CN111807926A - Reaction system and method for preparing ethanol from coal - Google Patents
Reaction system and method for preparing ethanol from coal Download PDFInfo
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- CN111807926A CN111807926A CN202010683566.4A CN202010683566A CN111807926A CN 111807926 A CN111807926 A CN 111807926A CN 202010683566 A CN202010683566 A CN 202010683566A CN 111807926 A CN111807926 A CN 111807926A
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 130
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 119
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000003245 coal Substances 0.000 title claims abstract description 24
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 224
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims abstract description 180
- 238000005810 carbonylation reaction Methods 0.000 claims abstract description 55
- 230000006315 carbonylation Effects 0.000 claims abstract description 35
- 239000002994 raw material Substances 0.000 claims abstract description 30
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 12
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910002091 carbon monoxide Inorganic materials 0.000 claims abstract description 11
- 230000003197 catalytic effect Effects 0.000 claims abstract description 11
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 9
- 238000002309 gasification Methods 0.000 claims abstract description 3
- 239000012071 phase Substances 0.000 claims description 36
- 239000000047 product Substances 0.000 claims description 36
- 238000005984 hydrogenation reaction Methods 0.000 claims description 34
- 239000007789 gas Substances 0.000 claims description 33
- 238000005406 washing Methods 0.000 claims description 26
- 238000000926 separation method Methods 0.000 claims description 23
- 239000007795 chemical reaction product Substances 0.000 claims description 16
- 239000007791 liquid phase Substances 0.000 claims description 16
- 238000000605 extraction Methods 0.000 claims description 14
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 12
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 238000000746 purification Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000004891 communication Methods 0.000 claims description 2
- 150000002431 hydrogen Chemical class 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 9
- 239000006185 dispersion Substances 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 description 16
- 239000003054 catalyst Substances 0.000 description 13
- 230000000694 effects Effects 0.000 description 13
- 239000000126 substance Substances 0.000 description 12
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 230000008901 benefit Effects 0.000 description 6
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- 238000004519 manufacturing process Methods 0.000 description 5
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- 238000003860 storage Methods 0.000 description 5
- 239000002351 wastewater Substances 0.000 description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 3
- 239000005977 Ethylene Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000000855 fermentation Methods 0.000 description 3
- 230000004151 fermentation Effects 0.000 description 3
- 238000013467 fragmentation Methods 0.000 description 3
- 238000006062 fragmentation reaction Methods 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 239000003345 natural gas Substances 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 240000008042 Zea mays Species 0.000 description 2
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 2
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003034 coal gas Substances 0.000 description 2
- 235000005822 corn Nutrition 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- 240000003183 Manihot esculenta Species 0.000 description 1
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 1
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910003158 γ-Al2O3 Inorganic materials 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/09—Preparation of ethers by dehydration of compounds containing hydroxy groups
-
- 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
- C07C29/132—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 an oxygen containing functional group
- C07C29/136—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 an oxygen containing functional group of >C=O containing groups, e.g. —COOH
- C07C29/147—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 an oxygen containing functional group of >C=O containing groups, e.g. —COOH of carboxylic acids or derivatives thereof
- C07C29/149—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 an oxygen containing functional group of >C=O containing groups, e.g. —COOH of carboxylic acids or derivatives thereof with hydrogen or hydrogen-containing gases
-
- 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
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
- C07C41/42—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/58—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/36—Preparation of carboxylic acid esters by reaction with carbon monoxide or formates
- C07C67/37—Preparation of carboxylic acid esters by reaction with carbon monoxide or formates by reaction of ethers with carbon monoxide
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
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Abstract
The invention provides a reaction system and a method for preparing ethanol from coal, wherein the reaction system comprises: the system comprises a methanol-to-dimethyl ether reaction unit and a dimethyl ether-to-ethanol reaction unit which are connected in sequence, wherein the methanol is prepared by coal gasification; the reaction unit for preparing dimethyl ether from methanol comprises: a dimethyl ether reactor; introducing methanol into the dimethyl ether reactor to perform gas phase catalytic dehydration reaction; the dimethyl ether-to-ethanol reaction unit comprises: the carbonylation reactor the outside of carbonylation reactor is provided with first little interface generator, first little interface generator lets in follow dimethyl ether and carbon monoxide that the strip tower separated out, process the broken back entering of dispersion of first little interface generator the carbonylation reactor reacts. The reaction system provided by the invention reduces the energy consumption, reduces the reaction temperature, improves the utilization rate of raw materials, and effectively improves the productivity.
Description
Technical Field
The invention relates to the field of ethanol preparation from coal, and particularly relates to a reaction system and method for preparing ethanol from coal.
