CN115006862B - Energy-saving high-purity n-butanol extraction system and method - Google Patents
Energy-saving high-purity n-butanol extraction system and method Download PDFInfo
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- CN115006862B CN115006862B CN202210684326.5A CN202210684326A CN115006862B CN 115006862 B CN115006862 B CN 115006862B CN 202210684326 A CN202210684326 A CN 202210684326A CN 115006862 B CN115006862 B CN 115006862B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/007—Energy recuperation; Heat pumps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
- B01D3/322—Reboiler specifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- 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
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Abstract
The invention relates to an n-butanol extraction system, in particular to an energy-saving high-purity n-butanol extraction system and method. An energy-saving high-purity n-butanol extraction system is mainly formed by a preheater, an n-butanol light-removal tower, an n-butanol heavy-removal tower and an n-isobutyraldehyde separation tower in sequence, wherein raw n-butanol raw materials enter the system through the preheater and are subjected to heat exchange with n-butanol products obtained by the n-butanol heavy-removal tower in the preheater; the n-butyl alcohol light component removing tower, the n-butyl alcohol heavy component removing tower and the n-isobutyl aldehyde separating tower are respectively connected with a reboiler for heat recovery, and the top of the n-butyl alcohol heavy component removing tower is connected with the reboiler pipeline of the n-isobutyl aldehyde separating tower. The system can effectively improve the rectification effect so as to obtain high-purity n-butanol.
Description
Technical Field
The invention relates to an n-butanol extraction system, in particular to an energy-saving high-purity n-butanol extraction system and method, and belongs to the technical field of n-butanol production.
Background
N-butanol is an important organic chemical raw material, has very wide application, and is mainly used for n-butyl phthalate, fatty dibasic acid, butyl phosphate, butyl acrylate, butyl acetate and the like; can be oxidized to produce butyraldehyde or butyric acid; can also be used as extraction solvent for oil, medicine and perfume, and alkyd resin additive. Can also be used as solvent for organic dye and printing ink, and dewaxing agent. The butanol in China is mainly used for producing butyl acetate, butyl acrylate, dibutyl phthalate, medical intermediates and the like, and the large dosage of the butanol is butyl acetate, butyl acrylate and dibutyl phthalate (DBP).
N-butanol has the chemical formula of CH 3 (CH 2 ) 3 OH is colorless transparent liquid, and emits strong flame during combustion. Has smell similar to fusel oil, and vapor is irritating and can cause cough. Boiling point 117-118 deg.c and relative density 0.810. 63% n-butanol and 37% water to form an azeotropic liquid.
N-butanol is industrially obtained mainly by hydrogenation of n-butyraldehyde, and more impurities such as: the problems of high rectification difficulty, poor product quality and high energy consumption in the rectification process are caused by the fact that the boiling point of impurities is close to that of n-butanol in the production process, and under the conditions of increasingly severe energy crisis and extremely rapid increase of demands of downstream customers on high-end n-butanol products, the pressure of n-butanol production enterprises is high.
Disclosure of Invention
The invention aims at an energy-saving high-purity n-butanol extraction system which can effectively improve the rectification effect so as to obtain high-purity n-butanol.
The invention also provides an energy-saving high-purity n-butanol extraction method, which can obtain high-purity n-butanol products and solve the problems of poor quality of the n-butanol products and high energy consumption in the rectification process.
