CN105130749B - A kind of technique that coke-stove gas low-carbon alcohols are combined by synthesis gas - Google Patents
A kind of technique that coke-stove gas low-carbon alcohols are combined by synthesis gas Download PDFInfo
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- CN105130749B CN105130749B CN201510464737.3A CN201510464737A CN105130749B CN 105130749 B CN105130749 B CN 105130749B CN 201510464737 A CN201510464737 A CN 201510464737A CN 105130749 B CN105130749 B CN 105130749B
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- 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
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Abstract
A kind of technique for combining coke-stove gas low-carbon alcohols by synthesis gas is that coke-stove gas and synthesis gas are mixed to form to the coarse raw materials gas for meeting higher alcohols synthesis；Coarse raw materials gas is washed through low-temp methanol, removes the impurity such as hydrogen sulfide and carbon dioxide, and the pure gas of synthesis of low-carbon alcohol are made, and the hydrogen sulfide of abjection removes sulfur recovery, the carbon dioxide high altitude discharge of removing；Pure gas after purification carry out synthesis of low-carbon alcohol reaction, and obtained gas-liquid two-phase product carries out gas-liquid separation, and the gas of separation mainly includes CO, H2And CO2A part is sent to low-temp methanol and washes circulation, and another part sends to torch burning discharge as periodic off-gases, and the liquid product of separation is alcohol-water mixture, and alcohol-water mixture carries out alcohol-water separation, obtains low-carbon alcohols product.The present invention has product diversification, adjusts superfluous production capacity, promotes energy-saving and emission-reduction, the advantages of readjusting the energy structure.
Description
Technical field
The invention belongs to a kind of synthesis of low-carbon alcohol technique, and in particular to a kind of to combine coke-stove gas low-carbon alcohols by synthesis gas
Technique.
Background technology
Low-carbon alcohols are often referred to C1~C5 alcohol-based mixtures.Application prospect is quite varied：Both it can be used as alternative fuel, it is also possible to
Make fuel additive.Burnt when low-carbon alcohols are as alternative fuel abundant, and the CO, NOx, the hydro carbons etc. that are discharged in burning are less,
It is environmentally compatible fuels；Low-carbon alcohols have a extensive future as fuel additive, used methyl tertiary-butyl ether because
The problems such as in the presence of storage, transport, progressive with science and technology eventually can be disabled, and this provides opportunity for the exploitation of low-carbon alcohols.And
Low-carbon alcohols octane number is higher, explosion-proof, anti-seismic performance is good.Low-carbon alcohols have as chemical products and large Chemical Manufacture raw material simultaneously
There is immense value.At present, Global Oil resource increasingly consumes, and energy security problem is increasingly severe, the research of new energy system
It is extremely urgent with developing.
China is the first big coke production state in the world, production coke a large amount of coke-stove gas of by-product simultaneously.Coke-stove gas
Main component is (volume ratio)：50-60% hydrogen, 20-28% methane, 10-18% CO+CO2.It is in addition, also micro
H2S, the harmful components such as COS, HCN.These coke-stove gas part is used for methanol processed, synthesis ammonia and factory's combustion gas, and inclined
Remote area is then discharged in vain.Nearly 300 billion cubic meter more than needed is burnt every year in addition to production synthesis ammonia and methanol for coke-stove gas at present
Furnace gas, due to coke-stove gas form " the more carbon of hydrogen are few " the characteristics of, it is about 55% to cause the capacity usage ratio of coke-stove gas at this stage
Left and right, cause huge energy waste and environmental pollution.
The low-quality lignite on the ground such as rich coal resources in China, particularly Inner Mongol, Xinjiang enters through synthesis gas made from gasification furnace
The synthesis of row chemical products, the few feature of the more hydrogen of carbon of synthesis gas, (gas of synthesis gas forms percent by volume：CO：45-
60%, H2：20-28%, CO2：8-18, CH4：7-15%, H2S：0.15-0.35%)；It can be seen that by coke-stove gas or synthesis gas list
Only production low-carbon alcohols, component all be present and utilize the problem of insufficient：The more carbon of coke-stove gas hydrogen are few, and separately synthesized low-carbon alcohols necessarily go out
Now a large amount of hydrogen are remaining, or need other supplementary carbon source；And synthesize that the more hydrogen of gas carbon are few, and separately synthesized low-carbon alcohols will occur largely
Carbon is remaining, or needs other supplemental hydrogen source.If coke-stove gas and synthesis gas mixed in proportion, it can reach and learn from other's strong points to offset one's weaknesses,
Form hydrogen-carbon ratio condition (the H:Cmoleratio H for meeting higher alcohols synthesis2/ CO=2.3-4.5), will realize coke-stove gas and
Synthesis gas " gas its use to the greatest extent ", turns waste into wealth, not only produces obvious economic benefit and environmental benefit, also have to Energy restructuring
It is significant.
