CN116534933A - Device and process for recovering and extracting furfural from process wastewater - Google Patents
Device and process for recovering and extracting furfural from process wastewater Download PDFInfo
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- CN116534933A CN116534933A CN202211530226.3A CN202211530226A CN116534933A CN 116534933 A CN116534933 A CN 116534933A CN 202211530226 A CN202211530226 A CN 202211530226A CN 116534933 A CN116534933 A CN 116534933A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/38—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with substituted hydrocarbon radicals attached to ring carbon atoms
- C07D307/40—Radicals substituted by oxygen atoms
- C07D307/46—Doubly bound oxygen atoms, or two oxygen atoms singly bound to the same carbon atom
- C07D307/48—Furfural
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a device and a process for recovering and extracting furfural from process wastewater; the dehydration deacidification tower in the previous procedure is connected with an inlet of a process wastewater storage tank, an outlet of the process wastewater storage tank is connected with a process wastewater feed pump, an outlet of the process wastewater feed pump is connected with an inlet of a preheater, an outlet of the preheater is connected with an inlet of a light removal rectifying tower, a liquid phase of a tower bottom of the light removal rectifying tower is connected with an inlet of a recovery distillation tower, a top gas phase of the recovery distillation tower is connected with an inlet of a recovery condenser, the recovery condenser is connected with an inlet of an aldehyde separating tank, and an outlet of a lower part of the aldehyde separating tank is connected with an inlet of a crude furfural removing storage tank; the top of the light component removal rectifying tower is provided with a vapor phase, a light component removal condenser inlet, a light component removal condenser outlet, a liquid separating tank inlet, a light component storage tank outlet and a light component conveying pump. The tower is distilled within a stable temperature range, the technical process of recovering and extracting furfural from wastewater is realized, the refining yield can be improved by 3-6 percent, and the relative economic benefit is improved by 3-5 percent.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a device and a process for recovering and extracting furfural from process wastewater.
Background
CN102086180B discloses a production process for improving the yield of furfural, wherein dilute aldehyde hydrolysate containing furfural is separated by a primary distillation tower and an aldehyde-water separation device, the lower aldehyde phase is further processed into a finished product of furfural after entering a water washing tower for water washing and a dehydration tower for dehydration, and the upper water phase of the aldehyde-water separation device is recycled into the primary distillation tower after further water washing and light removal. The invention also discloses a special device aldehyde-water separation device for the process, which comprises an outer cylinder, a middle cylinder and an inner cylinder, wherein a plurality of sieve holes are distributed on the wall of the inner cylinder, the liquid inlet is connected with the inner cylinder, a first sedimentation chamber is arranged between the inner cylinder and the middle cylinder, and a second sedimentation chamber is arranged between the middle cylinder and the outer cylinder. The light component removing tower is only applicable to one sieve plate type, the tower structure is sized, the operable elastic range is small, the process wastewater (water phase generated by the dehydrating tower) only refers to one process wastewater generated in the process of preparing commercial furfural by washing, deacidifying and continuously rectifying crude furfural, and the refining yield is low.
At present, in domestic furfural production enterprises, the content of furfural in crude furfural produced by distillation in a primary distillation tower is generally about 90%, the crude furfural is refined into commodity furfural by different rectification modes (such as alkali-adding neutralization deacidification batch rectification, alkali-adding neutralization deacidification continuous rectification, alkali-free neutralization tower deacidification dehydration continuous rectification and the like), and the refining yield is generally between 82 and 85%, and the theoretical yield is more than 89%. The reason is that the process waste water containing a large amount of furfural (the production amount of the process waste water is 15-20% of the weight of the crude furfural and the content of the furfural in the process waste water is 8-20%) is distilled out from the top of the tower in the first step of rectification, and the waste water is discharged to an in-plant waste water treatment system, so that the loss of the furfural in the waste water results in lower yield and poor enterprise production benefit.