The technical scheme adopted for solving the technical problems is as follows:
an energy-saving high-purity n-butanol extraction system is mainly formed by a preheater, an n-butanol light-removal tower, an n-butanol heavy-removal tower and an n-isobutyraldehyde separation tower in sequence, wherein raw n-butanol raw materials enter the system through the preheater and are subjected to heat exchange with n-butanol products obtained by the n-butanol heavy-removal tower in the preheater; the n-butyl alcohol light component removing tower, the n-butyl alcohol heavy component removing tower and the n-isobutyl aldehyde separating tower are respectively connected with a reboiler for heat recovery, and the top of the n-butyl alcohol heavy component removing tower is connected with a reboiler pipeline of the n-isobutyl aldehyde separating tower;
the n-butanol light component removing tower and the n-butanol heavy component removing tower are rectifying towers with packing combined with a floating valve tray, the top of the n-butanol light component removing tower is sequentially connected with a first condenser and a first reflux tank, and a reflux pipeline is arranged between the first reflux tank and the n-butanol light component removing tower; the first reflux tank is also provided with an exhaust pipeline with a first tail gas discharge valve, a drainage pipeline and an impurity extraction line pipeline for discharging light components, and one end of the impurity extraction line pipeline is connected to the reflux pipeline;
the top of the n-butanol heavy removal tower is also connected with a second reflux tank, the top of the second reflux tank is connected with a reboiler of the n-isobutyraldehyde separation tower, a reflux pipeline is arranged between the bottom of the second reflux tank and the n-butanol heavy removal tower, and the reflux pipeline is provided with a second reflux valve; the return pipeline is connected with a n-butyl alcohol product extraction pipeline.
The system adopts two rectifying towers which are sequentially connected in series to carry out rectifying purification on crude n-butanol, light component separation is carried out firstly, then heavy component separation is carried out, the rectifying towers adopt a mode of combining filler and a floating valve tray, and thermal coupling is carried out on hot materials at the top of the rectifying tower and a reboiler of the n-isobutyraldehyde separating tower through feeding heat exchange, so that the energy is saved while the n-butanol extraction is finished.
The n-butanol light component removing tower adopts the upper packing, and the structure of the lower tray can effectively reduce the pressure difference in the tower and improve the rectification effect.
The preheater and the second condenser are of a fixed tube plate structure. The preheater in the invention adopts the finally obtained n-butanol product to preheat the raw material crude n-butanol. The first condenser is an air-cooled heat exchanger, and the air-cooled heat exchanger has a variable frequency adjusting function and can freely adjust the cooling effect. The reboiler of the n-isobutyraldehyde separating tower is a vertical fixed tube plate heat exchanger.
Preferably, the top of the n-butanol light component removing tower is provided with a packing layer, the bottom of the n-butanol light component removing tower is provided with a floating valve structure, and the floating valve is a tray which can float on a tray plate and change the opening degree along with the change of the gas flow;
the top of the n-butanol heavy removal tower is of a floating valve structure, the bottom of the n-butanol heavy removal tower is provided with a packing layer, and the floating valve is a tray which can float on a tray plate and change the opening degree along with the change of gas flow.
Preferably, the floating valves in the n-butanol light component removing tower and the n-butanol heavy component removing tower are double overflow trays, the packing is structured packing, and a plurality of temperature measuring points are arranged on the tower body.
Preferably, the first reflux tank is a horizontal tank or a vertical tank with a water collecting bag and a coalescer, the top of the first reflux tank is connected with a first condenser, and the bottom of the first reflux tank is connected with an n-butanol light component removing tower.
Preferably, a first reflux valve is arranged on a reflux pipeline of the first reflux tank, a light component extraction regulating valve is arranged on an impurity extraction line pipeline, a water collecting bag outlet of the first reflux tank is connected with a drainage pipeline, and a water extraction regulating valve is arranged on the drainage pipeline.
Preferably, an n-butyl alcohol extraction valve is arranged between the n-butyl alcohol product extraction pipeline and the preheater, and a second condenser and a second tail gas discharge valve are arranged on the exhaust pipeline of the second reflux tank.
Preferably, a feeding valve of the n-butanol heavy-removal tower is arranged between the n-butanol light-removal tower and the n-butanol heavy-removal tower.
