CN113461490A - Method for treating mixed liquid containing isopropanol, isopropyl acetate and water - Google Patents
Method for treating mixed liquid containing isopropanol, isopropyl acetate and water Download PDFInfo
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- CN113461490A CN113461490A CN202110707000.5A CN202110707000A CN113461490A CN 113461490 A CN113461490 A CN 113461490A CN 202110707000 A CN202110707000 A CN 202110707000A CN 113461490 A CN113461490 A CN 113461490A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/86—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by liquid-liquid treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/58—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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Abstract
The invention relates to a method for treating a mixed solution containing isopropanol, isopropyl acetate and water, which comprises the following steps: the mixed solution is rectified to form a first azeotrope of isopropanol and isopropyl acetate, water is added into the first azeotrope to carry out liquid-liquid extraction and phase separation to obtain a first light phase rich in isopropyl acetate and a first heavy phase rich in water and isopropanol. The mixed liquid treatment method can effectively separate the isopropanol and the isopropyl acetate in the mixed liquid, so that the isopropanol and the isopropyl acetate in the mixed liquid can be recycled and utilized, and the pollution of the mixed liquid to the environment is reduced.
Description
Technical Field
The present invention relates to a method for treating a mixed liquid containing isopropyl alcohol, isopropyl acetate and water.
Background
Isopropanol (IPA for short) is an important chemical product and raw material. It is mainly used in pharmacy, cosmetics, plastics, perfume, paint, etc.
Isopropyl acetate (IPAC) is used as solvent for paint, printing ink, etc. and is also used as dewatering agent, extractant and perfume component in medicine production.
Isopropyl alcohol is also a hydrolysate of isopropyl acetate, and isopropyl alcohol is likely to be produced as a by-product during the production of isopropyl acetate, and the isopropyl alcohol and isopropyl acetate form an azeotrope, wherein the azeotropic ratio is about IPA to IPCA of 0.55 to 0.45, and the isopropyl alcohol and isopropyl acetate are difficult to separate by using a common rectification method.
Disclosure of Invention
The main object of the present invention is to provide a method capable of separating and recovering isopropyl alcohol and isopropyl acetate contained in a mixed liquid.
In order to achieve the above object, the present invention relates to a method for treating a mixed solution containing isopropyl alcohol, isopropyl acetate and water, comprising the steps of:
the mixed solution enters a first rectifying tower for continuous rectification to obtain a first material containing isopropanol and isopropyl acetate azeotrope at the tower top,
performing liquid-liquid extraction phase separation on the first material and water in a first liquid-liquid extraction tower to obtain a second material containing isopropyl acetate in a light phase and a third material containing water and isopropanol in a heavy phase,
dehydrating the second material by a first pervaporation membrane to obtain an isopropyl acetate product,
the third material enters a second rectifying tower for intermittent rectification to obtain a fourth material of azeotrope of water and isopropanol at the tower top,
and dehydrating the fourth material through a second pervaporation membrane to obtain an isopropanol product.
In some embodiments, the third material further contains isopropyl acetate, the third material enters a second rectifying tower for batch rectification, the head fraction of the tower top obtains a fifth material consisting of isopropyl acetate, isopropanol and water in a ternary azeotropic mode, and the second fraction obtains the fourth material.
In some embodiments, the fifth material and water are subjected to extraction phase separation in a second liquid-liquid extraction tower, a sixth material containing isopropyl acetate is obtained in a light phase, the sixth material enters the first pervaporation membrane to be dehydrated to obtain an isopropyl acetate product, a seventh material containing isopropanol and water is obtained in a heavy phase, and the seventh material flows back to the second rectification tower to be subjected to the batch rectification.
In some embodiments, the water is added in the first lle column in excess of the azeotropic ratio of water to isopropanol such that the bottoms of the second rectification column is pure water and the bottoms of the second rectification column are refluxed to the second lle column for the extractive phase separation.
In some embodiments, the water is added in the first lle column in excess of the azeotropic ratio of water to isopropanol so that the bottoms of the second rectification column is pure water and the bottoms of the second rectification column are refluxed to the first lle column for the extractive phase separation.
