CN1230131A - Electrostatic coalescence - Google Patents
Electrostatic coalescence Download PDFInfo
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- CN1230131A CN1230131A CN97197802A CN97197802A CN1230131A CN 1230131 A CN1230131 A CN 1230131A CN 97197802 A CN97197802 A CN 97197802A CN 97197802 A CN97197802 A CN 97197802A CN 1230131 A CN1230131 A CN 1230131A
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- dispersion
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/06—Separation of liquids from each other by electricity
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- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Water Treatment By Electricity Or Magnetism (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Electrostatic Separation (AREA)
- Colloid Chemistry (AREA)
- Other In-Based Heterocyclic Compounds (AREA)
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- Developing Agents For Electrophotography (AREA)
Abstract
Method for segregating a dispersion having a continuous organic phase and a disperse aqueous phase from a caprolactam production process, wherein electrostatic coalescence is applied to the dispersion at an electric field of at least 500 volts per centimetre and a frequency of at least 5 Hz, whereby the formation of a separate aqueous layer is induced.
Description
Background of invention
The present invention relates to a kind of method that has continuous organic facies in the caprolactam production process and disperse the dispersion of water of separating.
Prior art is discussed
In the production process of caprolactam, caprolactam prepares through Beckmann rearrangement in the presence of sulfuric acid or oleum by cyclohexanone oxime.Use in the ammonia then and neutralized rearrangement mixture, thereby formed ammonium sulfate.After this, extract caprolactam with organic solvent such as benzene.In resulting organic facies, also exist and disperse water.This water also has ammonium sulfate except that comprising caprolactam.The existence of ammonium sulfate is unfavorable for the subsequent treatment and the purification of caprolactam.Therefore be starved of the water of deviating from this dispersion as much as possible.
There are many processes to separate to dispersion.
Available subsider separates the enough big dispersion of two-phase density contrast.Than heavy phase fall to light mutually under, and have when enough the chien shih two-phase fully separate and extract out.But such method need be used very huge settling tank, and occupies quite big quantity space.In addition, this separation method can become fairly large the slowest stage in the production process of acyl ammonium in oneself, and has therefore determined the production capacity of overall process.
Another kind may be to adopt coalescer or method for treating water to remove decentralized photo, as German patent application 1,031, described in 308.In the production process of this caprolactam, add the alkaline washing material and be the quality that is unfavorable for caprolactam.
U.S. Pat P3,528,907 have introduced the method that adopts electric field is dispersed in the water in hydro carbons such as the crude oil from described oil possibility.But this piece patent is also mentioned, and the voltage that electric field applied must not surpass 1000 volts of per inch certainly, maybe must not surpass 400 volts every centimetre, otherwise can cause interelectrode short circuit.Particularly, the shortcoming of this method is, to only containing the decentralized photo of the water that accounts for total binding liquid phase 5% at the most, is difficult for separating from organic facies.
European patent application No.51463 has described employing electrostatic coalescence method sedimentation emulsion.But this method needs cubical content big as account for 50% conducting liquid (water) and exist.Especially need insulating electrode, otherwise will be short-circuited.
German patent application No.3,709,456 and european patent application 438790 all to have introduced water be the fluid film piece-rate system of continuous phase.
Generally, dispersion all is shown as the continuous distribution of granularity.Dispersion can be divided into once and the secondary dispersion.For a dispersion, the average particle size that forms decentralized photo is＞0.1mm.Under many situations, these dispersions are easy to be separated by gravity in settling tank.But for the secondary dispersion, the particle mean size that forms dispersion particle all only＜＜0.1mm.Yet, adopt the method for settling tank to separate a kind of dispersion in back, the time that commercial Application needs is oversize, can not be satisfactory.Therefore for shortening this disengaging time, adopt according to electrostatic coalescence method of the present invention be possible and favourable.
Summary of the invention
Main purpose of the present invention is, a kind of method that can very effectively be separated in the dispersion in the caprolactam production process is provided, and especially separates the dispersion that wherein only contains the water of about 5% (weight) at the most.
By employing be in application to less every centimetre of 500 volts of voltages and at least the electrostatic coalescence method in the electric field of 5Hz frequency reach this purpose.With the electric field of every centimetre at least 1000 volt (peak value) intensity, preferably at least 3000 volts every centimetre, more preferably every centimetre at least 5000 is lied prostrate, and especially every centimetre at least 10,000 volt, also can advantageously use, and do like this, the separating effect that is reached can be become better and better.No matter whether adopt high like this electric field, do not have short circuit to take place so far, and water phase separated and oil phase are also very effective.For example, it is found that, in organic liquid phase, behind following 10 minutes of frequency 50Hz and 733 volts/centimetre, 50% aqueous dispersion phase of separable existence.After under 6666 volts every centimetre 10 minutes, the water of existence with regard to separable 90%.Adopt settling tank then to need several days and even time in a week, just can reach such effect.
