CN106178571B - Azeotrope separation process - Google Patents
Azeotrope separation process Download PDFInfo
- Publication number
- CN106178571B CN106178571B CN201610788105.7A CN201610788105A CN106178571B CN 106178571 B CN106178571 B CN 106178571B CN 201610788105 A CN201610788105 A CN 201610788105A CN 106178571 B CN106178571 B CN 106178571B
- Authority
- CN
- China
- Prior art keywords
- rectifying
- tank
- tower
- receiving tank
- phase
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
An azeotrope separation process comprising the steps of: 1) Adding the raw materials into an extraction kettle, adding an extractant, stirring for a certain time, standing for phase separation, and separating into a water phase and an oil phase; 2) Transferring one phase of the water phase or the oil phase into a rectifying still, heating by a reboiler of the rectifying still, and lifting the vapor phase into the rectifying tower; 3) The vapor phase in the rectifying tower rises to the top of the tower to be condensed into liquid, after total reflux is stable, a proper reflux ratio is set, the front fraction is firstly extracted, then the product is extracted, and finally the transition fraction is extracted. The azeotrope separation process combines the advantages of batch rectification and extractive rectification, has flexible operation, good stability and small equipment investment, and is suitable for separating an azeotropic system and a near-boiling system.
Description
Technical Field
The invention relates to an azeotrope separation process, and belongs to the field of separation and purification of azeotropes.
Background
In petrochemical product separation, two products with very similar boiling points are often separated, and if a common rectification method is adopted, the required theoretical plate number and reflux ratio are large, and the investment and operation cost are high.
Extractive distillation is a special distillation separation technology, and is suitable for the separation of azeotropic systems. The separation is achieved by continuously adding an extractant to the top of the rectifying column to change the relative volatilities of the original components. By combining the extraction and the rectification together, the method combines the advantages of batch rectification and extractive rectification, has flexible operation, small equipment investment and cost saving, and is suitable for separating an azeotropic system and a near-boiling system, such as: acetonitrile and water (acetonitrile: -85%, the balance water), methylene chloride and methanol (methylene chloride: -94%, the balance methanol), toluene and methanol (toluene: -31%, the balance methanol), and other azeotrope-like systems.
Disclosure of Invention
The invention provides an azeotrope separation process aiming at the defects of the prior art and integrating extraction and rectification technologies.
The technical scheme for solving the technical problems is as follows: an azeotrope separation process comprising the steps of:
1) Adding the raw materials into an extraction kettle, adding an extractant, stirring for a certain time, standing for phase separation, and separating into a water phase and an oil phase;
2) According to the property of the substances to be separated, transferring one phase of the water phase or the oil phase into a rectifying still, heating by a reboiler of the rectifying still, and then lifting the vapor phase into the rectifying tower;
3) The vapor phase in the rectifying tower rises to the top of the tower to be condensed into liquid, after total reflux of the top of the tower is stable, a proper reflux ratio is set according to the analysis result of the product at the top of the tower, the front fraction is firstly extracted, then the product is extracted, and finally the transition fraction is extracted.
The rectifying tower adopts a plate type tower, a packed tower, and a plate type and packed type combined tower.
Wherein, the step 2) can be deleted according to the actual situation, the steps of the azeotrope separation process are as follows:
1) Adding the raw materials into an extraction kettle, adding an extractant, stirring for a certain time, standing for phase separation, and separating into a water phase and an oil phase;
2) Transferring one phase of the water phase or the oil phase into a rectifying tower according to the property of the substances to be separated, and carrying out normal pressure batch rectification; heating by a rectifying tower reboiler, then lifting the vapor phase to the top of the tower, condensing the vapor phase at the top of the tower into liquid, setting a proper reflux ratio according to the analysis result of the product at the top of the tower after total reflux is stable, firstly extracting the front fraction, then extracting the product, and finally extracting the transition fraction.
As a further improvement of the scheme, the invention provides an azeotrope separation device, which comprises a rectifying kettle, a rectifying tower and an extraction kettle; the bottom of the extraction kettle is provided with a water phase receiving tank and an oil phase receiving tank; the bottom of the water phase receiving tank is connected with the rectifying still and the rectifying tower respectively; the tank bottom of the oil phase receiving tank is connected with the rectifying still and the rectifying tower respectively; the rectifying still is connected with the rectifying tower still; the top of the rectifying tower is provided with a reflux tank which is connected with the extraction kettle.
Further, the bottom of the rectifying still is connected with a still residue barrel.
Further, a product receiving tank is arranged on the reflux tank, and a front fraction receiving tank, a transition fraction receiving tank and an extractant tank are arranged between the reflux tank and the extraction kettle in parallel.
Further, a condenser is arranged between the rectifying tower and the reflux tank.