A method for extracting high-purity n-butanol, comprising the following steps:
s1, raw n-butyl alcohol raw material obtained by gas phase or liquid phase hydrogenation production of n-butyl aldehyde is subjected to heat exchange with refined n-butyl alcohol product extracted from an n-butyl alcohol heavy removal tower in a preheater, then enters an n-butyl alcohol light removal tower, a first reboiler at the bottom of the n-butyl alcohol light removal tower is used for heating materials to generate ascending steam, heat and mass transfer are carried out on tower plates and fillers with reflux liquid, so that light components are gasified and enter a gas phase, the n-butyl alcohol product enters a liquid phase, and the gas phase at the top of the tower is condensed by a first condenser and then enters a first reflux tank,
the water is demulsified, coalesced and settled by a coalescer, the emulsified liquid is demulsified, the small water droplets after demulsification are agglomerated into large water droplets, the large water droplets are settled to the bottom of the coalescer, collected in a water collecting bag, discharged and sent to a water treatment device,
other light components such as n-butyraldehyde, isobutanol and other impurities contained in the crude n-butanol are extracted through an impurity extraction line pipeline at the top of the n-butanol light removal tower;
s2, crude n-butanol with light components removed enters an n-butanol heavy removal tower, ascending steam is generated by heating materials through a second reboiler at the tower bottom, heat transfer and mass transfer are carried out on the tower plate and filler with reflux liquid, so that n-butanol is gasified and enters a gas phase, main impurities such as butyl butyrate, trimer and heavy components enter a liquid phase, high-purity gas phase n-butanol at the tower top enters an n-isobutyraldehyde separation tower reboiler to recover heat, the condensed gas phase which is not condensed in a second reflux tank enters a second condenser, all n-butanol enters the second reflux tank after condensation,
part of the n-butanol in the second reflux tank is extracted as a product, enters a preheater for heat recovery and is extracted as n-butanol product, part of the n-butanol is refluxed into the tower as reflux of the tower,
and the impurities such as butyl butyrate, trimer, heavy components and the like are extracted from the tower bottom.
Preferably, the temperature of the tower bottom of the n-butyl alcohol light component removing tower is 120-140 ℃, the temperature of the tower top is 90-100 ℃, and the pressure of the tower top is 0.02-0.08 Mpag.
Preferably, the temperature of the tower bottom of the n-butyl alcohol heavy-removing tower is 130-150 ℃, the temperature of the tower top is 110-120 ℃, and the pressure of the tower top is 0.02-0.08 Mpag.
Compared with the prior art, the invention has the beneficial effects that: the invention adopts the composite novel rectifying tower with the combination of the filler and the floating valve, the pressure difference of the tower is lower than that of a plate-type tower, the mass transfer rate is increased, the retention time of the n-butyl alcohol material at high temperature is shortened, the heavy component generation amount caused by high-temperature polymerization in the rectifying process is reduced, the problems of high difficulty in refining the n-butyl alcohol and low product purity can be effectively solved, and the heat in the gas phase of the heavy-removed tower top of the n-butyl alcohol and the n-butyl alcohol product can be recovered, so that the problem of heat waste is solved.
Drawings
FIG. 1 is a schematic diagram of a high purity n-butanol extraction system according to the present invention;
description of the reference numerals: 1 is a butanol light component removing tower, 2 is a first condenser, 3 is a first reflux tank, 4 is a butanol heavy component removing tower, 5 is a second condenser, 6 is a second reflux tank, 7 is an n-isobutyraldehyde separating tower reboiler, 8 is an n-isobutyraldehyde separating tower, 9 is a preheater, 10 is a first reboiler, 11 is a second reboiler, 12 is a crude butanol feeding regulating valve, 13 is a first reflux valve, 14 is a light component extraction regulating valve, 15 is a water extraction regulating valve, 16 is a first tail gas discharge valve, 17 is a second tail gas discharge valve, 18 is an n-butanol extraction valve, 19 is a second reflux valve, 20 is a heavy component extraction valve, 21 is an n-butanol heavy component removing tower feeding valve, and 22 is a coalescer.
Detailed Description
The technical scheme of the invention is further specifically described by the following specific examples. It should be understood that the practice of the invention is not limited to the following examples, but is intended to be within the scope of the invention in any form and/or modification thereof.
In the present invention, unless otherwise specified, all parts and percentages are by weight, and the equipment, materials, etc. used are commercially available or are conventional in the art. The methods in the following examples are conventional in the art unless otherwise specified.
