CN102179059A - Hydrolysis separation device of methyl acetate and process method thereof - Google Patents

Hydrolysis separation device of methyl acetate and process method thereof Download PDF

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CN102179059A
CN102179059A CN2011100490990A CN201110049099A CN102179059A CN 102179059 A CN102179059 A CN 102179059A CN 2011100490990 A CN2011100490990 A CN 2011100490990A CN 201110049099 A CN201110049099 A CN 201110049099A CN 102179059 A CN102179059 A CN 102179059A
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tower
section
pipeline
methyl acetate
stripping section
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李军
孙兰义
宁亚南
周宪田
李青松
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China University of Petroleum East China
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Abstract

The invention provides a hydrolysis separation device of methyl acetate and a process method thereof, and in particular relates to a process of utilizing an inner thermally-coupled reaction rectifying tower to carry out a catalytic hydrolysis reaction and product separation on methyl acetate. The device comprises an inner thermally-coupled reaction rectifying section, a stripping section, a heat exchanger, a compressor, a throttling valve, a condenser, a reboiler, a methanol separation tower and accessory equipment (the condenser and the reboiler), wherein the compressor is arranged between the inner thermally-coupled reaction rectifying section and the stripping section; steam from the tower top of the stripping section enters the tower bottom of the rectifying section after being pressurized by the compressor; the tower bottom of the rectifying section is provided with the throttling valve so as to guarantee the stable pressure of the stripping section; and the heat exchange is realized between the rectifying section and the stripping section by the heat exchanger. In the invention, the advantages of the inner thermally-coupled reaction rectifying tower and the reactive rectification can be fully exerted, and the catalytic hydrolysis reaction and target product purification can be simultaneously achieved. In the device and the process flow, the hydrolysis rate of the methyl acetate is more than 99%, and the mass fraction of a high-purity methanol product is more than 99%, and simultaneously, the energy coupling between the two tower sections can greatly reduce energy consumption.

Description

A kind of hydrolysis device of methyl acetate and process thereof
Technical field
The present invention relates to a kind of chemical reaction separator and process thereof, specifically be meant a kind of new device and technology of utilizing internal thermal coupled reaction fractionating tower to carry out the methyl acetate catalyzing hydrolysis, catalyzing hydrolysis, the product that can finish methyl acetate separate, and compare with the popular response rectifier unit and can save energy 30~50%.
Background technology
Methyl acetate is the byproduct in the polyvinyl alcohol production process, and each PVA producer all is that acetate and Methanol Recovery are used with methyl acetate hydrolysis at present.The methyl acetate hydrolysis technology of domestic and foreign current mainly adopts exchange resin catalyzed hydrolysis process of fixed bed cation and reactive distillation hydrolysis process.
The shortcoming of the exchange resin catalyzed hydrolysis process of fixed bed cation is: the methyl acetate hydrolysis rate is low, is 1: 1 o'clock in the mol ratio of water and methyl acetate, only reaches 23%~25%; There are a plurality of azeotropic systems, the separation process complexity in the methyl acetate hydrolysis product simultaneously; The recovery that need circulate of a large amount of unhydrolysed methyl acetates adds complicated separation process, causes equipment investment big, the separating energy consumption height.
Afterwards, many scholars have improved fixed-bed catalytic hydrolysis flow process, the methyl acetate that they will react after the hydrolysis mixes product earlier through after the simple rectifying separation, unreacted methyl acetate Returning reactor is further reacted, can improve percent hydrolysis like this, alleviate the later separation task, as patent CN101012162A, CN1333204A, US4352940, JP59036631 etc.But this method is not still broken away from the intrinsic drawback of fixed-bed catalytic hydrolysis flow process.
