CN109052774A - Solvent is recycled efficient ethane nitrile wastewater recovery system - Google Patents
Solvent is recycled efficient ethane nitrile wastewater recovery system Download PDFInfo
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- CN109052774A CN109052774A CN201810640844.0A CN201810640844A CN109052774A CN 109052774 A CN109052774 A CN 109052774A CN 201810640844 A CN201810640844 A CN 201810640844A CN 109052774 A CN109052774 A CN 109052774A
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- acetonitrile
- discharge port
- tower
- solvent
- feed inlet
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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
-
- 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
- C02F1/26—Treatment of water, waste water, or sewage by extraction
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/32—Separation; Purification; Stabilisation; Use of additives
- C07C253/34—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/343—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the pharmaceutical industry, e.g. containing antibiotics
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/002—Construction details of the apparatus
- C02F2201/007—Modular design
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of solvents to be recycled efficient ethane nitrile wastewater recovery system, including head tank, azeotropy rectification column, acetonitrile lightness-removing column, acetonitrile refining tower, solvent knockout tower, extractor, heater and multiple condensers, head tank discharge port connects feed inlet in the middle part of azeotropy rectification column, the tower top discharge port of azeotropy rectification column connects azeotropic mixture storage tank V1 feed inlet by a condenser, a reflux line is arranged in discharge port, overhead reflux mouth is connected, the tower bottom discharge port of azeotropy rectification column is directly connected to discharge outlet.This acetonitrile returns to production system and reuses, and waste water drains into sewage treatment plant.Entire process flow is reasonable, it is also an option that being automatically controlled using DCS, easy to operate, investment is small, and device height is low, does not generate VOC organic exhaust gas, cooling water using ordinary cycle water, is particularly suitable for pharmacy corporation.
Description
Technical field
The invention belongs to separation equipment field, especially a kind of solvent is recycled efficient ethane nitrile wastewater recovery system.
Background technique
Acetonitrile is widely applied in polypeptide pharmaceutical industry.Acetonitrile have excellent solubility property, and can make a variety of inorganic matters and
The feature of organic matter dissociation, is used as solvent, catalyst and intermediate in many reactions.What many pharmaceutical factories generated largely contains second
In nitrile waste water, according to current national requirements for environmental protection, because acetonitrile toxicity is big, acetonitrile waste liquid can only be burned by specialized company and be destroyed, pin
Ruin 5 times that price is commodity acetonitrile.If acetonitrile is not added on recycling in ethane nitrile wastewater, not only the economic expense of producer is big, but also endangers
Evil environment, pollutes.Acetonitrile and water form azeotropic mixture under normal pressure, are difficult completely to divide them with common rectificating method
It opens.Currently, the conventional method that one aqueous mixtures of acetonitrile separate is had following several:
Variable-pressure rectification method: using pressurizing tower rectifying and vacuum tower rectifying thermal coupling, changes acetonitrile water by changing pressure
Azeotropic composition, finally obtain the acetonitrile of high-content；Constant boiling rectification method: change group by the way that nonvariant boiling reagent is added in return tank of top of the tower
Relative volatility between point reaches separation purpose, obtains the anhydrous acetonitrile of high-content.Extraction fractional distillation: added by the top in tower
Enter extractant to change the relative volatility between component, reach separation purpose, obtain the anhydrous acetonitrile of high-content, needs to increase extraction
Take agent recovery tower.Salting-out method: by layering of saltouing, dewatered acetonitrile enters back into acetonitrile tower and produces finished product acetonitrile from tower reactor.
Dehydrating agent dehydration: being added the dehydration of the dehydrating agents such as calcium chloride or piece solid base, then rectifying obtains qualified acetonitrile.Methylene chloride method: two
Chloromethanes is the technique combined using extraction and rectifying, obtains the anhydrous acetonitrile of high-content.
There are processing method complexity, equipment cost height and low separation efficiency, energy consumption height, acetonitrile yield for above-mentioned several method
The problems such as low.Transformation method, constant boiling rectification method and extraction fractional distillation rectifying column are very high, and water content is higher, are not suitable for pharmaceutical factory second
Nitrile wastewater treatment.Salting out method and dehydrating agent method can generate secondary pollution, be not suitable for industrial production.The shortcomings that methylene chloride method is two
38 ° of chloromethanes boiling point, VOC gas discharge can be generated, and need refrigerating plant.