In order to solve the problem of low refining yield, the process wastewater containing furfural is analyzed: mainly contains a large amount of water, and secondarily contains furfural, acetic acid, acetone, methanol and other components. Just because the content of the mixed components is relatively close, if a conventional distillation method is adopted, the furfural in the wastewater is difficult to recover and extract.
Disclosure of Invention
In order to overcome the defects, the invention aims to provide a device and a process for recovering and extracting furfural from process wastewater, which are suitable for any furfural production enterprises, and the comprehensive accounting and refining yield can be improved by 3-6 percent on the basis of the original, and the economic benefit is improved by 3-5 percent.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the device for recovering and extracting furfural from the process wastewater comprises a process wastewater storage tank, a process wastewater feed pump, a preheater, a light component removal rectifying tower, a recovery distilling tower, a recovery condenser, a light component removal condenser, an aldehyde separating tank, a crude furfural removing storage tank, a liquid separating tank, a light component storage tank and a light component conveying pump; the dehydration deacidification tower in the previous procedure is connected with the inlet of the process wastewater storage tank, the outlet of the process wastewater storage tank is connected with the inlet of the process wastewater feed pump, the outlet of the process wastewater feed pump is connected with the inlet of the preheater, the outlet of the preheater is connected with the inlet of the light removal rectifying tower, the liquid phase of the bottom of the light removal rectifying tower is connected with the inlet of the recovery distillation tower, the gas phase of the top of the recovery distillation tower is connected with the inlet of the recovery condenser, the recovery condenser is connected with the inlet of the aldehyde separating tank, and the outlet of the lower part of the aldehyde separating tank is connected with the inlet of the crude removal furfural storage tank; the light component conveying pump is characterized in that the top of the light component stripping rectifying tower is connected with the top of the light component stripping rectifying tower through a vapor phase, the top of the light component stripping rectifying tower is connected with the top of the light component stripping rectifying tower, the light component stripping tower.
Optionally, the light component removing rectifying tower comprises a tower top gas phase outlet, a distillation process liquid reflux port, a rectifying section, a process wastewater feed inlet, a stripping section, a tower kettle heater and a tower kettle liquid phase outlet which are sequentially arranged from top to bottom; the stripping section tower internals adopt a floating valve, a sieve plate, a tongue plate or a packing structure; the tower kettle heater adopts an external circulation type, a central circulation type or a coil pipe type structure; the rectifying section tower internals adopt a floating valve, a sieve plate, a tongue plate or a packing structure form.
Optionally, the process wastewater storage tank has a capacity of 10m 3 -40m 3 The method comprises the steps of carrying out a first treatment on the surface of the The process wastewater feed pump is set to have a flow rate ranging from 500L/h to 3000L/h.
Optionally, the process waste water storage tank is provided with a process waste water storage tank liquid level gauge; a light component removal tower feeding flowmeter is arranged between the process wastewater feeding pump and the preheater; a light component removal tower kettle thermometer is arranged at the bottom of the light component removal rectifying tower; the top of the light component removal rectifying tower is provided with a light component removal tower top thermometer; a light component removing tower kettle liquid level meter is arranged between the light component removing rectifying tower and the recovery distilling tower; the bottom of the recovery distillation tower is provided with a recovery tower kettle thermometer and is connected with a recovery tower kettle liquid level meter; the top of the recovery distillation tower is provided with a recovery tower top thermometer; the bottom of the aldehyde separating tank is provided with an aldehyde separating tank liquid level meter; a light component removal tower liquid-separating filling level gauge is arranged in the liquid-separating tank; and a light component storage tank liquid level meter is arranged in the light component storage tank.
