CN105906488A - Method applied to refining purification device for by-product diisopropylether during isopropanol production - Google Patents
Method applied to refining purification device for by-product diisopropylether during isopropanol production Download PDFInfo
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- CN105906488A CN105906488A CN201610425351.6A CN201610425351A CN105906488A CN 105906488 A CN105906488 A CN 105906488A CN 201610425351 A CN201610425351 A CN 201610425351A CN 105906488 A CN105906488 A CN 105906488A
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- diisopropyl ether
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
- C07C41/42—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/38—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method applied to a refining purification device for a by-product diisopropylether during isopropanol production. According to the technical scheme, the top of an extraction tower is connected with an azeotropy tower through an extraction tower buffer tank, the bottom of the extraction tower is connected with an extraction tower kettle pump, and isopropanol is removed through the extraction tower; the top of the azeotropy tower is connected with an azeotropy tower return tank through an azeotropy tower condenser, and the bottom of the azeotropy tower is connected to a de-weight tower through an azeotropy tower kettle pump; the top of the de-weight tower is connected with a de-weight tower return tank through a de-weight tower condenser, the upper portion of the de-weight tower is connected to a refining tower through a pipeline, and a de-weight tower kettle pump is installed at the bottom of the de-weight tower; the top of the refining tower is connected with a refining tower return tank through a refining tower condenser, and the product diisopropylether is obtained through a tower kettle. The method has the advantages that the problem that the by-product diisopropylether is hard to purify and poor in quality during isopropanol production is solved, a continuous production process is adopted, and the defects of cumbersome operation and high energy consumption are overcome.
Description
Technical field
The present invention relates to a kind of chemical industry process for refining and purifying, particularly to a kind of method of the refined purifying plant of by-product diisopropyl ether in isopropanol produces.
Background technology
Diisopropyl ether is important industrial chemicals, is widely used in the industry such as chemical industry and medicine as organic solvent and synthesis material.From the by-product producing isopropanol, separating-purifying diisopropyl ether is a kind of traditional method producing diisopropyl ether.
Isopropanol by-product thick diisopropyl ether complicated components, possibly together with several isomerss and other heavy constituent impurity of C6 alkene in addition to water, isopropanol.Water, isopropanol and diisopropyl ether azeotropic, several isomers boiling points of C6 alkene and diisopropyl ether boiling point are close, differ about 1 DEG C, and the refined purification making diisopropyl ether is more difficult.What traditional method of purification was through rectification or pickling partition method obtains diisopropyl ether product, and owing in isopropanol device by-product, Component comparison is complicated, rectification separates relatively difficult, and poor product quality, yield are low；And pickling is very strong to the corrosion of equipment, environment is also had certain pollution, therefore actual production is seldom applied.
Summary of the invention
The purpose of the present invention is aiming at the drawbacks described above that prior art exists, a kind of method of the refined purifying plant of by-product diisopropyl ether in isopropanol produces is provided, the removing isopropanol combined through extraction process and azeotropic distillation technique produce in by-product diisopropyl ether in the impurity such as isopropanol, water, C6 alkene and n-butyl alcohol, removing difficult separation impurity in thick ether, diisopropyl ether product purity entirely reaches more than 99%.
A kind of method of the refined purifying plant of by-product diisopropyl ether in isopropanol produces that the present invention mentions, concrete steps include the following:
Step 1, thick diisopropyl ether extraction removing isopropanol:
Thick diisopropyl ether and demineralized water from raw material tank field are squeezed in extraction tower (1) respectively, demineralized water feeds from upper feed inlet, thick diisopropyl ether is from bottom throat-fed, the charge proportion controlling thick ether and demineralized water is 1:2, extracting operation is carried out under room temperature, tower top ether phase materials enters extraction tower surge tank (2) and stores, the tower reactor aqueous phase material containing isopropanol returns isopropanol refinement by extraction tower tower reactor pump (14) and reclaims isopropanol, and ether is entered in extraction tower surge tank (2) by tower top mutually；
Step 2, azeotropy rectification column:
Thick diisopropyl ether material after extraction is through azeotrope column feed pump (12), it is delivered in azeotrope column (3), entrainer is methanol, entering in azeotrope column (3) after mixing in the pipeline of input, control thick ether inlet amount 1000Kg/h, the inlet amount controlling entrainer methanol is 30 Kg/h, control this column overhead temperatures 69 DEG C, bottom temperature is at 76 DEG C, and tower top pressure 110 KPa, control of reflux ratio is 12；In the azeotrope column return tank (5) of tower top, material returns in azeotrope column (3) through azeotrope column reflux pump (15) part as backflow, and a part is delivered to entrainer recovery system and reclaims entrainer and isopropanol, and controlling load is 100 Kg/h；Materials at bottom of tower is delivered in diisopropyl ether weight-removing column (6), and controlling load is 930 Kg/h；
Step 3, the de-weight of diisopropyl ether:
Diisopropyl ether crude product in step 2 is removing heavy constituent in azeotrope column tower reactor pump (16) is delivered to weight-removing column (6), control this column overhead operation temperature: 71 DEG C, tower reactor operation temperature 85 DEG C, tower top operation pressure: 110KPa, control of reflux ratio: 7, the diisopropyl ether crude product that tower top obtains is in dehvery pump is delivered to treating column (9), control load is 870Kg/h, kettle material is mainly heavy constituent impurity n-butyl alcohol, being delivered in mixed alcohol storage tank take out as mixed alcohol through weight-removing column tower reactor pump (19), controlling load is 60 Kg/h；
Step 4, diisopropyl ether refines:
Diisopropyl ether crude product in step 3 enters in treating column (9), controls the tower top operation temperature for the treatment of column (9): 67 DEG C, tower reactor operation temperature 72 DEG C, tower top operates pressure: 105KPa, control of reflux ratio: 26；What tower top obtained returns in step 2 containing diisopropyl ether crude product, and it is 85 Kg/h that control tower ejects doses, and tower reactor obtains the purity diisopropyl ether product more than 99%, enters diisopropyl ether finished product tank field after cooling.
