CN203602526U - Reactive distillation device for producing ethanol from methyl acetate by adding hydrogen - Google Patents
Reactive distillation device for producing ethanol from methyl acetate by adding hydrogen Download PDFInfo
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- CN203602526U CN203602526U CN201320740304.2U CN201320740304U CN203602526U CN 203602526 U CN203602526 U CN 203602526U CN 201320740304 U CN201320740304 U CN 201320740304U CN 203602526 U CN203602526 U CN 203602526U
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Abstract
The utility model relates to a reactive distillation method and device for producing ethanol from methyl acetate by adding hydrogen. The device comprises a reactive distillation tower, a methanol refining tower, a methyl acetate recycling tower, condensers, reboilers, a compressor, a pump and pipelines for connecting the equipment, wherein the condensers and the reboilers are arranged at the tops and bottoms of the reactive distillation tower, the methanol refining tower and the methyl acetate recycling tower, gas phase outlets of the condensers at the tower tops are connected to the compressor, liquid phase outlets are connected to a feed port of the methanol refining tower, and an ethanol product is obtained at the bottom of the methanol refining tower; a compressor outlet is connected to the hydrogen inlet of the reactive distillation tower, a material discharged from the top of the methanol refining tower is fed into the methyl acetate recycling tower, and the product at the bottom of the methyl acetate recycling tower is methanol; a material discharged from the top of the methyl acetate recycling tower is returned to the methanol refining tower, and a material discharged from the methyl acetate recycling tower is returned to the reactive distillation tower and is used as fed methyl acetate. The operations of two units, namely methyl acetate hydrogenation reaction and ethanol purification rectification separation, are coupled and simultaneously performed in one piece of equipment, and a high-purity ethanol product is synchronously obtained when the reaction is accomplished, so that equipment investment is saved, and later operation expense is reduced.
Description
Technical field
The utility model relates to alcohol production technical field, particularly relates to a kind of reaction and rectification device of ritalin hydrogenation production ethanol.
Background technology
Ethanol can be divided into fermenting alcohol and synthesizing alcohol by the mode of production, world's ethanol production 93% by fermentative Production.Its raw material sources are very extensive.Biomass, after fermentation, obtain volume fraction of ethanol content and are 5%～30% fermentation liquid, after fermentation liquid rectifying and dehydration, can obtain dehydrated alcohol product.Dehydrated alcohol is widely used in Chemical Manufacture raw material, organic solvent and railroad fuel etc., wherein claims again alcohol fuel as the dehydrated alcohol of railroad fuel.The external interdependency of China's energy constantly increases at present, and energy security problem becomes increasingly conspicuous; The problem of environmental pollution of China has seriously restricted the fast development of national economy; China's agriculture, rural areas and farmers outstanding problem.Greatly develop fuel ethanol production technology significant to addressing the above problem.
Except fermentation method, also has ethene aquation method and the carboxylicesters Hydrogenation method for alcohol about the technology of preparing of ethanol.There is in the past methods involving narration by carboxylicesters Hydrogenation for alcohol: DE892958 discloses 75-300 ℃, 0.1-100kg/cm
2under absolute pressure, gas phase ester reacts and prepares alcohol with hydrogen catalysis.CN86105765A discloses the method for carboxylicesters alcohol processed, reacts under existing containing copper and at least one magnesium, lanthanide series metal or actinide metals catalyzer with under high temperature, normal pressure or high pressure.CN102976892A discloses take mesopore molecular sieve as carrier, supported copper series catalysts, and temperature of reaction is 220 ℃, pressure 3MPa, hydrogen ester mol ratio 30, ritalin air speed is 2h
-1time, acetic ester transformation efficiency is 98.5%.CN1230458A discloses a kind of method of preparing ethanol from acetaldehyde, ethyl acetate, acetic acid or its mixture gas phase hydrogenation, and catalyzer is CuO and auxiliary agent, Al
2o
3for carrier.In addition, also there is Patents to report the catalyzer of reaction, as JP6259632, JP61178940, JP61178942, USP4405819, CN102327774A, CN101411990A, CN1935375A etc.