Examples:
an energy-saving high-purity n-butanol extraction system is shown in figure 1, and is formed by a preheater 9, an n-butanol light-removal tower 1, an n-butanol heavy-removal tower 4 and an n-isobutyraldehyde separation tower 8 in sequence, wherein raw n-butanol raw materials enter the system through the preheater and are subjected to heat exchange with an n-butanol product obtained by the n-butanol heavy-removal tower in the preheater; the n-butyl alcohol light component removing tower, the n-butyl alcohol heavy component removing tower and the n-isobutyl aldehyde separating tower are respectively connected with a reboiler for heat recovery, and the top of the n-butyl alcohol heavy component removing tower is connected with the reboiler pipeline of the n-isobutyl aldehyde separating tower.
The reboilers of the n-butyl alcohol light component removing tower and the n-butyl alcohol heavy component removing tower for heat recovery are respectively a first reboiler 10 and a second reboiler 11, and the reboilers of the n-isobutyl aldehyde separating tower for heat recovery are n-isobutyl aldehyde separating tower reboilers 7.
The n-butanol light component removing tower and the n-butanol heavy component removing tower are rectifying towers with packing combined with a floating valve tray,
the top of the n-butanol light component removing tower is sequentially connected with a first condenser 2 and a first reflux tank 3, and a reflux pipeline is arranged between the first reflux tank and the n-butanol light component removing tower; the first reflux drum is also provided with an exhaust pipe with a first exhaust gas discharge valve 16, a drain pipe and an impurity extraction line pipe for discharging light components, one end of the impurity extraction line pipe being connected to the reflux pipe;
the top of the n-butanol heavy removal tower is also connected with a second reflux tank 6, the top of the second reflux tank is connected with a reboiler 7 of the n-isobutyraldehyde separation tower, a reflux pipeline is arranged between the bottom of the second reflux tank and the n-butanol heavy removal tower, and the reflux pipeline is provided with a second reflux valve 19; the return pipeline is connected with a n-butyl alcohol product extraction pipeline. An n-butyl alcohol extraction valve 18 is arranged between the n-butyl alcohol product extraction pipeline and the preheater, and a second condenser 5 and a second tail gas discharge valve 17 are arranged on the exhaust pipeline of the second reflux tank.
The n-butanol light component removing tower adopts the upper packing, and the structure of the lower tray can effectively reduce the pressure difference in the tower and improve the rectification effect. The top of the n-butanol light component removing tower is provided with a packing layer, the bottom of the n-butanol light component removing tower is provided with a floating valve structure, and the floating valve is a tray which can float on a tray plate and change the opening degree along with the change of the gas flow; the top of the n-butanol heavy removal tower is of a floating valve structure, the bottom of the n-butanol heavy removal tower is provided with a packing layer, and the floating valve is a tray which can float on a tray plate and change the opening degree along with the change of gas flow. The floating valves in the n-butanol light component removing tower and the n-butanol heavy component removing tower are double overflow trays, the packing is structured packing, and a plurality of temperature measuring points are arranged on the tower body.
The first reflux tank is a horizontal tank or a vertical tank with a water collecting bag and a coalescer, the top of the first reflux tank is connected with a first condenser, and the bottom of the first reflux tank is connected with an n-butanol light component removing tower. The reflux pipeline of the first reflux tank is provided with a first reflux valve 13, the impurity extraction line pipeline is provided with a light component extraction regulating valve 14, the water collecting bag outlet of the first reflux tank is connected with a drainage pipeline, and the drainage pipeline is provided with a water extraction regulating valve 15.
An n-butanol heavy-removal tower feeding valve 21 is arranged between the n-butanol light-removal tower and the n-butanol heavy-removal tower.
A high-purity n-butanol extraction method comprises the following specific steps:
s1, raw n-butyl alcohol raw material obtained by gas phase or liquid phase hydrogenation production of n-butyl aldehyde is subjected to heat exchange with refined n-butyl alcohol product extracted from an n-butyl alcohol heavy removal tower in a preheater, then enters an n-butyl alcohol light removal tower, a first reboiler at the bottom of the n-butyl alcohol light removal tower is used for heating materials to generate ascending steam, heat and mass transfer are carried out on tower plates and fillers with reflux liquid, so that light components are gasified and enter a gas phase, the n-butyl alcohol product enters a liquid phase, and the gas phase at the top of the tower is condensed by a first condenser and then enters a first reflux tank,
the water is demulsified, coalesced and settled by a coalescer, the emulsified liquid is demulsified, the small water droplets after demulsification are agglomerated into large water droplets, the large water droplets are settled to the bottom of the coalescer, collected in a water collecting bag, discharged and sent to a water treatment device,
other light components such as n-butyraldehyde, isobutanol and other impurities contained in the crude n-butanol are extracted through an impurity extraction line pipeline at the top of the n-butanol light removal tower;
s2, crude n-butanol with light components removed enters an n-butanol heavy removal tower, ascending steam is generated by heating materials through a second reboiler at the tower bottom, heat transfer and mass transfer are carried out on the tower plate and filler with reflux liquid, so that n-butanol is gasified and enters a gas phase, main impurities such as butyl butyrate, trimer and heavy components enter a liquid phase, high-purity gas phase n-butanol at the tower top enters an n-isobutyraldehyde separation tower reboiler to recover heat, the condensed gas phase which is not condensed in a second reflux tank enters a second condenser, all n-butanol enters the second reflux tank after condensation,
part of the n-butanol in the second reflux tank is extracted as a product, enters a preheater for heat recovery and is extracted as n-butanol product, part of the n-butanol is refluxed into the tower as reflux of the tower,
and the impurities such as butyl butyrate, trimer, heavy components and the like are extracted from the tower bottom.
In general, the temperature of the tower bottom of the n-butyl alcohol light component removing tower is 120-140 ℃, the temperature of the tower top is 90-100 ℃, and the pressure of the tower top is 0.02-0.08 Mpag. The temperature of the tower bottom of the n-butyl alcohol heavy-removing tower is 130-150 ℃, the temperature of the tower top is 110-120 ℃, and the pressure of the tower top is 0.02-0.08 Mpag.
In the embodiment, crude n-butanol generated by hydrogenating n-butyraldehyde enters a preheater 9 to be heated to 70-90 ℃, the flow rate is controlled by a crude butanol feeding regulating valve 12 to enter an n-butanol light-removing tower 1, the bottom of the n-butanol light-removing tower 1 is a tray, the top of the n-butanol light-removing tower 1 is a filler, the material is heated by a first reboiler 10 at the tower bottom, the temperature of the tower bottom is controlled at 120-140 ℃, the temperature of the tower top is controlled at 90-100 ℃, and the pressure of the tower top is 0.02-0.08 Mpa. The gas phase material at the top of the tower enters the first condenser 2 to be cooled to 60-75 ℃, then enters the first reflux tank 3, gas-liquid separation and water separation are carried out in the first reflux tank 3, and uncondensed gas phase such as hydrogen, nitrogen, methane and the like is discharged through the first tail gas discharge valve 16. The trace water mixed in the first reflux tank 3 breaks emulsion, coalesces and settles water dissolved in n-butanol through the effect of a coalescer 22, the emulsified liquid is broken, small water droplets after breaking emulsion are agglomerated into large water droplets, the water is settled to the bottom of the first reflux tank due to density difference, collected in a water collecting bag and discharged through a water extraction regulating valve 15. The overhead mixture after removal of water is mainly: the majority of n-butanol, n-butyraldehyde, isobutanol and the like flow back to the top of the tower, the minority of n-butanol, n-butyraldehyde, isobutanol and the like are extracted according to the temperature of a sensitive plate, and the temperature of the sensitive plate is controlled between 90 and 130 ℃. The temperature reduction of the sensitive plate shows that the accumulation amount of the light components on the top of the tower is greatly increased, the temperature of the sensitive plate is high, the extraction is reduced, the proper temperature of the sensitive plate is maintained, and the total light components are removed by reasonably adjusting the extraction of the light components in combination with the chromatographic analysis data of the tower bottom of the butanol light component removing tower.