Summary of the invention
Reasonable, easy to operate, investment that it is an object of the invention to overcome the deficiencies of the prior art and provide a kind of process flows
Solvent small, that device height is low is recycled efficient ethane nitrile wastewater recovery system.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of solvent is recycled efficient ethane nitrile wastewater recovery system, including head tank, azeotropy rectification column, acetonitrile lightness-removing column,
Acetonitrile refining tower, solvent knockout tower, extractor, heater and multiple condensers, head tank discharge port connect azeotropy rectification column
The tower top discharge port of middle part feed inlet, azeotropy rectification column connects azeotropic mixture storage tank V1 feed inlet by a condenser, and discharge port is set
A reflux line is set, overhead reflux mouth is connected, the tower bottom discharge port of azeotropy rectification column is directly connected to discharge outlet；
Azeotropic mixture reservoir outlet connects one feed inlet of extractor, and the feed inlet of extractor is also connected with solvent tank discharging
Mouthful, the feed inlet of extractor is connecting an ionic liquid reservoir outlet, installs blender, the discharge port of extractor in extractor
It is connected in parallel a water phase storage tank and an oily phase storage tank respectively, water phase storage tank connects one feed inlet of head tank, oily phase storage tank discharging
Mouth connects feed inlet in the middle part of acetonitrile lightness-removing column by a heater；
Acetonitrile lightness-removing column tower top discharge port is connected in parallel acetonitrile lightness-removing column refluxing opening and azeotropic mixture storage after passing through a condenser
Tank feed inlet, acetonitrile lightness-removing column tower bottom discharge port connect feed inlet in the middle part of acetonitrile refining tower；
Acetonitrile refining column overhead discharge port is connected in parallel acetonitrile storage tank and the reflux of acetonitrile lightness-removing column after passing through a condenser
Mouthful.Acetonitrile refining tower tower bottom discharge port connects solvent knockout tower, the tower top discharge port of solvent knockout tower by after a condenser simultaneously
The overhead reflux mouth and solvent tank of connection connection solvent knockout tower.
Moreover, heating mantle is installed in extractor lower part, for heating to extractor.
The advantages and positive effects of the present invention are as follows:
The application extracts ethane nitrile wastewater by the way of increasing higher boiling double solvents, and higher boiling double solvents is common
High boiling solvent adds a certain proportion of ionic liquid solvent, obtains content using high-efficiency packing tower isolation technics again after extraction
99.9% anhydrous acetonitrile.The acetonitrile returns to production system and reuses, and waste water drains into sewage treatment plant.Entire process flow is closed
Reason, it is easy to operate it is also an option that automatically controlled using DCS, invest small, device height is low, does not generate VOC organic exhaust gas, cold
But water uses ordinary cycle water, is particularly suitable for pharmacy corporation.
The application continues to use after high boiling solvent can also be separately recovered, very saving solvent usage.
Detailed description of the invention
Fig. 1 is structural schematic diagram of the invention.
Specific embodiment
For that can further appreciate that the contents of the present invention, feature and effect, following embodiment is provided, and cooperate attached drawing specifically
It is bright as follows, it should be noted that the present embodiment be it is descriptive, be not restrictive, cannot thus limit protection of the invention
Range.
The purpose of the application is in order to recycle acetonitrile that content in raw material is 10% and by content has been purified to
99.9% anhydrous acetonitrile, the application devise efficient ethane nitrile wastewater recovery system, behaviour reasonable with process flow
Make simple, small, the low advantage of device height of investment, specific structure and connection relationship are as follows:
A kind of solvent is recycled efficient ethane nitrile wastewater recovery system, including head tank 1, azeotropy rectification column T1, acetonitrile are de- light
Tower T2, acetonitrile refining tower T3, solvent knockout tower T4, extractor V3, heater E2 and multiple condensers (E1, E3, E4), raw material
Tank discharge port connects feed inlet in the middle part of azeotropy rectification column, and the tower top discharge port of azeotropy rectification column connects azeotropic mixture by a condenser
A reflux line is arranged in storage tank V1 feed inlet, discharge port, connects overhead reflux mouth, and the tower bottom discharge port of azeotropy rectification column directly connects
Connect discharge outlet；
Azeotropic mixture reservoir outlet connects one feed inlet of extractor, and it is (high that the feed inlet of extractor is also connected with solvent tank V2
Boiling point solvent) discharge port, the installation stirring in one ion liquid storage tank V7 discharge port of connection, extractor of the feed inlet of extractor
Device, the discharge port of extractor are connected in parallel the oily phase storage tank V5 of a water phase storage tank V4 and one respectively, and water phase storage tank connects head tank one
A feed inlet, oily phase reservoir outlet connect feed inlet in the middle part of acetonitrile lightness-removing column by a heater.
Acetonitrile lightness-removing column tower top discharge port is connected in parallel acetonitrile lightness-removing column refluxing opening and azeotropic mixture storage after passing through a condenser
Tank feed inlet, acetonitrile lightness-removing column tower bottom discharge port connect feed inlet in the middle part of acetonitrile refining tower.