In some embodiments, the operating conditions of the second liquid-liquid extraction column are: normal pressure, light phase discharging temperature of 10-40 deg.c and heavy phase discharging temperature of 10-40 deg.c.
In some embodiments, the fifth material is collected in the temporary storage tank and then enters the second liquid-liquid extraction tower.
In some embodiments, the operating conditions of the first rectification column are: under normal pressure, the temperature at the top of the tower is 75-80 ℃, the temperature at the bottom of the tower is 80-85 ℃, the reflux ratio is 4-7, and the azeotrope is discharged from the top of the first rectifying tower.
In some embodiments, the operating conditions of the second rectification column are: the first fraction is discharged from the top of the tower under normal pressure, the temperature at the top of the tower is 70-80 ℃, the temperature at the bottom of the tower is 80-85 ℃, the reflux ratio is 1-4.
In some embodiments, the operating conditions of the first lle column are: normal pressure, light phase discharging temperature of 10-45 deg.c and heavy phase discharging temperature of 10-45 deg.c.
The mixed liquid treatment method can effectively separate the isopropanol and the isopropyl acetate in the mixed liquid, so that the isopropanol and the isopropyl acetate in the mixed liquid can be recycled and utilized, and the pollution of the mixed liquid to the environment is reduced.
Drawings
FIG. 1 is a process flow chart of a method for treating a mixed solution of isopropyl alcohol and isopropyl acetate.
In the figure: the method comprises the following steps of 1, a first rectifying tower, 2, a first liquid-liquid extraction tower, 3, a first pervaporation membrane, 4, a transfer tank, 5, a second rectifying tower, 6, a temporary storage tank, 7, a second liquid-liquid extraction tower, 8, an extractant storage tank, 9, an IPAC finished product tank, 10, a second pervaporation membrane, 11, an IPA finished product tank, 100 mixed liquor, 101, a first material, 102, a second material, 103, a third material, 104, a fourth material, 105, a fifth material, 106, a sixth material and 107, a seventh material. 108. And (3) water.
Detailed Description
The rectifying tower in this embodiment includes not only the tower body, but also relevant corollary equipment and instrumentation systems, such as a relevant pump, a pipeline, a valve, a control system, etc., configured for the rectifying tower body to achieve rectification.
In this embodiment, the transportation of each material may be controlled by a pipeline, a pump, a valve, and a control system, and the temperature of the material may be adjusted by various heaters, heat exchangers, and other devices.
The extraction tower in this embodiment includes not only a tower body, but also relevant corollary equipment and instrumentation systems, such as relevant pumps, pipelines, valves, control systems, and the like, configured for the extraction tower in order to realize extraction split-phase extraction.
The contents in the present example are weight percentages unless otherwise specified.
The method for treating the mixed liquid containing isopropanol, isopropyl acetate and water mainly comprises the following steps:
the mixed solution enters a first rectifying tower for continuous rectification to obtain a first material containing isopropanol and isopropyl acetate azeotrope at the tower top,
performing liquid-liquid extraction phase separation on the first material and water in a first liquid-liquid extraction tower to obtain a second material containing isopropyl acetate in a light phase and a third material containing water and isopropanol in a heavy phase,
dehydrating the second material by a first pervaporation membrane to obtain an isopropyl acetate product,
the third material enters a second rectifying tower for intermittent rectification to obtain a fourth material of azeotrope of water and isopropanol at the tower top,
and dehydrating the fourth material through a second pervaporation membrane to obtain an isopropanol product.
The invention will be further illustrated with reference to fig. 1 and the examples.
The liquid mixture treated in this example contained 80.93% IPA, 17.87% IPAC, and 1.2% water. The mixed liquid firstly enters a first rectifying tower 1 for rectification, the feeding flow of the mixed liquid is 1000kg/h, and the operating conditions of the first rectifying tower 1 are as follows: the first azeotrope of IPA and IPAC was distilled off from the top of the first distillation column 1 at normal pressure, the top temperature of 78.2 ℃ and the bottom temperature of 83.4 ℃ at a reflux ratio of 6, and a small amount of water was also contained, and the top discharge of the first distillation column 1 in this example was a first material containing 53.4% IPA, 43.6% IPAC and 3% water at a flow rate of 400kg/h, and the bottom discharge was an IPA product containing 99.3% IPA and 0.7% IPAC at a flow rate of 600 kg/h. IPA purity in the tower cauldron ejection of compact has accorded with the requirement of IPA product in this embodiment, can directly send into IPA product jar 11 and store, when the tower cauldron ejection of compact has different compositions, can handle according to actual conditions.
