CN104058932A - Production system and method for producing ethyl alcohol through adding of hydrogen in methyl acetate - Google Patents
Production system and method for producing ethyl alcohol through adding of hydrogen in methyl acetate Download PDFInfo
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- CN104058932A CN104058932A CN201410318790.8A CN201410318790A CN104058932A CN 104058932 A CN104058932 A CN 104058932A CN 201410318790 A CN201410318790 A CN 201410318790A CN 104058932 A CN104058932 A CN 104058932A
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- methyl acetate
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- heat exchanger
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- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 title claims abstract description 82
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 title claims abstract description 79
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 41
- 239000001257 hydrogen Substances 0.000 title claims abstract description 30
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 30
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 235000019441 ethanol Nutrition 0.000 title abstract description 21
- 239000007789 gas Substances 0.000 claims abstract description 106
- 239000007788 liquid Substances 0.000 claims abstract description 91
- 239000002994 raw material Substances 0.000 claims abstract description 47
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000012495 reaction gas Substances 0.000 claims abstract description 31
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims description 93
- 238000010438 heat treatment Methods 0.000 claims description 44
- 238000011084 recovery Methods 0.000 claims description 41
- 239000002918 waste heat Substances 0.000 claims description 40
- 238000012856 packing Methods 0.000 claims description 18
- 239000007921 spray Substances 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 7
- 230000008020 evaporation Effects 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 5
- 238000007701 flash-distillation Methods 0.000 claims description 3
- 230000006835 compression Effects 0.000 claims description 2
- 238000007906 compression Methods 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 abstract description 15
- 238000000926 separation method Methods 0.000 abstract 1
- 229960004756 ethanol Drugs 0.000 description 18
- 238000000034 method Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 description 6
- 238000009833 condensation Methods 0.000 description 5
- 230000005494 condensation Effects 0.000 description 5
- 239000000945 filler Substances 0.000 description 5
- 239000007795 chemical reaction product Substances 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 239000007858 starting material Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000009834 vaporization Methods 0.000 description 3
- 230000008016 vaporization Effects 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- 241001253206 Andrias Species 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- -1 hydrogen ester Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000013022 venting Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/582—Recycling of unreacted starting or intermediate materials
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a production system and method for producing ethyl alcohol through adding of hydrogen in methyl acetate. The system comprises a methyl acetate feed pump, a mixed evaporator, a gas-gas heat exchanger, a hydrogenation reactor, a methyl acetate preheater, a water cooler and a gas-liquid separator. The preheated methyl acetate and the preheated hydrogen are fed into a tube pass of the mixed evaporator from the top and the bottom respectively, and the obtained mixed raw material gas enters a tube pass of the gas-gas heat exchanger to be heated to be at the temperature range from 160 DEG C to 250 DEG C and then enters the hydrogenation reactor to be reacted. Thermal reaction gas generated through reaction enters the tube pass of the gas-gas heat exchanger, enters a tube pass of the mixed evaporator and a tube pass of the methyl acetate preheater from the outlet of the tube pass of the gas-gas heat exchanger, enters the water cooler to be cooled to be at the temperature below 40 DEG C and then enters the gas-liquid separator so that the mixture of crude ethyl alcohol and crude methyl alcohol and non-reacted hydrogen can be obtained through separation. The methyl alcohol serves as raw materials to be repeatedly used, absolute ethyl alcohol serves as a product to be sold, and the market price of the absolute ethyl alcohol is improved by one or more times that of acetic acid.
Description
Technical field
The present invention relates to the treatment technology of by product-methyl acetate of producing in a kind of polyvinyl alcohol (PVA) production process, relate in particular to production system and method that a kind of methyl acetate hydrogenation is produced ethanol.
Background technology
Methyl acetate is the by product producing in polyvinyl alcohol (PVA) production process, in traditional polyvinyl alcohol production equipment, by the hydrolysis of by-product acetic acid methyl esters, then produces acetic acid and methyl alcohol by rectifying, as the raw materials for production recycling of polyvinyl alcohol.On the one hand, methyl acetate is reduced to raw acetic acid and methyl alcohol needs very high production cost, and on the other hand, the value of acetic acid is very low, upper and lower at 3000 yuan/ton at present.