The content of the invention
It is an object of the invention to provide a kind of product diversification, adjusts superfluous production capacity, promotes energy-saving and emission-reduction, adjusts energy knot
The technique that coke-stove gas low-carbon alcohols are combined by synthesis gas of structure.
Present invention process is few according to the coke-stove gas composition more carbon of hydrogen, and synthesizes the characteristics of more hydrogen of gas carbon are few, and both are excellent
Gesture is complementary, reaches the hydrogen-carbon ratio for meeting synthesis of low-carbon alcohol, with solve individually using coke-stove gas production low-carbon alcohols need to mend carbon or
The shortcomings that person individually needs to mend hydrogen using low carbon alcohol by synthetic gas, a kind of effectively way is provided for reasonable utilize of coke-stove gas
Footpath, be advantageous to product diversification, adjust superfluous production capacity, promote energy-saving and emission-reduction, readjust the energy structure, moreover it is possible to significantly improve enterprise's warp
Benefit of helping and social environment benefit.
To achieve the above object, the present invention adopts the following technical scheme that：
(1) by coke-stove gas, (percent by volume composition is H2：50-60%, CH4：20-28%, CO+CO2:10-18%,
N2：3-8%) (percent by volume composition is CO with synthesis gas：45-60%, H2：20-28%, CO2：8-18, CH4：7-15%,
H2S：0.15-0.35%) it is passed through gas holder to be sufficiently mixed, forms the coarse raw materials gas for meeting higher alcohols synthesis hydrogen-carbon ratio；
(2) coarse raw materials gas is compressed carries out low temperature methanol cleaning, removes the impurity such as hydrogen sulfide and carbon dioxide, is made and closes
Into the pure gas of low-carbon alcohols, the hydrogen sulfide of abjection removes sulfur recovery, the carbon dioxide high altitude discharge of removing；
(3) pure gas after purifying carry out synthesis of low-carbon alcohol reaction, and obtained gas-liquid two-phase product carries out gas-liquid separation, point
From gas mainly include CO, H2And CO2A part is sent to low-temp methanol and washes circulation, and another part sends to torch as periodic off-gases
Burning and exhausting, the liquid product of separation is alcohol-water mixture, and alcohol-water mixture carries out alcohol-water separation, obtains water and low-carbon alcohols production
Product.
The operation temperature that low-temp methanol as described above is washed is -35~-55 DEG C, operating pressure 2.0-6.5MPa, is passed through
Low-temp methanol wash after synthesis gas in H2S<0.1ppm,CO2<20ppm。
The coarse raw materials gas complicated component formed due to synthesis gas and coke-stove gas.Its gas component includes CO, H2、CO2、CH4
The H of denier2S, organic sulfur, tar, aliphatic acid, naphtha etc..CO, H are removed in these components2Active principle, remaining all groups
Dividing includes CO2All it is the objectionable impurities for needing to remove with sulfide, it is seen that it purifies the arduousness of task.Make a general survey of current various gases
Purification technique, can take on this person with heavy responsibilities's non-cryogenic methanol and wash and do not belong to.Because only low temperature methanol cleaningization just can be same
All various harmful components, such as CO are neatly removed in one device2、H2S、COS、C4H4S、HCN、NH3、H2O、C2Above hydro carbons
(including light oil, aromatic hydrocarbon, naphtha, alkene and colloid etc.) and other carbonyls etc., and other any purification works
Skill can not all accomplish.In addition, low-temp methanol washing process also has following various significant excellent compared with other purification techniques
Point：
1. absorbability is strong, solution internal circulating load is small
2. methanol solvate is cheap and easy to get, regeneration energy consumption is low
3. gas purification degree is high
4. solvent heat endurance and chemical stability are good, solvent is non-degradable, non-foaming, and equipment is not corroded
5. first alcohol and water can be dissolved each other with arbitrary proportion, its dry feedstock gas can be used using this characteristic
Low-temp methanol washes the removing for realizing plurality of impurities in the same apparatus, relative to a variety of net of other purification methods
For changing process combination, process is relatively single, reasonable, management easy to operation.
Low-carbon alcohols reactor as described above uses one or more series connection fixed bed reactors, and reaction process condition is：
Reaction pressure 3-10MPa, reaction temperature are 240-410 DEG C, H:Cmoleratio H2/ CO=2.0-5.0, preferable 2.2-4.5,
Air speed is 5000-50000h-1Under the conditions of carry out low-carbon alcohols synthesis.