Ritalin hydrogenation products mainly contains hydrogen, unreacted ritalin, methyl alcohol and ethanol, and after cooling, liquid phase is mainly ritalin, methyl alcohol and ethanol.At present, for mixture separation, mainly concentrate on the separation of ritalin, methyl alcohol and water, as CN1962587A discloses a kind of method of separating methyl acetate and methanol, the main azeotrope containing methyl acetate and methanol enters the first knockout tower middle part, tower reactor obtains pure methyl alcohol, the azeotrope that tower top obtains enters the second knockout tower, obtain pure ritalin through separating tower reactor, tower top obtains azeotrope and returns to the first knockout tower, the first knockout tower operates under normal pressure or negative pressure, and the second knockout tower is operation under pressurization.CN102757342A discloses the purification process of by-product methyl acetate in a kind of PVA production, comprises extracting rectifying, purifying and drying unit, thereby can obtain the ritalin that purity is higher.Correlative study does not relate to the separating of mixture of simultaneously containing ritalin, methyl alcohol and ethanol.
At present, have been reported reaction and catalysis for ethanol about ritalin Hydrogenation, the means that realize mostly adopt intermittently or flow reactor, and having reacted after product must could obtain high-purity alcohol product through a series of separation.Reaction rectification technique is day by day a kind of process intensification technology of will reaction simultaneously carrying out in same equipment with separation coupling widely of application in chemical industry.Reaction rectification technique can constantly shift out product by rectifying from reaction zone, make the reactant concn of reaction zone maintain higher degree, thereby keep the speed of reaction of reaction zone to maintain higher level, and can at the bottom of tower top or tower, obtain the higher product of purity.In addition, due to reaction and rectifying are coupling in an equipment and are carried out, aspect facility investment, this technology also than reaction and the flow process that separates separate operation more economically.Also reaction rectification technique is not applied at present to Patents and the report of ritalin preparation of ethanol by hydrogenating process.
Summary of the invention
The purpose of this utility model is to provide a kind of reaction and rectification device of ritalin hydrogenation production ethanol, the catalysis reaction rectifying device that provides of the utility model is provided, has that technical process is simple, facility investment is lower, easy to operate, energy consumption is lower and target product purity of alcohol advantages of higher.
Ritalin hydrogenation of the present utility model is produced the reaction and rectification device of ethanol, is mainly made up of pre-reactor, reactive distillation column, refining methanol tower and methyl acetate recovery tower, and main products is ethanol and methyl alcohol.The feature of method of the present utility model and device is the employing of reaction rectification technique and equipment, can when carrying out ritalin hydrogenation reaction, reactive distillation column obtain alcohol product at the bottom of tower, can also obtain methyl alcohol by later separation, and realize making full use of of raw material by the circulation of ritalin and hydrogen.
The technical solution of the utility model is as follows:
Ritalin hydrogenation of the present utility model is produced the reaction and rectification device of ethanol, comprises reactive distillation column, refining methanol tower, methyl acetate recovery tower, condenser, reboiler, compressor, pump and relevant feeding line and the pipeline that is connected above equipment; At the bottom of reactive distillation column, refining methanol tower and methyl acetate recovery column overhead and tower, condenser and reboiler are all set, reactive distillation column overhead condenser gaseous phase outlet is connected to compressor, and liquid-phase outlet is connected to refining methanol tower opening for feed, is alcohol product at the bottom of tower; Compressor outlet is connected to reactive distillation column hydrogen feed place; The discharging of refining methanol column overhead enters methyl acetate recovery tower, and bottom product is methyl alcohol; Refining methanol tower is returned in the discharging of methyl acetate recovery column overhead, and at the bottom of tower, the charging of reactive distillation column ritalin is returned in discharging.
Described ritalin hydrogenation is produced the reaction and rectification device of ethanol, and pre-reactor can be set before reactive distillation column, and raw material and circulating hydrogen and ritalin enter pre-reactor, and pre-reactor outlet is connected to reactive distillation column.
The reactive distillation method that ritalin hydrogenation of the present utility model is produced ethanol is: raw hydrogen (S01) and raw material ritalin (S02) enter reactive distillation column (T1); Reactive distillation column (T1) top gaseous phase (S04) enters reactive distillation column overhead condenser (E1), gas phase after condensation (S05) is returned to reactive distillation column (T1) charging as circulating hydrogen (S23) after compressor (C1) pressurization, liquid phase after condensation (S06) obtains liquid phase (S07) through reactive distillation column reflux-withdrawal pump (P1), a part is as reactive distillation column backflow (S08), another portion, as refining methanol tower (T2) charging (S09), is product ethanol (S10) at the bottom of reactive distillation column tower; Refining methanol tower (T2) top gaseous phase (S11) is the liquid phase (S13) through refining methanol tower reflux-withdrawal pump (P2) through condenser (E3) liquid phase (S12), a part is as reflux (S14), another part is as methyl acetate recovery tower (T3) charging (S15), extraction product methyl alcohol (S16) at the bottom of refining methanol tower tower; Methyl acetate recovery tower (T3) top gaseous phase (S17) obtains liquid phase (S19) through condenser (E5) liquid phase (S18) through methyl acetate recovery tower reflux-withdrawal pump (P3), a part is as reflux (S20), another part is that methyl alcohol and ritalin azeotrope (S21) return to refining methanol tower (T2), and at the bottom of tower, extraction circulation ritalin (S22) returns to reactive distillation column (T1) charging.
Raw hydrogen (S01) and raw material ritalin (S02) also can be introduced into pre-reactor (R1), and exported product (S03) enters reactive distillation column (T1).
Ritalin hydrogenation is produced in the reactive distillation method of ethanol: pre-reactor adopts copper-based catalysts, and temperature is 120-350 ℃, and pressure is 0.2-8.0MPa (a); Reactive distillation pressure tower 0.2-7.0MPa (a), reflux ratio is 0.01-100, catalyzer is copper-based catalysts; Refining methanol pressure tower 0.01-1.0MPa (a), reflux ratio is 0.01-100; Methyl acetate recovery pressure tower 0.05-2.0MPa (a), reflux ratio is 0.01-100.
The copper-based catalysts active ingredient adopting in pre-reactor and reactive distillation column is copper, and auxiliary agent is zinc or aluminium or its combination, can be silicon-dioxide, aluminum oxide molecular sieve or graphite if adopt carrier.
Ritalin hydrogenation of the present utility model is produced reactive distillation method and the device of ethanol, its advantage is ritalin hydrogenation reaction and two unit operations of ethyl alcohol purification rectifying separation, organically be coupled in an equipment and carry out simultaneously, react and obtained high-purity alcohol product simultaneously, both save facility investment, reduced again follow-up process cost.In addition, by refining methanol tower and the operation of methyl acetate recovery tower height low pressure recycle, can realize separating of methyl alcohol and ritalin azeotrope, saving equipment and energy consumption.
Accompanying drawing explanation
Fig. 1 is reactive distillation method and the device schematic diagram that ritalin hydrogenation is produced ethanol.
Fig. 2 is reactive distillation method and the device schematic diagram of producing ethanol with the ritalin hydrogenation of pre-reactor.
Equipment: R1. pre-reactor, T1. reactive distillation column, T2. refining methanol tower, T3. methyl acetate recovery tower, P1. reactive distillation column reflux-withdrawal pump, P2. refining methanol tower reflux-withdrawal pump, P3. methyl acetate recovery tower reflux-withdrawal pump, E1. reactive distillation column overhead condenser, E2. reactive distillation column reboiler, E3. refining methanol tower condenser, E4. refining methanol tower reboiler, E5. methyl acetate recovery tower condenser, E6. methyl acetate recovery tower reboiler, C1. compressor
Logistics: S01. raw hydrogen, S02. raw material ritalin, S03. pre-reactor outlet material, S04. reactive distillation column top gaseous phase, S05. gas phase after condensation, S06. liquid phase after condensation, S07. reactive distillation column reflux-withdrawal pump discharge liquid phase, S08. reactive distillation column refluxes, S09. refining methanol tower charging, S10. product ethanol, S11. refining methanol column overhead gas phase, S12. condensator outlet liquid phase, S14. refining methanol tower refluxes, S15. methyl esters recovery tower charging, S16. product methyl alcohol, S17. methyl acetate recovery column overhead gas phase, S18. liquid phase after condensation, S19. methyl acetate recovery tower reflux-withdrawal pump discharge liquid phase, S20. methyl acetate recovery tower refluxes, S21. methyl alcohol and ritalin azeotrope, S22. ritalin circulates
Embodiment
Below in conjunction with accompanying drawing, method provided by the utility model and device are further detailed.