Summary of the invention
The production system and the method that the object of this invention is to provide the methyl acetate hydrogenation production ethanol that a kind of energy consumption is low, energy-conservation, economic worth is high.
The object of the invention is to be achieved through the following technical solutions:
Methyl acetate hydrogenation of the present invention is produced the production system of ethanol, comprises methyl acetate fresh feed pump, mixing evaporator, gas-gas heat exchanger, hydrogenator, methyl acetate preheater, water cooler and gas-liquid separator;
Described mixing evaporator comprises cylindrical shell, and the top and bottom of described cylindrical shell are respectively equipped with upper cover and lower cover, is provided with successively top spray section, corrugated plate packing section, steam heating section, waste heat recovery section, liquid level control section in described cylindrical shell from top to bottom;
In described top spray section, be provided with a plurality of shower nozzles, described a plurality of shower nozzles are connected with the stock liquid entrance of being located on described cylindrical shell;
In described corrugated plate packing section, be provided with corrugated plate packing;
In described steam heating section, be longitudinally provided with many steam heating segment heat transfer tubes, the top and bottom of described many steam heating segment heat transfer tubes are fixed on described cylindrical shell by steam heating segment upper tubesheet and steam heating segment lower tubesheet respectively, cylindrical shell near described steam heating segment upper tubesheet position is provided with steam entry, and the cylindrical shell at close described steam heating segment lower tubesheet position is provided with condensation-water drain;
In described waste heat recovery section, be longitudinally provided with many waste heat recovery section heat transfer tubes, the top and bottom of described many waste heat recovery section heat transfer tubes are fixed on described cylindrical shell by waste heat recovery section upper tubesheet and waste heat recovery section lower tubesheet respectively, cylindrical shell near described waste heat recovery section upper tubesheet position is provided with reaction gas entrance, and the cylindrical shell at close described waste heat recovery section lower tubesheet position is provided with reaction gas outlet and condensate outlet;
Described liquid level control section is provided with unstripped gas entrance;
Described upper cover and lower cover are respectively equipped with the outlet of mixing raw material gas and stock liquid discharge outlet;
The mixing raw material gas outlet of described mixing evaporator is connected with the tube side entrance of described gas-gas heat exchanger bottom, the tube side outlet on described gas-gas heat exchanger top is connected with the entrance at described hydrogenator top, the outlet of described hydrogenator bottom is connected with the shell side entrance on described gas-gas heat exchanger top, the shell side outlet of described gas-gas heat exchanger bottom is connected respectively with the reaction gas entrance of described mixing evaporator and the shell side entrance of described methyl acetate preheater, the reaction gas outlet of described mixing evaporator and the shell side outlet of described methyl acetate preheater are connected with gas-liquid separator successively with described water cooler respectively, described methyl acetate charging pump outlet is connected by the tube side of described methyl acetate preheater and the stock liquid entrance of described mixing evaporator, the stock liquid discharge outlet of described mixing evaporator is connected with the tube side entrance of described methyl acetate preheater by methyl acetate recycle pump, the pneumatic outlet at described gas-liquid separator top is connected with the unstripped gas entrance of described mixing evaporator, the liquid exit of described gas-liquid separator bottom is connected with water distilling apparatus, the unstripped gas entrance pipe of described mixing evaporator is connected with hydrogen make pipeline.
Methyl acetate hydrogenation of the present invention is produced the production method of ethanol, comprises the following steps:
A, the methyl acetate after the preheating of methyl acetate preheater and hydrogen are sent into respectively to the tube side of mixing evaporator from top and bottom, methyl acetate evaporation therein is also mixed to form mixing raw material gas with hydrogen;
The mixing raw material gas that B, steps A obtain enters in the tube side of gas-gas heat exchanger and is heated to 160～250 ℃, enters in hydrogenator and reacts;
The thermal response gas that C, step B reaction generates enters the shell side of described gas-gas heat exchanger, by described gas-gas heat exchanger shell side outlet minute two-way, one tunnel enters the shell side of described mixing evaporator, another road enters the shell side of described methyl acetate preheater, after together with described mixing evaporator shell side outlet converges to the outlet of methyl acetate preheater shell side, enter water cooler and be cooled to below 40 ℃, then enter mixture and the unreacted hydrogen that gas-liquid separator separates obtains coarse ethanol and thick methyl alcohol.
