CN112374967A - System and method for recovering ethanol from organic waste liquid - Google Patents

System and method for recovering ethanol from organic waste liquid Download PDF

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Publication number
CN112374967A
CN112374967A CN202011231214.1A CN202011231214A CN112374967A CN 112374967 A CN112374967 A CN 112374967A CN 202011231214 A CN202011231214 A CN 202011231214A CN 112374967 A CN112374967 A CN 112374967A
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waste liquid
hole
ethanol
pipeline
kettle
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冯烈
孙琪
钱晔
吴方丽
王朝妹
蒋红华
刘小兵
蒋开炎
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Jiande Jianye Resource Recycling Technology Co ltd
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ZHEJIANG JIANYE CHEMICAL CO Ltd
Hangzhou Xinde Environmental Protection Technology Co ltd
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Priority to CN202011231214.1A priority Critical patent/CN112374967A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • B01D3/143Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
    • B01D3/146Multiple effect distillation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/66Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds

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  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
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  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The invention relates to the technical field of industrial sewage treatment, in particular to a system and a method for recovering ethanol from organic waste liquid, wherein the system comprises a waste liquid rectifying still, a waste liquid rectifying tower, a delayer, a front fraction collecting tank and an ethanol finished product tank, wherein the upper end of the waste liquid rectifying still is provided with a first feeding hole and a first discharging hole, and the first discharging hole is connected with the bottom of the waste liquid rectifying tower through a pipeline; the top of the waste liquid rectifying tower is provided with a second discharge hole and a second feed hole, the top of the delayer is provided with a third feed hole, the side of the delayer is provided with a third discharge hole, the second discharge hole is connected with the third feed hole through a pipeline, and the third discharge hole is respectively communicated with the second feed hole, the front fraction collecting tank and the ethanol finished product tank through a tee pipeline. The invention has simple structure, and can carry out rectification and recovery on the ethanol in the organic waste liquid by two times of rectification treatment to change the waste liquid into raw materials and finished products, thereby generating economic benefit and environmental protection benefit.