Background
The production routes of ethanol worldwide include grain fermentation routes, petrochemical routes, and carbon-chemical routes such as coal and natural gas. The grain fermentation route is widely applied internationally, and large-scale ethanol production enterprises mostly adopt grain fermentation processes. Influenced by the 'grain crisis', the new corn fuel ethanol project is stopped to be approved in China at present. The cellulose fuel ethanol project fermented by cassava and corn straws has poor economic benefit due to high production cost, excessive dependence on national subsidies, imperfect production technology and other factors. The petrochemical route uses ethylene as raw material to prepare fuel ethanol by ethylene hydration method. China depends on import of a large amount of petroleum, and the price of ethylene is often higher than that of ethanol, so that the application and popularization of the method in China are restricted.
The carbon chemical industrial route of coal, natural gas and the like is a method for preparing synthetic gas and methanol by using coal or natural gas as raw materials and then preparing ethanol by a dimethyl ether method or an acetic acid method. However, the method has a series of problems of high reaction pressure, high temperature, high energy consumption, low raw material utilization rate, low productivity and the like.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the present invention is to provide a reaction system for producing ethanol from coal, which combines the reaction system with a micro-interface generator, thereby reducing energy consumption, reducing reaction temperature, increasing reaction yield, particularly increasing the utilization rate of reaction gas phase, and effectively increasing productivity, further increasing product quality and yield, and further saving equipment cost and equipment floor space.
The second purpose of the invention is to provide a reaction method for preparing ethanol from coal by adopting the reaction system, the reaction method fully disperses and crushes reaction raw materials, improves the mass transfer efficiency of the reaction, improves the conversion rate of the reaction raw materials, and correspondingly improves the yield of products.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
the invention provides a reaction system for preparing ethanol from coal, which comprises: the system comprises a methanol-to-dimethyl ether reaction unit and a dimethyl ether-to-ethanol reaction unit which are connected in sequence, wherein the methanol is prepared by coal gasification;
the reaction unit for preparing dimethyl ether from methanol comprises: a dimethyl ether reactor; introducing methanol into the dimethyl ether reactor to carry out gas phase catalytic dehydration reaction, introducing a product after the reaction into a first rectifying tower to carry out dimethyl ether purification, sending a rectified gas phase to a washing tower to recover the dimethyl ether in the gas phase, sending a rectified liquid phase to a stripping tower to carry out separation of the methanol and the dimethyl ether, and sending the separated dimethyl ether to a dimethyl ether-to-ethanol reaction unit;
the dimethyl ether-to-ethanol reaction unit comprises: the device comprises a carbonylation reactor, wherein a first micro-interface generator is arranged on the outer side of the carbonylation reactor, dimethyl ether and carbon monoxide separated from a stripping tower are introduced into the first micro-interface generator, and enter the carbonylation reactor for reaction after being dispersed and crushed by the first micro-interface generator, the carbonylation reactor is connected with a second micro-interface generator so as to introduce carbonylation products into the second micro-interface generator, hydrogen is simultaneously introduced into the second micro-interface generator, the second micro-interface generator is dispersed and crushed by the second micro-interface generator and then enters a hydrogenation reactor for methyl acetate hydrogenation, and reaction products after the hydrogenation reaction are subjected to separation of methanol and ethanol through a second rectifying tower to obtain ethanol.
According to the reaction system for preparing the ethanol from the coal, the micro-interface generator is correspondingly arranged in front of the carbonylation reactor and the hydrogenation reactor, and the entering gas phase is dispersed and crushed into micro-bubbles, so that the mass transfer effect is improved.
In addition, in the reaction system of the invention, micro-interface generators are required to be arranged in front of the carbonylation reactor and the hydrogenation reactor, because the reactions in the two reactors are both gas-liquid two-phase reactions, the arranged micro-interface generators can just play a role of dispersing and crushing gas phase, and because the micro-interface generators are arranged, dimethyl ether does not need to be gasified firstly, and can be directly introduced into the micro-interface generators to be mixed, dispersed and crushed with carbon monoxide, thereby simplifying the operation steps.
Preferably, the number of the first micro-interface generator or the second micro-interface generator is not unique, and in order to increase the mass transfer effect, the number of the micro-interface generators can be correspondingly increased, the micro-interface generators are preferably arranged in a manner of being sequentially arranged from top to bottom, and the micro-interface generators are preferably in a parallel connection relationship.
The first micro-interface generator and the second micro-interface generator are both in a pneumatic type, and the gas phase is introduced into the micro-interface generator and then is broken into micro bubbles after being directly contacted with the liquid phase, so that the mass transfer effect is improved.
Certainly, except for the mode of arranging the micro-interface generator in the reactor, the micro-interface generator can also be correspondingly arranged in the reactor, but the optimal mode is to arrange the micro-interface generator in front of the reactor, and the micro-interface generator is required to be arranged in front of the carbonylation reactor and the hydrogenation reactor, so that the pressure in the reaction process is ensured not to be too high, the raw materials are not required to be gasified, the centralized control is facilitated, the safety of the equipment operation is also improved, if one micro-interface generator is arranged less, the controllability of the material pressure in the whole process flow is reduced, the pressure is different, and the effect of reducing the energy consumption cannot be fully achieved.