Many in recent years scholars have done big quantity research to the method and the technology of reactive distillation hydrolysis methyl acetate, and have several pieces of patents to occur.They load catalyst filling in common rectifying tower, hydrolysis is incorporated in the rectifying column carries out, and then through a series of separation process and obtain unreacted methyl acetate and each product completely, this thinking can in time shift out conversion zone with reactant, to improve hydrolysis reaction, as patent US5770770, CN1927792A, CN1380273A, CN1343649A etc.The reactive distillation hydrolysis process can improve the percent hydrolysis of methyl acetate, course of reaction and distillation process organically are coupled, reactant is separated with product when reacting, both improved the concentration of reactant in reaction zone, improve reaction rate, make product in time leave reaction zone again and suppressed the generation of back reaction.But still there are some defectives in this technology: all be the cat head total reflux operation as above-mentioned patent, for reaching enough percent hydrolysis, must operate under high water to ester ratio and high capacity of returns condition that energy consumption is bigger.
Simultaneously, in traditional rectifying column, introducing the heat of rectifying column reboiler is discharged by the condenser place by after the rectifying column, most energy loss is such as the pressure drop of tower and by on the temperature difference of heat exchanger, and have only portion of energy to be used to reduce the entropy of rectifying column product, its thermodynamic efficiency generally has only 5~10%.
Therefore, Chinese scholars has been carried out a large amount of research to the raising of distillation process energy utilization efficiency for many years, research work mainly concentrates on the integrated aspect of energy of system, comprises that the energy between tower is integrated, the rectifying heat-exchange network synthetic and the energy of single tower inside is integrated.Wherein, internal thermal coupled distillation technology is intended to improve the degree of reversibility that the rectifying column energy utilizes, and can cut down the consumption of energy significantly, and its good energy-saving effect has been subjected to various countries scholars' extensive concern.Internal thermally coupled distillation column is that conventional tower is punished into two rectifying columns from charging, be called rectifying section and stripping section, because the temperature of conventional tower rectifying section is lower than stripping section, the liquid that descends for the Steam Heating stripping section that rises with rectifying section, compressor is set between the two raises its temperature with the steam that pressurization stripping section cat head comes out, choke valve is set to guarantee the stable of stripping section pressure at the bottom of the rectifying section tower, can produce the liquid of decline and the steam of rising in the inside of rectifying section and stripping section respectively by two intersegmental energy couplings like this, provide withdrawing fluid and the steam that boils again by the coupling of the energy between tower, can reduce the reboiler energy consumption greatly.Therefore, can significantly cut down the consumption of energy and equipment investment, increase economic efficiency.
Patent US200501213031011 flows by analysing fluid and has proposed several heat transfer structure models of relevant internal thermally coupled distillation column, comprise horizontal heat transfer and vertical heat transfer structure, patent US200902607911011 discloses a kind of concrete structure of internal thermal coupled distillation technology, and rectifying section and stripping section adopt the concentric shaft type heat exchange mode of single tube.Patent 201N200951326Y discloses a kind of inside diathermanous formula coupling rectification energy saver, diathermanous mode adopts concentric shaft type heat exchanger or plate-fin heat exchanger, adopt the utility model device in this patent respectively benzene/methylbenzene, ethanol/water system to be separated, compare with traditional rectifier unit energy consumption cost, can save energy more than 30~40%.Patent 201N200955890Y is applied to air separation unit with this inside diathermanous formula coupling rectification tower, compare with the energy consumption of existing cryogenic air separation plant, can save energy more than 30%, improved rate of energy greatly, simultaneously the tower body height can reduce near half, help the equipment installation and maintenance, operation is implemented.Patent 201N201463462U discloses a kind of plate-fin thermal coupling rectification device, last tower hypomere in the Cryogenic air rectifying separation field and following tower epimere are thermally coupled in one, cancel traditional main condenser evaporimeter, reduced time tower operating pressure, saved the air compressor energy consumption.The internal thermal coupled destilling tower that patent 201N201454133U provides is arranged on rectifying section and stripping section outside with heat exchanger, makes the area of heat exchanger no longer be subjected to the restriction of destilling tower technology, has improved operating flexibility, dynamic characteristic and the controllability of destilling tower.