Optionally, the light component removing rectifying tower comprises a tower kettle liquid level meter connecting pipe, a tower top conical head, a tower top instrument interface, a tower kettle observation mirror, a tower kettle heating steam inlet and a tower kettle gas phase outlet; the tower top conical end enclosure is positioned at the top of the rectifying section and is narrow in upper part and wide in lower part; the side part of the tower top conical end socket is provided with a tower top instrument interface; the tower kettle liquid level meter connecting pipes are respectively arranged at the upper side part and the lower side part of the tower kettle, and the tower kettle heating steam inlet is arranged at the other side part of the tower kettle; the tower kettle gas phase outlet is arranged at the bottom of the tower kettle and is positioned above the tower kettle liquid phase outlet; the tower kettle observation mirror is arranged at the upper part of the outer side of the tower kettle.
The application also discloses a process for recovering and extracting furfural from process wastewater, which comprises the following steps:
the process wastewater distilled from the dehydration deacidification tower is stored in a process wastewater storage tank, and is sent into a light component removal rectifying tower through a process wastewater feed pump according to a set flow range;
introducing primary steam into a tower kettle heater to enable the tower to distill for removing light components in a stable temperature range, and continuously extracting water and aldehyde liquid from the tower kettle to enter a recovery distillation tower;
and synchronously introducing primary steam into a heater of a recovery distillation tower, distilling the tower in a stable temperature range, condensing a gas phase at the tower top, introducing the condensed gas phase into an aldehyde separating tank, layering the crude furfural at the lower part in the aldehyde separating tank, metering the crude furfural by a mass flowmeter, and delivering the crude furfural to a crude furfural storage tank.
Optionally, the process wastewater storage tank has a capacity of 10m 3 -40m 3 The method comprises the steps of carrying out a first treatment on the surface of the The process wastewater feed pump is set to have a flow range of 500-3000L/h; controlling the primary steam pressure to be 0.5-0.3 MPa; controlling the temperature of the light component removal rectifying tower to be 110-90 ℃; the extraction amount of the aqueous aldehyde liquid accounts for 70% -90% of the feeding amount; the gas phase condensation temperature at the top of the recovery distillation tower is 60-40 ℃; the temperature of the recovery distillation tower is controlled to be 110-90 ℃.
Crude furfural produced by distillation in a primary distillation tower of a furfural enterprise is refined into process wastewater generated in the commodity furfural process by different rectification modes (such as alkali neutralization deacidification batch rectification, alkali neutralization deacidification continuous rectification, alkali-free neutralization tower deacidification dehydration continuous rectification, water washing deacidification continuous rectification and the like). The light component removing distillation tower diameter and the tower height are designed and manufactured in a targeted mode according to the production scale and the investment cost of enterprises, and the operation flexibility range is wide.
The invention has the positive beneficial effects that:
the tower is distilled within a stable temperature range, the gas phase at the tower top is condensed and enters an aldehyde separating tank, the crude furfural at the lower part of the tower is metered by a mass flowmeter and then is sent to a crude furfural storage tank after layering in the aldehyde separating tank, the technical process of recovering and extracting furfural from the technical wastewater and the refining yield are realized, and the cost is reduced. The novel process distillation device is suitable for any domestic furfural production enterprises, the comprehensive accounting refining yield can be improved by 3-6 percent on the basis of the original, and the relative economic benefit is improved by 3-5 percent.
Drawings
Fig. 1 is a schematic diagram of a process flow for recovering and extracting furfural from process wastewater provided in embodiment 1 of the present invention;
fig. 2 is a schematic structural diagram of a light component removal rectifying tower provided in embodiment 1 of the present invention;
fig. 3 is a schematic diagram of a process flow for recovering and extracting furfural from process wastewater provided in embodiment 2 of the present invention;
fig. 4 is a schematic structural diagram of a light component removal rectifying tower according to embodiment 2 of the present invention.