As seen from the above technical solution provided by the invention, the methyl acetate hydrogenation that the embodiment of the present invention provides is produced production system and the method for ethanol, owing to comprising methyl acetate fresh feed pump, mixing evaporator, gas-gas heat exchanger, hydrogenator, methyl acetate preheater, water cooler and gas-liquid separator; Methyl acetate after the preheating of methyl acetate preheater and hydrogen are sent into respectively to the tube side of mixing evaporator from top and bottom, methyl acetate evaporation therein is also mixed to form mixing raw material gas with hydrogen; The mixing raw material gas obtaining enters in the tube side of gas-gas heat exchanger and is heated to 160～250 ℃, enters in hydrogenator and reacts; The thermal response gas that reaction generates enters the shell side of described gas-gas heat exchanger, by gas-gas heat exchanger shell side outlet minute two-way, one tunnel enters the shell side of described mixing evaporator, another road enters the shell side of described methyl acetate preheater, after together with described mixing evaporator shell side outlet converges to the outlet of methyl acetate preheater shell side, enter water cooler and be cooled to below 40 ℃, then enter mixture and the unreacted hydrogen that gas-liquid separator separates obtains coarse ethanol and thick methyl alcohol.By hydrogen addition technology, with methyl acetate, produce dehydrated alcohol and methyl alcohol, methyl alcohol is reused as raw material, and dehydrated alcohol is as production marketing, and its market value is enhanced about more than once than acetic acid.
Accompanying drawing explanation
The methyl acetate hydrogenation that Fig. 1 provides for the embodiment of the present invention is produced the structural representation of the production system of ethanol;
Fig. 2 is the structural representation of the mixing evaporator in the embodiment of the present invention.
In figure:
1, upper cover; 2, shower nozzle; 3, top cylindrical shell; 4, corrugated plate packing; 5, liquid distributor; 6, steam heating segment upper tubesheet; 7, traverse baffle; 8, heat transfer tube; 9, steam heating segment lower tubesheet; 10, condensation-water drain; 11, waste heat recovery section upper tubesheet; 12, waste heat recovery section heat transfer tube; 13, bottom cylindrical shell; 14, waste heat recovery section lower tubesheet; 15, condensate outlet; 16, unstripped gas entrance; 17, lower cover; 18, stock liquid discharge outlet; 19, interface of the level gauge; 20, reaction gas outlet; 21, reaction gas entrance; 22, middle cylinder; 23, steam entry; 24, stock liquid entrance; 25, mixing raw material gas outlet;
A, top spray section, B, corrugated plate packing section, C, steam heating section, D, waste heat recovery section, E, liquid level control section.
Embodiment
To be described in further detail the embodiment of the present invention below.