Above-mentioned two kinds of chemical coupling procedures are combined, reactive distillation is applied in the internal thermally coupled distillation column, be internal thermal coupled reaction fractionating tower.Internal thermal coupled reaction rectification technique be a reaction with separate simultaneously carry out, highly enriched complex technology, can further improve reaction conversion ratio and selectivity, cut down the consumption of energy.
Summary of the invention
The purpose of this invention is to provide a kind of process and device that utilizes internal thermal coupled reaction fractionating tower to realize the height coupling that methyl acetate catalyzing hydrolysis and product separate.The present invention organically combines course of reaction, product separation and carries out simultaneously, can directly obtain highly purified methanol product, and improves thermodynamic efficiency significantly by the energy coupling, cuts down the consumption of energy.Simultaneously, internal thermal coupled reaction fractionating tower adopts rectifying section, heat exchanger, the parallel successively continuous parallel construction of stripping section, and the height of tower is reduced greatly, helps plant maintenance, and operation is implemented and handling safety.
Device of the present invention is internal thermal coupled reaction fractionating tower and methyl alcohol knockout tower, and as shown in Figure 1, promptly raw water and methyl acetate are according to certain proportioning access to plant.This internal thermal coupled reaction fractionating tower rectifying section (1) has 15~25 theoretical plates, there are 5~10 theoretical plates its recovery area, middle and upper part (101), reaction zone (102) has 10~15 theoretical plates, stripping section (2) has 15~25 theoretical plates, wherein reaction zone (201) has 3~10 theoretical plates, and recovery area, bottom (202) have 12~15 theoretical plates.Methyl alcohol knockout tower (8) has 15~25 theoretical plates.Stripping section (2) (heat absorbing part) links to each other successively in internal thermal coupled reactive distillation enriching section (1) (giving hot part), heat exchanger (3) and the internal thermal coupled reaction fractionating tower, and reaction zone (102) bottom links to each other with choke valve (5) by compressor (4) with reaction zone (201) top.Heat exchanger (3) form is concentric shaft type of multitube or plate-fin, concentric shaft type heat exchanger of multitube such as accompanying drawing 3, and wherein the fluid of the fluid of rectifying section and stripping section is walked tube side d and shell side D respectively; Plate-fin heat exchanger is seen accompanying drawing 4.In order to realize that inner heat is from the transmission of rectifying section (1) to stripping section (2), introduce compressor (4) and regulate the pressure of the two, the gas phase on stripping section (2) top carries out rectifying section (1) entering the compression of the preceding elder generation of rectifying section (1) by compressor (4) under higher pressure and temperature conditions.In order to guarantee that stripping section (2) moves under lower pressure, the liquid phase of rectifying section (1) bottom is passed through choke valve (5) earlier before entering stripping section, to keep the pressure difference on both sides.
Method of the present invention is: as the water of reactant by the metering proportion preheating after pipeline (11) enters reaction zone (102) top of rectifying section (1), reactant methyl acetate fresh feed mixes after pipeline (14) enters reaction zone (201) bottom of stripping section (2) with recycle stream from pipeline (13) through pipeline (12).Like this, under the effect of catalyst, catalytic hydrolysis reaction generation methyl alcohol and acetate take place with the reverse reaction zone (201) that contacts at reaction zone that is filled with the rectifying section of hydrolyst (1) (102) and stripping section (2) of water in methyl acetate.The azeotropic mixture that unreacted methyl acetate and product methyl alcohol form gets off a part of methanol wash through the washing effect of the recovery area, top (101) of rectifying section (1), and squeezes into the further reaction of reaction zone (201) bottom of stripping section (2) remove low amounts of water under rectifying action after successively as recycle stream through pipeline (17), condenser (6), pipeline (31), pipeline (13) from the cat head discharging.Reaction zone (102) bottom liquid phases of rectifying section (1) enters reaction zone (201) the top continuation generation catalytic hydrolysis reaction of stripping section (2) successively through pipeline (16), choke valve (5), pipeline (25), reaction zone (201) the top gas phase of stripping section (2) enters reaction zone (102) the bottom continuation generation catalytic hydrolysis reaction and the centrifugation of rectifying section (1) successively through pipeline (15), compressor (4), pipeline (24).Product and excessive water are removed the small amount of acetic acid methyl esters after pipeline (18) is discharged the tower still through the effect of heating up in a steamer of carrying of stripping section (2) recovery area, bottom (202), the part logistics enters reboiler (7) through pipeline (30) and produces the steam that boils again and return the tower still through pipeline (26), another part enters methyl alcohol knockout tower (8) as product stream through pipeline (19), the rectifying action of the rectification zone (801) of process methyl alcohol knockout tower (8) obtains the high purity methanol product successively through pipeline (20) at cat head, condenser (9), pipeline (32), pipeline (22) discharger, heat up in a steamer through carrying of methyl alcohol knockout tower (8) stripping zone (802) and to act on the mixture that obtains acetate and water at the bottom of the tower and discharge the tower still through pipeline (21), the part logistics enters reboiler (10) through pipeline (33) and produces the steam that boils again and return the tower still through pipeline (29), and another part goes later separation as product stream through pipeline (23) discharger.Catalytic hydrolysis reaction occurs in the reaction zone (102) of rectifying section (1) and the reaction zone (201) of stripping section (2).
