydrogen for synthesis
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C1/00—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon
    • C07C1/02—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon
    • C07C1/04—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon from carbon monoxide with hydrogen
    • C07C1/0485—Set-up of reactors or accessories; Multi-step processes
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
    • C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
    • C10L3/08—Production of synthetic natural gas

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a serial methanol and methane synthesis process taking coke-oven gas as a raw material. The serial methanol and methane synthesis process comprises the following steps: capturing CO2 from fume, adding into the coke-oven gas to adjust the hydrogen-carbon ratio; performing an NHD-process rough desulfuration and dry-process fine desulfuration, thereby obtaining a purified qualified synthesis gas; synthesizing methanol by using the synthesis gas in a methanol synthesis unit under the action of a methanol synthesis catalyst firstly, and performing heat exchange and cooling separation, thereby obtaining crude methanol; refining the crude methanol, thereby obtaining a fine methanol product; feeding the gas (generated after the crude methanol is separated) into a methane synthesis unit, completing methane synthesis reaction through three serially connected methane synthesis reactors, and performing cryogenic refrigeration on the generated gas, thereby obtaining liquefied natural gas of which the content of alkane is greater than 94%. According to the process, since the methanol synthesis unit is serially connected in front of the methane synthesis units, COX(CO+CO2) in the synthesis gas is reduced to be within 13%, the synthesis gas can be directly fed into the methane synthesis units without being diluted, and the whole synthesis process is simplified.