It will be appreciated by those skilled in the art that the micro-interface generator used in the present invention is described in the prior patents of the present inventor, such as the patents of application nos. CN201610641119.6, 201610641251.7, CN201710766435.0, CN106187660, CN105903425A, CN109437390A, CN205833127U and CN 207581700U. The detailed structure and operation principle of the micro bubble generator (i.e. micro interface generator) is described in detail in the prior patent CN201610641119.6, which describes that "the micro bubble generator comprises a body and a secondary crushing member, wherein the body is provided with a cavity, the body is provided with an inlet communicated with the cavity, the opposite first end and second end of the cavity are both open, and the cross-sectional area of the cavity decreases from the middle of the cavity to the first end and second end of the cavity; the secondary crushing member is disposed at least one of the first end and the second end of the cavity, a portion of the secondary crushing member is disposed within the cavity, and an annular passage is formed between the secondary crushing member and the through holes open at both ends of the cavity. The micron bubble generator also comprises an air inlet pipe and a liquid inlet pipe. "the specific working principle of the structure disclosed in the application document is as follows: liquid enters the micro-bubble generator tangentially through the liquid inlet pipe, and gas is rotated at a super high speed and cut to break gas bubbles into micro-bubbles at a micron level, so that the mass transfer area between a liquid phase and a gas phase is increased, and the micro-bubble generator in the patent belongs to a pneumatic micro-interface generator.
In addition, the first patent 201610641251.7 describes that the primary bubble breaker has a circulation liquid inlet, a circulation gas inlet and a gas-liquid mixture outlet, and the secondary bubble breaker communicates the feed inlet with the gas-liquid mixture outlet, which indicates that the bubble breakers all need to be mixed with gas and liquid, and in addition, as can be seen from the following drawings, the primary bubble breaker mainly uses the circulation liquid as power, so that the primary bubble breaker belongs to a hydraulic micro-interface generator, and the secondary bubble breaker simultaneously introduces the gas-liquid mixture into an elliptical rotating ball for rotation, thereby realizing bubble breaking in the rotating process, so that the secondary bubble breaker actually belongs to a gas-liquid linkage micro-interface generator. In fact, the micro-interface generator is a specific form of the micro-interface generator, whether it is a hydraulic micro-interface generator or a gas-liquid linkage micro-interface generator, however, the micro-interface generator adopted in the present invention is not limited to the above forms, and the specific structure of the bubble breaker described in the prior patent is only one of the forms that the micro-interface generator of the present invention can adopt.
Furthermore, the prior patent 201710766435.0 states that the principle of the bubble breaker is that high-speed jet flows are used to achieve mutual collision of gases, and also states that the bubble breaker can be used in a micro-interface strengthening reactor to verify the correlation between the bubble breaker and the micro-interface generator; moreover, in the prior patent CN106187660, there is a related description on the specific structure of the bubble breaker, see paragraphs [0031] to [0041] in the specification, and the accompanying drawings, which illustrate the specific working principle of the bubble breaker S-2 in detail, the top of the bubble breaker is a liquid phase inlet, and the side of the bubble breaker is a gas phase inlet, and the liquid phase coming from the top provides the entrainment power, so as to achieve the effect of breaking into ultra-fine bubbles, and in the accompanying drawings, the bubble breaker is also seen to be of a tapered structure, and the diameter of the upper part is larger than that of the lower part, and also for better providing the entrainment power for the liquid phase. Since the micro-interface generator was just developed in the early stage of the prior patent application, the micro-interface generator was named as a micro-bubble generator (CN201610641119.6), a bubble breaker (201710766435.0) and the like in the early stage, and is named as a micro-interface generator in the later stage along with the continuous technical improvement, and the micro-interface generator in the present invention is equivalent to the micro-bubble generator, the bubble breaker and the like in the prior art, and has different names.
In summary, the micro-interface generator of the present invention belongs to the prior art, although some bubble breakers belong to the type of pneumatic bubble breakers, some bubble breakers belong to the type of hydraulic bubble breakers, and some bubble breakers belong to the type of gas-liquid linkage bubble breakers, the difference between the types is mainly selected according to the different specific working conditions, and in addition, the connection between the micro-interface generator and the reactor and other equipment, including the connection structure and the connection position, is determined according to the structure of the micro-interface generator, which is not limited.
The reaction system comprises a reaction unit for preparing dimethyl ether from methanol and a reaction unit for preparing ethanol from dimethyl ether.