Adopt electrostatic coalescence, also obviously may change frequency, as long as frequency is at least 20Hz, can reach good effect according to the present invention.The frequency height also can be used very goodly to 500Hz.Frequency exceeds preferable range, also can obtain good effect.
The accompanying drawing summary
Fig. 1 schematic construction ground illustrates a kind of device type of the present invention that can be used for implementing.
Explanation another kind in Fig. 2 schematic construction ground can be used for implementing device type of the present invention.
Detailed Description Of The Invention
The shape of carrying out the container of electrostatic coalescence or vessel is not too important. Container can be cylindrical shape, square or rectangle etc.
Electrostatic coalescence technology of the present invention can be carried out continuously or off and on. But, when carrying out continuous electrostatic coalescence, need the careful inner surface structure of paying close attention to container or vessel, to guarantee to form laminar flow; Draw ratio is important just for this reason. Particularly, should avoid turbulent flow, because such turbulent flow is harmful to separating, or owing to exist this situation can affect the separation required time.
The electrode that can use can be with various material preparations, such as electro-conductive glass, metal etc. The electrode used therein shape is not main to the present invention. Embodiment comprises rod or plate shape electrode. These electrodes can be insulation or uninsulated. Use uninsulated electrode, it is contemplated that to cause low cost. But, because safety and energy consumption can be selected insulating electrode in addition.
By the temperature that electrostatic coalescence separates, in fact neither be basic to the present invention, and preferably can be room temperature.Although general higher temperature helps finishing sooner the separation process of phase, need prevent that generally temperature from rising too high, otherwise separated dispersion can come to life, or cause generating gas, thereby cause turbulent flow and form dispersion again again.
Certainly under elevated pressures, electrostatic coalescence is also always possible, can prevent the dispersion boiling like this.
The two all can use alternating current and direct current.When adopting alternating current, its pulse or can be sinusoidal waveform or rectangle, zigzag, or its combined waveform, they have only distant influence for separating effect.
The term " organic facies " that is used for this patent refers to a kind of or several organic compounds of being made up of carbon and hydrogen, for example straight chain and hydro carbons ring-type, and also they also can contain other atom such as oxygen, sulphur, nitrogen, halogen etc.The embodiment of these compounds comprises benzene, toluene, cyclohexane, heptane, dimethyl sulfoxide (DMSO), chloroform and trichloroethanes etc.
Outside dewatering, water also can contain other compound, for example salt or even the organic compound that is soluble in the aqueous phase.Water even can contain the heavy organic compound of as many as 60%, for example caprolactam.However, in text of the present invention, if when water content at least 20% is heavy, " water " just is considered to moisture.
Water also can contain water soluble salt, for example at the heavy ammonium sulfate of 0.1-5%.
Separated aqueous dispersion phase adopts obvious method well known to those skilled in the art at present, all can make it to separate with organic continuous phase, for example adopts methods such as extracting aqueous layer, decant out.Also separated water may be circulated in the caprolactam production process.
The preparation of caprolactam relates to the various preparation processes that wherein form such dispersion.The technology that general these steps all need effective liquid/liquid to separate.Embodiment in each processing step comprises oxidation, the hydroxyl amine salt preparation of cyclohexane and from top and bottoms that extraction tower comes out.
Inventive embodiments
Accompanying drawing describes in detail
Referring now to following embodiment the present invention is more at large illustrated, and therefore the present invention is not constituted any restriction.
Embodiment
Adopt a kind of Ultra-Torrax7 T50 blender, change the rotating speed of (rpm) with per minute 5000, use accounts for the water dispersant of mixture total weight amount 2%, in 5 minutes, the caprolactam of water-soluble (50%) is scattered in the benzene as organic facies (reaching 50% weight).In 1 minute, this dispersion is introduced in the electrostatic coalescer, and follows setpoint frequency and voltage.These embodiment use alternating current in each case, and at room temperature finish.
The coalescer that is used for embodiment I-III is by Fig. 1 illustrative in addition, and wherein 1 is the insulating glass electrode, and 2 glass jacket that sulfuric acid 3 are housed in being are as external electrode, and 4 for having the voltage source of frequency regulator.Gap between electrode 1 and 3 is 1.5cm.