Acetonitrile refining column overhead discharge port is connected in parallel acetonitrile storage tank V6 after passing through a condenser and acetonitrile lightness-removing column returns
Head piece.Acetonitrile refining tower tower bottom discharge port connects solvent knockout tower, and the tower top discharge port of solvent knockout tower passes through after a condenser
It is connected in parallel the overhead reflux mouth and solvent tank of solvent knockout tower, before entering solvent tank, can be exchanged heat by heat exchanger, solvent
The tower bottom discharge port of knockout tower connects ionic liquid reservoir inlet.
In order to accelerate the rate of extraction of extractor, heating mantle 2 can be installed in extractor lower part, for adding to extractor
Heat.
Solvent tank feed inlet is connected by heat exchanger.
The operating process of the present apparatus is as follows:
For the application by taking the ethane nitrile wastewater of polypeptide industry as an example, waste water generally contains acetonitrile 10%, and 10% ethane nitrile wastewater is first adopted
With azeotropic distillation, azeotropy rectification column T1 tower top obtains the azeotropic mixture of acetonitrile and water, and ethane nitrile content is the left and right 80% (wt), collects
To azeotropic mixture storage tank V1.The purpose is to reduce high boiling solvent dosages for low-concentration acetonitrile elder generation azeotropic concentration.If ethane nitrile content exists
25% or more, azeotropic distillation can not also be used directly to go to extract, its advantage is that saving steam.
80% acetonitrile solution and higher boiling composite extractant are added under normal temperature and pressure, in extractor V3, extractant is used
Measuring is 1-2 times of acetonitrile quality, and after agitated in extractor, extracting and demixing, extractant and acetonitrile, raffinate are obtained in extraction phase
It is water and micro-content organism in phase, is substantially free of acetonitrile, raffinate phase enters water phase storage tank V4, can directly throw sewage treatment system into
System.According to the output size of ethane nitrile wastewater, continuous extraction process can also be used.
Extraction phase is collected into oily phase storage tank V5, and the mixture of extractant and acetonitrile continuously enters acetonitrile lightness-removing column T2, takes off light
Tower atmospheric operation, tower top temperature are that 70 ° of tower tops obtain a small amount of acetonitrile and aqueous mixtures, return to azeotropic mixture storage tank V1 in extracting system
Again it extracts, tower bottom is higher boiling composite extractant and acetonitrile.
Moving material from acetonitrile lightness-removing column T1 tower reactor enters acetonitrile refining tower T3, since tower reactor is the compound extraction of higher boiling
Solvent is taken, and 70 ° of the tower top acetonitrile temperature difference or more, separating difficulty is small, and 81.7 ° of tower top temperature, reflux ratio R=0.1-1.0, tower top is very
It is easy to get 99.9% qualified anhydrous acetonitrile, is collected into acetonitrile storage tank V6 after the assay was approved, tower bottom extractant is free of acetonitrile.
Tower bottom solvent be separately input into after solvent knockout tower separates high-temperature solvent with ionic liquid solvent tank and
Ion liquid storage tank is recycled respectively, and high-temperature solvent can also return to the storage of extracting system solvent after T2 preheater E2 cooling
Tank V2 is reused.
Claims (2)
1. a kind of solvent is recycled efficient ethane nitrile wastewater recovery system, it is characterised in that: including head tank, azeotropy rectification column, second
Nitrile lightness-removing column, acetonitrile refining tower, solvent knockout tower, extractor, heater and multiple condensers, the connection of head tank discharge port is altogether
Feed inlet in the middle part of rectifying column is boiled, the tower top discharge port of azeotropy rectification column connects azeotropic mixture storage tank V1 feed inlet by a condenser,
A reflux line is arranged in discharge port, connects overhead reflux mouth, and the tower bottom discharge port of azeotropy rectification column is directly connected to discharge outlet；
Azeotropic mixture reservoir outlet connects one feed inlet of extractor, and the feed inlet of extractor is also connected with solvent tank discharge port, extracts
It takes the feed inlet of tank connecting an ionic liquid reservoir outlet, blender, the discharge port difference of extractor is installed in extractor
It is connected in parallel a water phase storage tank and an oily phase storage tank, water phase storage tank connects one feed inlet of head tank, and oily phase reservoir outlet is logical
Cross feed inlet in the middle part of heater connection acetonitrile lightness-removing column；
Acetonitrile lightness-removing column tower top discharge port pass through a condenser after be connected in parallel acetonitrile lightness-removing column refluxing opening and azeotropic mixture storage tank into
Material mouth, acetonitrile lightness-removing column tower bottom discharge port connect feed inlet in the middle part of acetonitrile refining tower；
Acetonitrile refining column overhead discharge port is connected in parallel acetonitrile storage tank and acetonitrile lightness-removing column refluxing opening after passing through a condenser.Second
Nitrile treating column tower bottom discharge port connects solvent knockout tower, and the tower top discharge port of solvent knockout tower after a condenser by being connected in parallel
The overhead reflux mouth and solvent tank of solvent knockout tower.