Wherein, the reaction unit for preparing dimethyl ether from methanol mainly comprises the following equipment: the dimethyl ether reactor, a first rectifying tower, a washing tower and a stripping tower.
The methanol is firstly subjected to gas phase catalytic dehydration reaction in a dimethyl ether reactor to generate dimethyl ether, the reaction temperature is 250-270 ℃, the pressure is 1.2MPa, and the catalyst is generally a molecular sieve, such as a ZSM molecular sieve, aluminum phosphate or gamma-Al2O3. The dimethyl ether generated by methanol dehydration is an exothermic reaction, and the temperature of the product gas at the outlet of the reactor is 320-330 ℃. The main reaction products are dimethyl ether and water, and the side reaction products are carbon oxide, methane, hydrocarbon and the like.
Preferably, the methanol-to-dimethyl ether reaction unit comprises a methanol pump, and the methanol is transported by the methanol pump to a part of the dimethyl ether reactor and a part of the washing tower as the washing solvent. That is, the methanol raw material in the dimethyl ether reactor is delivered by a methanol pump, and a part of the methanol which is led to the washing tower is used for absorbing and recovering the dimethyl ether by taking the methanol or the methanol-water solution as a washing solvent in the washing tower.
Preferably, the reaction unit for preparing dimethyl ether from methanol comprises a heat exchanger, and the heat exchanger is used for carrying out heat exchange on raw material methanol and a gas-phase catalytic dehydration reaction product.
Preferably, the heat exchanger is arranged between the dimethyl ether reactor and the first rectifying tower, and a preheater is further arranged between the heat exchanger and the dimethyl ether reactor. Just because the dimethyl ether prepared by dehydrating methanol belongs to exothermic reaction, a preheater and a heat exchanger are correspondingly arranged, and the heat exchanger can exchange heat between a reaction product and a raw material, thereby achieving the purpose of effectively utilizing heat.
After heat exchange, the reaction product enters the first rectifying tower and the stripping tower in sequence for purification, and then a pure dimethyl ether product can be formed for subsequent ethanol synthesis.
Preferably, the top of the first rectification column and the top of the stripping column are in communication with the wash column via a conduit for returning methanol for reuse.
The first rectifying tower is mainly used for purifying dimethyl ether products, the stripping tower is mainly used for recovering methanol, after the gas-phase methanol recovered from the top of the first rectifying tower is liquefied by the tower top condenser, one part of the gas-phase methanol flows back to the first rectifying tower, the other part of the gas-phase methanol flows to the washing tower, and the returned methanol can also be directly used as reaction raw materials. The material that comes out from first rectifying column bottom is the dimethyl ether for the majority, and a small amount of methanol, then enters into the stripper and carries out the recovery of methanol, and the methanol that goes out from the stripper top is sent to the scrubbing tower, also can directly be as the reaction raw materials similarly, and the stripper bottom has set up the circulation steam line that provides power for the strip, still is provided with the waste water discharge port in addition for directly discharging the waste water that produces in the stripping process.
Preferably, the first rectifying tower and the stripping tower are both provided with side draws, and the side draws of the first rectifying tower and the stripping tower are converged and then connected with the first micro-interface generator. The main product extraction of the first rectifying tower and the stripping tower is carried out through side extraction, and the dimethyl ether product is conveyed to the first micro-interface generator after the two side extraction outlets are jointly converged for subsequent ethanol synthesis process.
The reaction unit for preparing ethanol from dimethyl ether mainly comprises the following equipment: the device comprises a carbonylation reactor, a separation tower, a hydrogenation reactor and a second rectifying tower.
Preferably, the carbonylation reactor for carrying out the carbonylation reaction is a fixed bed reaction kettle, the catalyst in the fixed bed reaction kettle is fixed on the bed layer, and the fixed bed layer is generally arranged on 3 layers to meet the reaction requirement of catalysis.
Dimethyl ether products from a reaction unit for preparing dimethyl ether from methanol do not need to be gasified and are directly introduced into a first micro-interface generator, carbon monoxide is also introduced into the first micro-interface generator, the carbon monoxide is crushed into micro-bubbles under the action of liquid-phase dimethyl ether and then enters a carbonylation reactor to carry out carbonylation reaction, in order to improve the reaction effect, feed inlets are arranged on the side wall and the top of the carbonylation reactor, and the feed inlets on the side wall are preferably arranged between two fixed bed layers.
Preferably, a separation column is provided between the carbonylation reactor and the second micro-interface generator for removing gas phase impurities from the carbonylation product. The method comprises the steps that carbon monoxide and dimethyl ether are subjected to carbonylation reaction under the action of a catalyst to obtain a carbonylation product, the main component of the carbonylation product is methyl acetate, and then some unreacted dimethyl ether exists, after the carbonylation product is subjected to steam stripping through a separation tower, the top of the separation tower is mainly unreacted dimethyl ether, the unreacted dimethyl ether can be directly returned to a first micro-interface generator through a separation tank arranged at the top of the separation tower to serve as reaction feeding of carbonylation, and a liquid phase discharged from the bottom of the separation tank is directly returned to the separation tower to be subjected to steam stripping separation and purification again.