Coalescer used in embodiment IV and V is illustrated with Fig. 2.Wherein 10 is thermostatic container, lays a glass container 20 in it, (100:30:100mm), is sealed with lid 30 again, passes this lid and settles two uninsulated stainless steel electrodes 40.Electrode gap is 1.5cm.Take the sample of dispersion at interval according to different time, and analyzed.
These tests are at room temperature carried out.Separated for defining how much water, or determine aqueous-phase concentration in dispersion, according to DIN method (" Deutsche Einheitsverfahren ") C2, DIN38404, the 2nd joint determination of test method turbidity, this also is a kind of yardstick of the percentage of water phase separated.With the related turbidity of calibration curve with divided dried up percentage.
The embodiment I is to III
Embodiment I to III is carried out according to above-mentioned formality.Frequency is 50Hz.Electric field is sine-shaped.Voltage changes, and is shown in the table I, and comprises corresponding separating resulting.
The table I
| Embodiment | Voltage, volt/cm | Separate weight % after 1 minute | Separate weight % after 5 minutes | Separate weight % after 10 minutes |
| ????Ⅰ | ????733 | ????15 | ????40 | ????51 |
| ????Ⅱ | ????3333 | ????42 | ????68 | ????80 |
| ????Ⅲ | ????6666 | ????60 | ????88 | ????90 |
The table I clearlys show that voltage is high more, and separating effect is good more, and complete more.
Embodiment IV and V
These embodiment carry out according to above-mentioned formality.Frequency is 50hz, and voltage changes.The voltage electric field is sine-shaped.The results are shown in the table II.
The table II
| Embodiment | Voltage, volt/cm | Separate weight % after 1 minute | Separate weight % after 5 minutes | Separate weight % after 10 minutes |
| ????Ⅳ | ????733 | ????48 | ????70 | ????73 |
| ????Ⅴ | ????2067 | ????62 | ????91 | ????92 |
Reference examples A
The dispersion sample of certain embodiment is introduced in the cylindrical vessel, makes it does not using sedimentation under the electrostatic coalescence condition.After 1 minute, have only 6% water-bearing layer separation, its quantity has only 12% after reaching 9%, 10 minute after 5 minutes.
The present invention now is illustrated by the reference specific embodiment, but according to the applicable patent method, the scope of right and degree only are subjected to the term restriction of following claim item.
Claims (11)
1, a kind of method that has continuous organic facies in the caprolactam production process and disperse the dispersion of water of separating, it is characterized in that, this dispersion is used electrostatic coalescence, electric field is every centimetre of 500 volts of (V) voltage and frequency at least 5 He Zhi (Hz) at least, forms the aqueous layer that separates thereby induce.
2,, it is characterized in that adopting the electric field of every centimetre of 1000 volts of voltages at least according to the method for claim 1.
3,, it is characterized in that adopting the electric field of every centimetre of 5000 volts of voltages at least according to the method for claim 2.
4,, it is characterized in that adopting the electric field of every centimetre of 10,000 volts of voltages at least according to the method for claim 3.
5,, it is characterized in that frequency is 20Hz at least according to each method of claim 1-4.
6,, it is characterized in that frequency is 500Hz at the most according to the method for claim 5.
7,, it is characterized in that water quantity is at most total liquid phase 5% weight of combination according to each method of claim 1-6.
8, according to each method of claim 1-7, it is characterized in that organic facies is a benzene.
9, according to each method of claim 1-8, it is characterized in that decentralized photo is a water.
10,, it is characterized in that decentralized photo comprises the caprolactam that 60% weight is following according to the method for claim 9.