Adding a first material and water into a first liquid-liquid extraction tower 2 together to carry out extraction phase separation, wherein the feeding flow rate of the first material is 400kg/h, the feeding flow rate of the water is 550kg/h, the water extracts isopropanol in a first azeotrope and forms phase separation with isopropyl acetate, the addition amount of the water is related to the amount of the isopropanol in the first azeotrope, the water at least has the dosage capable of absorbing all the isopropanol to form stable phase separation and is excessive in azeotropic composition of the water and the isopropanol, and the operating conditions of the first liquid-liquid extraction tower 2 are as follows: the normal pressure is realized, the discharge temperature of the light phase is 12.0 ℃, the discharge temperature of the heavy phase is 41.8 ℃, the light phase in the first liquid-liquid extraction tower contains a second material containing 0.5 percent of IPA, 98.1 percent of IPAC and 1.4 percent of water, the discharge flow rate of the second material is 143kg/h, the heavy phase contains 26.4 percent of IPA, 4.2 percent of IPAC and 69.4 percent of water, and the discharge flow rate of the third material is 807 kg/h. The second material is sent into the first pervaporation membrane 3 to be separated to obtain an IPAC product, and the IPAC product is sent into an IPAC finished product tank 9 to be stored.
And the third material is sent into a second rectifying tower 5 for intermittent rectification after passing through a transit tank 4, the flow rate of the material in the transit tank entering the second rectifying tower 5 is 975kg/h, and the operating conditions of the second rectifying tower 5 are as follows: the atmospheric pressure, the overhead temperature of 75.4 ℃, the bottom temperature of 84.4 ℃, the reflux ratio of 3, a small amount of first distillate distilled from the top of the second rectifying tower is a fifth material containing 37.5% IPA, 51.3% IPAC and 11.2% water, the flow rate is 77.5kg/h, the second distillate after the first distillate is a fourth material containing 85.2% IPA and 14.8% water, the flow rate is 250kg/h, the tower bottom discharge is 100% pure water, and the flow rate is 647.5 kg/h. A small amount of fifth material can be temporarily stored in the temporary storage tank 6, the fifth material is sent to the second liquid-liquid extraction tower 7 after waiting for a large amount of fifth material, the second liquid-liquid extraction tower 7 is extracted by water, the flow rate of the material entering the second liquid-liquid extraction tower in the temporary storage tank is 500kg/h, and the operation conditions of the second liquid-liquid extraction tower 7 are as follows: normal pressure, light phase discharging temperature 11.1 deg.c and heavy phase discharging temperature 37.9 deg.c. After extraction phase separation, the light phase is a sixth material containing 0.2% of IPA, 98.4% of IPAC and 79.2% of water, the discharge flow rate is 244kg/h, the heavy phase is a seventh material containing 17.3% of IPA, 3.5% of IPAC and 79.2% of water, the discharge flow rate is 856kg/h, and the sixth material is sent to the first pervaporation membrane 3 to be subjected to dewatering separation to obtain an IPAC product, and the IPAC product is stored by an IPAC finished product tank 9. The seventh material can be returned to the second rectifying tower 5 for continuous treatment after being refluxed to the transit tank. The fourth material of the second fraction enters the second pervaporation membrane 10 to be separated to obtain IPA product, and the IPA product can be stored by an IPA product tank 11.
The embodiments of the present invention are merely illustrative, and not restrictive, of the scope of the claims, and other substantially equivalent alternatives may occur to those skilled in the art and are within the scope of the present invention.
Claims (10)
1. A method for treating a mixed liquid containing isopropyl alcohol, isopropyl acetate and water, comprising the steps of:
the mixed solution enters a first rectifying tower for continuous rectification to obtain a first material containing isopropanol and isopropyl acetate azeotrope at the tower top,
performing liquid-liquid extraction phase separation on the first material and water in a first liquid-liquid extraction tower to obtain a second material containing isopropyl acetate in a light phase and a third material containing water and isopropanol in a heavy phase,
dehydrating the second material by a first pervaporation membrane to obtain an isopropyl acetate product,
the third material enters a second rectifying tower for intermittent rectification to obtain a fourth material of azeotrope of water and isopropanol at the tower top,
and dehydrating the fourth material through a second pervaporation membrane to obtain an isopropanol product.