And the substances discharged from the bottom of the separation tower are mainly methyl acetate and are conveyed into the second micro-interface generator through a pump, and in order to improve the action effect of the second micro-interface generator, the methyl acetate is preheated by a preheater and then is introduced into the second micro-interface generator. And simultaneously introducing hydrogen into the second micro-interface generator, and after the hydrogen is crushed into micro bubbles under the action of the liquid-phase methyl acetate, feeding the micro bubbles into the hydrogenation reactor for hydrogenation reaction.
Preferably, the hydrogenation reactor for hydrogenation reaction is a fixed bed reactor, the catalyst in the fixed bed reactor is fixed on the bed layer, the catalyst for hydrogenation reaction is generally nickel-based catalyst, preferably the catalyst can be supported nickel-based catalyst, or nickel-based catalyst modified by alkaline earth metal oxide or rare earth metal oxide is more preferable.
Methyl acetate generates methanol and ethanol after hydrogenation reaction, and then enters a second rectifying tower for ethanol refining, the operating pressure of the top of the second rectifying tower is about 0.03MPa, steam at the top of the second rectifying tower is condensed to 61.7 ℃, and part of a condensed liquid phase (a large amount of methanol) returns to the second rectifying tower and part of the condensed liquid phase goes to a reaction unit for preparing dimethyl ether from methanol, and is used as a reaction raw material for preparing dimethyl ether.
Preferably, the top of the second rectifying tower is provided with a methanol outlet, the methanol outlet is communicated with the washing tower through a pipeline so as to be used for returning methanol to be recycled, and the bottom of the second rectifying tower is provided with a product extraction outlet for extracting ethanol products.
And after the substances discharged from the methanol outlet are condensed by the overhead condenser, one part of the substances returns to the second rectifying tower again, and the other part of the substances is communicated with the washing tower through a pipeline so as to return the methanol for recycling.
And a product extraction port arranged at the bottom of the second rectifying tower is used for extracting refined ethanol, the temperature is about 101 ℃, the refined ethanol extracted from the extraction port is cooled to 40 ℃ in an ethanol cooler, then the cooled refined ethanol passes through an ethanol buffer tank and is conveyed to an ethanol product tank area by a pump, and an ethanol unqualified product tank is arranged in an intermediate tank area and is used when the automobile is started or the production is abnormal. And a small amount of rectification waste liquid, mainly comprising acetic acid, is generated at the bottom of the second rectifying tower in the process of refining the ethanol, and is cooled to normal temperature and then sent to a heavy component tank for storage.
The invention also provides a reaction method for preparing ethanol from coal, which comprises the following steps:
carrying out gas phase catalytic dehydration, rectification and steam stripping on the raw material methanol to obtain dimethyl ether;
after dimethyl ether and carbon monoxide are mixed, dispersed and crushed, carbonylation reaction is carried out to obtain a carbonylation reaction product;
and mixing, dispersing and crushing the carbonylation reaction product and hydrogen, carrying out hydrogenation reaction, and rectifying to obtain the ethanol.
Preferably, the pressure of the carbonylation reaction is 2.5-3.0MPa, and the temperature of the carbonylation reaction is 200-230 ℃.
Preferably, the pressure of the hydrogenation reaction is 2.5-3.0MPa, and the temperature of the hydrogenation reaction is 200-210 ℃.
In the prior art, the temperature of the dimethyl ether carbonylation reaction is selected to be 240-260 ℃, the pressure is selected to be 5.0MPa, the temperature of the hydrogenation reaction is selected to be 230-260 ℃, and the pressure is 5.0MPa, although the reaction activity of the catalyst and the selectivity of the product can be obviously improved by increasing the temperature, the catalyst deactivation can be accelerated by increasing the reaction temperature too high; the higher reaction pressure is beneficial to the carbonylation reaction and promotes the dimethyl ether conversion, but the liquefaction of raw materials or products and the inactivation of the catalyst are accelerated due to the overhigh reaction pressure, so that the reaction method not only properly reduces the reaction temperature and the reaction pressure and ensures the activity of the catalyst, but also reduces the energy consumption and ensures the reaction effect, and the yield and the conversion rate of the raw materials are still kept at a higher level.
The ethanol obtained by the coal-to-ethanol reaction has high yield and high purity, and the purity can reach 99.9%.