The utility model is achieved by the following technical solution:
Ritalin hydrogenation is produced the reaction and rectification device of ethanol, as shown in Figure 1, comprises reactive distillation column, refining methanol tower, methyl acetate recovery tower, condenser, reboiler, compressor, pump and relevant feeding line and the pipeline that is connected above equipment; It is characterized in that: at the bottom of reactive distillation column, refining methanol tower and methyl acetate recovery column overhead and tower, condenser and reboiler are all set, reactive distillation column overhead condenser gaseous phase outlet is connected to compressor, liquid-phase outlet is connected to refining methanol tower opening for feed, is alcohol product at the bottom of tower; Compressor outlet is connected to reactive distillation column hydrogen feed place; The discharging of refining methanol column overhead enters methyl acetate recovery tower, and bottom product is methyl alcohol; Refining methanol tower is returned in the discharging of methyl acetate recovery column overhead, and at the bottom of tower, the charging of reactive distillation column ritalin is returned in discharging.
Described ritalin hydrogenation is produced the reaction and rectification device of ethanol, can pre-reactor be set before reactive distillation column, and as shown in Figure 2, raw material and circulating hydrogen and ritalin enter pre-reactor, and pre-reactor outlet is connected to reactive distillation column.
The reactive distillation method that ritalin hydrogenation of the present utility model is produced ethanol is: raw hydrogen (S01) and raw material ritalin (S02) enter reactive distillation column (T1); Reactive distillation column (T1) top gaseous phase (S04) enters reactive distillation column overhead condenser (E1), gas phase after condensation (S05) is returned to reactive distillation column (T1) charging as circulating hydrogen (S23) after compressor (C1) pressurization, liquid phase after condensation (S06) obtains liquid phase (S07) through reactive distillation column reflux-withdrawal pump (P1), a part is as reactive distillation column backflow (S08), another portion, as refining methanol tower (T2) charging (S09), is product ethanol (S10) at the bottom of reactive distillation column tower; Refining methanol tower (T2) top gaseous phase (S11) is the liquid phase (S13) through refining methanol tower reflux-withdrawal pump (P2) through condenser (E3) liquid phase (S12), a part is as reflux (S14), another part is as methyl acetate recovery tower (T3) charging (S15), extraction product methyl alcohol (S16) at the bottom of refining methanol tower tower; Methyl acetate recovery tower (T3) top gaseous phase (S17) obtains liquid phase (S19) through condenser (E5) liquid phase (S18) through methyl acetate recovery tower reflux-withdrawal pump (P3), a part is as reflux (S20), another part is that methyl alcohol and ritalin azeotrope (S21) return to refining methanol tower (T2), and at the bottom of tower, extraction circulation ritalin (S22) returns to reactive distillation column (T1) charging.
Raw hydrogen (S01) and raw material ritalin (S02) also can be introduced into pre-reactor (R1), and exported product (S03) enters reactive distillation column (T1).
Ritalin hydrogenation is produced in the reactive distillation method of ethanol: pre-reactor adopts copper-based catalysts, and temperature is 120-350 ℃, and pressure is 0.2-8.0MPa (a); Reactive distillation column adopts copper-based catalysts, pressure 0.2-7.0MPa (a), and reflux ratio is 0.01-100; Refining methanol pressure tower 0.01-1.0MPa (a), reflux ratio is 0.01-100; Methyl acetate recovery pressure tower 0.05-2.0MPa (a), reflux ratio is 0.01-100.
The copper-based catalysts active ingredient adopting in pre-reactor and reactive distillation column is copper, and auxiliary agent is zinc or aluminium or its combination, can be silicon-dioxide, aluminum oxide molecular sieve and graphite if adopt carrier.
Technology and equipment of the present utility model is widely used in the reactive distillation processes of ritalin hydrogenation production ethanol, in order to illustrate that better the utility model is in the advantage aspect product purity and yield, choosing wherein four application examples is illustrated, but therefore do not limit the scope of application of this technology and equipment, accompanying drawing is drawn for explanation the utility model, concrete application form of the present utility model is not construed as limiting.
Embodiment 1
Process by the utility model method for ritalin preparation of ethanol by hydrogenating, as shown in Figure 1, comprise reactive distillation column, refining methanol tower, methyl acetate recovery tower, condenser, reboiler, compressor, pump and relevant feeding line and the pipeline that is connected above equipment; It is characterized in that: at the bottom of reactive distillation column, refining methanol tower and methyl acetate recovery column overhead and tower, condenser and reboiler are all set, reactive distillation column overhead condenser gaseous phase outlet is connected to compressor, liquid-phase outlet is connected to refining methanol tower opening for feed, is alcohol product at the bottom of tower; Compressor outlet is connected to reactive distillation column hydrogen feed place; The discharging of refining methanol column overhead enters methyl acetate recovery tower, and bottom product is methyl alcohol; Refining methanol tower is returned in the discharging of methyl acetate recovery column overhead, and at the bottom of tower, the charging of reactive distillation column ritalin is returned in discharging.
Raw hydrogen (S01) and raw material ritalin (S02) enter reactive distillation column (T1), and reactive distillation pressure tower is 0.2MPa (a), and reflux ratio is 0.01, adopt copper-based catalysts; Reactive distillation column (T1) top gaseous phase (S04) enters reactive distillation column overhead condenser (E1), gas phase after condensation (S05) is returned to reactive distillation column (T1) charging as circulating hydrogen (S23) after compressor (C1) pressurization, liquid phase after condensation (S06) obtains liquid phase (S07) through reactive distillation column reflux-withdrawal pump (P1), a part is as reactive distillation column backflow (S08), another portion, as refining methanol tower (T2) charging (S09), is product ethanol (S10) at the bottom of reactive distillation column tower; Refining methanol pressure tower 0.01MPa (a), reflux ratio is 0.01, refining methanol tower (T2) top gaseous phase (S11) is the liquid phase (S13) through refining methanol tower reflux-withdrawal pump (P2) through condenser (E3) liquid phase (S12), a part is as reflux (S14), another part is as methyl acetate recovery tower (T3) charging (S15), extraction product methyl alcohol (S16) at the bottom of refining methanol tower tower; Methyl acetate recovery tower (T3) methyl acetate recovery pressure tower 0.05MPa (a), reflux ratio is 0.01, top gaseous phase (S17) obtains liquid phase (S19) through condenser (E5) liquid phase (S18) through methyl acetate recovery tower reflux-withdrawal pump (P3), a part is as reflux (S20), another part is that methyl alcohol and ritalin azeotrope (S21) return to refining methanol tower (T2), and at the bottom of tower, extraction circulation ritalin (S22) returns to reactive distillation column (T1) charging.
By ritalin hydrogenation reaction and two unit operations of ethyl alcohol purification rectifying separation, be organically coupled in an equipment and carry out simultaneously, react and obtained high-purity alcohol product simultaneously, both saved facility investment, reduce again follow-up process cost.In addition, by refining methanol tower and the operation of methyl acetate recovery tower height low pressure recycle, can realize separating of methyl alcohol and ritalin azeotrope, saving equipment and energy consumption.Finally obtain obtaining at the bottom of reactive distillation column tower purity and be 90% ethanol, at the bottom of refining methanol tower tower, obtaining methanol concentration is 90%.
Embodiment 2
Process by the utility model method for ritalin preparation of ethanol by hydrogenating, as shown in Figure 2, comprise pre-reactor, reactive distillation column, refining methanol tower, methyl acetate recovery tower, condenser, reboiler, compressor, pump and relevant feeding line and the pipeline that is connected above equipment; It is characterized in that: raw material and circulating hydrogen and ritalin enter pre-reactor, pre-reactor outlet is connected to reactive distillation column; At the bottom of reactive distillation column, refining methanol tower and methyl acetate recovery column overhead and tower, condenser and reboiler are all set, reactive distillation column overhead condenser gaseous phase outlet is connected to compressor, and liquid-phase outlet is connected to refining methanol tower opening for feed, is alcohol product at the bottom of tower; Compressor outlet is connected to reactive distillation column hydrogen feed place; The discharging of refining methanol column overhead enters methyl acetate recovery tower, and bottom product is methyl alcohol; Refining methanol tower is returned in the discharging of methyl acetate recovery column overhead, and at the bottom of tower, the charging of reactive distillation column ritalin is returned in discharging.