Methyl acetate hydrogenation of the present invention is produced the production system of ethanol, its preferably embodiment be:
Comprise methyl acetate fresh feed pump, mixing evaporator, gas-gas heat exchanger, hydrogenator, methyl acetate preheater, water cooler and gas-liquid separator;
Described mixing evaporator comprises cylindrical shell, and the top and bottom of described cylindrical shell are respectively equipped with upper cover and lower cover, is provided with successively top spray section, corrugated plate packing section, steam heating section, waste heat recovery section, liquid level control section in described cylindrical shell from top to bottom;
In described top spray section, be provided with a plurality of shower nozzles, described a plurality of shower nozzles are connected with the stock liquid entrance of being located on described cylindrical shell;
In described corrugated plate packing section, be provided with corrugated plate packing;
In described steam heating section, be longitudinally provided with many steam heating segment heat transfer tubes, the top and bottom of described many steam heating segment heat transfer tubes are fixed on described cylindrical shell by steam heating segment upper tubesheet and steam heating segment lower tubesheet respectively, cylindrical shell near described steam heating segment upper tubesheet position is provided with steam entry, and the cylindrical shell at close described steam heating segment lower tubesheet position is provided with condensation-water drain;
In described waste heat recovery section, be longitudinally provided with many waste heat recovery section heat transfer tubes, the top and bottom of described many waste heat recovery section heat transfer tubes are fixed on described cylindrical shell by waste heat recovery section upper tubesheet and waste heat recovery section lower tubesheet respectively, cylindrical shell near described waste heat recovery section upper tubesheet position is provided with reaction gas entrance, and the cylindrical shell at close described waste heat recovery section lower tubesheet position is provided with reaction gas outlet and condensate outlet;
Described liquid level control section is provided with unstripped gas entrance;
Described upper cover and lower cover are respectively equipped with the outlet of mixing raw material gas and stock liquid discharge outlet;
The mixing raw material gas outlet of described mixing evaporator is connected with the tube side entrance of described gas-gas heat exchanger bottom, the tube side outlet on described gas-gas heat exchanger top is connected with the entrance at described hydrogenator top, the outlet of described hydrogenator bottom is connected with the shell side entrance on described gas-gas heat exchanger top, the shell side outlet of described gas-gas heat exchanger bottom is connected respectively with the reaction gas entrance of described mixing evaporator and the shell side entrance of described methyl acetate preheater, the reaction gas outlet of described mixing evaporator and the shell side outlet of described methyl acetate preheater are connected with gas-liquid separator successively with described water cooler respectively, described methyl acetate charging pump outlet is connected by the tube side of described methyl acetate preheater and the stock liquid entrance of described mixing evaporator, the stock liquid discharge outlet of described mixing evaporator is connected with the tube side entrance of described methyl acetate preheater by methyl acetate recycle pump, the pneumatic outlet at described gas-liquid separator top is connected with the unstripped gas entrance of described mixing evaporator, the liquid exit of described gas-liquid separator bottom is connected with water distilling apparatus, the unstripped gas entrance pipe of described mixing evaporator is connected with hydrogen make pipeline.
The pneumatic outlet at described gas-liquid separator top is connected with loop compression device, and the liquid exit of described gas-liquid separator bottom is connected with flash distillation plant.
Tube side outlet and the connecting pipeline of described hydrogenator top entrance on described gas-gas heat exchanger top are provided with electric heater.
Described hydrogenator is heat-insulating hydrogenator, and its inside is provided with Cu-series catalyst bed.
Methyl acetate hydrogenation of the present invention is produced the production method of ethanol, its preferably embodiment be:
Comprise the following steps:
A, the methyl acetate after the preheating of methyl acetate preheater and hydrogen are sent into respectively to the tube side of mixing evaporator from top and bottom, methyl acetate evaporation therein is also mixed to form mixing raw material gas with hydrogen;
The mixing raw material gas that B, steps A obtain enters in the tube side of gas-gas heat exchanger and is heated to 160～250 ℃, enters in hydrogenator and reacts;
The thermal response gas that C, step B reaction generates enters the shell side of described gas-gas heat exchanger, by described gas-gas heat exchanger shell side outlet minute two-way, one tunnel enters the shell side of described mixing evaporator, another road enters the shell side of described methyl acetate preheater, after together with described mixing evaporator shell side outlet converges to the outlet of methyl acetate preheater shell side, enter water cooler and be cooled to below 40 ℃, then enter mixture and the unreacted hydrogen that gas-liquid separator separates obtains coarse ethanol and thick methyl alcohol.
Described unreacted hydrogen returns to the unstripped gas entrance of described mixing evaporator.
The stock liquid that described mixing evaporator does not gasify returns to the stock liquid entrance of described mixing evaporator.
The methyl acetate hydrogenation that the embodiment of the present invention provides is produced production system and the method for ethanol, and energy consumption is low, energy-conservation, economic worth is high.
Specific embodiment:
Embodiment 1, production system:
As shown in Figure 1, comprise a mixing evaporator, a heat exchanger, a reactor, a condenser and a separator.