The reaction method for preparing the ethanol from the coal has the advantages of low reaction temperature, greatly reduced pressure and high liquid hourly space velocity, and is equivalent to improving the productivity and the product yield.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the reaction system for preparing the ethanol from the coal, the carbonylation reactor, the hydrogenation reactor and the micro-interface generator are combined, so that the energy consumption is reduced, the reaction temperature is reduced, the reaction yield is improved, and the utilization rate of raw materials is improved;
(2) according to the reaction system for preparing the ethanol from the coal, the micro-interface generator is arranged at a specific position, so that the operation steps are simplified, and the energy consumption of the whole process is reduced;
(3) the reaction method for preparing the ethanol from the coal has the advantages of low reaction temperature, greatly reduced pressure, high liquid hourly space velocity, capacity improvement, high yield of the ethanol obtained by the reaction, high purity and high product purity of 99.9%.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
fig. 1 is a schematic structural diagram of a reaction system for producing ethanol from coal according to an embodiment of the present invention.
Description of the drawings:
a 10-dimethyl ether reactor; 20-a preheater;
30-a heat exchanger; 40-a first rectification column;
401-overhead condenser; 402-column bottoms reboiler;
50-a first micro-interface generator; 60-CO storage tank;
a 70-carbonylation reactor; 80-a separation column;
90-a second micro-interface generator; 100-a hydrogen storage tank;
110-a hydrogenation reactor; 120-a second rectification column;
1201-methanol outlet; 1202-product extraction and export;
130-methanol pump; 140-a washing column;
150-stripper column.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings and the detailed description, but those skilled in the art will understand that the following described embodiments are some, not all, of the embodiments of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
In order to more clearly illustrate the technical solution of the present invention, the following description is made in the form of specific embodiments.
Examples
Referring to fig. 1, a schematic diagram of a specific structure of a reaction system for producing ethanol from coal according to an embodiment of the present invention is shown, where the reaction system includes two units, i.e., a reaction unit for producing dimethyl ether from methanol and a reaction unit for producing ethanol from dimethyl ether.
Wherein the dimethyl ether reaction unit comprises: the dimethyl ether reactor 10, the first rectifying tower 40, the washing tower 140 and the stripping tower 150, wherein a part of raw material methanol is conveyed to the dimethyl ether reactor 10 by a methanol pump 130, and the other part of raw material methanol is conveyed to the washing tower 140 to form washing solvent in the form of methanol or methanol-water solution in the washing tower 140 to absorb dimethyl ether in a gas phase. After methanol enters the dimethyl ether reactor 10 for gas-phase catalytic dehydration reaction, reaction products enter the first rectifying tower 40 for dimethyl ether purification, and the rectified tower top gas phase (mainly a small amount of gas-phase dimethyl ether, methanol and the like) goes to the washing tower 140 for gas-phase dimethyl ether recovery, and can also be directly returned to the dimethyl ether reactor 10 to be used as reaction raw materials.
The top of the first rectifying tower 40 is provided with an overhead condenser 401, and after the overhead gas phase passes through the overhead condenser 401, a part of the overhead gas phase returns to the first rectifying tower 40 again, and the other part of the overhead gas phase goes out of the overhead condenser 401 to the washing tower 140. The bottom of the first rectifying tower 40 is provided with a tower kettle reboiler 402, under the action of the tower kettle reboiler 402, the product (mainly liquid-phase dimethyl ether) flowing out of the tower kettle is sent to the stripping tower 150 to be stripped and purified, the tower kettle of the stripping tower 150 is provided with a steam pipeline to provide stripping power, the substance flowing out of the top of the stripping tower 150 is mainly gas-phase methanol and returns to the washing tower 140, or directly returns to the dimethyl ether reactor 10 to be reacted as a methanol raw material, and the bottom of the stripping tower 150 is provided with a wastewater discharge port for directly discharging wastewater generated in the stripping process.
Both the first rectifying tower 40 and the stripping tower 150 are provided with side line extraction mechanisms for extracting the product dimethyl ether, and side line extractions of the first rectifying tower and the stripping tower are converged and then sent to a dimethyl ether-to-ethanol reaction unit to serve as reaction raw materials of ethanol.
A heat exchanger 30 for exchanging heat between the raw material methanol and the gas phase catalytic dehydration reaction product is arranged between the dimethyl ether reactor 10 and the first rectifying tower 40, and a preheater 20 for preheating the raw material entering the dimethyl ether reactor 10 is also arranged between the heat exchanger 30 and the dimethyl ether reactor 10, so as to improve the reaction efficiency of the dimethyl ether reactor 10.
The reaction unit for preparing ethanol from dimethyl ether comprises: carbonylation reactor 70, first micro-interface generator 50, separation column 80, second micro-interface generator 90, hydrogenation reactor 110, and second rectification column 120.