It is 0.15~0.5MPa that the internal thermal coupled reaction fractionating tower rectifying section of the present invention (1) tower is pressed, stripping section (2) atmospheric operation, methyl alcohol knockout tower (8) atmospheric operation.In the operating process, internal thermal coupled reaction fractionating tower rectifying section (1) cat head top reflux ratio is 0.2~10, rectifying section (1) tower top temperature is 60~90 ℃, the temperature of reaction zone (102) is 70~100 ℃, tower still temperature is 80~100 ℃, stripping section (2) tower top temperature is 50~70 ℃, and the temperature of reaction zone (201) is 50~70 ℃, and tower still temperature is 70~100 ℃.Methyl alcohol knockout tower (8) tower top temperature is 50~80 ℃, and tower still temperature is 100~120 ℃.Charging is liquid phase feeding, and temperature is 20~80 ℃, and the methyl acetate charging can be the methyl acetate pure component, also can be methyl acetate and methanol mixture, wherein, the methyl acetate mass fraction is greater than 70%, and raw water and methyl acetate mol ratio are 4: 1~10: 1.
Methyl alcohol knockout tower cat head methanol quality mark reaches more than 99% among the present invention, and the methyl acetate hydrolysis rate reaches same percent hydrolysis and product separation requirement more than 99%, can save energy 30~50% than popular response distillation process.
Description of drawings
Fig. 1: the internal thermal coupled reaction fractionating tower of methyl acetate hydrolysis and methyl alcohol separator schematic flow sheet
Fig. 2: the popular response rectifying double-column process schematic diagram of methyl acetate hydrolysis
Fig. 3: the structural representation of the concentric shaft type heat exchanger of multitube
Fig. 4: the structural representation of plate-fin heat exchanger.
Among the figure, 1, rectifying section, 2, stripping section, 3, heat exchanger, 4, compressor, 5, choke valve, 6, condenser, 7, reboiler, 8, the methyl alcohol knockout tower, 9, condenser, 10, reboiler, 11~40, pipeline
Specific embodiments
The present invention is described in further detail below in conjunction with accompanying drawing and example:
Example 1: flow process as shown in Figure 1.Each Region Theory plate number is as shown in table 1, feed rate and form as shown in table 2, raw water and methyl acetate raw materials components mole ratio are 5: 1, the feed entrance point of water and methyl acetate (counting from top to bottom) is respectively the 6th theoretical plate of rectifying section (1) and the 3rd theoretical plate of stripping section (2), and charging is 50 ℃.Internal thermal coupled reaction fractionating tower rectifying section (1) top reflux ratio is 3.45, methyl alcohol knockout tower (8) top reflux ratio is 5.38, each logistics flux and form as shown in table 2, rectifying section (1) top temperature is 80 ℃, stripping section (2) still temperature is 83.3 ℃, and methyl alcohol knockout tower (8) top temperature is 67.8 ℃, and the still temperature is 106.5 ℃, stripping section (2) and methyl alcohol knockout tower atmospheric operation, rectifying section (1) pressure is 0.25MPa.The total percent hydrolysis of gained methyl acetate is 99.5%, and finishing the required total heat conduction area that conducts heat is 544m 2Reach same percent hydrolysis and product separation requirement, the required total energy consumption of this technological process is 7223.5kW, and the old process total energy consumption is 10702.36kW, compares and can save energy 32.51%.