Description

A kind of series connection methyl alcohol with oven gas as raw material, process for synthesizing methane
Technical field
The invention belongs to new energy field, it is related to a kind of series connection methyl alcohol with oven gas as raw material, process for synthesizing methane.
Background technology
Coke-stove gas is the byproduct in process of coking, and its main component is hydrogen（55%~60%）And methane（23%~ 27%）, in addition also contain a small amount of carbon monoxide（5%~8%）, more than C2 unsaturated hydrocarbons（2%~4%）, carbon dioxide（1.5%~3%)、 Oxygen (0.3% ~ 0.8%), nitrogen (3% ~ 7%).Oven gas can be used as combustion gas, is also used as the unstripped gas of Chemical Manufacture.
At present, the chemical utilization of oven gas is mainly used to produce methyl alcohol.According to incompletely statistics, domestic oven gas methyl alcohol at present Device has nearly 70 sets, and more than 9,000,000 t/a, feature is that unit scale is relatively small to aggregated capacity, and most is 100,000 t/a ~ 200,000 t/ a.Under the seriously superfluous background of China's methyl alcohol production capacity, methanol market is weak, and coke-stove gas methyl alcohol prospect allows of no optimist.And China Natural gas insufficiency of supply-demand is very big, and in the long run, China's natural gas price will be in progressively up-trend.
Oven gas is a kind of gas of hydrogen-rich, therein（H2-CO2/CO+CO2）Reach 6 ~ 8, no matter for produce methyl alcohol, Still it is used for producing liquefied natural gas and all there is H2Excessive problem, in order to maximally utilise resource, needs to oven gas Mend carbon.Can mix with oven gas to adjust with the gas compared with low hydrogen-carbon ratio（H2-CO2/CO+CO2）To 2.3 ~ 3.0.In coking Cheng Zhong, 45% ~ 50% coke oven to be returned of oven gas total amount, as heating combustion gas, contains substantial amounts of in the flue gas of post combustion emission CO2, CO can be trapped2It is supplemented to regulation hydrogen-carbon ratio in oven gas, reach the purpose increasing methyl alcohol and liquefied natural gas (LNG)-throughput.
Mend CO2CO in synthesis gas afterwardsXContent reaches 17%, and being directly entered methane synthesis reactor can make beds temperature Degree is raised to more than 900 DEG C, causes catalyst to inactivate.
Content of the invention
It is an object of the invention to provide a kind of series connection methyl alcohol with oven gas as raw material, process for synthesizing methane.
The series connection methyl alcohol with oven gas as raw material for the present invention, process for synthesizing methane, it is qualified to mend carbon after-purification to it is characterized in that Oven gas be raw material, using methyl alcohol, methane connect synthesis technique combined production of methanol, liquefied natural gas.
The qualified gas of described purification first passes through methanol synthesis unit, is then passed through methane synthesis unit, all of reaction Device is single pass reactors.
Described after methanol-fueled CLC, CO and CO in synthesis gas2Concentration sum<13%, it is directly entered first without dilution Methane synthesis reactor, the temperature rise of the first methane synthesis reactor control the scope allowing in wide temperature methane synthesizing catalyst it Interior.
The temperature rise of described first methane synthesis reactor controls in 440 DEG C.
Described methane synthesis unit is completed using three adiabatic methane synthesis reactor series connection, and wherein, first methane closes Become reactor using wide temperature operation, reactor inlet temperature is 260 DEG C ~ 300 DEG C, 650 DEG C ~ 700 DEG C of outlet temperature, the second methane Synthesis reactor inlet temperature is 260 DEG C ~ 300 DEG C, 500 DEG C ~ 600 DEG C of outlet temperature, leucoaurin synthesis reactor entrance temperature Spend for 260 DEG C ~ 280 DEG C, 300 DEG C ~ 350 DEG C of outlet temperature.
It is raw material that this technique mends the qualified oven gas of carbon after-purification, using methyl alcohol, methane series connection synthesis technique coproduction first Alcohol, liquefied natural gas.Methanol synthesis unit is set before methane synthesis, methanol-fueled CLC can be first passed through and consume a part of COX, Make the CO of entrance methane synthesis unitXControl within the range of permission, the first methane synthesis reactor just can be using thermal insulation Reactor, and synthesis gas can be directly entered without dilution, and beds temperature rise can control to synthesize in wide temperature methane urges Within the scope of 440 DEG C that agent allows.
A kind of typical technique of the present invention, comprises following unit process：
(1) synthesis gas prepares：Oven gas carries out detar, naphthalene, benzene, ammonia etc. and processes, and is subsequently adding from coke oven discharge The CO of trapping in flue gas2, adjust gas（H2-CO2/CO+CO2）To 2.3 ~ 3.0.Then compression boosts to 3.0 ~ 8.0MPa, then Through NHD method desulfurization, Organic sulfur hydro-conversion, fine de-sulfur, total sulfur content is removed to below 0.1ppm.
(2) methanol synthesis unit：Purify qualified unstripped gas one way and pass through methyl alcohol synthetic reactor, close in efficient low pressure methanol Carry out methanol-fueled CLC, reacted gas obtains crude carbinol by heat exchange refrigerated separation in the presence of becoming catalyst, then through rectifying Obtain refined methanol.Separate the gas after methyl alcohol and wash the methyl alcohol removing remnants through scrubbing tower with water.
(3) methane synthesis unit：Through washing except the gas of methyl alcohol is through three adiabatic methane synthesis reactors connected Carry out methane synthetic reaction, CO content in gas is reduced to 50ppm, CO2Content is reduced to less than 1.5%.
(4) cryogenic refrigeration unit：From methane synthesis reactor gas out pass through cryogenic refrigeration by the methane gas, The liquefaction of many carbon hydrocarbon is separated, and obtains the liquefied natural gas of hydrocarbon content more than 94%, is rich in hydrogen in remaining gas phase.
The present invention produces methyl alcohol and liquefied natural gas with oven gas for raw material simultaneously, with traditional preparing methanol from coke oven gas technique Compare, flow process greatly simplifies, eliminate air separation unit, pure oxygen catalytic partial oxidation reburner and methanol synthesis loop compressibility Deng substantially reducing plant investment, reduce operating cost.
Mend the qualified synthesis gas of carbon after-purification can directly connect production methyl alcohol and liquefied natural gas, methanol-fueled CLC therein and Methane synthesis is one way reaction, and methanol synthesis reactor and the first methane synthesis reactor are all not required to be equipped with gas cyclic system System, simplifies flow process.