1. A process waste water storage tank; 2. a process wastewater feed pump; 3. a preheater; 4. a light component removing rectifying tower; 5. recovering the distillation tower; 6. a recovery condenser; 7. an aldehyde separating tank; 8. a light-off condenser; 9. a liquid separating tank; 10. a light component storage tank; 11. a light component delivery pump; 12. a tower kettle; 13. connecting a tower kettle liquid level meter with the pipe; 14. a stripping section; 15. stripping section tower internals; 16. a rectifying section; 17. rectifying section column internals; 18. a conical end enclosure at the top of the tower; 19. a gaseous phase outlet at the top of the column; 20. a tower top instrument interface; 21. a distillation process liquid reflux port; 22. a process wastewater feed inlet; 23. observing the sight glass at the tower kettle; 24. heating a steam inlet at the tower kettle; 25. a tower kettle heater; 26. a gas phase outlet of the tower kettle; 27. a tower kettle liquid phase outlet; 201. a process waste water storage tank level gauge; 202. a light component removal tower feeding flowmeter; 203. a liquid level meter of a tower bottom of the light component removing tower; 204. a tower kettle thermometer of the light component removing tower; 205. a light component removal tower top thermometer; 206. a recovery tower kettle liquid level meter; 207. a recovery tower kettle thermometer; 208. a recovery tower top thermometer; 209. aldehyde separating tank level gauge; 210. a liquid level meter is filled in a light component removing tower; 211. a light component storage tank level gauge. CWS, circulating cooling water to water; CWR, circulating cooling water backwater; LS, low pressure saturated steam.
Detailed Description
The invention will be further described with reference to the following embodiments.
Example 1
As shown in fig. 1 and 2, the device for recovering and extracting furfural from the process wastewater comprises a process wastewater storage tank, a process wastewater feed pump, a preheater, a light component removal rectifying tower, a recovery distilling tower, a recovery condenser and a light component removal condenser, an aldehyde separating tank, a crude furfural removing storage tank, a liquid separating tank, a light component storage tank and a light component conveying pump; the dehydration deacidification tower in the previous procedure is connected with the inlet of the process wastewater storage tank, the outlet of the process wastewater storage tank is connected with the inlet of the process wastewater feed pump, the outlet of the process wastewater feed pump is connected with the inlet of the preheater, the outlet of the preheater is connected with the inlet of the light removal rectifying tower, the liquid phase of the bottom of the light removal rectifying tower is connected with the inlet of the recovery distillation tower, the gas phase of the top of the recovery distillation tower is connected with the inlet of the recovery condenser, the recovery condenser is connected with the inlet of the aldehyde separating tank, and the outlet of the lower part of the aldehyde separating tank is connected with the inlet of the crude removal furfural storage tank; the top evaporation gas phase of the light component removal rectifying tower is connected with the inlet of the light component removal condenser, the outlet of the light component removal condenser is connected with the inlet of the liquid separating tank, the outlet of the liquid separating tank is connected with the inlet of the light component storage tank, the outlet of the light component storage tank is connected with the light component conveying pump, and the light component conveying pump can convey the light component to an in-plant light component (waste liquid) disposal system or a furfural residue burning boiler for burning; and (3) recovering liquid-phase wastewater (containing 0.07% of furfural) at the tower bottom of the distillation tower and discharging the wastewater to an in-plant wastewater treatment system.
The novel process distillation device is suitable for any domestic furfural production enterprises, the comprehensive accounting refining yield can be improved by 3-6 percent on the basis of the original, and the relative economic benefit is improved by 3-5 percent.
Specifically, the recovery distillation tower is a float valve tower; the light component removing condenser is in a tubular or plate type structure form; the device comprises a water cooling circulation system (condenser cooling water) and a steam heating system (tower kettle heating steam); referring to fig. 2, the light component removal rectifying tower comprises a tower top gas phase outlet 15, a distillation process liquid reflux port, a rectifying section, a process wastewater feed port, a stripping section, a tower kettle heater and a tower kettle liquid phase outlet which are sequentially arranged from top to bottom; the internal parts of the stripping section tower adopt the structural forms of floating valves, sieve plates, tongue plates or fillers and the like; the tower kettle heater adopts an external circulation type, a central circulation type, a coil pipe type or a straight pipe type and other structural forms; the rectifying section tower internals adopt the structural forms of floating valves, sieve plates, tongue plates or fillers and the like.