2. The process according to claim 1, wherein the third material further comprises isopropyl acetate, the third material is fed into the second rectifying tower for batch rectification, the overhead fraction of the tower obtains a fifth material consisting of ternary azeotropic composition of isopropyl acetate, isopropanol and water, and the sub-fraction obtains the fourth material.
3. The process according to claim 2, wherein the fifth material and water are subjected to extraction phase separation in a second liquid-liquid extraction column, a sixth material containing isopropyl acetate is obtained in a light phase, the sixth material enters the first pervaporation membrane for dehydration to obtain an isopropyl acetate product, a seventh material containing isopropanol and water is obtained in a heavy phase, and the seventh material flows back to the second rectification column for batch rectification.
4. The process according to claim 3, wherein the water is added in an amount in excess of the amount of water added to form an azeotropic mixture of water and isopropanol, such that the bottoms of the second distillation column are purified water and the bottoms of the second distillation column are refluxed to the second liquid-liquid extraction column for the extractive phase separation.
5. The process according to claim 1 or 4, wherein the water is added in an amount in excess of the amount of water to form an azeotropic mixture of water and isopropanol in the first liquid-liquid extraction column, so that the bottom discharge of the second distillation column is pure water and the bottom discharge of the second distillation column is refluxed to the first liquid-liquid extraction column for the extractive phase separation.
6. The process of claim 3, wherein the second liquid-liquid extraction column is operated under the following conditions: normal pressure, light phase discharging temperature of 10-40 deg.c and heavy phase discharging temperature of 10-40 deg.c.
7. The process of claim 3 wherein the fifth stream is collected in a holding tank and then introduced into the second liquid-liquid extraction column.
8. The process according to claim 1, characterized in that the operating conditions of the first rectification column are: under normal pressure, the temperature at the top of the tower is 75-80 ℃, the temperature at the bottom of the tower is 80-85 ℃, the reflux ratio is 4-7, and the azeotrope is discharged from the top of the first rectifying tower.
9. The process according to claim 1, characterized in that the operating conditions of the second rectification column are: the first fraction is discharged from the top of the tower under normal pressure, the temperature at the top of the tower is 70-80 ℃, the temperature at the bottom of the tower is 80-85 ℃, the reflux ratio is 1-4.
10. The process of claim 1, wherein the first lle column is operated under the following conditions: normal pressure, light phase discharging temperature of 10-45 deg.c and heavy phase discharging temperature of 10-45 deg.c.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110707000.5A CN113461490A (en) | 2021-06-24 | 2021-06-24 | Method for treating mixed liquid containing isopropanol, isopropyl acetate and water |
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| CN202110707000.5A CN113461490A (en) | 2021-06-24 | 2021-06-24 | Method for treating mixed liquid containing isopropanol, isopropyl acetate and water |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114315581A (en) * | 2021-12-29 | 2022-04-12 | 扬州贝尔新环境科技有限公司 | Method for pressure swing separation of isopropyl acetate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2003232246A1 (en) * | 2002-05-07 | 2003-11-11 | Basf Aktiengesellschaft | Method for producing an aqueous alkali acrylate solution |
| CN1733685A (en) * | 2005-07-20 | 2006-02-15 | 上海吴泾化工有限公司 | Method for preparing and purifying propyl acetate |
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2021
- 2021-06-24 CN CN202110707000.5A patent/CN113461490A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2003232246A1 (en) * | 2002-05-07 | 2003-11-11 | Basf Aktiengesellschaft | Method for producing an aqueous alkali acrylate solution |
| CN1733685A (en) * | 2005-07-20 | 2006-02-15 | 上海吴泾化工有限公司 | Method for preparing and purifying propyl acetate |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114315581A (en) * | 2021-12-29 | 2022-04-12 | 扬州贝尔新环境科技有限公司 | Method for pressure swing separation of isopropyl acetate |
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Application publication date: 20211001 |