The first rectifying tower 40 and the side line extraction for extracting the dimethyl ether product arranged on the stripping tower 150 are jointly converged and then sent to the first micro-interface generator 50, CO is introduced into the first micro-interface generator 50, carbon monoxide is conveyed from a CO storage tank 60, the carbon monoxide is jointly mixed with the dimethyl ether in the first micro-interface generator 50 and then dispersed and crushed, the mixture enters the carbonylation reactor 70 for carbonylation reaction, the main components of the carbonylation reaction product are methyl acetate and some unreacted dimethyl ether, after being stripped by the separation column 80, the unreacted dimethyl ether is mainly at the top of the separation column 80, the liquid phase from the bottom of the knockout drum is directly returned to the knockout drum 80 for stripping separation and purification again, and the liquid phase from the bottom of the knockout drum is directly returned to the first micro-interface generator 50 as the reaction feed for carbonylation.
The substance that goes out from the bottom of knockout tower 80 is mainly methyl acetate, convey into second micro interface generator 90 through the pump, in order to improve the effect of second micro interface generator 90, methyl acetate passes through preheater 20 and preheats earlier and then enters into second micro interface generator 90, meanwhile lets in hydrogen in second micro interface generator 90 simultaneously, hydrogen is conveyed through hydrogen storage tank 100, hydrogen enters into hydrogenation ware 110 after fully mixing with liquid phase methyl acetate in second micro interface generator 90 and smashing into the microbubble and carrying out hydrogenation.
Methyl acetate generates methanol and ethanol after hydrogenation reaction, the methanol and the ethanol are conveyed to the second rectifying tower 120 for ethanol refining, a methanol outlet 1201 is formed in the top of the second rectifying tower 120, the methanol outlet 1201 is communicated with the washing tower 140 through a pipeline so as to be used for returning the methanol to be recycled, and a product extraction outlet 1202 is formed in the bottom of the second rectifying tower 120 and is used for extracting product ethanol. The top of the second rectifying tower 120 is provided with a tower top condenser, the tower bottom is provided with a tower bottom reboiler, a part of substances discharged from the methanol outlet 1201 is condensed by the tower top condenser and returns to the second rectifying tower 120, and a part of the substances is discharged, and the discharged part can be sent to the washing tower 140 to be used as a washing agent to wash the gas phase dimethyl ether, and can also be directly returned to the dimethyl ether reactor 10 to be used as a reaction raw material.
The reaction system of the embodiment is provided with the micro-interface generator at a specific position, so that the mass transfer effect of the whole reaction is improved, the energy consumption is reduced, and the utilization rate of raw materials is improved.
In the above embodiment, it is not limited to setting a single micro-interface generator, and in order to increase the dispersion and mass transfer effects, additional micro-interface generators may be additionally provided, the installation position is not limited in practice, and the micro-interface generators may be external or internal, and when the micro-interface generators are internally installed, the micro-interface generators may be installed on the side wall in the kettle and arranged oppositely, so as to realize the opposite flushing of the micro-bubbles coming out from the outlet of the micro-interface generator, which is of course the best for the solution of the present invention, is to use the external micro-interface generator.
In the above embodiment, the number of the pump bodies is not specifically required, and the pump bodies may be arranged at corresponding positions as required.
The working process and principle of the coal-to-ethanol reaction system of the invention are briefly explained as follows:
nitrogen purges each device in the reaction system, then operation is carried out by starting, raw material methanol firstly carries out gas phase catalytic dehydration reaction in a dimethyl ether reactor 10, then goes to a first rectifying tower 40 for rectification, substances from the bottom of the first rectifying tower 40 go to a stripping tower 150 for steam stripping to generate dimethyl ether, substances from the top of the first rectifying tower 40 go to a washing tower 140 for gas phase dimethyl ether recovery, dimethyl ether extracted from a side line extraction mechanism of the first rectifying tower 40 and a side line extraction mechanism of the stripping tower 150 go to a first micro interface generator 50 to be mixed with CO for dispersion and fragmentation, the mixture after dispersion and fragmentation enters a carbonylation reactor 70 for carbonylation, reaction products after carbonylation go to a separation tower 80 for steam stripping separation, then goes to a second micro interface generator 90 after going from the bottom of the separation tower 80 to be mixed with hydrogen for dispersion and fragmentation and then goes to a hydrogenation reactor 110 for hydrogenation reaction, finally, the hydrogenation reaction product is sent to a second rectifying tower 120 for rectification to obtain the final product refined ethanol.
Wherein the pressure of the carbonylation reaction is 2.5-3.0MPa, and the temperature of the carbonylation reaction is 200-230 ℃.
The pressure of the hydrogenation reaction is 2.5-3.0MPa, and the temperature of the hydrogenation reaction is 200-210 ℃.
The above steps are repeated circularly to make the whole synthesis system run smoothly.