Wherein, the entrance of mixing evaporator tube side is the entrance of unstripped gas, the outlet of mixing evaporator tube side is connected with the entrance of heat exchanger tube side, the outlet of heat exchanger tube side is connected with the entrance of reactor, the outlet of reactor is connected with the entrance of heat exchanger shell side, the outlet of heat exchanger shell side is connected with the entrance of feed preheater shell side with mixing evaporator shell side respectively, after the outlet reaction gas of mixing evaporator shell side and feed preheater shell side converges, is connected successively with condenser with separator again.
Described mixing evaporator is provided with raw material liq circulation device, make unevaporated raw material liq from mixing evaporator bottom out, by recycle pump, be driven into the raw material liq entrance at mixing evaporator top.
Described production system also comprises a recycle compressor and a flash drum, is connected respectively with separator.
Described recycle compressor is connected with the entrance of mixing evaporator tube side.
Described flash drum is also connected with rectifier unit.
Described reactor is adiabatic reactor, and its inside is provided with Cu-series catalyst bed.
In above-mentioned production system, heat exchanger adopts the common tube and shell heat exchanger of chemical field, separator adopts the common gas-liquid separator of chemical field, and all the other equipment all adopt the conventional equipment of chemical field as condenser, recycle compressor, flash drum, rectifier unit etc.
In above-mentioned production system, the concrete structure of mixing evaporator as shown in Figure 2, comprises that top spray section, metal corrugated plate packing section, top tubulation steam heating segment, bottom tubulation waste heat recovery section, bottoms level control section six parts form.Concrete structure is: upper cover, shower nozzle, metal corrugated plate filler, top cylindrical shell, steam heating segment (liquid distributor, upper tubesheet, heat transfer tube, lower tubesheet, middle cylinder), waste heat recovery section (liquid distributor, upper tubesheet, heat transfer tube, lower tubesheet, bottom cylindrical shell), lower cover, interface of the level gauge, steam entry, condensation-water drain, reaction gas entrance, reaction gas outlet, unstripped gas entrance, stock liquid entrance, the outlet of mixing raw material gas, condensate outlet, bottom leakage fluid dram forms.
Upper cover and top cylindrical shell, the welding of steam heating segment upper tubesheet, middle space has formed upper tube box, and upper tube box top is shower nozzle, is down metal corrugated plate filler, then is down liquid distributor.Middle cylindrical shell and the upper and lower Tube-sheet Welding of steam heating segment.Between cylindrical shell, tube sheet, tube bank and traverse baffle, formed shell side flow of water vapor passage.Lower shell and the upper and lower Tube-sheet Welding of waste heat recovery section.Between cylindrical shell, tube sheet, tube bank and traverse baffle, formed the mobile passage of reaction gas of shell side.From bottom to top, tube side has formed the circulation passage of unstripped gas.
Mixing evaporator is the equipment that shell and tube heat exchanger and packing tower combine.
Unstripped gas enters from bottom unstripped gas entrance 16, along the tube side of waste heat recovery section, upwards flow, and with from up to down mobile raw material liq counter current contact, constantly heat up after absorbing the heat of shell side reaction gas, unstripped gas is heated, raw material liq is vaporized.Then upwards upwards mobile along the tube side of steam heating segment, the heat of absorption shell side water vapour, continues unstripped gas heating, the process of raw material liq vaporization.Unstripped gas continues upwards to flow, and in top filler 4, with the sufficient counter current contact of the raw material liq flowing downward, compares mass transfer process thoroughly.The mixing raw material gas that is mixed with vaporization raw material liq is discharged from top mixing raw material gas outlet 25.
Raw material liq enters from top feed liquid entrance 24, by gravity, flow downward, successively by packing section 4, steam heating segment heat transfer tube 8 and waste heat recovery section heat transfer tube 12, constantly and unstripped gas counter current contact, absorb the heat of shell side thermal medium, constantly be heated and evaporate, unevaporated liquid is discharged from bottom leakage fluid dram 18.
The reaction gas of heat enters from reaction gas entrance 21, between the traverse baffle 7 of shell side, from up to down flows, and with unstripped gas and the stock liquid heat exchange in pipe, emits sensible heat and condensation latent heat, is cooled and condensation.Reaction gas after cooling is discharged from reaction gas outlet 20.