Further, a cooler is arranged on the pipeline among the front cut receiving tank, the transition cut receiving tank, the extractant tank, the product receiving tank and the reflux tank.
Further, the condenser is connected with a tail cooler, and the other end of the tail cooler is respectively connected with a front fraction receiving tank, a transition fraction receiving tank, an extractant tank and a product receiving tank.
Further, a rectifying tower reboiler is arranged at the rectifying tower kettle.
Further, a rectifying still reboiler is arranged at the bottom of the rectifying still.
The invention has the characteristics of low energy consumption, low pollution, high recovery rate and high product purity, and has remarkable practicality and economic benefit.
Drawings
FIG. 1 is a schematic diagram of an azeotrope separation apparatus.
Wherein, 1, rectifying still; 2. a rectifying tower; 3. an extraction kettle; 4. a water phase receiving tank; 5. an oil phase receiving tank; 6. a reflux drum; 7. a product receiving tank; 8. a front cut receiving tank; 9. a transition fraction receiving tank; 10. an extractant tank; 11. a condenser; 12. a cooler; 13. a tail cooler; 14. a kettle residue barrel; 15. a rectifying still reboiler; 16. a rectifying tower reboiler.
Detailed Description
The principles and features of the present invention are described below with reference to the drawings, the examples are illustrated for the purpose of illustrating the invention and are not to be construed as limiting the scope of the invention.
Example 1
The pretreated raw material is mainly acetonitrile and water
Firstly, raw materials enter an extraction kettle 3, then an extractant is added, stirring is started for a certain time, standing is carried out for phase separation, and a water phase is extracted to a wastewater treatment working section; the oil phase is transferred into a rectifying still 1, heated by a rectifying still reboiler 15, vapor phase rises into a rectifying tower 2, condensed by a tower top condenser 11, and after total reflux of the tower top is stable, a proper reflux ratio is set according to the analysis result of the tower top product, a front fraction (an azeotrope of an extractant and water and a transition fraction of the extractant and acetonitrile) is firstly extracted, and the front fraction can be returned to the extracting still for recycling along with the next batch as the extractant; the acetonitrile product is then withdrawn to product receiving tank 7.
Example 2
The pretreated raw material mainly comprises dichloromethane and methanol
Firstly, raw materials enter an extraction kettle 3, then an extractant is added, stirring is started for a certain time, standing is carried out, phase separation is carried out, an oil phase (methylene dichloride product) and a water phase (methanol aqueous solution containing a small amount of methylene dichloride) are obtained after phase separation, the water phase (methanol aqueous solution containing a small amount of methylene dichloride) is transferred into a rectification kettle 1, after being heated by a rectification kettle reboiler 15, the vapor phase rises into a rectification tower 2, is condensed by a tower top condenser 11, after total reflux of the tower top is stable, a proper reflux ratio is set according to the analysis result of the tower top product, and front fractions (methylene dichloride/methanol/water), methanol and water are sequentially extracted; the water can be used as the extractant for the working section for recycling.
Example 3
The pretreated raw materials mainly comprise toluene and methanol
Liquid-liquid extraction is carried out through an extraction kettle 3, and toluene products are obtained after phase separation; the water phase is methanol aqueous solution, which is transferred into a rectifying still 1, heated by a rectifying still reboiler 15, vapor phase rises into a rectifying tower 2, condensed by a tower top condenser 11, and after total reflux of the tower top is stabilized, a proper reflux ratio is set according to the analysis result of the tower top product, and a small amount of front cut fraction, methanol product and transition cut fraction (methanol and water) are sequentially extracted; when methanol is not contained in the distillate at the top of the rectifying tower 2, the heating can be stopped. The process waste water in the kettle can be used as extractant circulating water in the process after being cooled.
An azeotrope separation device used in the azeotrope separation process is shown in figure 1, and comprises a rectifying still 1, a rectifying tower 2 and an extracting still 3; the bottom of the extraction kettle 3 is provided with a water phase receiving tank 4 and an oil phase receiving tank 5; the bottom of the water phase receiving tank 4 is respectively connected with the rectifying still 1 and the rectifying tower 2; the tank bottom of the oil phase receiving tank 5 is connected with the rectifying still 1 and the rectifying tower 2 respectively; the rectifying still 1 is connected with the rectifying still 2; the rectifying tower 2 tower kettle is provided with a rectifying tower reboiler 16, the rectifying tower 2 tower top is provided with a reflux tank 6, and the reflux tank 6 is connected with the extraction kettle 3.