The distillation tower and the rectifying tower are in gas-liquid two-phase contact for phase mass transfer, a condenser positioned at the top of the tower enables the gas phase distilled out of the top of the tower to be partially condensed, part of condensate is returned to the top of the tower as reflux liquid, and the rest distillate is tower top products. A heater located at the bottom of the column vaporizes a portion of the liquid, the vapor rises along the column, and the remaining liquid serves as a high concentration heavy ends product at the bottom of the column. The feed is added in the middle of the column, the liquid in the feed and the liquid from the upper column section descend along the column, and the vapor in the feed and the vapor from the lower column section ascend along the column. In the whole distillation tower, the gas phase and the liquid phase are in countercurrent contact to carry out phase mass transfer. Volatile components in the liquid phase enter the vapor phase and less volatile components in the vapor phase go into the liquid phase. For systems that do not form constant boiling materials, the overhead will be a high purity volatile component (low boiling point light component) and the bottoms will be a high purity less volatile component (high boiling point material) as long as designed and operated properly. The tower section above the feed inlet is used for further concentrating volatile components in the rising vapor and is called a rectifying section; and a tower section below the feed inlet is used for extracting volatile components from the descending liquid and is called stripping section. The combination of the two operations allows for more complete separation of the components in the liquid mixture to produce two products of the desired purity.
The rectification results in complete separation of the liquid mixture, the key being the use of reflux. Reflux includes both high concentration volatile component liquid at the top of the column and high concentration less volatile component vapor at the bottom of the column being returned to the column. The gas-liquid reflux forms a countercurrent contact gas-liquid two-phase, thereby obtaining relatively pure single-component products at the two ends of the tower respectively. The ratio of the amount of liquid flowing back into the column at the top of the column to the amount of product at the top of the column, called reflux ratio, is an important control parameter for the rectification operation, and its variation affects the separation effect and the energy consumption of the rectification operation. The light component removing distillation column can be in various structural forms, the stripping section column internal part can be in a structural form of combining a floating valve, a sieve plate and a tongue plate with the rectifying section column internal part by adopting a filler (the rectifying efficiency is higher when the stripping section column internal part is tracked by a plurality of technological parameters and the stripping section column internal part can be in a structural form of combining the floating valve, the sieve plate and the tongue plate with the rectifying section column internal part by adopting the filler).
Example 2
Referring to fig. 3, further, the process waste water tank is provided with a process waste water tank level gauge; a light component removal tower feeding flowmeter is arranged between the process wastewater feeding pump and the preheater, and a certain flow rate is arranged to be interlocked with the feeding pump so as to ensure stable feeding amount; a light component removal tower kettle thermometer is arranged at the bottom of the light component removal rectifying tower; the top of the light component removal rectifying tower is provided with a light component removal tower top thermometer; a light component removing tower kettle liquid level meter is arranged between the light component removing rectifying tower and the recovery distilling tower, and is interlocked with a liquid outlet regulating valve to ensure the stable liquid level of the tower kettle; the bottom of the recovery distillation tower is provided with a recovery tower kettle thermometer and is connected with a recovery tower kettle liquid level meter, and the liquid level meter is interlocked with a liquid outlet regulating valve to ensure the stable liquid level of the tower kettle; the top of the recovery distillation tower is provided with a recovery tower top thermometer; the bottom of the aldehyde separating tank is provided with an aldehyde separating tank liquid level meter which is a density interface liquid level meter and is interlocked with a liquid outlet regulating valve, so that the layered interface liquid level is ensured to be stable; a light component removal tower liquid-separating filling level gauge is arranged in the liquid-separating tank; and a light component storage tank liquid level meter is arranged in the light component storage tank.