Table 1 example 1 each Region Theory plate number
Figure BSA00000442128500041
Figure BSA00000442128500051
Table 2 example 1 each logistics quality flow and each constituent mass mark
Figure BSA00000442128500052
Example 2: flow process as shown in Figure 1.Feed heat state, feed entrance point and each Region Theory plate number be with example 1, methyl acetate pure component charge raw material, and water and methyl acetate raw materials components mole ratio are 4.2: 1, rectifying section (1) pressure is 0.15MPa.Internal thermal coupled reaction fractionating tower rectifying section (1) top reflux ratio is 3.5, methyl alcohol knockout tower (8) top reflux ratio is 5.38, each logistics flux and form as shown in table 3, rectifying section (1) top temperature is 80 ℃, stripping section (2) still temperature is 85.4 ℃, and methyl alcohol knockout tower (8) top temperature is 67.7 ℃, and the still temperature is 106.6 ℃, stripping section (2) and methyl alcohol knockout tower atmospheric operation, rectifying section (1) pressure is 0.15MPa.Gained methyl acetate hydrolysis rate is 99.22%, and finishing the required total heat conduction area that conducts heat is 525m 2Reach same percent hydrolysis and product separation requirement, the required total energy consumption of this technological process is 6345.6kW, and the old process total energy consumption is 12063.7kW, compares and can save energy 47.4%.
Table 3 example 2 each logistics quality flow and each constituent mass mark
Figure BSA00000442128500053
Example 3: flow process as shown in Figure 1.Feed composition, feed heat state, feed entrance point and each Region Theory plate number are with example 1, and just raw water and methyl acetate raw materials components mole ratio are 10: 1.Internal thermal coupled reaction fractionating tower rectifying section (1) top reflux ratio is 3.6, methyl alcohol knockout tower (8) top reflux ratio is 5.38, each logistics flux and form as shown in table 4, rectifying section (1) top temperature is 79.8 ℃, stripping section (2) still temperature is 87.7 ℃, and methyl alcohol knockout tower (8) top temperature is 67.7 ℃, and the still temperature is 105.8 ℃, stripping section (2) and methyl alcohol knockout tower atmospheric operation, rectifying section (1) pressure is 0.25MPa.Gained methyl acetate hydrolysis rate is 99.42%, and finishing the required total heat conduction area that conducts heat is 858m 2Reach same percent hydrolysis and product separation requirement, the required total energy consumption of this technological process is 7624kW, and the old process total energy consumption is 11065.9kW, compares and can save energy 31.1%.
Table 4 example 3 each logistics quality flow and each constituent mass mark
Figure BSA00000442128500061
Example 4: flow process as shown in Figure 1.Feed heat state, feed entrance point and each Region Theory plate number are with example 1, and the methyl acetate charging is methyl acetate and methanol mixture, and wherein, the methyl acetate mass fraction is 70.6%, and water and methyl acetate raw materials components mole ratio are 6.4: 1.Internal thermal coupled reaction fractionating tower rectifying section (1) top reflux ratio is 3.5, methyl alcohol knockout tower (8) top reflux ratio is 5.38, each logistics flux and form as shown in table 5, rectifying section (1) top temperature is 80 ℃, stripping section (2) still temperature is 83.1 ℃, and methyl alcohol knockout tower (8) top temperature is 67.6 ℃, and the still temperature is 106.3 ℃, stripping section (2) and methyl alcohol knockout tower atmospheric operation, rectifying section (1) pressure is 0.25MPa.Gained methyl acetate hydrolysis rate is 99.6%, and finishing the required total heat conduction area that conducts heat is 1067m 2Reach same methyl acetate hydrolysis rate and product separation requirement, the required total energy consumption of this technological process is 7230.4kW, and the old process total energy consumption is 10684.2kW, compares and can save energy 32.3%.