Description

System and method for recovering ethanol from organic waste liquid
Technical Field
The invention relates to the technical field of industrial sewage treatment, in particular to a system and a method for recovering ethanol from organic waste liquid.
Background
The industrial production or the pharmaceutical industry for disinfection and cleaning can generate a large amount of organic waste liquid, the main components are ethanol and water (the ethanol content is 73 percent and the water content is 24 percent), the other components are acid, methanol, high-boiling impurities and the like, at present, the waste ethanol is treated by burning mostly in China, but the waste ethanol has high energy consumption, large investment or incomplete treatment and high operating cost.
The recovered waste ethanol is a good solvent, can dissolve a plurality of inorganic substances and a plurality of organic substances, so that the ethanol is commonly used for dissolving the plant pigment or the medicinal components in the plant pigment, and the ethanol is also commonly used as the solvent for reaction, so that the organic substances and the inorganic substances which participate in the reaction can be dissolved, the contact area is increased, and the reaction rate is improved.
Chinese patent literature discloses "a system for ethanol recovery", its application publication number is CN207667179U, this utility model increases the film evaporator before the ethanol recovery tower, the reboiler only needs a little heat can guarantee the normal recovery of ethanol recovery tower, has improved the handling capacity and the recovery efficiency of ethanol recovery tower, simultaneously, the steam energy consumption that uses the reboiler heating to use in getting into ethanol recovery tower with solvent form than aqueous solvent is lower. However, the utility model has the advantages of complex structure, complex operation process, low purity of recovered ethanol and low economic benefit.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention provides a system for recovering ethanol from organic waste liquid, which has a simple structure and compact assembly, changes the waste liquid into raw materials and finished products, and generates economic benefits and environmental protection benefits.
The invention also provides a method for recovering ethanol from the organic waste liquid, which is simple to operate, easy to control conditions, green, environment-friendly and easy to industrialize.
In order to achieve the purpose, the invention adopts the following technical scheme:
a system for recovering ethanol from organic waste liquid comprises a waste liquid rectifying kettle, a waste liquid rectifying tower, a delayer, a front fraction collecting tank and an ethanol finished product tank, wherein a first feeding hole and a first discharging hole are formed in the upper end of the waste liquid rectifying kettle, and the first discharging hole is connected with the bottom of the waste liquid rectifying tower through a pipeline; the top of the waste liquid rectifying tower is provided with a second discharge hole and a second feed hole, the top of the delayer is provided with a third feed hole, the side of the delayer is provided with a third discharge hole, the second discharge hole is connected with the third feed hole through a pipeline, and the third discharge hole is respectively communicated with the second feed hole, the front fraction collecting tank and the ethanol finished product tank through a tee pipeline.
The system for recovering ethanol from the organic waste liquid has a simple structure, ethanol in the organic waste liquid is rectified and recovered through two times of rectification treatment, on one hand, the design of the delayer can perform rectification and purification on part of organic phase materials again to improve the extraction rate of ethanol, on the other hand, front fractions (low boiling and ethanol) can be used for producing ethyl acetate, middle fractions (recovered ethanol) are sold as finished ethanol, waste liquid is changed into raw materials and finished products, and economic benefits and environmental protection benefits are generated.
As preferred, still include alkali lye bin, preliminary treatment cauldron and low condenser that boils, preliminary treatment cauldron's top is equipped with fourth feed inlet and fourth discharge gate, the alkali lye bin is connected with the fourth feed inlet through the pipeline, the fourth discharge gate is connected with the first feed inlet of waste liquid rectifying still through the low condenser that boils of pipeline.
The alkali liquor storage tank is filled with alkali liquor for adjusting the pH value of the organic waste liquid in the pretreatment kettle. Preferably, the device further comprises a waste liquid conveying pump, a first discharge port is further formed in the bottom of the pretreatment kettle, and the first discharge port is connected with the top of the waste liquid rectifying kettle through the waste liquid conveying pump through a pipeline.
Preferably, the system also comprises an overhead condenser, and the second discharge port is connected with the third feed port through the overhead condenser through a pipeline.
Preferably, the device also comprises a waste liquid feeding pump, and the waste liquid feeding pump is connected with the fourth feeding hole through a pipeline.