The crude n-butanol which has been completely removed of light components enters the n-butanol heavy ends removal column 4 at a temperature of 120-140 ℃ under flow control through the n-butanol heavy ends removal column feed valve 21. The bottom of the butanol heavy-removal tower is filled, the top of the butanol heavy-removal tower is provided with a tray, the tower kettle heats the materials through a second reboiler 11, the temperature of the tower kettle is controlled to be 130-150 ℃, the temperature of the tower top is controlled to be 110-120 ℃, and the pressure of the tower top is 0.02-0.08 MPag. The gas phase n-butanol at the top of the tower enters a reboiler 7 of the n-isobutyl aldehyde separating tower to heat and recover heat, partial condensate of the gas phase n-butanol and the gas phase n-butanol which is not condensed enter a second reflux tank 6 to carry out gas-liquid two-phase separation, and the gas phase enters a second condenser 5 to carry out secondary condensation on the gas phase of the n-butanol and then returns to the second reflux tank 6. At this time, n-butanol having a purity of more than 99.85% was contained in the second reflux drum 6. N-butanol in the second reflux tank 6 is recovered by the preheater 9 according to the material balance part and then is sent to the n-butanol product storage tank, and part of n-butanol is refluxed to the n-butanol heavy removal tower 4. The heavy components accumulate in the column bottoms and pass through heavy component extraction valve 20.
The method has good use effect in the refining of the n-butanol, can effectively remove water dissolved in the n-butanol, effectively reduce the water content, improve the purity of the n-butanol product, and reduce the pressure drop in operation by combining the novel filler with the tray, thereby reducing the probability of flooding in the operation process. The heat is recycled, so that the problem of heat energy waste in the n-butyl alcohol production process can be well solved.
In this specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, so that the same or similar parts between the embodiments are referred to each other. For the device disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and the relevant points refer to the description of the method section.
The energy-saving high-purity n-butanol extraction system and the method provided by the invention are described in detail. The principles and embodiments of the present invention have been described herein with reference to specific examples, the description of which is intended only to facilitate an understanding of the method of the present invention and its core ideas. It should be noted that it will be apparent to those skilled in the art that various modifications and adaptations of the invention can be made without departing from the principles of the invention and these modifications and adaptations are intended to be within the scope of the invention as defined in the following claims.
Claims (4)
1. An energy-conserving high purity n-butyl alcohol extraction system, characterized in that: the system is mainly formed by a preheater (9), an n-butyl alcohol light component removing tower (1), an n-butyl alcohol heavy component removing tower (4) and an n-isobutyl aldehyde separating tower (8) in sequence, wherein raw n-butyl alcohol enters the system through the preheater, and heat exchange is carried out between the raw n-butyl alcohol and an n-butyl alcohol product obtained by the n-butyl alcohol heavy component removing tower in the preheater; the n-butyl alcohol light component removing tower, the n-butyl alcohol heavy component removing tower and the n-isobutyl aldehyde separating tower are respectively connected with a reboiler for heat recovery, and the top of the n-butyl alcohol heavy component removing tower is connected with a reboiler pipeline of the n-isobutyl aldehyde separating tower;
the n-butanol light component removing tower and the n-butanol heavy component removing tower are rectifying towers with packing combined with a floating valve tray,
the top of the n-butanol light component removing tower is sequentially connected with a first condenser (2) and a first reflux tank (3), and a reflux pipeline is arranged between the first reflux tank and the n-butanol light component removing tower; the first reflux tank is also provided with an exhaust pipeline with a first tail gas discharge valve (16), a drainage pipeline and an impurity extraction line pipeline for discharging light components, and one end of the impurity extraction line pipeline is connected to the reflux pipeline;
the top of the n-butanol heavy removal tower is also connected with a second reflux tank (6), the top of the second reflux tank is connected with a reboiler of the n-isobutyraldehyde separation tower, a reflux pipeline is arranged between the bottom of the second reflux tank and the n-butanol heavy removal tower, and the reflux pipeline is provided with a second reflux valve (19); the return pipeline is connected with a n-butyl alcohol product extraction pipeline;