The recovery distillation tower is a common normal pressure float valve distillation tower; the light component removal tower condenser and the recovery condenser are heat exchangers in tubular, plate type and other structural forms; related devices include industrial control instrumentation systems (level gauges, flow meters, pressure gauges, thermometer and regulating valves); and the system also comprises matched public engineering: a low-pressure saturated steam system (steam for heating a distillation column) and a circulating cooling water system (water for cooling a condenser),
the light component removing distillation column and the recovery distillation column are distilled within a stable temperature range.
Referring to fig. 4, the light component removing rectifying tower comprises a tower kettle liquid level meter connecting pipe, a tower top conical head, a tower top instrument interface, a tower kettle observation mirror, a tower kettle heating steam inlet and a tower kettle gas phase outlet; the tower top conical end enclosure is positioned at the top of the rectifying section and is narrow in upper part and wide in lower part; the side part of the tower top conical end enclosure is provided with a tower top instrument interface, so that instruments such as a thermocouple thermometer and the like can be installed; the tower kettle liquid level meter connecting pipes are respectively arranged at the upper side part and the lower side part of the tower kettle, and the tower kettle heating steam inlet is arranged at the other side part of the tower kettle; the tower kettle gas phase outlet is arranged at the bottom of the tower kettle and is positioned above the tower kettle liquid phase outlet; the tower kettle observation mirror is arranged on the upper part of the outer side of the tower kettle, so that the internal condition of the tower kettle can be observed in real time.
Example 3
The process for recovering and extracting furfural from the process wastewater comprises the following steps:
s1, storing the process wastewater distilled from the dehydration deacidification tower in a process wastewater storage tankThe process wastewater generated in the refining process of crude furfural is stored in a process wastewater storage tank) and is fed through a process wastewater feed pump (flow 3m 3 And/h, the lift is 10-40 m), the wastewater is sent into a light component removal rectifying tower according to the set flow range;
s2, when the liquid level of the tower kettle of the light component removal rectifying tower reaches 60-70%, introducing primary steam into a tower kettle heater, so that the tower is distilled to remove light components in a stable temperature range (110-70 ℃), and continuously extracting water aldehyde liquid (70-90% of the extracting amount of the water aldehyde liquid) from the tower kettle enters a recovery distilling tower;
s3, when the liquid level of the tower bottom of the recovery distillation tower reaches 60-70% of the liquid level, synchronously introducing primary steam (low-pressure saturated steam) into a heater of the recovery distillation tower, distilling the tower in a stable temperature range (110-90 ℃), condensing a gas phase at the tower top (60-40 ℃) and then introducing the condensed gas phase into an aldehyde separating tank, and metering crude furfural at the lower part of the layered crude furfural in the aldehyde separating tank by a mass flowmeter and then delivering the crude furfural to a crude furfural storage tank (the crude furfural contains about 90 percent of furfural);
the upper water phase (containing about 10% of furfural) flows into the recovery distillation tower from the overflow port of the aldehyde separating tank.
The gas phase distilled from the top of the light component removal rectifying tower enters a light component removal condenser, the condensed liquid phase (liquid phase temperature is 50-30 ℃) flows into a liquid separating tank, the removed light component flows out from an overflow port at the upper part of the liquid separating tank and enters a light component storage tank, and the liquid at the lower part in the liquid separating tank flows back into a reflux port of the light component removal rectifying tower; the light components in the light component storage tank are used as organic fuel to be sent to a furfuraldehyde slag burning boiler hearth for burning through a light component conveying pump. The bottom of the recovery distillation tower continuously discharges the waste water (the waste water contains furfural which is less than or equal to 0.07 percent) at the bottom of the recovery distillation tower through the linkage control of the liquid level of the tower bottom and the regulating valve, and the waste water is sent to the waste water treatment device.