Organic waste liquid passes through the waste liquid charge pump and carries to the preliminary treatment cauldron in, sample waste liquid test acid value, add the alkali lye in the alkali lye hold up tank in the preliminary treatment cauldron and neutralize to neutral, the temperature risees during neutralization during and gets into in the waste liquid rectifying still after low boiling condenser condensation, waste liquid after the neutralization passes through waste liquid transfer pump and carries into in the waste liquid rectifying still, waste liquid rectifying still gas phase export to waste liquid rectifying column, waste liquid rectifying column ejection of compact is to in the delayer, divide water to go the wastewater disposal basin from the delayer, partly backward flow of organic phase material to rectifying column in the delayer, partly ejection of compact is to in the collecting vat. And (3) controlling the waste liquid rectifying tower according to the temperature at the top of the tower, collecting the front fraction into a front fraction collecting tank to be used as an ethanol raw material for producing ethyl acetate, and collecting the finished product ethanol into an ethanol finished product tank to be used as an ethanol finished product for selling. And conveying the finally residual components in the waste liquid rectifying kettle, namely water and high-boiling residues, to a waste water pool for collection and treatment.
Preferably, the waste liquid rectifying tower is internally provided with stainless steel perforated plate corrugated packing.
Preferably, the surface of the corrugated packing of the stainless steel orifice plate is loaded with temperature-responsive gel, and the temperature-responsive gel factor is poly isopropyl acrylamide (PNIPAm) gel, and the structural formula of the gel is as follows:
Figure BDA0002765275010000021
the response mechanism of the temperature response type gel factor is as follows: the gel structure has a certain proportion of hydrophobic and hydrophilic groups, and the change of temperature can affect the hydrophobic effect of the groups and the hydrogen bonding effect among macromolecules, so that the conformation of the macromolecular chains of the gel stretches or curls due to the response to the stimulation of the temperature, and the volume of the gel expands or contracts.
The existing waste liquid rectifying kettle mostly adopts stainless steel pore plate corrugated packing, the gap between the packing and the joint of the tower is large, the secondary rectifying efficiency of ethanol is greatly reduced, the processing cannot meet the process requirement, in addition, the existing packing has no reinforcing rib design, when the diameter of the tower is too large, the packing is extruded when being installed, the packing is easy to collapse and deform, liquid is easy to enrich, gas passes through the two ends when rising, the mixing time of the gas and the liquid is reduced, and the service life of the packing is shortened.
The invention loads the temperature responsive gel factor on the surface of the corrugated filler of the stainless steel orifice plate, and has the following functions:
(1) the compactness of the joint of the filler and the tower can be enhanced and the secondary rectification efficiency can be improved by controlling the rectification temperature in the waste liquid rectification tower to regulate the expansion and the contraction of the temperature-responsive gel factor; (2) the pore diameter of the filler in the rectification process is regulated and controlled in real time through temperature control, so that the strength of the filler is increased, collapse is prevented, liquid enrichment is avoided, and the energy consumption is reduced; (3) the hydrophobic and hydrophilic groups in the gel structure can adsorb a large amount of ethanol molecules, the resistance of gas phase rising in the rectification process is reduced, the gas-liquid distribution is uniform, the efficiency is high, the flux is large, the secondary rectification effect is greatly improved, and the gel structure can be applied to negative pressure, normal pressure and pressurization operation.
Preferably, the pretreatment kettle is made of an enamel material.
A method for recovering ethanol from organic waste liquid by using the system comprises the following steps:
(1) pumping organic waste liquid into a waste liquid rectifying kettle, heating for primary rectifying treatment, and allowing generated gas phase to enter a waste liquid rectifying tower through a first discharge port through a pipeline;
(2) heating the waste liquid rectifying tower for secondary rectification treatment, and enabling the generated gas phase to enter a delayer through a second discharge hole through a pipeline; (3) one part of the organic phase material in the delayer flows back to the waste liquid rectifying tower through a third discharge hole for rectifying and purifying again, and the other part of the organic phase material is discharged; in the discharging process, the front fraction is collected into a front fraction collecting tank and the finished product ethanol is collected into an ethanol finished product tank by controlling the temperature of the top of the waste liquid rectifying tower.
Preferably, in the step (1), before the organic waste liquid is pumped into the waste liquid rectifying still, the pH value is adjusted to be neutral.
Preferably, in the step (3), the front fraction below 78 ℃ is extracted into a front fraction collecting tank, the middle fraction above 78 ℃ is extracted into an ethanol finished product tank, the tower top temperature of the waste liquid rectifying tower reaches 90 ℃ and the rectification is finished, and water and high-boiling residues remained in the waste liquid rectifying kettle are conveyed to a waste water pool for collection and treatment.
Therefore, the invention has the following beneficial effects: the structure is simple, ethanol in the organic waste liquid is rectified and recovered through twice rectification treatment, on one hand, the design of the delayer can be used for rectifying and purifying part of organic phase materials again to improve the extraction rate of the ethanol, on the other hand, front fraction (low boiling and ethanol) can be used for producing ethyl acetate, middle fraction (recovered ethanol) is sold as finished ethanol, waste liquid is changed into raw materials and finished products, and economic benefit and environmental protection benefit are generated.