11,, it is characterized in that decentralized photo comprises the ammonium sulfate that 0.1-5% is heavy according to the method for claim 9.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| NL1003591A NL1003591C2 (en) | 1996-07-15 | 1996-07-15 | Electrostatic coalescence. |
| NL1003591 | 1996-07-15 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1230131A true CN1230131A (en) | 1999-09-29 |
Family
ID=19763204
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97197802A Pending CN1230131A (en) | 1996-07-15 | 1997-07-08 | Electrostatic coalescence |
Country Status (17)
| Country | Link |
|---|---|
| EP (1) | EP0920349A1 (en) |
| JP (1) | JP2000514352A (en) |
| KR (1) | KR20000023771A (en) |
| CN (1) | CN1230131A (en) |
| AU (1) | AU3361597A (en) |
| BG (1) | BG103086A (en) |
| CA (1) | CA2260248A1 (en) |
| CO (1) | CO4790158A1 (en) |
| CZ (1) | CZ13899A3 (en) |
| EA (1) | EA199900105A1 (en) |
| GE (1) | GEP20002017B (en) |
| ID (1) | ID18566A (en) |
| NL (1) | NL1003591C2 (en) |
| PL (1) | PL331170A1 (en) |
| SK (1) | SK5099A3 (en) |
| TW (1) | TW374083B (en) |
| WO (1) | WO1998002225A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100339146C (en) * | 2001-11-07 | 2007-09-26 | 艾贝尔公司 | Electrostatic coalescer device and use of the device |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NO20044265L (en) * | 2004-10-08 | 2006-04-10 | Sintef Energiforskning As | Method of electrocoalescence of emulations and apparatus for carrying out the method |
| JP5034485B2 (en) * | 2006-12-20 | 2012-09-26 | ダイキン工業株式会社 | Refrigeration equipment |
| KR101425412B1 (en) | 2013-01-17 | 2014-08-01 | 한국기계연구원 | Combined separation system to separate dispersed water droplets in emulsions of continuous phase materials |
| KR101453500B1 (en) | 2013-01-17 | 2014-10-23 | 한국기계연구원 | Electrostatic coagulation apparatus for growth of water droplets in water-dispersed emulsions |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4415426A (en) * | 1980-09-30 | 1983-11-15 | Exxon Research And Engineering Co. | Electrodes for electrical coalescense of liquid emulsions |
| DE3176445D1 (en) * | 1980-11-01 | 1987-10-22 | Univ Bradford | Settling of liquid dispersions |
| US4409078A (en) * | 1981-04-20 | 1983-10-11 | Exxon Research And Engineering Co. | Methods and apparatus for electrostatically resolving emulsions |
| DE3709456A1 (en) * | 1987-03-23 | 1988-10-06 | Univ Hannover | Process and apparatus for breaking liquid membrane emulsions from metal extraction processes |
| US5326441A (en) * | 1990-01-19 | 1994-07-05 | European Economic Community | Process for separating and concentrating gallium from an aqueous solution containing gallium, together with aluminum, zinc and copper |
-
1996
- 1996-07-15 NL NL1003591A patent/NL1003591C2/en not_active IP Right Cessation
-
1997
- 1997-07-08 EA EA199900105A patent/EA199900105A1/en unknown
- 1997-07-08 CN CN97197802A patent/CN1230131A/en active Pending
- 1997-07-08 AU AU33615/97A patent/AU3361597A/en not_active Abandoned
- 1997-07-08 CZ CZ99138A patent/CZ13899A3/en unknown
- 1997-07-08 SK SK50-99A patent/SK5099A3/en unknown
- 1997-07-08 JP JP10505871A patent/JP2000514352A/en active Pending
- 1997-07-08 CA CA002260248A patent/CA2260248A1/en not_active Abandoned
- 1997-07-08 EP EP97929593A patent/EP0920349A1/en not_active Withdrawn
- 1997-07-08 GE GEAP19974636A patent/GEP20002017B/en unknown
- 1997-07-08 PL PL97331170A patent/PL331170A1/en unknown
- 1997-07-08 WO PCT/NL1997/000396 patent/WO1998002225A1/en not_active Application Discontinuation
- 1997-07-09 CO CO97038166A patent/CO4790158A1/en unknown
- 1997-07-15 ID IDP972450A patent/ID18566A/en unknown
- 1997-08-01 TW TW086111028A patent/TW374083B/en active
-
1999
- 1999-01-14 KR KR1019997000241A patent/KR20000023771A/en not_active Application Discontinuation
- 1999-01-15 BG BG103086A patent/BG103086A/en unknown
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100339146C (en) * | 2001-11-07 | 2007-09-26 | 艾贝尔公司 | Electrostatic coalescer device and use of the device |
Also Published As
| Publication number | Publication date |
|---|---|
| KR20000023771A (en) | 2000-04-25 |
| BG103086A (en) | 1999-08-31 |
| CZ13899A3 (en) | 1999-08-11 |
| PL331170A1 (en) | 1999-06-21 |
| ID18566A (en) | 1998-04-23 |
| AU3361597A (en) | 1998-02-09 |
| EP0920349A1 (en) | 1999-06-09 |
| GEP20002017B (en) | 2000-04-10 |
| SK5099A3 (en) | 1999-05-07 |
| JP2000514352A (en) | 2000-10-31 |
| WO1998002225A1 (en) | 1998-01-22 |
| EA199900105A1 (en) | 1999-06-24 |
| TW374083B (en) | 1999-11-11 |
| CA2260248A1 (en) | 1998-01-22 |
| CO4790158A1 (en) | 1999-05-31 |
| NL1003591C2 (en) | 1998-01-21 |
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