In steam-heated cal(l)andria section, shell side provides heat with water vapour, continues to unstripped gas and raw material liq heating.Steam-heated cal(l)andria Duan Yousan special effect, is first when revivification of catalyst, and starting all provides heat by water vapour, when reduction latter temperature is too high, then opens electric heater additional heat; Its two, when initial start-up, in reaction gas, seldom, the heat of condensation producing can not meet caloric requirement to reaction product, now mainly by water vapour, provides heat.It three is when shortage of heat that waste heat recovery section reclaims, can make up with a small amount of water vapor the deficiency of heat.
The packing section on top, is one safeguards, due to the raw material liq of the unstripped gas rising in filler and decline counter current contact fully, can guarantee that liquid starting material vaporizes fully, thereby guarantee to reach the stock liquid steam output that meets need of production.
Embodiment 2, produce the production process of 100,000 tons of ethanol per year:
21 tons/hour of liquid acetic acid methyl esters material flows, incoming stock pump intake, be pressurized to 5.0-7.0Mpa (g), converge with the circulation fluid of methyl acetate recycle pump discharge, the tube side of incoming stock liquid preheater, by reaction gas, be heated to 60--80 ℃, from the stock liquid entrance 24 at mixing evaporator top, enter into mixing evaporator.Enter after mixing evaporator, first through shower nozzle, raw material is sprayed on filler, carry out sufficient gas-to-liquid contact with the mobile unstripped gas that makes progress, carry out mass-transfer progress, stock liquid is partly evaporated.Unevaporated stock liquid flows downward by gravity, by liquid distributor, enter uniformly in every heat transfer tube of water vapour heating zone, become membranaceous flowing downward, with the unstripped gas counter current contact that makes progress mobile, the heat of simultaneously accepting shell side water vapour is heated and evaporates.Unevaporated stock liquid continues to flow downward, and enters in every heat transfer tube of waste heat recovery section the heat of acceptable response gas and be heated and evaporate through liquid distributor.
In order to guarantee that raw material liq can be heat transfer tube interrupt flow and withered (the withered time have not been grown meeting fouling blocking pipe); For liquid film can be full of inner-walls of duct to guarantee mass-and heat-transfer effect; Be two liquid distributors liquid that can distribute uniformly, all need the flow of suitable increasing raw material liq, still, can strengthen out like this stock liquid scale of construction of mixing evaporator bottom, be provided with stock liquid recycle pump for this reason.From mixing evaporator bottom raw material liq out, enter pump entry, pressurization stock liquid rear and feedstock pump outlet is mixed into liquid starting material preheater.With recycle pump, control the liquid feeding amount of mixing evaporator, with feedstock pump, control the liquid level of mixing evaporator bottom.
After hydrogen make-up is mixed with circulating hydrogen, flow 200000Nm3/h, enter circulating hydrogen compressor, be pressurized to 4.0-6.0MPa (g), 40 ℃ of bottom unstripped gas entrances that enter mixing evaporator (seeing Fig. 2), successively upwards by waste heat recovery section tube side, steam heating section tube side and top packing section.
Unstripped gas enters the tube side of waste heat recovery section, with from the top down along inside pipe wall flowing fluid methyl acetate raw material counter current contact, absorb the sensible heat of shell side thermal response gas and the condensation latent heat of reaction product, gas is heated, liquid acetic acid methyl esters is evaporated and mix with hydrogen.Unstripped gas from waste heat recovery section tube side out, enters water vapour heating zone tube side, continues heating raw gas, the process of evaporation raw material liq.
Under the normal condition of production, the needs of the enough heating raw gas of heat reclaiming in waste heat recovery section and vaporization raw material liq, the water vapour of water vapour heating zone is not opened or is opened less.But sometimes because of liquid starting material in pipe skewness or produce the factor such as undesired cause conduct heat and evaporation effect bad, the heat of waste heat recovery section recovery can not meet the needs of production.Just need to supplement a part of heat by water vapour heating zone.