In a word, compared with the reaction system for preparing ethanol from coal in the prior art, the reaction system for preparing ethanol from coal has the advantages of fewer equipment components, small occupied area, low energy consumption, low cost, high safety, controllable reaction and high raw material conversion rate, is equivalent to providing a reaction system with stronger operability for the field of preparing ethanol from coal, and is worthy of wide popularization and application.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A reaction system for preparing ethanol from coal is characterized by comprising: the system comprises a methanol-to-dimethyl ether reaction unit and a dimethyl ether-to-ethanol reaction unit which are connected in sequence, wherein the methanol is prepared by coal gasification;
the reaction unit for preparing dimethyl ether from methanol comprises: a dimethyl ether reactor; introducing methanol into the dimethyl ether reactor to carry out gas phase catalytic dehydration reaction, introducing a product after the reaction into a first rectifying tower to carry out dimethyl ether purification, sending a rectified gas phase to a washing tower to recover the dimethyl ether in the gas phase, sending a rectified liquid phase to a stripping tower to carry out separation of the methanol and the dimethyl ether, and sending the separated dimethyl ether to a dimethyl ether-to-ethanol reaction unit;
the dimethyl ether-to-ethanol reaction unit comprises: the device comprises a carbonylation reactor, wherein a first micro-interface generator is arranged on the outer side of the carbonylation reactor, dimethyl ether and carbon monoxide separated from a stripping tower are introduced into the first micro-interface generator, and enter the carbonylation reactor for reaction after being dispersed and crushed by the first micro-interface generator, the carbonylation reactor is connected with a second micro-interface generator so as to introduce carbonylation products into the second micro-interface generator, hydrogen is simultaneously introduced into the second micro-interface generator, the second micro-interface generator is dispersed and crushed by the second micro-interface generator and then enters a hydrogenation reactor for methyl acetate hydrogenation, and reaction products after the hydrogenation reaction are subjected to separation of methanol and ethanol through a second rectifying tower to obtain ethanol.
2. The reaction system of claim 1, wherein the methanol to dimethyl ether reaction unit comprises a methanol pump, and the methanol is transported by the methanol pump to pass a part to the dimethyl ether reactor and a part to the washing tower as the washing solvent.
3. The reaction system of claim 1, wherein the methanol-to-dimethyl ether reaction unit comprises a heat exchanger for exchanging heat between the raw material methanol and the product of the gas phase catalytic dehydration reaction.
4. The reaction system of claim 3, wherein the heat exchanger is arranged between the dimethyl ether reactor and the first rectification column, and a preheater is further arranged between the heat exchanger and the dimethyl ether reactor.
5. The reaction system of claim 1, wherein the top of the first rectification column and the top of the stripping column are in communication with the scrubber via a conduit for returning methanol for reuse.
6. The reaction system of claim 1, wherein side draws are arranged on the first rectifying tower and the stripping tower, and the side draws of the first rectifying tower and the side draws of the stripping tower are combined and then connected with the first micro-interface generator.
7. A reaction system according to claim 1 wherein a separation column is provided between the carbonylation reactor and the second micro-interface generator for removing gas phase impurities from the carbonylation product.
8. The reaction system of claim 7, wherein a methanol outlet is arranged at the top of the second rectifying tower, the methanol outlet is communicated with the washing tower through a pipeline for returning methanol to be recycled, and a product extraction outlet is arranged at the bottom of the second rectifying tower for extracting product ethanol.
9. The reaction method using the coal-to-ethanol reaction system according to any one of claims 1 to 8, comprising:
carrying out gas phase catalytic dehydration, rectification and steam stripping on the raw material methanol to obtain dimethyl ether;
after dimethyl ether and carbon monoxide are mixed, dispersed and crushed, carbonylation reaction is carried out to obtain a carbonylation reaction product;
and mixing, dispersing and crushing the carbonylation reaction product and hydrogen, carrying out hydrogenation reaction, and rectifying to obtain the ethanol.
10. The reaction process as claimed in claim 9, wherein the pressure of the carbonylation reaction is 2.5-3.0MPa, and the temperature of the carbonylation reaction is 200-230 ℃;
preferably, the pressure of the hydrogenation reaction is 2.5-3.0MPa, and the temperature of the hydrogenation reaction is 200-210 ℃.
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| CN202010683566.4A CN111807926A (en) | 2020-07-16 | 2020-07-16 | Reaction system and method for preparing ethanol from coal |
| PCT/CN2020/122727 WO2022011870A1 (en) | 2020-07-16 | 2020-10-22 | Reaction system and method for coal-to-ethanol |
| JP2022600018U JP3238823U (en) | 2020-07-16 | 2020-10-22 | Reaction system for producing ethanol from coal |
| DE212020000670.9U DE212020000670U1 (en) | 2020-07-16 | 2020-10-22 | Coal-to-Ethanol Reaction System |
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| DE212020000670U1 (en) | 2022-04-25 |
| JP3238823U (en) | 2022-08-25 |
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