Table 5 example 4 each logistics quality flow and each constituent mass mark
Figure BSA00000442128500062
Example 5: flow process as shown in Figure 1.Feed composition, feed heat state, feed entrance point and each Region Theory plate number are with example 1, and rectifying section pressure is brought up to 0.5MPa, and raw water and methyl acetate raw materials components mole ratio are 4: 1.Internal thermal coupled reaction fractionating tower rectifying section (1) top reflux ratio is 10, methyl alcohol knockout tower (8) top reflux ratio is 5.38, each logistics flux and form as shown in table 6, rectifying section (1) top temperature is 84.4 ℃, stripping section (2) still temperature is 76.7 ℃, and methyl alcohol knockout tower (8) top temperature is 67.5 ℃, and the still temperature is 106.5 ℃, stripping section (2) and methyl alcohol knockout tower atmospheric operation, rectifying section (1) pressure is 0.5MPa.Gained methyl acetate hydrolysis rate is 99.2%, and finishing the required total heat conduction area that conducts heat is 348m 2Reach same acetate conversion ratio and product separation requirement, the required total energy consumption of this technological process is 9357.4kW, and the old process total energy consumption is 13515.2kW, compares and can save energy 30.8%.
Table 6 example 5 each logistics quality flow and each constituent mass mark
Figure BSA00000442128500063
Figure BSA00000442128500071

Claims (8)

1. the hydrolysis device of a methyl acetate, it is characterized in that, this device comprises rectifying section (1), stripping section (2), heat exchanger (3), compressor (4), choke valve (5), condenser (6), reboiler (7), methyl alcohol knockout tower (8), condenser (9), reboiler (10), described rectifying section (1), heat exchanger (3) links to each other successively with stripping section (2), the cat head gas phase delivery line (15) that described compressor (4) is installed on described stripping section (2) and rectifying section (1) tower spirit are mutually between the feed pipe (24), described choke valve (5) is installed at the bottom of the tower of rectifying section (1) between the liquid phase delivery line (16) and stripping section (2) cat head liquid phase feed pipe (25), described condenser (6) is installed on the product delivery line (17) of rectifying section (1) cat head, described reboiler (7) links to each other with product delivery line (18) at the bottom of stripping section (2) tower through pipeline (30), described methyl alcohol knockout tower (8) is connected on the product delivery line (19) at the bottom of stripping section (2) tower, described condenser (9) is connected with methyl alcohol knockout tower (8) cat head gas phase delivery line (20), and described reboiler (10) links to each other with liquid phase delivery line (21) at the bottom of methyl alcohol knockout tower (8) tower through pipeline (33).