When the original heating reduction of initial start-up, the initial stage is all carried out heated air with water vapour, when latter temperature is too high, need to drives electric heater and carry out additional heat.At the production initial stage, in reaction gas, reaction product does not have or seldom, heat of condensation seldom, relies on water vapour that heat is provided completely.
The packing section at top is a safeguards, when liquid starting material is in pipe during skewness, liquid evaporation effect is bad, steam output is not enough, and unstripped gas has undersaturated overheat condition and occurs, and can not meet need of production, now, the sufficient counter current contact in packing layer due to unstripped gas and raw material liq, can produce good mass transfer effect, thereby guarantees that the steam output of methyl acetate can meet the requirement of producing.
From mixing evaporator top exit out, the mixing raw material gas that meets production requirement hydrogen ester ratio, temperature 60--80 ℃, enter the tube side of gas-gas heat exchanger, continuation is heated to 160--210 ℃ by reaction gas, enters the mixing raw material gas entrance of reactor head, under the effect of inside reactor Cu-series catalyst, methyl acetate and hydrogen reaction, generate ethanol and methyl alcohol.
The reaction gas that reactor bottom exports out, temperature 180--230 ℃, enter the shell side of gas-gas heat exchanger, with the heat exchange of mixing raw material gas, cool to 80--130 ℃, the gas of the gas heat exchanger shell pass of giving vent to anger, is divided into two portions, main line enters the shell side of mixing evaporator, with mixing raw material gas and raw material liq heat exchange.Pay the incoming stock liquor preheater shell side of line, heating raw liquid is to 60--80 ℃.Another effect of paying line is, when mixing evaporator water vapour Close All, when the steam output of methyl acetate still surpasses the ratio needing, can increase the flow of paying line reaction gas, reduce the flow of main line reaction gas, thereby regulate the steam output of methyl acetate in mixing evaporator.
Together with two outlet reaction gases of mixing evaporator shell side and raw material liq preheater shell side converge to, enter water cooler tube side, with recirculated cooling water, be cooled to 40 ℃, now ethanol and the methyl alcohol overwhelming majority have been condensed into liquid.Gas-liquid mixture from water cooler out, enters gas-liquid separator, and unreacting gas and reaction product liquid are separated, and the mixture of coarse ethanol and methyl alcohol goes rectifier unit to produce product ethanol and methyl alcohol after flash distillation.The isolated gas overwhelming majority is hydrogen, and major part is returned to recycle compressor and recycled as unstripped gas, and a very little part is as speeding bleed air exhaust, to reduce the accumulation of rare gas element.Flash steam and the venting of speeding mix send device for producing hydrogen to use.
The above; be only the present invention's embodiment preferably, but protection scope of the present invention is not limited to this, is anyly familiar with in technical scope that those skilled in the art disclose in the present invention; the variation that can expect easily or replacement, within all should being encompassed in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (7)
1. methyl acetate hydrogenation is produced a production system for ethanol, it is characterized in that, comprises methyl acetate fresh feed pump, mixing evaporator, gas-gas heat exchanger, hydrogenator, methyl acetate preheater, water cooler and gas-liquid separator;
Described mixing evaporator comprises cylindrical shell, and the top and bottom of described cylindrical shell are respectively equipped with upper cover and lower cover, is provided with successively top spray section, corrugated plate packing section, steam heating section, waste heat recovery section, liquid level control section in described cylindrical shell from top to bottom;
In described top spray section, be provided with a plurality of shower nozzles, described a plurality of shower nozzles are connected with the stock liquid entrance of being located on described cylindrical shell;
In described corrugated plate packing section, be provided with corrugated plate packing;
In described steam heating section, be longitudinally provided with many steam heating segment heat transfer tubes, the top and bottom of described many steam heating segment heat transfer tubes are fixed on described cylindrical shell by steam heating segment upper tubesheet and steam heating segment lower tubesheet respectively, cylindrical shell near described steam heating segment upper tubesheet position is provided with steam entry, and the cylindrical shell at close described steam heating segment lower tubesheet position is provided with condensation-water drain;