Brief description
Fig. 1 is that the benefit carbon of the embodiment of the present invention prepares synthesis gas process general flow chart, and Fig. 2 is the series connection of the embodiment of the present invention Methyl alcohol, process for synthesizing methane general flow chart.
Specific embodiment
With accompanying drawing, the present invention is described in detail in reference to embodiments.
The technical process of embodiment is as shown in figure 1 and 2.
Embodiment 1
Oven gas supplements CO2Adjust（H2-CO2/CO+CO2）To 2.3 ~ 3.0, compressed boost to 8.4MPa, then wet method crude Desulfurization, fine desulfurization process by dry to below total sulfur content 0.1ppm, are purified qualified synthesis gas.
Synthesis gas enter methyl alcohol synthetic reactor when pressure be 8.1MPa, temperature be 220 DEG C, in low pressure methanol synthesis catalyst Carry out methanol synthesis reaction, reacted gas is crude carbinol by the liquid product that heat exchange refrigerated separation obtains under effect, then It is rectifying to obtain refined methanol.Separate in the gas after liquid product（H2-CO2/CO+CO2）It is about 3, COXContent<11%, entrance is washed Wash the methyl alcohol that tower washes remnants with water, subsequently into methane synthesis unit.
Methane synthesis unit is made up of the adiabatic methane synthesis reactor of two connecting, and gas is warmed up to 250 through heat exchange DEG C enter the first methane synthesis reactor, methane synthesis liberated heat make gas temperature rise to 600 DEG C；Synthesize from the first methane Reactor gas out reclaims its reaction heat, by-product super-pressure superheated steam by heat exchanger, waste heat boiler（11MPa）, After heat exchange, synthesis gas temperature is down to about 250 DEG C.Enter back into second level methane synthesis reactor, after reaction, gas temperature rises to 450 DEG C, in gas, CO content is reduced to 100ppm, CO2Content is reduced to 1.5%, obtains hydrocarbon after the water that refrigerated separation generates The gas-phase product of class content 88%.
By gas-phase product cryogenic refrigeration to -165 DEG C, the CH in gas4It is separated with more than C2 hydro carbons and obtain hydro carbons The liquefied natural gas of content more than 94%.
Embodiment 2
The flue gas of coke oven combustion chamber discharge is introduced CO2Capture unit, obtains purity 99% using pressure swing absorption process CO2；Oven gas CO with trapping from flue gas after the pretreatments such as detar, de- benzene, de- naphthalene2Mixing, compressed boosts to 5.4MPa, then through NHD method desulfurization, then it is warmed up to 220 DEG C, enter hydro-conversion stove and the organic sulfur conversion in oven gas is become no Machine sulphur, then through zinc peroxide fine de-sulfur, total sulfur is removed to below 0.1ppm, obtain consisting of H253%%、C2H62%、CH4 28%、CO 6%、CO210%、N21% synthesis gas.
Synthesis gas enter methyl alcohol synthetic reactor when pressure be 5.3MPa, temperature be 220 DEG C, in low pressure methanol synthesis catalyst Carry out methanol synthesis reaction, reacted gas is crude carbinol by the liquid product that heat exchange refrigerated separation obtains under effect, then It is rectifying to obtain refined methanol.Separate in the gas after liquid product（H2-CO2/CO+CO2）It is about 3, COXContent<13%, entrance is washed Wash the methyl alcohol that tower washes remnants with water, subsequently into methane synthesis unit.
Methane synthesis unit is made up of the adiabatic methane synthesis reactor of three connecting, and gas is warmed up to 250 through heat exchange DEG C enter the first methane synthesis reactor, methane synthesis liberated heat make gas temperature rise to 680 DEG C；Synthesize from the first methane Reactor gas out reclaims its reaction heat, by-product super-pressure superheated steam by heat exchanger, waste heat boiler（11MPa）, After heat exchange, synthesis gas temperature is down to about 250 DEG C.Enter back into second level methane synthesis reactor, after reaction, gas temperature rises to 600 DEG C, 260 DEG C of entrance leucoaurin synthesis reactor are cooled to by heat exchange, after reaction, gas temperature is 360 DEG C, in gas CO content is reduced to 50ppm, CO2Content is reduced to 1%, obtains the gas phase of hydrocarbon content 90% after the water that refrigerated separation generates Product.
By gas-phase product cryogenic refrigeration to -165 DEG C, the CH in gas4It is separated with more than C2 hydro carbons and obtain hydro carbons The liquefied natural gas of content more than 94%.
Embodiment 3
The flue gas of coke oven combustion chamber discharge is introduced CO2Capture unit, obtains purity 99% using membrane separating method CO2；Oven gas CO with trapping from flue gas after the pretreatments such as detar, de- benzene, de- naphthalene2Mixing, compressed boosts to 6.4MPa, then through NHD method desulfurization, then it is warmed up to 220 DEG C, enter hydro-conversion stove and the organic sulfur conversion in oven gas is become no Machine sulphur, then through zinc peroxide fine de-sulfur, total sulfur is removed to below 0.1ppm, obtain consisting of H253%%、C2H62%、CH4 28%、CO 6%、CO210%、N21% synthesis gas.
Synthesis gas enter methyl alcohol synthetic reactor when pressure be 6.3MPa, temperature be 220 DEG C, in low pressure methanol synthesis catalyst Carry out methanol synthesis reaction, reacted gas is crude carbinol by the liquid product that heat exchange refrigerated separation obtains under effect, then It is rectifying to obtain refined methanol.Separate in the gas after liquid product（H2-CO2/CO+CO2）It is about 3, COXContent<12%, entrance is washed Wash tower to wash the methyl alcohol of remnants with water and make gas carry 20% moisture, subsequently into methane synthesis unit.
Methane synthesis unit is made up of the adiabatic methane synthesis reactor of three connecting, and gas is warmed up to 250 through heat exchange DEG C enter the first methane synthesis reactor, methane synthesis liberated heat make gas temperature rise to 650 DEG C；Synthesize from the first methane Reactor gas out reclaims its reaction heat, by-product super-pressure superheated steam by heat exchanger, waste heat boiler（11MPa）, After heat exchange, synthesis gas temperature is down to about 250 DEG C.Enter back into second level methane synthesis reactor, after reaction, gas temperature rises to 560 DEG C, 260 DEG C of entrance leucoaurin synthesis reactor are cooled to by heat exchange, after reaction, gas temperature is 370 DEG C, in gas CO content is reduced to 80ppm, CO2Content is reduced to 1.2%, obtains the gas of hydrocarbon content 90% after the water that refrigerated separation generates Phase product.
By gas-phase product cryogenic refrigeration to -165 DEG C, the CH in gas4It is separated with more than C2 hydro carbons and obtain hydro carbons The liquefied natural gas of content more than 94%.

Claims (3)

1. a kind of series connection methyl alcohol with oven gas as raw material, methane synthetic method, including following unit step：Synthesis gas prepares, Methanol synthesis unit, methane synthesis unit, cryogenic refrigeration unit, it is characterized in that to mend the qualified oven gas of carbon after-purification be former Material, using methyl alcohol, methane series connection synthesis technique combined production of methanol, liquefied natural gas；The qualified gas of described purification first passes through methyl alcohol Synthesis unit, is then passed through methane synthesis unit, and all of reactor is single pass reactors；Described through methanol-fueled CLC it Afterwards, CO and CO in synthesis gas2Concentration sum<13%, it is directly entered the first methane synthesis reactor without dilution, the first methane closes The temperature rise becoming reactor controls within the scope of wide temperature methane synthesizing catalyst allows；Described synthesis gas is prepared as：Coke oven Gas carries out detar, naphthalene, benzene, ammonia treatment, is subsequently adding the CO of trapping from the flue gas of coke oven discharge2, adjust gas（H2- CO2/CO+CO2）To 2.3 ~ 3.0, then compress and boost to 3.0 ~ 8.0MPa, then through NHD method desulfurization, Organic sulfur hydro-conversion, essence Desulfurization, total sulfur content is removed to below 0.1ppm；Described methane synthesis unit adopts three adiabatic methane synthesis reactor strings Connection completes, and wherein, using wide temperature operation, reactor inlet temperature is 260 DEG C ~ 300 DEG C to first methane synthesis reactor, outlet 650 DEG C ~ 700 DEG C of temperature, temperature rise controls in 440 DEG C, and the second methane synthesis reactor inlet temperature is 260 DEG C ~ 300 DEG C, goes out 500 DEG C ~ 600 DEG C of temperature of mouth, leucoaurin synthesis reactor inlet temperature is 260 DEG C ~ 280 DEG C, outlet temperature 300 DEG C ~ 350 ℃；Described cryogenic refrigeration unit is：From methane synthesis reactor gas out pass through cryogenic refrigeration by the methane gas, The liquefaction of many carbon hydrocarbon is separated, and the liquid-phase product obtaining is the liquefied natural gas of hydrocarbon content more than 94%, is rich in hydrogen in gas phase Gas.
2. the method for claim 1 is it is characterised in that described methanol synthesis unit is：Purify qualified unstripped gas list Journey passes through methyl alcohol synthetic reactor, carries out methanol-fueled CLC in the presence of low pressure methanol synthesis catalyst, and reacted gas passes through to change Hot refrigerated separation obtains crude carbinol, then is rectifying to obtain refined methanol, and the gas after separation methyl alcohol washes with water through scrubbing tower and removes Remove the methyl alcohol of remnants.
3. method as claimed in claim 2 is it is characterised in that described methane synthesis unit is：Through washing except the gas of methyl alcohol Body, carries out methane synthetic reaction through the adiabatic methane synthesis reactor of three series connection, CO content in gas is reduced to 50ppm, CO2Content is reduced to less than 1.5%.
CN201310396839.7A 2013-09-04 2013-09-04 Serial methanol and methane synthesis process taking coke-oven gas as raw material Active CN104418703B (en)

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CN105294394A (en) * 2015-05-08 2016-02-03 徐州伟天化工有限公司 Methanol co-production recycling system
CN114349602A (en) * 2020-10-12 2022-04-15 中石化南京化工研究院有限公司 Process for synthesizing low-carbon mixed alcohol by taking coal synthesis gas as raw material and carrying out methanation in series
CN114082287A (en) * 2021-11-25 2022-02-25 中化学科学技术研究有限公司 Method and system for directly hydrogenating flue gas

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