The invention has the beneficial effects as follows: the present invention successfully solves side-product diisopropyl ether product purification difficult, ropy problem during isopropanol produces, through having entirely reached more than 99% with the diisopropyl ether product purity after water extraction, addition entrainer azeotropic distillation, de-weight and refined purification, substantially increase device benefit.Meanwhile, use continuous production technology, solve complex operation, energy consumption high defect.
Accompanying drawing explanation
Accompanying drawing 1 is the structural representation of the present invention；
In figure: extraction tower 1, extraction tower surge tank 2, azeotrope column 3, azeotrope column condenser 4, azeotrope column return tank 5, weight-removing column 6, weight-removing column condenser 7, weight-removing column return tank 8, treating column 9, treating column condenser 10, treating column return tank 11, azeotrope column feed pump 12, azeotrope column reboiler 13, extraction tower tower reactor pump 14, azeotrope column reflux pump 15, azeotrope column tower reactor pump 16, weight-removing column reboiler 17, weight-removing column reflux pump 18, weight-removing column tower reactor pump 19, treating column reboiler 20, treating column reflux pump 21, treating column tower reactor pump 22.
Detailed description of the invention
A kind of refined purifying plant of by-product diisopropyl ether in isopropanol produces that the present invention mentions, including extraction tower 1, extraction tower surge tank 2, azeotrope column 3, azeotrope column condenser 4, azeotrope column return tank 5, weight-removing column 6, weight-removing column condenser 7, weight-removing column return tank 8, treating column 9, treating column condenser 10, treating column return tank 11, the top of described extraction tower 1 connects azeotrope column 3 by extraction tower surge tank 2, bottom connects extraction tower tower reactor pump 14, removes isopropanol by extraction tower 1；Described azeotrope column 3 top connects azeotrope column return tank 5 by azeotrope column condenser 4, and the bottom of azeotrope column 3 is connected to weight-removing column 6 by azeotrope column tower reactor pump 16, and the thick diisopropyl ether still liquid that azeotrope column tower reactor obtains enters weight-removing column 6；The top of described weight-removing column 6 connects weight-removing column return tank 8 by weight-removing column condenser 7, and the top of weight-removing column 6 is connected to treating column 9 by pipeline, and weight-removing column tower reactor pump 19 is installed in the bottom of weight-removing column 6, and what tower top obtained enters treating column 9 containing diisopropyl ether crude product；The top of described treating column 9 connects treating column return tank 11 by treating column condenser 10, the purity that tower reactor the obtains diisopropyl ether product higher than 99%, enters diisopropyl ether finished product tank field after cooling.
The bottom of above-mentioned azeotrope column 3 is provided with azeotrope column reboiler 13, and the bottom of weight-removing column 6 is provided with weight-removing column reboiler 17, and the bottom for the treatment of column 9 is provided with treating column reboiler 20.
The bottom of above-mentioned treating column 9 is provided with treating column tower reactor pump 22.
Above-mentioned extraction tower 1 is packed tower, built-in 250Y wire packing, and the number of plates is 30 pieces, plays the purpose of isopropanol in strengthening mass transfer, the multitple extraction thick diisopropyl ether of separation；Extraction tower material uses 304 rustless steels.
Above-mentioned azeotrope column 3 is mainly made up of rectifying section and stripping section, and using plate number is 65 pieces, and feed entrance point is at the 35th block of plate, and equipment body material is 304 rustless steels.
Above-mentioned weight-removing column 6 uses tray structure, plate number to be 45 pieces, and feed entrance point is 304 rustless steels in the 20th block of plate, equipment body material, and tower internals is 304 rustless steels.
Above-mentioned treating column 9 uses filling-material structure, has 70 blocks of plates, and feed entrance point is 304 rustless steels in the 30th block of plate, equipment body material, and inner-tower filling material is 700Y type wire packing.
A kind of method of the refined purifying plant of by-product diisopropyl ether in isopropanol produces that the present invention mentions, concrete steps include the following:
Step 1, thick diisopropyl ether extraction removing isopropanol:
Thick diisopropyl ether and demineralized water from raw material tank field are squeezed in extraction tower 1 respectively, demineralized water feeds from upper feed inlet, thick diisopropyl ether is from bottom throat-fed, the charge proportion controlling thick ether and demineralized water is 1:2, extracting operation is carried out under room temperature, tower top ether phase materials enters extraction tower surge tank 2 and stores, and the tower reactor aqueous phase material containing isopropanol returns isopropanol refinement by extraction tower tower reactor pump 14 and reclaims isopropanol, and ether is entered in extraction tower surge tank 2 by tower top mutually；
Step 2, azeotropy rectification column:
Thick diisopropyl ether material after extraction is through azeotrope column feed pump 12, it is delivered in azeotrope column 3, entrainer is methanol, entering in azeotrope column 3 after mixing in the pipeline of input, control thick diisopropyl ether inlet amount 1000Kg/h, the inlet amount controlling entrainer methanol is 30 Kg/h, control this column overhead temperatures 69 DEG C, bottom temperature is at 76 DEG C, and tower top pressure 110 KPa, control of reflux ratio is 12；In the azeotrope column return tank 5 of tower top, material returns in azeotrope column 3 through azeotrope column reflux pump 15 part as backflow, and a part is delivered to entrainer recovery system and reclaims entrainer and isopropanol, and controlling load is about 100 Kg/h；Materials at bottom of tower is delivered in diisopropyl ether weight-removing column 6, and controlling load is about 930 Kg/h；
Controlling consumption is C6 olefin(e) centent in thick diisopropyl ether 50%～the 150% of entrainer, control tower top temperature 60 C～80 DEG C, control bottom temperature 80 DEG C～100 DEG C, tower top pressure is 80-200 KPa.
Step 3, the de-weight of diisopropyl ether:
Diisopropyl ether crude product in step 2 is delivered in weight-removing column 6 remove heavy constituent through azeotrope column tower reactor pump 16, control this column overhead operation temperature: 71 DEG C, tower reactor operation temperature 85 DEG C, tower top operation pressure: 110KPa, control of reflux ratio: 7, the diisopropyl ether crude product that tower top obtains is in dehvery pump is delivered to treating column 9, control load is 870Kg/h, kettle material is mainly heavy constituent impurity n-butyl alcohol, being delivered in mixed alcohol storage tank take out as mixed alcohol through weight-removing column tower reactor pump 19, controlling load is 60 Kg/h；
Step 4, diisopropyl ether refines:
Diisopropyl ether crude product in step 3 enters in treating column 9, controls the tower top operation temperature for the treatment of column 9: 67 DEG C, tower reactor operation temperature 72 DEG C, tower top operates pressure: 105KPa, control of reflux ratio: 26；What tower top obtained returns in step 2 containing diisopropyl ether crude product, and it is 85 Kg/h that control tower ejects doses, and tower reactor obtains the purity diisopropyl ether product more than 99%, enters diisopropyl ether finished product tank field after cooling.
Claims (1)
1. a method for the refined purifying plant of by-product diisopropyl ether in isopropanol produces, is characterized in that concrete steps include the following:
Step 1, thick diisopropyl ether extraction removing isopropanol:
Thick diisopropyl ether and demineralized water from raw material tank field are squeezed in extraction tower (1) respectively, demineralized water feeds from upper feed inlet, thick diisopropyl ether is from bottom throat-fed, the charge proportion controlling thick ether and demineralized water is 1:2, extracting operation is carried out under room temperature, tower top ether phase materials enters extraction tower surge tank (2) and stores, the tower reactor aqueous phase material containing isopropanol returns isopropanol refinement by extraction tower tower reactor pump (14) and reclaims isopropanol, and ether is entered in extraction tower surge tank (2) by tower top mutually；
Step 2, azeotropy rectification column:
Thick diisopropyl ether material after extraction is through azeotrope column feed pump (12), it is delivered in azeotrope column (3), entrainer is methanol, entering in azeotrope column (3) after mixing in the pipeline of input, control thick ether inlet amount 1000Kg/h, the inlet amount controlling entrainer methanol is 30 Kg/h, control this column overhead temperatures 69 DEG C, bottom temperature is at 76 DEG C, and tower top pressure 110 KPa, control of reflux ratio is 12；In the azeotrope column return tank (5) of tower top, material returns in azeotrope column (3) through azeotrope column reflux pump (15) part as backflow, and a part is delivered to entrainer recovery system and reclaims entrainer and isopropanol, and controlling load is 100
Kg/h；Materials at bottom of tower is delivered in diisopropyl ether weight-removing column (6), and controlling load is 930
Kg/h；
Step 3, the de-weight of diisopropyl ether:
Diisopropyl ether crude product in step 2 is removing heavy constituent in azeotrope column tower reactor pump (16) is delivered to weight-removing column (6), control this column overhead operation temperature: 71 DEG C, tower reactor operation temperature 85 DEG C, tower top operation pressure: 110KPa, control of reflux ratio: 7, the diisopropyl ether crude product that tower top obtains is in dehvery pump is delivered to treating column (9), control load is 870Kg/h, kettle material is mainly heavy constituent impurity n-butyl alcohol, being delivered in mixed alcohol storage tank take out as mixed alcohol through weight-removing column tower reactor pump (19), controlling load is 60 Kg/h；
Step 4, diisopropyl ether refines:
Diisopropyl ether crude product in step 3 enters in treating column (9), controls the tower top operation temperature for the treatment of column (9): 67 DEG C, tower reactor operation temperature 72 DEG C, tower top operates pressure: 105KPa, control of reflux ratio: 26；What tower top obtained returns in step 2 containing diisopropyl ether crude product, and it is 85 Kg/h that control tower ejects doses, and tower reactor obtains the purity diisopropyl ether product more than 99%, enters diisopropyl ether finished product tank field after cooling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610425351.6A CN105906488B (en) | 2014-08-06 | 2014-08-06 | A kind of purification purifying plant for by-product diisopropyl ether in isopropyl alcohol production |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610425351.6A CN105906488B (en) | 2014-08-06 | 2014-08-06 | A kind of purification purifying plant for by-product diisopropyl ether in isopropyl alcohol production |
| CN201410383277.7A CN104177234B (en) | 2014-08-06 | 2014-08-06 | The refined purifying plant of a kind of by-product diisopropyl ether in isopropanol produces and method |
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| CN201410383277.7A Division CN104177234B (en) | 2014-08-06 | 2014-08-06 | The refined purifying plant of a kind of by-product diisopropyl ether in isopropanol produces and method |
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| CN105906488A true CN105906488A (en) | 2016-08-31 |
| CN105906488B CN105906488B (en) | 2019-11-15 |
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| CN201410383277.7A Active CN104177234B (en) | 2014-08-06 | 2014-08-06 | The refined purifying plant of a kind of by-product diisopropyl ether in isopropanol produces and method |
| CN201610425351.6A Active CN105906488B (en) | 2014-08-06 | 2014-08-06 | A kind of purification purifying plant for by-product diisopropyl ether in isopropyl alcohol production |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115353442A (en) * | 2022-09-23 | 2022-11-18 | 青岛科技大学 | Control method for separating isopropanol/diisopropyl ether/water azeotrope by azeotropic distillation |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633597A (en) * | 2012-03-22 | 2012-08-15 | 河北工业大学 | Process of recovering ethanol, propyl alcohol and isobutyl alcohol from polyalcohol-water mixture |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4510022A (en) * | 1983-08-08 | 1985-04-09 | Lloyd Berg | Separation of isopropyl ether from isopropanol and water by extractive distillation |
| CN1045001C (en) * | 1996-06-07 | 1999-09-08 | 南开大学新技术集团公司丹阳分厂 | Prodn. tech for isopropyl ether |
| IT1290449B1 (en) * | 1997-04-02 | 1998-12-03 | Snam Progetti | PROCEDURE FOR THE PRODUCTION OF ALCOHOL ETHERS |
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2014
- 2014-08-06 CN CN201410383277.7A patent/CN104177234B/en active Active
- 2014-08-06 CN CN201610425351.6A patent/CN105906488B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633597A (en) * | 2012-03-22 | 2012-08-15 | 河北工业大学 | Process of recovering ethanol, propyl alcohol and isobutyl alcohol from polyalcohol-water mixture |
Non-Patent Citations (1)
| Title |
|---|
| 宋世晶等: ""异丙醇装置副产二异丙醚精制过程模拟研究"", 《山东化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115353442A (en) * | 2022-09-23 | 2022-11-18 | 青岛科技大学 | Control method for separating isopropanol/diisopropyl ether/water azeotrope by azeotropic distillation |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104177234B (en) | 2016-08-17 |
| CN105906488B (en) | 2019-11-15 |
| CN104177234A (en) | 2014-12-03 |
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