the n-butanol light component removing tower adopts an upper filler, and the structure of a lower tray can effectively reduce the internal pressure difference of the tower and improve the rectification effect;
the top of the n-butanol light component removing tower is provided with a packing layer, the bottom of the n-butanol light component removing tower is provided with a floating valve structure, and the floating valve is a tray which can float on a tray plate and change the opening degree along with the change of the gas flow;
the top of the n-butanol heavy removal tower is of a floating valve structure, the bottom of the n-butanol heavy removal tower is provided with a packing layer, and the floating valve is a tray which can float on a tray plate and change the opening degree along with the change of the gas flow;
the floating valves in the n-butyl alcohol light component removing tower and the n-butyl alcohol heavy component removing tower are double overflow trays, the packing is structured packing, and a plurality of temperature measuring points are arranged on the tower body;
the first reflux tank is a horizontal tank or a vertical tank with a water collecting bag and a coalescer, the top of the first reflux tank is connected with a first condenser, and the bottom of the first reflux tank is connected with an n-butyl alcohol light component removing tower;
the extraction method of the extraction system comprises the following steps:
s1, raw n-butyl alcohol raw material obtained by gas phase or liquid phase hydrogenation production of n-butyl aldehyde is subjected to heat exchange with refined n-butyl alcohol product extracted from an n-butyl alcohol heavy removal tower in a preheater, then enters an n-butyl alcohol light removal tower, a first reboiler at the bottom of the n-butyl alcohol light removal tower is used for heating materials to generate ascending steam, heat and mass transfer are carried out on tower plates and fillers with reflux liquid, so that light components are gasified and enter a gas phase, the n-butyl alcohol product enters a liquid phase, and the gas phase at the top of the tower is condensed by a first condenser and then enters a first reflux tank,
the water is demulsified, coalesced and settled by a coalescer, the emulsified liquid is demulsified, the small water droplets after demulsification are agglomerated into large water droplets, the large water droplets are settled to the bottom of the coalescer, collected in a water collecting bag, discharged and sent to a water treatment device,
other light component impurities contained in the crude n-butanol are extracted through an impurity extraction line pipeline at the top of the n-butanol light removal tower;
s2, crude n-butanol with light components removed enters an n-butanol heavy removal tower, ascending steam is generated by heating materials through a second reboiler at the tower bottom, heat transfer and mass transfer are carried out on the tower plate and the filler with reflux liquid, so that n-butanol is gasified to enter a gas phase, main impurity heavy components enter a liquid phase, high-purity gas phase n-butanol at the tower top enters an n-isobutyraldehyde separation tower reboiler to recover heat, the condensed gas phase which is not condensed in a second reflux tank enters a second condenser, all n-butanol after condensation enters the second reflux tank,
part of the n-butanol in the second reflux tank is extracted as a product, enters a preheater for heat recovery and is extracted as n-butanol product, part of the n-butanol is refluxed into the tower as reflux of the tower,
heavy component impurities are extracted from the tower bottom;
the temperature of the tower bottom of the n-butyl alcohol light component removing tower is 120-140 ℃, the temperature of the tower top is 90-100 ℃, and the pressure of the tower top is 0.02-0.08 MPaG;
the temperature of the tower bottom of the n-butyl alcohol heavy-removal tower is 130-150 ℃, the temperature of the tower top is 110-120 ℃, and the pressure of the tower top is 0.02-0.08 MPaG.
2. The high purity n-butanol extraction system of claim 1 wherein: a first reflux valve (13) is arranged on a reflux pipeline of the first reflux tank, a light component extraction regulating valve (14) is arranged on an impurity extraction line pipeline, a water collecting bag outlet of the first reflux tank is connected with a drainage pipeline, and a water extraction regulating valve (15) is arranged on the drainage pipeline.
3. The high purity n-butanol extraction system of claim 1 wherein: an n-butyl alcohol extraction valve (18) is arranged between the n-butyl alcohol product extraction pipeline and the preheater, and a second condenser (5) and a second tail gas discharge valve (17) are arranged on the exhaust pipeline of the second reflux tank.
4. The high purity n-butanol extraction system of claim 1 wherein: an n-butanol heavy-removal tower feeding valve (21) is arranged between the n-butanol light-removal tower and the n-butanol heavy-removal tower.
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