The catalyst that higher alcohols synthesis as described above uses is using the MoS of DOW chemical companies of the U.S.2- M-K is catalyzed
Agent, the modification Cu-Zn-Al-K series catalysts of German Lurgi companies, the Cu-Co-Cr-K catalysis of IFP (IFP)
Agent, the Zn-Cr catalyst of Shanxi Inst. of Coal Chemistry, Chinese Academy of Sciences or one kind in Japanese Cu-Ni-Zr-Na catalyst or
It is several.
Return as described above low-temp methanol wash circulation gas account for separation volume of gas for 30-90%.
Alcohol-water separation as described above is taken off using benzene azeotropic distillation technology, ion exchange resin, membrane separation technique, molecular sieve
One kind of water technology, operating condition are：80-150 DEG C of temperature, pressure are normal pressure or decompression,
Mass percent composition hilltop methanol accounts for 20-30%, ethanol 40-60%, propyl alcohol in low-carbon alcohols product as described above
12-20%, other alcohol 8-20%.
The present invention has the following advantages that compared with prior art：
The present invention makes full use of the coke-stove gas composition more carbon of hydrogen few, and synthesizes the characteristics of more hydrogen of gas carbon are few, and both are pressed into one
Certainty ratio mixes, and has complementary advantages, reaches the hydrogen-carbon ratio for meeting synthesis of low-carbon alcohol, solves individually given birth to using coke-stove gas well
Produce low-carbon alcohols need it is a large amount of mend carbon or a large amount of the shortcomings that mending hydrogen individually needed using low carbon alcohol by synthetic gas, be coke-stove gas and
Reasonable utilize of synthesis gas provides a kind of effective way, realizes good and bad complementation, makes the best use of everything, be advantageous to product diversification, adjusts
Superfluous production capacity is saved, promotes energy-saving and emission-reduction, readjusts the energy structure, moreover it is possible to significantly improve Business Economic Benefit and social environment benefit.
Brief description of the drawings
The process chart of Fig. 1 present invention.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail, and these embodiments are only used in more detail specifically
The bright present invention, and the scope that should not be construed as the above-mentioned theme of the present invention is only limitted to the limitation of following embodiments.
Embodiment 1
By coke-stove gas, (percent by volume composition is H2：54%, CH4：23%, CO:10%, CO2:7%, N2：6%) and
(percent by volume composition is CO to synthesis gas：50%, H2：25%, CO2：12, CH4：12%, H2S：0.16%) by volume 7:1
It is passed through gas holder to be sufficiently mixed, formation meets that higher alcohols synthesis H:Cmoleratio is H2/ CO=3.5 coarse raw materials gas.
Coarse raw materials gas is compressed to be put to 4.0MPa into low temperature methanol cleaning makeup, and removing hydrogen sulfide and carbon dioxide etc. is miscellaneous
Matter, by H in coarse raw materials gas under the conditions of -40 DEG C2S is taken off to less than 0.1ppm, CO2Less than 20ppm, the pure of synthesis of low-carbon alcohol is made
Net gas, the hydrogen sulfide H of removing2S removes sulfur recovery, the CO of removing2High altitude discharge.
Pure gas after purification enter two series connection fixed bed low-carbon alcohols reactors, changing using German Lurgi companies
Property Cu-Zn-Al-K series catalysts, are 4MPa in reaction pressure, 350 DEG C of reaction temperature, H:Cmoleratio H2/ CO=3.5, it is empty
Speed is 25000h-1Under the conditions of carry out synthesis of low-carbon alcohol reaction,
Obtained gas-liquid two-phase product enters gas-liquid separator, and the gas of separation mainly includes CO, H2And CO2, by volume hundred
Point being sent to low-temp methanol than will separate the 60% of gas washes circulation, and another 40% sends to torch burning as periodic off-gases discharges,
The liquid product (alcohol-water mixture) of separation is sent into alcohol-water separation device, using membrane separation technique, in normal pressure and 95
Alcohol-water mixture is isolated to water and low-carbon alcohols product (mass percent product form under the conditions of DEG C：Methanol accounts for 25%, second
Alcohol 50%, propyl alcohol 15%, other alcohol 10%).
Embodiment 2
By coke-stove gas, (percent by volume composition is H2：60%, CH4：22%, CO:9%, CO2:6%, N2：3%) and close
Into gas, (percent by volume composition is CO：50%, H2：27%, CO2：11%, CH4：12%, H2S：0.20%) by volume 5:1
It is passed through gas holder to be sufficiently mixed, formation meets that higher alcohols synthesis H:Cmoleratio is H2/ CO=4.0 coarse raw materials gas.
Coarse raw materials gas is compressed to be put to 4.5MPa into low temperature methanol cleaning makeup, and removing hydrogen sulfide and carbon dioxide etc. is miscellaneous
Matter, by H in coarse raw materials gas under the conditions of -43 DEG C2S is taken off to less than 0.1ppm, CO2Less than 20ppm, the pure of synthesis of low-carbon alcohol is made
Net gas, the hydrogen sulfide H of removing2S removes sulfur recovery, the CO of removing2High altitude discharge.
Pure gas after purification enter two series connection fixed bed low-carbon alcohols reactors, and first fixed bed reactors is adopted
With the Zn-Cr catalyst of Shanxi Inst. of Coal Chemistry, Chinese Academy of Sciences, second fixed bed reactors is ground using french petroleum
Study carefully the Cu-Co-Cr-K catalyst of institute (IFP), be 4.5MPa in reaction pressure, 270 DEG C of reaction temperature, H:Cmoleratio H2/
CO=4.0, air speed 20000h-1Under the conditions of carry out synthesis of low-carbon alcohol reaction,
Obtained gas-liquid two-phase product enters gas-liquid separator, and the gas of separation mainly includes CO, H2And CO2, by volume hundred
Point being sent to low-temp methanol than will separate the 70% of gas washes circulation, and another 30% sends to torch burning as periodic off-gases discharges,
The liquid product (alcohol-water mixture) of separation is sent into alcohol-water separation device, using benzene azeotropic distillation technology, in normal pressure
With 105 DEG C under the conditions of alcohol-water mixture is isolated to water and low-carbon alcohols product (mass percent product form：Methanol accounts for
23%, ethanol 56%, propyl alcohol 12%, other alcohol 9%).
Embodiment 3
By coke-stove gas, (percent by volume composition is H2：58%, CH4：24%, CO:8%, CO2:6%, N2：4%) and close
Into gas, (percent by volume composition is CO：50%, H2：26%, CO2：11%, CH4：13%, H2S：0.24%) by volume 3:1
It is passed through gas holder to be sufficiently mixed, formation meets that higher alcohols synthesis H:Cmoleratio is H2/ CO=2.7 coarse raw materials gas.
Coarse raw materials gas is compressed to be put to 3.8MPa into low temperature methanol cleaning makeup, and removing hydrogen sulfide and carbon dioxide etc. is miscellaneous
Matter, by H in coarse raw materials gas under the conditions of -49 DEG C2S is taken off to less than 0.1ppm, CO2Less than 20ppm, the pure of synthesis of low-carbon alcohol is made
Net gas, the hydrogen sulfide H of removing2S removes sulfur recovery, the CO of removing2High altitude discharge.
Pure gas after purification enter three series connection fixed bed low-carbon alcohols reactors, and first fixed bed reactors is using beautiful
The MoS of DOW chemical companies of state2- M-K catalyst, latter two fixed bed catalyst use the modification Cu- of German Lurgi companies
Zn-Al-K catalyst, it is 3.8MPa in reaction pressure, 340 DEG C of reaction temperature, H:Cmoleratio H2/ CO=2.6, air speed are
32000h-1Under the conditions of carry out synthesis of low-carbon alcohol reaction,
Obtained gas-liquid two-phase product enters gas-liquid separator, and the gas of separation mainly includes CO, H2And CO2, by volume hundred
Point being sent to low-temp methanol than will separate the 50% of gas washes circulation, and another 50% sends to torch burning as periodic off-gases discharges,
The liquid product (alcohol-water mixture) of separation is sent into alcohol-water separation device, using ion-exchange resin technique, subtracted
Alcohol-water mixture is isolated to water and low-carbon alcohols product (mass percent product form under the conditions of pressure and 85 DEG C：Methanol accounts for
28%, ethanol 51%, propyl alcohol 10%, other alcohol 11%).
Embodiment 4
By coke-stove gas, (percent by volume composition is H2：53%, CH4：26%, CO:9%, CO2:7%, N2：5%) and close
Into gas, (percent by volume composition is CO：52%, H2：23%, CO2：14%, CH4：11%, H2S：0.31%) by volume 7.6:
1, which is passed through gas holder, is sufficiently mixed, and formation meets that higher alcohols synthesis H:Cmoleratio is H2/ CO=4.1 coarse raw materials gas,
Coarse raw materials gas is compressed to be put to 5.0MPa into low temperature methanol cleaning makeup, and removing hydrogen sulfide and carbon dioxide etc. is miscellaneous
Matter, by H in coarse raw materials gas under the conditions of -35 DEG C2S is taken off to less than 0.1ppm, CO2Less than 20ppm, the pure of synthesis of low-carbon alcohol is made
Net gas, the hydrogen sulfide H of removing2S removes sulfur recovery, the CO of removing2High altitude discharge.
Pure gas after purification enter single fixed bed low-carbon alcohols reactor, and catalyst is using DOW chemical companies of the U.S.
MoS2- M-K catalyst, it is 5.0MPa in reaction pressure, 320 DEG C of reaction temperature, H:Cmoleratio H2/ CO=4.1, air speed are
37000h-1Under the conditions of carry out synthesis of low-carbon alcohol reaction,
Obtained gas-liquid two-phase product enters gas-liquid separator, and the gas of separation mainly includes CO, H2And CO2, by volume hundred
Point being sent to low-temp methanol than will separate the 75% of gas washes circulation, and another 25% sends to torch burning as periodic off-gases discharges,
The liquid product (alcohol-water mixture) of separation is sent into alcohol-water separation device, using molecular sieve dehydration technology, depressurized
With 90 DEG C under the conditions of alcohol-water mixture is isolated to water and low-carbon alcohols product (mass percent product form：Methanol accounts for
21%, ethanol 53%, propyl alcohol 11%, other alcohol 15%).
Claims (3)
1. a kind of technique that coke-stove gas low-carbon alcohols are combined by synthesis gas, it is characterised in that comprise the following steps：
(1) coke-stove gas and synthesis gas are passed through into gas holder to be sufficiently mixed, form the coarse raw materials gas for meeting higher alcohols synthesis hydrogen-carbon ratio；
(2) coarse raw materials gas is compressed carries out low temperature methanol cleaning, removes the impurity such as hydrogen sulfide and carbon dioxide, it is low that synthesis is made
The pure gas of carbon alcohol, the hydrogen sulfide of abjection remove sulfur recovery, the carbon dioxide high altitude discharge of removing；
(3) pure gas after purifying carry out synthesis of low-carbon alcohol reaction, and obtained gas-liquid two-phase product carries out gas-liquid separation, separation
Gas mainly includes CO, H2And CO2A part is sent to low-temp methanol and washes circulation, and another part sends to torch burning as periodic off-gases
Discharge, the liquid product of separation is alcohol-water mixture, and alcohol-water mixture carries out alcohol-water separation, obtains water and low-carbon alcohols product；
The coke-stove gas percent by volume composition is H2：50-60%, CH4：20-28%, CO+CO2:10-18%, N2：3-8%,
Synthesis gas percent by volume composition is CO：45-60%, H2：20-28%, CO2：8-18, CH4：7-15%, H2S：0.15-
0.35%；
The operation temperature that described low-temp methanol is washed is -35~-55 DEG C, operating pressure 2.0-6.5MPa, by low-temp methanol
H in synthesis gas after washing2S<0.1ppm,CO2<20ppm；
Described alcohol-water separation using benzene azeotropic distillation technology, ion exchange resin, membrane separation technique, molecular sieve dehydration technology
One kind, operating condition are：80-150 DEG C of temperature, pressure are normal pressure or decompression；
Described low-carbon alcohols reaction uses one or more series connection fixed bed reactors, and reaction process condition is：Reaction pressure 3-
10MPa, reaction temperature are 240-410 DEG C, H:Cmoleratio H2/ CO=2.0-5.0, air speed 5000-50000h-1Under the conditions of
Carry out the synthesis of low-carbon alcohols；
The catalyst that described higher alcohols synthesis uses is using the MoS of DOW chemical companies of the U.S.2- M-K catalyst, Germany
The modification Cu-Zn-Al-K series catalysts of Lurgi companies, the Cu-Co-Cr-K catalyst of IFP, the Chinese Academy of Sciences
One or more in the Zn-Cr catalyst of Shanxi coal chemistry institute or Japanese Cu-Ni-Zr-Na catalyst；
Mass percent composition methanol accounts for 20-30%, ethanol 40-60%, propyl alcohol 12-20% in described low-carbon alcohols product, its
Its alcohol 8-20%.
2. a kind of technique that coke-stove gas low-carbon alcohols are combined by synthesis gas as claimed in claim 1, it is characterised in that described
H:Cmoleratio be H2/ CO=2.2-4.5.
3. a kind of technique that coke-stove gas low-carbon alcohols are combined by synthesis gas as claimed in claim 1, it is characterised in that described
Return low-temp methanol wash circulation gas account for separation volume of gas for 30-90%.
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