A rectifying still reboiler 15 is arranged at the bottom of the rectifying still 1, and a still residue barrel 14 is connected to the bottom of the rectifying still 1; a product receiving tank 7 is arranged on the reflux tank 6, and a front fraction receiving tank 8, a transition fraction receiving tank 9 and an extractant tank 10 are arranged between the reflux tank 6 and the extraction kettle 3 in parallel; a condenser 11 is arranged between the rectifying tower 2 and the reflux tank 6; a cooler 12 is arranged on the pipeline among the front cut receiving tank 8, the transition cut receiving tank 9, the extractant tank 10, the product receiving tank 7 and the reflux tank 6; the pipelines among the front cut receiving tank 8, the transition cut receiving tank 9, the extractant tank 10, the product receiving tank 7 and the condenser 11 are provided with a tail cooler 13.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (7)
1. An azeotrope separation process comprising the steps of:
1) Adding the raw materials into an extraction kettle, adding an extractant, stirring for a certain time, standing for phase separation, and separating into a water phase and an oil phase;
2) Transferring one phase of the water phase or the oil phase into a rectifying still, heating by a reboiler of the rectifying still, and lifting the vapor phase into the rectifying tower;
3) The vapor phase in the rectifying tower rises to the top of the tower to be condensed into liquid, after total reflux is stable, a proper reflux ratio is set, a front fraction is firstly extracted, then a product is extracted, and finally a transition fraction is extracted;
the azeotrope separation device used in the process comprises a rectifying kettle, a rectifying tower and an extraction kettle; the bottom of the extraction kettle is provided with a water phase receiving tank and an oil phase receiving tank; the bottom of the water phase receiving tank is connected with the rectifying still and the rectifying tower respectively; the tank bottom of the oil phase receiving tank is connected with the rectifying still and the rectifying tower respectively; the rectifying still is connected with the rectifying tower still; the top of the rectifying tower is provided with a reflux tank which is connected with the extraction kettle; the reflux tank is provided with a product receiving tank, and a front fraction receiving tank, a transition fraction receiving tank and an extractant tank are arranged in parallel between the reflux tank and the extraction kettle.
2. An azeotrope separation process according to claim 1, wherein:
the rectifying tower adopts a plate tower, a packed tower, and a plate and packed combined tower.
3. An azeotrope separation process according to claim 1, wherein:
a condenser is arranged between the rectifying tower and the reflux tank.
4. An azeotrope separation process according to claim 1, wherein:
and coolers are arranged on pipelines among the front cut receiving tank, the transition cut receiving tank, the extractant tank, the product receiving tank and the reflux tank.
5. A process for the separation of azeotropes according to claim 3, wherein:
the condenser is connected with a tail cooler, and the other end of the tail cooler is respectively connected with a front fraction receiving tank, a transition fraction receiving tank, an extractant tank and a product receiving tank.
6. An azeotrope separation process according to claim 1, wherein:
and a rectifying tower reboiler is arranged at the bottom of the rectifying tower.
7. An azeotrope separation process according to claim 1, wherein:
and a rectifying still reboiler is arranged at the bottom of the rectifying still.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610788105.7A CN106178571B (en) | 2016-08-31 | 2016-08-31 | Azeotrope separation process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610788105.7A CN106178571B (en) | 2016-08-31 | 2016-08-31 | Azeotrope separation process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106178571A CN106178571A (en) | 2016-12-07 |
| CN106178571B true CN106178571B (en) | 2023-07-14 |
Family
ID=58086333
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610788105.7A Active CN106178571B (en) | 2016-08-31 | 2016-08-31 | Azeotrope separation process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106178571B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107840808B (en) * | 2017-10-30 | 2024-06-14 | 烟台国邦化工机械科技有限公司 | Device for producing cyanoacetic acid ester and malonic acid ester by continuous reaction rectification and production process thereof |
| CN107998678B (en) * | 2017-10-30 | 2023-08-18 | 烟台国邦化工机械科技有限公司 | Environment-friendly cleaning device and process method for separating organic azeotrope |
| CN108046992B (en) * | 2017-12-29 | 2021-02-02 | 山东华安新材料有限公司 | Method and equipment for purifying 2, 2-difluoroethanol |
| CN109231635B (en) * | 2018-11-20 | 2023-05-09 | 江苏九天高科技股份有限公司 | Wastewater treatment process |
| CN112661731B (en) * | 2019-10-15 | 2022-08-05 | 中国石油化工股份有限公司 | Device and method for decoloring and purifying maleic anhydride refined heavy components |