Drawings
FIG. 1 is a schematic view showing the structure of a system for recovering ethanol from an organic waste liquid according to example 1.
In the figure: the device comprises a waste liquid rectifying kettle 1, a waste liquid rectifying tower 2, a delayer 3, a front fraction collecting tank 4, an ethanol finished product tank 5, an alkali liquor storage tank 6, a pretreatment kettle 7, a low boiling condenser 8, a waste liquid conveying pump 9, a tower top condenser 10, a waste liquid feeding pump 11, a first feeding hole 12, a first discharging hole 13, a second discharging hole 14, a second feeding hole 15, a third feeding hole 16, a third discharging hole 17, a fourth feeding hole 18 and a fourth discharging hole 19.
Detailed Description
The technical solution of the present invention is further specifically described below by using specific embodiments and with reference to the accompanying drawings.
In the present invention, all the equipment and materials are commercially available or commonly used in the art, and the methods in the following examples are conventional in the art unless otherwise specified.
Example 1
As shown in fig. 1: a system for recovering ethanol from organic waste liquid comprises a waste liquid rectifying kettle 1, a waste liquid rectifying tower 2 with stainless steel pore plate corrugated packing, a delayer 3, a front fraction collecting tank 4, an ethanol finished product tank 5, an alkali liquor storage 6, a pretreatment kettle 7, a low-boiling condenser 8, a waste liquid conveying pump 9, a tower top condenser 10 and a waste liquid feeding pump 11, wherein the top of the pretreatment kettle is provided with a fourth feeding hole 18 and a fourth discharging hole 19, the alkali liquor storage tank is connected with the fourth feeding hole 18 through a pipeline, the fourth discharging hole 19 is connected with a first feeding hole of the waste liquid rectifying kettle 1 through the low-boiling condenser 8 through a pipeline, the upper end of the waste liquid rectifying kettle is provided with a first feeding hole 12 and a first discharging hole 13, and the first discharging hole is connected with the bottom of the waste liquid rectifying tower through a pipeline; a second discharge hole 14 and a second feed hole 15 are formed in the top of the waste liquid rectifying tower, a third feed hole 16 is formed in the top of the delayer, a third discharge hole is formed in the side face of the delayer, the second discharge hole is connected with the third feed hole through a pipeline, and a third discharge hole 17 is respectively communicated with the second feed hole 15, the front fraction collecting tank 4 and the ethanol finished product tank 5 through a three-way pipeline; the second discharge port is connected with a third feed port 16 through a pipeline by the overhead condenser 10; the waste liquid feed pump is connected to the fourth feed port 18 via a pipe.
A method for recovering ethanol from organic waste liquid by using the system comprises the following steps:
(1) firstly, pumping organic waste liquid into a pretreatment kettle 7 through a fourth feed inlet 18 along a pipeline through a waste liquid feed pump 11, sampling the organic waste liquid to test an acid value, opening an alkali liquid storage tank 6, adding alkali liquid into the pretreatment kettle to adjust the organic waste liquid to be neutral, wherein the temperature during neutralization is normal temperature, low-boiling substances are condensed through a low-boiling condenser 8 and then enter a waste liquid rectifying kettle 2 through a first feed inlet 12, other substances are input into the waste liquid rectifying kettle 2 through a waste liquid conveying pump 9, heating is carried out for primary rectifying treatment, the temperature of the waste liquid rectifying kettle is 90 ℃, and generated gas phase enters a waste liquid rectifying tower through a pipeline through a first discharge outlet and then enters a delayer;
(2) heating the waste liquid rectifying tower to carry out secondary rectification treatment, wherein the temperature of a waste liquid rectifying kettle is 90 ℃, the generated gas phase enters the delayer through a second discharge port through a pipeline, and the waste liquid is discharged to a waste water tank through a discharge port;
(3) one part of the organic phase material in the delayer flows back to the waste liquid rectifying tower through a third discharge hole for rectifying and purifying again, and the other part of the organic phase material is discharged; in the discharging process, by controlling the temperature of the top of the waste liquid rectifying tower, front fraction below 78 ℃ is extracted into a front fraction collecting tank, middle fraction above 78 ℃ is extracted into an ethanol finished product tank, the temperature of the top of the waste liquid rectifying tower reaches 90 ℃ and the rectification is finished, and water and high-boiling residues remained in a waste liquid rectifying kettle are conveyed to a wastewater pool for collection and treatment.
The recovery of ethanol recovered in this example was 90% and the purity of the ethanol product was 91%.
Example 2
The difference between the embodiment 2 and the embodiment 1 is that a stainless steel orifice plate corrugated filler with poly isopropyl acrylamide (PNIPAm) gel loaded on the surface is arranged in the waste liquid rectifying tower 2, and the structural formula of the stainless steel orifice plate corrugated filler is as follows:
Figure BDA0002765275010000051
the recovery of ethanol recovered in this example was 92% and the purity of the ethanol product was 93%.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.