Further, the capacity of the process wastewater storage tank is 10m 3 -40m 3 The method comprises the steps of carrying out a first treatment on the surface of the The process wastewater feed pump is set to have a flow range of 500-3000L/h; controlling the primary steam pressure to be 0.5-0.3 MPa; controlling the temperature of the light component removal rectifying tower to be 110-90 ℃; the extraction amount of the aqueous aldehyde liquid accounts for 70% -90% of the feeding amount; the gas phase condensation temperature at the top of the recovery distillation tower is 60-40 ℃; controlling the temperature of the recovery distillation columnThe temperature is 110-90 ℃.
The process wastewater distilled from the dehydration deacidification tower is sent into the middle part of the light component removal rectifying tower through a feed pump; introducing primary steam into a heater of a light component removal rectifying tower to enable gas-liquid two phases to be in contact for carrying out phase mass transfer, so that the distillation of removing light components is carried out on the tower within a stable temperature range, and the gas phase at the top of the tower is condensed to obtain the distilled light components; the water aldehyde liquid continuously extracted from the tower kettle enters a recovery distillation tower; and synchronously introducing primary steam into a recovery distillation tower heater, distilling the tower in a stable temperature range, condensing a gas phase at the tower top, introducing the gas phase into an aldehyde separating tank, metering the crude furfural at the lower part of the layered part in the aldehyde separating tank through a mass flowmeter, and delivering the metered crude furfural to a crude furfural storage tank to realize the technical process of recovering and extracting furfural from the process wastewater. Has higher refining yield.
Finally, it is noted that the above-mentioned embodiments are merely for illustrating the technical solution of the present invention, and that other modifications and equivalents thereof by those skilled in the art should be included in the scope of the claims of the present invention without departing from the spirit and scope of the technical solution of the present invention.
Claims (7)
1. The device for recovering and extracting the furfural from the process wastewater is characterized by comprising a process wastewater storage tank, a process wastewater feed pump, a preheater, a light component removal rectifying tower, a recovery distilling tower, a recovery condenser, a light component removal condenser, an aldehyde separating tank, a crude furfural removing storage tank, a liquid separating tank, a light component storage tank and a light component conveying pump; the dehydration deacidification tower in the previous procedure is connected with the inlet of the process wastewater storage tank, the outlet of the process wastewater storage tank is connected with the inlet of the process wastewater feed pump, the outlet of the process wastewater feed pump is connected with the inlet of the preheater, the outlet of the preheater is connected with the inlet of the light removal rectifying tower, the liquid phase of the bottom of the light removal rectifying tower is connected with the inlet of the recovery distillation tower, the gas phase of the top of the recovery distillation tower is connected with the inlet of the recovery condenser, the recovery condenser is connected with the inlet of the aldehyde separating tank, and the outlet of the lower part of the aldehyde separating tank is connected with the inlet of the crude removal furfural storage tank; the light component conveying pump is characterized in that the top of the light component stripping rectifying tower is connected with the top of the light component stripping rectifying tower through a vapor phase, the top of the light component stripping rectifying tower is connected with the top of the light component stripping rectifying tower, the light component stripping tower.
2. The device for recovering and extracting furfural from process wastewater as claimed in claim 1, wherein the light component removal rectifying tower comprises a tower top gas phase outlet, a distillation process liquid reflux port, a rectifying section, a process wastewater feed port, a stripping section, a tower bottom heater and a tower bottom liquid phase outlet which are sequentially arranged from top to bottom; the stripping section tower internals adopt a floating valve, a sieve plate, a tongue plate or a packing structure; the tower kettle heater adopts an external circulation type, a central circulation type or a coil pipe type structure; the rectifying section tower internals adopt a floating valve, a sieve plate, a tongue plate or a packing structure form.
3. The device for recovering and extracting furfural from process wastewater as claimed in claim 1, wherein the capacity of the process wastewater storage tank is 10m 3 -40m 3 The method comprises the steps of carrying out a first treatment on the surface of the The process wastewater feed pump is set to have a flow rate ranging from 500L/h to 3000L/h.