2. solvent according to claim 1 is recycled efficient ethane nitrile wastewater recovery system, it is characterised in that: under extractor
Portion is installed by heating mantle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810640844.0A CN109052774A (en) | 2018-06-21 | 2018-06-21 | Solvent is recycled efficient ethane nitrile wastewater recovery system |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810640844.0A CN109052774A (en) | 2018-06-21 | 2018-06-21 | Solvent is recycled efficient ethane nitrile wastewater recovery system |
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| Publication Number | Publication Date |
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| CN109052774A true CN109052774A (en) | 2018-12-21 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810640844.0A Pending CN109052774A (en) | 2018-06-21 | 2018-06-21 | Solvent is recycled efficient ethane nitrile wastewater recovery system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112851550A (en) * | 2021-01-20 | 2021-05-28 | 山东亿盛实业股份有限公司 | Method and equipment for continuously extracting and separating acetonitrile water azeotrope |
Citations (9)
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|---|---|---|---|---|
| US3281450A (en) * | 1963-09-27 | 1966-10-25 | Goodrich Co B F | Purification of acetonitrile |
| US3870746A (en) * | 1971-01-22 | 1975-03-11 | Degussa | Process for recovery of pure acetonitrile |
| US3896007A (en) * | 1971-11-17 | 1975-07-22 | Snam Progetti | PH Control of recycle water in the plural stage distillation of a crude acrylonitrile feed |
| US4238295A (en) * | 1978-12-04 | 1980-12-09 | Standard Oil Company | Energy efficient recovery of acrylonitrile |
| US6843890B1 (en) * | 1999-07-23 | 2005-01-18 | The Standard Oil Company | Purification and recovery of acetonitrile from waste solvent acetonitrile |
| CN102068831A (en) * | 2010-12-15 | 2011-05-25 | 天津大学 | Batch extractive distillation device and separation method for acetonitrile-methanol azeotropic mixture |
| CN202688238U (en) * | 2012-06-30 | 2013-01-23 | 湖北杜文化工科技有限公司 | Device for refining high-purity acetonitrile |
| CN103601653A (en) * | 2013-11-22 | 2014-02-26 | 天津大学 | Method for extracting, rectifying and separating acetonitrile-water azeotropic mixture |
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-
2018
- 2018-06-21 CN CN201810640844.0A patent/CN109052774A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3281450A (en) * | 1963-09-27 | 1966-10-25 | Goodrich Co B F | Purification of acetonitrile |
| US3870746A (en) * | 1971-01-22 | 1975-03-11 | Degussa | Process for recovery of pure acetonitrile |
| US3896007A (en) * | 1971-11-17 | 1975-07-22 | Snam Progetti | PH Control of recycle water in the plural stage distillation of a crude acrylonitrile feed |
| US4238295A (en) * | 1978-12-04 | 1980-12-09 | Standard Oil Company | Energy efficient recovery of acrylonitrile |
| US6843890B1 (en) * | 1999-07-23 | 2005-01-18 | The Standard Oil Company | Purification and recovery of acetonitrile from waste solvent acetonitrile |
| CN102068831A (en) * | 2010-12-15 | 2011-05-25 | 天津大学 | Batch extractive distillation device and separation method for acetonitrile-methanol azeotropic mixture |
| CN202688238U (en) * | 2012-06-30 | 2013-01-23 | 湖北杜文化工科技有限公司 | Device for refining high-purity acetonitrile |
| CN103601653A (en) * | 2013-11-22 | 2014-02-26 | 天津大学 | Method for extracting, rectifying and separating acetonitrile-water azeotropic mixture |
| CN103922963A (en) * | 2014-04-17 | 2014-07-16 | 河北工业大学 | Process for separating acetonitrile-water azeotrope system by adopting ionic liquid extraction distillation |
Non-Patent Citations (1)
| Title |
|---|
| 吴国忠等: "《辐射技术与先进材料》", 31 March 2016, 上海交通大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112851550A (en) * | 2021-01-20 | 2021-05-28 | 山东亿盛实业股份有限公司 | Method and equipment for continuously extracting and separating acetonitrile water azeotrope |
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Application publication date: 20181221 |
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