Claims (10)

1. A system for recovering ethanol from organic waste liquid is characterized by comprising a waste liquid rectifying kettle, a waste liquid rectifying tower, a delayer, a front fraction collecting tank and an ethanol finished product tank, wherein the upper end of the waste liquid rectifying kettle is provided with a first feeding hole and a first discharging hole, and the first discharging hole is connected with the bottom of the waste liquid rectifying tower through a pipeline; the top of the waste liquid rectifying tower is provided with a second discharge hole and a second feed hole, the top of the delayer is provided with a third feed hole, the side of the delayer is provided with a third discharge hole, the second discharge hole is connected with the third feed hole through a pipeline, and the third discharge hole is respectively communicated with the second feed hole, the front fraction collecting tank and the ethanol finished product tank through a tee pipeline.
2. The system for recovering ethanol from organic waste liquid according to claim 1, further comprising an alkali liquor storage tank, a pretreatment kettle and a low-boiling condenser, wherein a fourth feeding hole and a fourth discharging hole are formed in the top of the pretreatment kettle, the alkali liquor storage tank is connected with the fourth feeding hole through a pipeline, and the fourth discharging hole is connected with the first feeding hole of the waste liquid rectifying kettle through the low-boiling condenser through a pipeline.
3. The system for recovering ethanol from organic waste liquid according to claim 2, further comprising a waste liquid conveying pump, wherein the bottom of the pretreatment kettle is further provided with a first discharge port, and the first discharge port is connected with the top of the waste liquid rectification kettle through a pipeline via the waste liquid conveying pump.
4. The system for recovering ethanol from organic waste liquid according to claim 1, further comprising an overhead condenser, wherein the second discharge port is connected with a third feed port through the overhead condenser via a pipeline.
5. The system for recovering ethanol from organic waste liquid according to claim 1, further comprising a waste liquid feeding pump, wherein the waste liquid feeding pump is connected with the fourth feeding hole through a pipeline.
6. The system for recovering ethanol from organic waste liquid according to claim 1, wherein the waste liquid rectifying tower is internally provided with stainless steel perforated plate corrugated packing.
7. The system for recovering ethanol from organic waste liquid according to claim 6, wherein the surface of the stainless steel pore plate corrugated packing is loaded with temperature-responsive gel.
8. The system for recovering ethanol from organic waste liquid according to claim 1, wherein the pretreatment kettle is made of enamel material.
9. A method for recovering ethanol from organic waste liquid by using the system according to any one of claims 1 to 8, comprising the steps of:
(1) pumping organic waste liquid into a waste liquid rectifying kettle, heating for primary rectifying treatment, and allowing generated gas phase to enter a waste liquid rectifying tower through a first discharge port through a pipeline;
(2) heating the waste liquid rectifying tower for secondary rectification treatment, and enabling the generated gas phase to enter a delayer through a second discharge hole through a pipeline;
(3) one part of the organic phase material in the delayer flows back to the waste liquid rectifying tower through a third discharge hole for rectifying and purifying again, and the other part of the organic phase material is discharged; in the discharging process, the front fraction is collected into a front fraction collecting tank and the finished product ethanol is collected into an ethanol finished product tank by controlling the temperature of the top of the waste liquid rectifying tower.
10. The method of claim 9,
in the step (1), before the organic waste liquid is pumped into a waste liquid rectifying still, the pH is adjusted to be neutral;
in the step (3), the front fraction below 78 ℃ is extracted into a front fraction collecting tank, the middle fraction above 78 ℃ is extracted into an ethanol finished product tank, the tower top temperature of the waste liquid rectifying tower reaches 90 ℃ and the rectification is finished, and water and high-boiling residues remained in the waste liquid rectifying kettle are conveyed to a waste water pool for collection and treatment.
CN202011231214.1A 2020-11-06 2020-11-06 System and method for recovering ethanol from organic waste liquid Pending CN112374967A (en)

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Cited By (3)

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CN112999679A (en) * 2021-03-12 2021-06-22 建德建业资源再生技术有限公司 System and method for recovering isopropanol from waste organic solvent
CN113262509A (en) * 2021-04-30 2021-08-17 浙江建业化工股份有限公司 Treatment system and treatment method for isobutanol recovered from diisobutyl preparation process
CN113559536A (en) * 2021-08-08 2021-10-29 建德建业资源再生技术有限公司 System and method for recycling methanol from waste organic solvent

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