| CN113461568A (en) * | 2021-06-24 | 2021-10-01 | 索闻特环保科技(上海)有限公司 | Method for treating toluene in acetonitrile waste liquid |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5152876A (en) * | 1991-03-27 | 1992-10-06 | Lloyd Berg | Separation of methylene chloride from the lower alcohols by extractive distillation |
| CN101492391A (en) * | 2008-01-25 | 2009-07-29 | 天津普莱化工技术有限公司 | Process for separating ethane nitrile wastewater with combination of abstraction and distillation |
| CN201279398Y (en) * | 2008-10-09 | 2009-07-29 | 上海宝钢化工有限公司 | Rectifier |
| CN103449981A (en) * | 2013-08-22 | 2013-12-18 | 无锡中天固废处置有限公司 | Azeotropic rectification device and method for separating propylene glycol monomethyl ether and water |
| CN104262079A (en) * | 2014-09-16 | 2015-01-07 | 山东特普化工技术有限公司 | Method and device for separating carbon tetrachloride and methanol through heterogeneous batch extractive distillation |
| CN105418430A (en) * | 2015-12-16 | 2016-03-23 | 东营市海科新源化工有限责任公司 | Device and method for preparing high-purity dimethyl carbonate through batch rectification |
| CN206198730U (en) * | 2016-08-31 | 2017-05-31 | 烟台国邦化工机械科技有限公司 | A kind of Azeotrope separation device |
-
2016
- 2016-08-31 CN CN201610788105.7A patent/CN106178571B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5152876A (en) * | 1991-03-27 | 1992-10-06 | Lloyd Berg | Separation of methylene chloride from the lower alcohols by extractive distillation |
| CN101492391A (en) * | 2008-01-25 | 2009-07-29 | 天津普莱化工技术有限公司 | Process for separating ethane nitrile wastewater with combination of abstraction and distillation |
| CN201279398Y (en) * | 2008-10-09 | 2009-07-29 | 上海宝钢化工有限公司 | Rectifier |
| CN103449981A (en) * | 2013-08-22 | 2013-12-18 | 无锡中天固废处置有限公司 | Azeotropic rectification device and method for separating propylene glycol monomethyl ether and water |
| CN104262079A (en) * | 2014-09-16 | 2015-01-07 | 山东特普化工技术有限公司 | Method and device for separating carbon tetrachloride and methanol through heterogeneous batch extractive distillation |
| CN105418430A (en) * | 2015-12-16 | 2016-03-23 | 东营市海科新源化工有限责任公司 | Device and method for preparing high-purity dimethyl carbonate through batch rectification |
| CN206198730U (en) * | 2016-08-31 | 2017-05-31 | 烟台国邦化工机械科技有限公司 | A kind of Azeotrope separation device |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106178571A (en) | 2016-12-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106178571B (en) | Azeotrope separation process | |
| CN103755559B (en) | A kind of method of ion liquid abstraction rectifying separation ethyl acetate-isopropanol | |
| CN101050159B (en) | Method for separating butane and butylenes, and dedicated installation | |
| CN109206291A (en) | A kind of separation method of chloromethanes-dimethyl ether | |
| CN105330514A (en) | Purification process for preparation of ethylene glycol from synthesis gas | |
| CN102675029B (en) | A kind of differential pressure heat coupling separation of extractive distillation hexahydrotoluene and the method for toluene | |
| CN203923057U (en) | Improved Butanol Recycling device | |
| CN104230657A (en) | Novel energy-saving three-tower continuous extractive distillation technology and extractive distillation system thereof | |
| CN103394209A (en) | Method for rectifying and separating ethanol and tetrahydrofuran azeotrope system by low-pressure tower and high-pressure tower | |
| CN101700916B (en) | Process and system for treating industrial normal propyl alcohol waste liquor | |
| CN101412671B (en) | Method for separating isobutyl acetate, ethanol and water by azeotropic distillation | |
| CN110066226B (en) | Refining process of acetonitrile-containing wastewater | |
| CN103408513A (en) | Method for separation of ethanol-tetrahydrofuran azeotrope by high-low pressure double-tower distillation | |
| CN107998677B (en) | Environment-friendly cleaning device and process method for solvent recovery | |
| CN101890249A (en) | Energy-saving process method for rectifying and separating three fractions | |
| CN106986751B (en) | Method for extracting crude phenol from phenol oil | |
| CN106349107B (en) | A kind of method and device of heterogeneous azeotropic rectification separating acetonitrile-triethylamine mixture | |
| CN206198730U (en) | A kind of Azeotrope separation device | |
| CN104370696A (en) | Novel method for separating ethylene glycol and 1,2-pentanediol | |
| CN104151137B (en) | High pressure normal pressure two-tower rectification is separated the method for propyl carbinol and MIBK azeotropic system | |
| CN108358754B (en) | Process method and system for separating ethanol, ethyl acetate and water mixture | |
| CN108358808B (en) | Method for recovering dimethylacetamide in waste oil of cyclohexanone device | |
| CN203060873U (en) | Continuous rectifying tower for N-methylaniline | |
| CN102795957A (en) | Method for separating m-ethyltoluene and p-ethyltoluene by extractive distillation | |
| CN104693005A (en) | New process for separating methanol-propyl formate azeotrope through extractive distillation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |