CN104230658A - New method for separating ethanediol and 1, 2-pentanediol from corn fermentation liquid - Google Patents
New method for separating ethanediol and 1, 2-pentanediol from corn fermentation liquid Download PDFInfo
- Publication number
- CN104230658A CN104230658A CN201410497334.4A CN201410497334A CN104230658A CN 104230658 A CN104230658 A CN 104230658A CN 201410497334 A CN201410497334 A CN 201410497334A CN 104230658 A CN104230658 A CN 104230658A
- Authority
- CN
- China
- Prior art keywords
- ethylene glycol
- pentanediol
- entrainer
- extraction
- tower
- 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.)
- Pending
Links
Classifications
-
- 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
- C07C29/82—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by azeotropic distillation
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a new method for separating ethanediol and 1, 2-pentanediol from corn fermentation liquid through azeotropic distillation. According to the new method, through ASPEN modeling simulation, a proper entrainer and a proper extractant are selected and distillation and extraction conditions are initially identified; a liquid polyol mixture and the entrainer enter a distillation tower, a mixture of the ethanediol and the entrainer is obtained at the top of the tower, and the 1, 2-pentanediol with the content higher than 99.5% can be obtained in the kettle of the tower; the extractant is insoluble in the entrainer, but the extractant and ethanediol can be dissolved with each other; mixed liquid of the extractant and the ethanediol can be separated by an ordinary distillation method; the content of the ethanediol is higher than 99.5%; the entrainer and the extractant can be recycled. The new method is easy to operate; by the new method, the ethanediol and the 1, 2-pentanediol with high purity can be obtained.
Description
Technical field
The present invention relates to and a kind ofly utilize the method for azeotropic distillation separating ethylene glycol and 1,2-pentanediol from corn fermentation treatment solution, obtain the novel method of ethylene glycol product and 1,2-pentanediol, belong to the separation engineering field in chemical engineering.
Background technology
In recent years, the development of world economy and the raising of people's environmental protection consciousness impelled the reproducible biomass resource of exploitation to become study hotspot.Traditional polyvalent alcohol raw materials multi-source is in fossil resources such as oil.Corn is utilized to prepare polyvalent alcohol as ethylene glycol, 1; 2-pentanediol belongs to emerging technology; not only can in the energy petroleum replacing matter polyvalent alcohol; alleviate the crisis that oil is day by day in short supply; but also numerous chemical or chemical intermediate can be synthesized, play an important role in environment protection and overcoming in energy dilemma.
Biological fermentation treatment solution separating multicomponent alcohol is promising, is the production technique of necessity of following chemical industry, both at home and abroad also in the project of Gong the suitability for industrialized production of the similar energy cycling and reutilization of research.Corn fermentation liquid can obtain the mixture of ethylene glycol and 1,2-pentanediol through the thick product of dehydration, cracking and initial gross separation, and wherein ethylene glycol is for the production of vibrin, Synolac, softening agent, frostproofer, also for makeup and explosive; As analytical reagent, stratographic analysis reagent and capacitor dielectric; Also can be used for producing synthetic resins, solvent, lubricant, tensio-active agent, tenderizer, moistening agent, explosive etc.; And 1,2-pentanediol also has higher economic worth.Therefore this processing method, has important economic worth and realistic meaning.
This raw material derives from corn fermentation treatment solution, and containing ethylene glycol, 1,2-pentanediol etc., but both ethylene glycol and 1,2-pentanediol boiling point is very near, and very difficult ordinary method is isolated.
The isolated ethylene glycol of the method and 1,2-pentanediol have important economic worth and realistic meaning.The domestic demand for ethylene glycol and 1,2-pentanediol is very big at present, and import most, works out the route of a separating-purifying ethylene glycol and 1,2-pentanediol, has a extensive future
.
Summary of the invention
The object of the present invention is to provide a kind of novel method utilizing the method for homogeneous phase azeotropic distillation separating ethylene glycol and 1,2-pentanediol from corn fermentation treatment solution.
The present invention realizes by the following method: adopt azeotropic distillation, select suitable entrainer to come to be separated ethylene glycol and 1,2-pentanediol.To azeotropic distillation, can select to be rich in entrainer backflow or entrainer and form with certain azeotropic with stock blend and reflux, so the working pressure of reflux ratio and tower affects liquid phase in tower to a great extent and to distribute and tower top, each concentration of component at the bottom of tower change.By the adjustment to homogeneous phase azeotropic distillation reflux ratio and tower working pressure, desirable separating effect can be obtained.Homogeneous phase azeotropic distillation equipment is simple, and can be separated multicomponent mixture by single tower, highly versatile, can regulate reflux ratio flexibly, has the advantages such as very large turndown ratio.
The present invention have chosen suitable entrainer, is tentatively determined azeotrope composition, azeotropic temperature and the separation sequence of testing system by ASPENPLUS.Azeotropy rectification column is by following conditional operation, and under normal or reduced pressure, entrainer and mixture send into rectifying tower, and operating reflux ratio is 10-30, by overhead extraction ethylene glycol and the entrainer of rectifying tower, and 1, the 2-pentanediol product that extraction at the bottom of tower is qualified.Because entrainer and ethylene glycol dissolve each other define homogeneous phase solution, so also need further separation and azeotropic liquid.Need to add another kind of extraction agent the two to be separated.Extraction agent is insoluble to entrainer and but can dissolves each other with ethylene glycol, uses extraction agent can realize the separation of azeotrope.Extraction agent can be separated by the method for conventional distillation with the mixed solution of ethylene glycol, and ethylene glycol content reaches more than 99. 5%.And recycling use entrainer and extraction agent.This is simple to operate, can reach separation requirement.
Idiographic flow (see accompanying drawing 1,2): ethylene glycol-1,2-pentanediol-entrainer mixture enters in tower, and tower top azeotrope is after condenser condenses, and the extraction of partial reflux part, reflux ratio is 10-30, finally obtains 1,2-qualified pentanediol product at the bottom of tower.Overhead extraction liquid is azeotropic mixture, and make its layering by adding extraction agent, upper strata is entrainer, lower floor is ethylene glycol and extraction agent solution, or uses extraction tower to be separated, and extraction phase is ethylene glycol and extractant mixture, extracting phase is mainly entrainer, and entrainer can continue after reclaiming to use.Ethylene glycol after separation and the mixture of extraction agent carry out normal pressure or decompression operation in rectifying tower can realize effectively being separated of ethylene glycol and extraction agent, qualified ethylene glycol product can be obtained, and extraction agent can be made to recycle, the method good separating effect, product purity can reach the requirement of technical indicator.
The invention has the advantages that and adopt entrainer and ethylene glycol to form azeotrope, azeotrope and 1, the relative volatility of 2-pentanediol and boiling point differ larger, thus isolate high purity 1,2-pentanediol product, continues through extraction and distillation operation can obtain ethylene glycol product and reclaim entrainer and extraction agent.The present invention has highly versatile, and device operational stability is strong, the advantages such as treatment capacity is large.
The inventive method, by the restriction of above-mentioned concrete device, is carried out the adjustment of technical process or conversion according to this patent, is undertaken amplifying by treatment capacity, carries out the behavior that lab scale, pilot scale and suitability for industrialized production all belong to the infringement of patent according to this patent requirement.
Accompanying drawing explanation
Fig. 1 is azeotropic distillation cell process schema, and Fig. 2 is conventional distillation cell process schema.
Embodiment
Example one
Design, manufacture, azeotropy rectification column is installed and carries out periodical operation, raw material is ethylene glycol-1, the mixture (wherein containing ethylene glycol: 1,2-pentanediol: entrainer mass ratio is 2:1:7.5) of 2-pentanediol-entrainer, working pressure is set to 80kpa, and reflux ratio is 25.Tower top temperature is stabilized in about 150 DEG C, and bottom temperature changes to 179 DEG C by 170 DEG C.Tower top obtains the azeotropic liquid of ethylene glycol and entrainer.Batch fractionating operation obtains good separating effect, demonstrates the azeotropic liquid that the available rectifying tower of this experiment obtains ethylene glycol and entrainer.
Example two
In employing, routine equipment and operational condition carry out continuous rectification operation, from rectifier bottoms or middle part normal temperature charging.Tower top still can obtain azeotrope, after stablizing extraction, regulates reflux ratio, continues rectifying and make tower reactor obtain 1,2-pentanediol of high density under this condition, and, purity qualified through the rear product colour of 1,2-pentanediol rectifying tower separation reaches more than 99.5%.
Example three
Collect the tower top azeotrope of above-mentioned two examples, extract with extraction agent, form heterogeneous solution, upper strata is entrainer, and lower floor is the mixing solutions of ethylene glycol and extraction agent; Obtaining extracting phase with extraction tower separation is entrainer, and the concentration finally obtaining entrainer is 99.5%, and extraction phase goes extraction agent rectifying tower to be separated.Extraction phase is the mixing solutions of ethylene glycol and extraction agent, and being extracted agent through the separation of extraction agent rectifying tower can recycle, and the ethylene glycol crude product obtained obtains pure ethylene glycol product through ethylene glycol rectifying tower, and ethylene glycol purity is more than 99.5%.
Claims (6)
1. one kind utilizes the method for azeotropic distillation separating ethylene glycol and 1 from corn fermentation treatment solution, 2-pentanediol, obtain ethylene glycol product and 1, the novel method of 2-pentanediol product, step is as follows: polyvalent alcohol mixed solution enters in rectifying tower, the azeotropic liquid of overhead extraction ethylene glycol and entrainer, extraction purity at the bottom of tower reaches more than 99.5% 1,2-pentanediol product; The entrainer that azeotropic distillation column overhead obtains and ethylene glycol dissolve each other and define homogeneous phase solution, and adding another kind of extraction agent can separate the two.
2. azeotropic distillation column plate number is 60-150 block, working pressure normal pressure or decompression, tower top temperature controls at 120 ~ 160 DEG C, and bottom temperature remains on 130 ~ 180 DEG C, operating reflux ratio is under the azeotropic distillation condition of 10-30, can obtain good azeotropic distillation separating effect.
3. extraction agent is insoluble to entrainer and but can dissolves each other with ethylene glycol, is joined by extraction agent in azeotropic liquid, and make tower top azeotrope layering (or using extraction tower to realize being separated object), extracting phase is entrainer, can recycle; The extraction phase solution that ethylene glycol and extraction agent are formed can effectively realize being separated by normal pressure or rectification under vacuum, and can obtain purity and reach more than 99.5% ethylene glycol product, extraction agent also can recycle.
4., according to described in claims 1, the entrainer that the processing method of azeotropic distillation separating ethylene glycol and 1,2-pentanediol mixture uses is one or more in aromatic hydroxy compound, alkane compound, alcohols, ethers, ketone compounds.
5., according to described in claims 3, the extraction agent used is the one in benzene, methyl alcohol, ethanol, butanols, water, methyl ethyl ether, dme, sherwood oil and ketone compounds.
6. utilize the method for homogeneous phase azeotropic distillation separating ethylene glycol and 1 from corn fermentation treatment solution according to a kind of described in claim 1,2,3,2-pentanediol, obtain ethylene glycol product and 1, the novel method of 2-pentanediol product, it is characterized in that not patenting and utilizing the method to carry out lab scale, pilot scale and suitability for industrialized production all belongs to infringement act.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410497334.4A CN104230658A (en) | 2014-09-26 | 2014-09-26 | New method for separating ethanediol and 1, 2-pentanediol from corn fermentation liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410497334.4A CN104230658A (en) | 2014-09-26 | 2014-09-26 | New method for separating ethanediol and 1, 2-pentanediol from corn fermentation liquid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104230658A true CN104230658A (en) | 2014-12-24 |
Family
ID=52219674
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410497334.4A Pending CN104230658A (en) | 2014-09-26 | 2014-09-26 | New method for separating ethanediol and 1, 2-pentanediol from corn fermentation liquid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104230658A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110878007A (en) * | 2018-09-05 | 2020-03-13 | 长春美禾科技发展有限公司 | Refining method of non-petroleum-based ethylene glycol |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2150392A1 (en) * | 1995-05-29 | 1996-11-30 | Jurgen Mohr | Recovery of glycols from used glycol-containing technical fluids |
| CN103772148A (en) * | 2013-07-08 | 2014-05-07 | 吉林化工学院 | Novel method for separating mixture of ethylene glycol and 1, 2-butanediol by adopting azeotropic distillation and extraction coupling technologies |
-
2014
- 2014-09-26 CN CN201410497334.4A patent/CN104230658A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2150392A1 (en) * | 1995-05-29 | 1996-11-30 | Jurgen Mohr | Recovery of glycols from used glycol-containing technical fluids |
| CN103772148A (en) * | 2013-07-08 | 2014-05-07 | 吉林化工学院 | Novel method for separating mixture of ethylene glycol and 1, 2-butanediol by adopting azeotropic distillation and extraction coupling technologies |
Non-Patent Citations (1)
| Title |
|---|
| 鲍妮娜等: "生物基化工醇重组分中多元醇的分离提取", 《化工进展》, vol. 30, no. 5, 31 December 2011 (2011-12-31), pages 957 - 961 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110878007A (en) * | 2018-09-05 | 2020-03-13 | 长春美禾科技发展有限公司 | Refining method of non-petroleum-based ethylene glycol |
| JP2022503653A (en) * | 2018-09-05 | 2022-01-12 | チャンチュン メイヘ サイエンス アンド テクノロジー ディベロップメント カンパニー リミテッド | How to Purify Non-Petroleum Ethylene Glycol |
| CN110878007B (en) * | 2018-09-05 | 2023-04-28 | 长春美禾科技发展有限公司 | Refining method of non-petroleum ethylene glycol |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103772148A (en) | Novel method for separating mixture of ethylene glycol and 1, 2-butanediol by adopting azeotropic distillation and extraction coupling technologies | |
| CN103396290A (en) | Novel process for separating ethylene glycol and 1,2-butanediol | |
| CN106588579B (en) | A method of extracting phenolic compound from carbolic oil | |
| CN103435482B (en) | Separation method and separation device of synthesis gas ethylene glycol product | |
| CN106178571B (en) | Azeotrope separation process | |
| CN105330514B (en) | A kind of purifying technique of synthesis gas preparing ethylene glycol | |
| CN105503522A (en) | Recycling and refining device for methylbenzene-methyl alcohol/ethyl alcohol and separating method | |
| CN203923057U (en) | Improved Butanol Recycling device | |
| CN101700916B (en) | Process and system for treating industrial normal propyl alcohol waste liquor | |
| CN103215058A (en) | Method for extracting and separating light component from coal tar at low temperature | |
| CN105152882B (en) | Method for preparing DMM3-5 from hypercoagulable polyoxymethylene dimethyl ether component DMM6+ and dimethoxymethane DMM | |
| CN105218305B (en) | A kind of byproduct recovery process of synthesis gas preparing ethylene glycol | |
| CN105152860A (en) | Method for refining mixed alcohol by rectification-pervaporation coupling process | |
| CN102627556B (en) | Technology of extractive distillation separation of ethyl acetate-ethanol-water | |
| CN104370696A (en) | Novel method for separating ethylene glycol and 1,2-pentanediol | |
| CN106518618B (en) | A kind of method of mixed solvent continuous extraction rectifying separating isopropanol-isopropyl ether azeotropic mixture | |
| CN108484368A (en) | A method of phenolic compound being extracted from coal tar using ethanol amine | |
| CN104230658A (en) | New method for separating ethanediol and 1, 2-pentanediol from corn fermentation liquid | |
| CN101891589B (en) | Method for extracting fatty alcohols | |
| CN106966852B (en) | The method of continuous extraction rectifying separation high-carbon n-alkane and normal olefine | |
| CN102911139A (en) | Recovery and separation method for solvent containing tetrahydrofuran-carbinol system | |
| CN104591952A (en) | Method for refining mesitylene by virtue of differential pressure thermal coupling rectification | |
| CN106380403B (en) | The method for efficiently separating dimethyl oxalate and dimethyl carbonate | |
| CN104693005A (en) | New process for separating methanol-propyl formate azeotrope through extractive distillation | |
| CN104829426A (en) | Continuous isopropyl ether-isopropyl alcohol azeotrope extraction and rectification technology based on choline chloride/urea low-co-melting solvent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20141224 |