2. the methyl acetate hydrolysis process that utilization is installed according to claim 1 is characterized in that, methyl acetate catalyzing hydrolysis and obtain separate purifying in internal thermal coupled reaction fractionating tower, and this process is made up of following steps:
A) as the water of reactant by the metering proportion preheating after pipeline (11) enters reaction zone (102) top of rectifying section (1), reactant methyl acetate fresh feed mixes after pipeline (14) enters reaction zone (201) bottom of stripping section (2) with recycle stream from pipeline (13) through pipeline (12);
B) under the effect of catalyst, the raw acetic acid methyl esters generates methyl alcohol and acetate with water reverse generation catalytic hydrolysis reaction that contacts in the reaction zone (201) of reaction zone that is filled with the rectifying section of hydrolyst (1) (102) and stripping section (2);
C) the unreacted azeotropic mixture that forms of methyl acetate and product methyl alcohol completely, the washing effect of the recovery area, top (101) of process rectifying section (1) gets off a part of methanol wash, and mixes the further reaction of reaction zone (201) bottom of squeezing into stripping section (2) through pipeline (14) from the cat head discharging with fresh methyl acetate charging as recycle stream through pipeline (13) remove low amounts of water under rectifying action after;
D) reaction zone (102) bottom liquid phases of rectifying section (1) enters reaction zone (201) the top continuation generation catalytic hydrolysis reaction of stripping section (2) successively through pipeline (16), choke valve (5), pipeline (25);
E) reaction zone (201) the top gas phase of stripping section (2) enters reaction zone (102) the bottom continuation generation catalytic hydrolysis reaction and the centrifugation of rectifying section (1) successively through pipeline (15), compressor (4), pipeline (24);
F) product and excessive water are removed the small amount of acetic acid methyl esters through the effect of heating up in a steamer of carrying of the recovery area, bottom (202) of stripping section (2);
G) stripping section (2) tower kettle product enters methyl alcohol knockout tower (8) through pipeline (18), (19) successively, the rectifying action of rectification zone (801) through methyl alcohol knockout tower (8) obtains the high purity methanol product successively through pipeline (20), condenser (9), pipeline (32), pipeline (22) discharger at cat head, heats up in a steamer through carrying of methyl alcohol knockout tower (8) stripping zone (802) to act on the mixture that obtains acetate and water at the bottom of the tower and go later separation through pipeline (21), (23) discharger successively.
3. the hydrolysis device of methyl acetate as claimed in claim 1 is characterized in that, described heat exchanger (3) is concentric shaft type heat exchanger of multitube or plate-fin heat exchanger.
4. as claim 1,2 described device and processes thereof, it is characterized in that catalytic hydrolysis reaction occurs in the reaction zone (102) of rectifying section (1) and the reaction zone (201) of stripping section (2).
5. process as claimed in claim 2 is characterized in that described methyl acetate charging can be the methyl acetate pure component, also can be methyl acetate and methanol mixture, and when charging was described mixture, the methyl acetate mass fraction was greater than 70%.
6. process as claimed in claim 2 is characterized in that described raw water and methyl acetate mol ratio are 4: 1~10: 1.
7. process as claimed in claim 2 is characterized in that rectifying section (1) tower top temperature is 60~90 ℃, and reaction zone (102) temperature is 70~100 ℃, and stripping section (2) tower still temperature is 70~100 ℃, and reaction zone (201) temperature is 50~70 ℃; It is 0.15~0.5MPa that rectifying section (1) tower is pressed, stripping section (2) atmospheric operation.
8. process as claimed in claim 2 is characterized in that methyl alcohol knockout tower (8) tower top temperature is 50~80 ℃, and tower still temperature is 100~120 ℃, methyl alcohol knockout tower (8) atmospheric operation.
CN2011100490990A 2011-02-24 2011-02-24 Hydrolysis separation device of methyl acetate and process method thereof Pending CN102179059A (en)

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CN103113614A (en) * 2013-02-28 2013-05-22 天津普莱化工技术有限公司 PVA (Polyvinyl alcohol) energy-saving and consumption-reducing production new technology method
CN111606797A (en) * 2020-06-12 2020-09-01 天津大学 New reaction rectification process for separating methyl acetate hydrolysate by using bulkhead column
CN111689836A (en) * 2020-06-12 2020-09-22 天津大学 Methyl acetate hydrolysis process of middle steam compression reaction rectifying tower integrated partition wall tower

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CN103113614A (en) * 2013-02-28 2013-05-22 天津普莱化工技术有限公司 PVA (Polyvinyl alcohol) energy-saving and consumption-reducing production new technology method
CN103113614B (en) * 2013-02-28 2014-10-29 天津普莱化工技术有限公司 PVA (Polyvinyl Alcohol) Energy-Saving and Consumption-Reducing Production New Technology Method
CN111606797A (en) * 2020-06-12 2020-09-01 天津大学 New reaction rectification process for separating methyl acetate hydrolysate by using bulkhead column
CN111689836A (en) * 2020-06-12 2020-09-22 天津大学 Methyl acetate hydrolysis process of middle steam compression reaction rectifying tower integrated partition wall tower

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Application publication date: 20110914