In described waste heat recovery section, be longitudinally provided with many waste heat recovery section heat transfer tubes, the top and bottom of described many waste heat recovery section heat transfer tubes are fixed on described cylindrical shell by waste heat recovery section upper tubesheet and waste heat recovery section lower tubesheet respectively, cylindrical shell near described waste heat recovery section upper tubesheet position is provided with reaction gas entrance, and the cylindrical shell at close described waste heat recovery section lower tubesheet position is provided with reaction gas outlet and condensate outlet;
Described liquid level control section is provided with unstripped gas entrance;
Described upper cover and lower cover are respectively equipped with the outlet of mixing raw material gas and stock liquid discharge outlet;
The mixing raw material gas outlet of described mixing evaporator is connected with the tube side entrance of described gas-gas heat exchanger bottom, the tube side outlet on described gas-gas heat exchanger top is connected with the entrance at described hydrogenator top, the outlet of described hydrogenator bottom is connected with the shell side entrance on described gas-gas heat exchanger top, the shell side outlet of described gas-gas heat exchanger bottom is connected respectively with the reaction gas entrance of described mixing evaporator and the shell side entrance of described methyl acetate preheater, the reaction gas outlet of described mixing evaporator and the shell side outlet of described methyl acetate preheater are connected with gas-liquid separator successively with described water cooler respectively, described methyl acetate charging pump outlet is connected by the tube side of described methyl acetate preheater and the stock liquid entrance of described mixing evaporator, the stock liquid discharge outlet of described mixing evaporator is connected with the tube side entrance of described methyl acetate preheater by methyl acetate recycle pump, the pneumatic outlet at described gas-liquid separator top is connected with the unstripped gas entrance of described mixing evaporator, the liquid exit of described gas-liquid separator bottom is connected with water distilling apparatus, the unstripped gas entrance pipe of described mixing evaporator is connected with hydrogen make pipeline.
2. methyl acetate hydrogenation according to claim 1 is produced the production system of ethanol, it is characterized in that, the pneumatic outlet at described gas-liquid separator top is connected with loop compression device, and the liquid exit of described gas-liquid separator bottom is connected with flash distillation plant.
3. methyl acetate hydrogenation according to claim 2 is produced the production system of ethanol, it is characterized in that, tube side outlet and the connecting pipeline of described hydrogenator top entrance on described gas-gas heat exchanger top are provided with electric heater.
4. methyl acetate hydrogenation according to claim 3 is produced the production system of ethanol, it is characterized in that, described hydrogenator is heat-insulating hydrogenator, and its inside is provided with Cu-series catalyst bed.
5. the production system of the production of the methyl acetate hydrogenation described in claim 1 to 4 any one ethanol realizes the production method that methyl acetate hydrogenation is produced ethanol, it is characterized in that, comprises the following steps:
A, the methyl acetate after the preheating of methyl acetate preheater and hydrogen are sent into respectively to the tube side of mixing evaporator from top and bottom, methyl acetate evaporation therein is also mixed to form mixing raw material gas with hydrogen;
The mixing raw material gas that B, steps A obtain enters in the tube side of gas-gas heat exchanger and is heated to 160～250 ℃, enters in hydrogenator and reacts;
The thermal response gas that C, step B reaction generates enters the shell side of described gas-gas heat exchanger, by described gas-gas heat exchanger shell side outlet minute two-way, one tunnel enters the shell side of described mixing evaporator, another road enters the shell side of described methyl acetate preheater, after together with described mixing evaporator shell side outlet converges to the outlet of methyl acetate preheater shell side, enter water cooler and be cooled to below 40 ℃, then enter mixture and the unreacted hydrogen that gas-liquid separator separates obtains coarse ethanol and thick methyl alcohol.
6. methyl acetate hydrogenation according to claim 5 is produced the production method of ethanol, it is characterized in that, described unreacted hydrogen returns to the unstripped gas entrance of described mixing evaporator.
7. methyl acetate hydrogenation according to claim 6 is produced the production method of ethanol, it is characterized in that, the stock liquid that described mixing evaporator does not gasify returns to the stock liquid entrance of described mixing evaporator.
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| CN111732497A (en) * | 2020-07-21 | 2020-10-02 | 濮阳永金化工有限公司 | Device for improving hydrogen-ester ratio and application method |
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