Raw hydrogen (S01) and raw material ritalin (S02) are introduced into pre-reactor (R1), and pre-reactor adopts copper-based catalysts, and temperature is 120 ℃, and pressure is 0.2MPa (a), and exported product (S03) enters reactive distillation column (T1), reactive distillation column (T1) adopts copper-based catalysts, pressure is 2.0MPa (a), reflux ratio is 20, top gaseous phase (S04) enters reactive distillation column overhead condenser (E1), gas phase after condensation (S05) is returned to reactive distillation column (T1) charging as circulating hydrogen (S23) after compressor (C1) pressurization, liquid phase after condensation (S06) obtains liquid phase (S07) through reactive distillation column reflux-withdrawal pump (P1), a part is as reactive distillation column backflow (S08), another portion is as refining methanol tower (T2) charging (S09), at the bottom of reactive distillation column tower, be product ethanol (S10), refining methanol tower (T2) pressure 0.1MPa (a), reflux ratio is 20, top gaseous phase (S11) is the liquid phase (S13) through refining methanol tower reflux-withdrawal pump (P2) through condenser (E3) liquid phase (S12), a part is as reflux (S14), another part is as methyl acetate recovery tower (T3) charging (S15), extraction product methyl alcohol (S16) at the bottom of refining methanol tower tower, methyl acetate recovery tower (T3) pressure 0.2MPa (a), reflux ratio is 20, top gaseous phase (S17) obtains liquid phase (S19) through condenser (E5) liquid phase (S18) through methyl acetate recovery tower reflux-withdrawal pump (P3), a part is as reflux (S20), another part is that methyl alcohol and ritalin azeotrope (S21) return to refining methanol tower (T2), and at the bottom of tower, extraction circulation ritalin (S22) returns to reactive distillation column (T1) charging.The copper-based catalysts active ingredient adopting in pre-reactor (R1) and reactive distillation column (T1) is copper, and auxiliary agent is zinc, and employing carrier is silicon-dioxide.
By ritalin hydrogenation reaction and two unit operations of ethyl alcohol purification rectifying separation, be organically coupled in an equipment and carry out simultaneously, react and obtained high-purity alcohol product simultaneously, both saved facility investment, reduce again follow-up process cost.In addition, by refining methanol tower and the operation of methyl acetate recovery tower height low pressure recycle, can realize separating of methyl alcohol and ritalin azeotrope, saving equipment and energy consumption.Finally obtain obtaining at the bottom of reactive distillation column tower purity and be 95% ethanol, at the bottom of refining methanol tower tower, obtaining methanol concentration is 95%.
Embodiment 3
Process by the utility model method for ritalin preparation of ethanol by hydrogenating, as shown in Figure 2, comprise pre-reactor, reactive distillation column, refining methanol tower, methyl acetate recovery tower, condenser, reboiler, compressor, pump and relevant feeding line and the pipeline that is connected above equipment; It is characterized in that: raw material and circulating hydrogen and ritalin enter pre-reactor, pre-reactor outlet is connected to reactive distillation column; At the bottom of reactive distillation column, refining methanol tower and methyl acetate recovery column overhead and tower, condenser and reboiler are all set, reactive distillation column overhead condenser gaseous phase outlet is connected to compressor, and liquid-phase outlet is connected to refining methanol tower opening for feed, is alcohol product at the bottom of tower; Compressor outlet is connected to reactive distillation column hydrogen feed place; The discharging of refining methanol column overhead enters methyl acetate recovery tower, and bottom product is methyl alcohol; Refining methanol tower is returned in the discharging of methyl acetate recovery column overhead, and at the bottom of tower, the charging of reactive distillation column ritalin is returned in discharging.
Raw hydrogen (S01) and raw material ritalin (S02) are introduced into pre-reactor (R1), and pre-reactor adopts copper-based catalysts, and temperature is 200 ℃, and pressure is 3.0MPa (a), and exported product (S03) enters reactive distillation column (T1), reactive distillation column (T1) adopts copper-based catalysts, pressure is 3.0MPa (a), reflux ratio is 50, top gaseous phase (S04) enters reactive distillation column overhead condenser (E1), gas phase after condensation (S05) is returned to reactive distillation column (T1) charging as circulating hydrogen (S23) after compressor (C1) pressurization, liquid phase after condensation (S06) obtains liquid phase (S07) through reactive distillation column reflux-withdrawal pump (P1), a part is as reactive distillation column backflow (S08), another portion is as refining methanol tower (T2) charging (S09), at the bottom of reactive distillation column tower, be product ethanol (S10), refining methanol tower (T2) pressure 0.5MPa (a), reflux ratio is 50, top gaseous phase (S11) is the liquid phase (S13) through refining methanol tower reflux-withdrawal pump (P2) through condenser (E3) liquid phase (S12), a part is as reflux (S14), another part is as methyl acetate recovery tower (T3) charging (S15), extraction product methyl alcohol (S16) at the bottom of refining methanol tower tower, methyl acetate recovery tower (T3) pressure 1.0MPa (a), reflux ratio is 50, top gaseous phase (S17) obtains liquid phase (S19) through condenser (E5) liquid phase (S18) through methyl acetate recovery tower reflux-withdrawal pump (P3), a part is as reflux (S20), another part is that methyl alcohol and ritalin azeotrope (S21) return to refining methanol tower (T2), and at the bottom of tower, extraction circulation ritalin (S22) returns to reactive distillation column (T1) charging.The copper-based catalysts active ingredient adopting in pre-reactor (R1) and reactive distillation column (T1) is copper, and auxiliary agent is aluminium, and employing carrier is aluminum oxide molecular sieve.
By ritalin hydrogenation reaction and two unit operations of ethyl alcohol purification rectifying separation, be organically coupled in an equipment and carry out simultaneously, react and obtained high-purity alcohol product simultaneously, both saved facility investment, reduce again follow-up process cost.In addition, by refining methanol tower and the operation of methyl acetate recovery tower height low pressure recycle, can realize separating of methyl alcohol and ritalin azeotrope, saving equipment and energy consumption.Finally obtain obtaining at the bottom of reactive distillation column tower purity and be 99.9% ethanol, at the bottom of refining methanol tower tower, obtaining methanol concentration is 99.9%.
Embodiment 4
Process by the utility model method for ritalin preparation of ethanol by hydrogenating, as shown in Figure 2, comprise pre-reactor, reactive distillation column, refining methanol tower, methyl acetate recovery tower, condenser, reboiler, compressor, pump and relevant feeding line and the pipeline that is connected above equipment; It is characterized in that: raw material and circulating hydrogen and ritalin enter pre-reactor, pre-reactor outlet is connected to reactive distillation column; At the bottom of reactive distillation column, refining methanol tower and methyl acetate recovery column overhead and tower, condenser and reboiler are all set, reactive distillation column overhead condenser gaseous phase outlet is connected to compressor, and liquid-phase outlet is connected to refining methanol tower opening for feed, is alcohol product at the bottom of tower; Compressor outlet is connected to reactive distillation column hydrogen feed place; The discharging of refining methanol column overhead enters methyl acetate recovery tower, and bottom product is methyl alcohol; Refining methanol tower is returned in the discharging of methyl acetate recovery column overhead, and at the bottom of tower, the charging of reactive distillation column ritalin is returned in discharging.
Raw hydrogen (S01) and raw material ritalin (S02) are introduced into pre-reactor (R1), and pre-reactor adopts copper-based catalysts, and temperature is 350 ℃, and pressure is 8.0MPa (a), and exported product (S03) enters reactive distillation column (T1), reactive distillation column (T1) adopts copper-based catalysts, pressure is 7.0MPa (a), reflux ratio is 100, top gaseous phase (S04) enters reactive distillation column overhead condenser (E1), gas phase after condensation (S05) is returned to reactive distillation column (T1) charging as circulating hydrogen (S23) after compressor (C1) pressurization, liquid phase after condensation (S06) obtains liquid phase (S07) through reactive distillation column reflux-withdrawal pump (P1), a part is as reactive distillation column backflow (S08), another portion is as refining methanol tower (T2) charging (S09), at the bottom of reactive distillation column tower, be product ethanol (S10), refining methanol tower (T2) pressure 1.0MPa (a), reflux ratio is 100, top gaseous phase (S11) is the liquid phase (S13) through refining methanol tower reflux-withdrawal pump (P2) through condenser (E3) liquid phase (S12), a part is as reflux (S14), another part is as methyl acetate recovery tower (T3) charging (S15), extraction product methyl alcohol (S16) at the bottom of refining methanol tower tower, methyl acetate recovery tower (T3) pressure 2.0MPa (a), reflux ratio is 100, top gaseous phase (S17) obtains liquid phase (S19) through condenser (E5) liquid phase (S18) through methyl acetate recovery tower reflux-withdrawal pump (P3), a part is as reflux (S20), another part is that methyl alcohol and ritalin azeotrope (S21) return to refining methanol tower (T2), and at the bottom of tower, extraction circulation ritalin (S22) returns to reactive distillation column (T1) charging.The copper-based catalysts active ingredient adopting in pre-reactor (R1) and reactive distillation column (T1) is copper, and auxiliary agent is the combination of zinc and aluminium, and employing carrier is graphite.
By ritalin hydrogenation reaction and two unit operations of ethyl alcohol purification rectifying separation, be organically coupled in an equipment and carry out simultaneously, react and obtained high-purity alcohol product simultaneously, both saved facility investment, reduce again follow-up process cost.In addition, by refining methanol tower and the operation of methyl acetate recovery tower height low pressure recycle, can realize separating of methyl alcohol and ritalin azeotrope, saving equipment and energy consumption.Finally obtain obtaining at the bottom of reactive distillation column tower purity and be 99.95% ethanol, at the bottom of refining methanol tower tower, obtaining methanol concentration is 99.98%.