4. The device for recovering and extracting furfural from process wastewater according to claim 1, wherein the process wastewater storage tank is provided with a process wastewater storage tank level gauge; a light component removal tower feeding flowmeter is arranged between the process wastewater feeding pump and the preheater; a light component removal tower kettle thermometer is arranged at the bottom of the light component removal rectifying tower; the top of the light component removal rectifying tower is provided with a light component removal tower top thermometer; a light component removing tower kettle liquid level meter is arranged between the light component removing rectifying tower and the recovery distilling tower; the bottom of the recovery distillation tower is provided with a recovery tower kettle thermometer and is connected with a recovery tower kettle liquid level meter; the top of the recovery distillation tower is provided with a recovery tower top thermometer; the bottom of the aldehyde separating tank is provided with an aldehyde separating tank liquid level meter; a light component removal tower liquid-separating filling level gauge is arranged in the liquid-separating tank; and a light component storage tank liquid level meter is arranged in the light component storage tank.
5. The apparatus for recovering and extracting furfural from process wastewater as claimed in claim 2, wherein said light ends removal and rectification column comprises a column bottom liquid level gauge connection tube, a column top conical head, a column top instrument interface, a column bottom observation mirror, a column bottom heating steam inlet and a column bottom gas phase outlet; the tower top conical end enclosure is positioned at the top of the rectifying section and is narrow in upper part and wide in lower part; the side part of the tower top conical end socket is provided with a tower top instrument interface; the tower kettle liquid level meter connecting pipes are respectively arranged at the upper side part and the lower side part of the tower kettle, and the tower kettle heating steam inlet is arranged at the other side part of the tower kettle; the tower kettle gas phase outlet is arranged at the bottom of the tower kettle and is positioned above the tower kettle liquid phase outlet; the tower kettle observation mirror is arranged at the upper part of the outer side of the tower kettle.
6. A process for recovering and extracting furfural from process wastewater is characterized by comprising the following steps:
the process wastewater distilled from the dehydration deacidification tower is stored in a process wastewater storage tank, and is sent into a light component removal rectifying tower through a process wastewater feed pump according to a set flow range;
introducing primary steam into a tower kettle heater to enable the tower to distill for removing light components in a stable temperature range, and continuously extracting water and aldehyde liquid from the tower kettle to enter a recovery distillation tower;
and synchronously introducing primary steam into a heater of a recovery distillation tower, distilling the tower in a stable temperature range, condensing a gas phase at the tower top, introducing the condensed gas phase into an aldehyde separating tank, layering the crude furfural at the lower part in the aldehyde separating tank, metering the crude furfural by a mass flowmeter, and delivering the crude furfural to a crude furfural storage tank.
7. The process for recovering and extracting furfural from process wastewater as claimed in claim 6, wherein said process wastewater storage tank has a capacity of 10m 3 -40m 3 The method comprises the steps of carrying out a first treatment on the surface of the The process wastewater feed pump is set to have a flow range of 500-3000L/h; controlling the primary steam pressure to be 0.5-0.3 MPa; controlling the temperature of the light component removal rectifying tower to be 110-90 ℃; the extraction amount of the aqueous aldehyde liquid accounts for 70% -90% of the feeding amount; the gas phase condensation temperature at the top of the recovery distillation tower is at60-40 ℃; the temperature of the recovery distillation tower is controlled to be 110-90 ℃.
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| CN202211530226.3A CN116534933A (en) | 2022-11-30 | 2022-11-30 | Device and process for recovering and extracting furfural from process wastewater |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117756207A (en) * | 2023-11-23 | 2024-03-26 | 重庆市三峡生态环境技术创新中心有限公司 | Alcohol rectification recovery device and method for sauce-flavor white spirit pit bottom water |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117756207A (en) * | 2023-11-23 | 2024-03-26 | 重庆市三峡生态环境技术创新中心有限公司 | Alcohol rectification recovery device and method for sauce-flavor white spirit pit bottom water |
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