The ritalin hydrogenation the utility model proposes is produced the reaction and rectification device of ethanol, be described by preferred embodiment, person skilled obviously can change or suitably change and combination equipment as herein described not departing from the utility model content, spirit and scope, realizes the utility model technology.Special needs to be pointed out is, all similar replacements and change apparent to those skilled in the artly, they are deemed to be included in the utility model spirit, scope and content.
Claims (2)
1. ritalin hydrogenation is produced a reaction and rectification device for ethanol, comprises reactive distillation column, refining methanol tower, methyl acetate recovery tower, condenser, reboiler, compressor, pump and relevant feeding line and the pipeline that is connected above equipment; It is characterized in that: at the bottom of reactive distillation column, refining methanol tower and methyl acetate recovery column overhead and tower, condenser and reboiler are all set, reactive distillation column overhead condenser gaseous phase outlet is connected to compressor, liquid-phase outlet is connected to refining methanol tower opening for feed, is alcohol product at the bottom of tower; Compressor outlet is connected to reactive distillation column hydrogen feed place; The discharging of refining methanol column overhead enters methyl acetate recovery tower, and bottom product is methyl alcohol; Refining methanol tower is returned in the discharging of methyl acetate recovery column overhead, and at the bottom of tower, the charging of reactive distillation column ritalin is returned in discharging.
2. device as claimed in claim 1, is characterized in that arranging pre-reactor before reactive distillation column, and raw material and circulating hydrogen and ritalin enter pre-reactor, and pre-reactor outlet is connected to reactive distillation column.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320740304.2U CN203602526U (en) | 2013-11-20 | 2013-11-20 | Reactive distillation device for producing ethanol from methyl acetate by adding hydrogen |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201320740304.2U CN203602526U (en) | 2013-11-20 | 2013-11-20 | Reactive distillation device for producing ethanol from methyl acetate by adding hydrogen |
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| CN203602526U true CN203602526U (en) | 2014-05-21 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588618A (en) * | 2013-11-20 | 2014-02-19 | 天津大学 | Reactive distillation method and device for producing ethanol from methyl acetate by adding hydrogen |
| CN105367384A (en) * | 2014-08-27 | 2016-03-02 | 中国石油化工股份有限公司 | Separation method for producing ethyl alcohol through acetate hydrogenation |
| CN105367386A (en) * | 2014-08-27 | 2016-03-02 | 中国石油化工股份有限公司 | Separation method of making ethyl alcohol and co-production of methyl alcohol by adding hydrogen to acetic ester |
| CN105439821A (en) * | 2014-08-27 | 2016-03-30 | 中国石油化工股份有限公司 | A separating process for ethanol production by methyl acetate hydrogenation |
-
2013
- 2013-11-20 CN CN201320740304.2U patent/CN203602526U/en not_active Withdrawn - After Issue
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588618A (en) * | 2013-11-20 | 2014-02-19 | 天津大学 | Reactive distillation method and device for producing ethanol from methyl acetate by adding hydrogen |
| CN105367384A (en) * | 2014-08-27 | 2016-03-02 | 中国石油化工股份有限公司 | Separation method for producing ethyl alcohol through acetate hydrogenation |
| CN105367386A (en) * | 2014-08-27 | 2016-03-02 | 中国石油化工股份有限公司 | Separation method of making ethyl alcohol and co-production of methyl alcohol by adding hydrogen to acetic ester |
| CN105439821A (en) * | 2014-08-27 | 2016-03-30 | 中国石油化工股份有限公司 | A separating process for ethanol production by methyl acetate hydrogenation |
| CN105367384B (en) * | 2014-08-27 | 2017-09-15 | 中国石油化工股份有限公司 | The separation method of acetate preparation of ethanol by hydrogenating |
| CN105439821B (en) * | 2014-08-27 | 2017-09-15 | 中国石油化工股份有限公司 | The process of methyl acetate preparation of ethanol by hydrogenating separation process |
| CN105367386B (en) * | 2014-08-27 | 2017-11-21 | 中国石油化工股份有限公司 | The separation method of acetate preparation of ethanol by hydrogenating co-production methanol |
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