EP2035107A1 - Verfahren zur spaltung von öl/wasser-emulsionen und dessen steuerung - Google Patents
Verfahren zur spaltung von öl/wasser-emulsionen und dessen steuerungInfo
- Publication number
- EP2035107A1 EP2035107A1 EP07702641A EP07702641A EP2035107A1 EP 2035107 A1 EP2035107 A1 EP 2035107A1 EP 07702641 A EP07702641 A EP 07702641A EP 07702641 A EP07702641 A EP 07702641A EP 2035107 A1 EP2035107 A1 EP 2035107A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- emulsion
- turbidity
- breaker
- organic
- amount
- 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.)
- Withdrawn
Links
Classifications
-
- 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
- B01D17/02—Separation of non-miscible liquids
- B01D17/04—Breaking emulsions
- B01D17/047—Breaking emulsions with separation aids
Definitions
- the invention relates to a method for controlling the cleavage of oil / water emulsions induced by organic breakers.
- oil-in-water emulsions such as cooling lubricant, thermoforming, cutting or Bohremulsionen whose oil phase mainly from natural or synthetic oils of different chemical Composition and origin, are not only subject to wear in their application, but are also contaminated by entry of foreign substances. They must therefore be disposed of regularly.
- the most important step in the - possibly continuous - disposal is the splitting of the processed emulsions. This means that the oil phase must be separated from the water phase as much as possible in order either to work up and recycle the separated oil phase or to be able to supply it and the likewise separated water phase in an ecologically safe manner to the usual disposal method.
- the optimum metering range has usually been determined by visual observation of the gap progression during emulsion splitting.
- This determination of the optimal metering range for the splitter i. of the end point for the addition of the surfactant compound used as cleavers, was usually done by adding cleavers until a floating oil / mud flake formed. In order to avoid overdosage, this had to be done with the addition of small cleavage amounts, which is why the splitting of oil / water emulsions with visual determination of the end point took a period of several hours to complete.
- EP-A-256 431 it is described that the optimum organic polisher dosing range for the organic cleavage-induced emulsion cleavage can be determined by measuring the haze profile as a function of the amount of organic cleavage added and the haze as an indicator of the organic cleavage Quality of the split water phase draws.
- This EP-A-256 431 describes a method for controlling the organic cleavage-induced cleavage of oil / water emulsions by measuring the turbidity of the split-water phase as a function of the added amount of organic breaker, characterized in that a known, consisting in principle of light source, sample chamber, detector for the transmitted light and detector for the forward scattered light apparatus arrangement during the addition of the organic cleavers emanating from the light source, through the sample chamber with the sample falling, non-adsorbed light ( Transmitted light) with the aid of the transmitted-light detector, simultaneously measuring the light forward-scattered by the light source and scattered by the oil droplets contained in the sample with the aid of the forward-scattered light detector; Turbidity calculated and if necessary s relates the result to the added cleavage amount and graphically records and interrupts the addition of the organic cleavage agent when the turbidity reaches a first minimum after the maximum.
- the object of the present invention is to improve the method of EP-A-256 431, in particular with regard to its application safety.
- turbidity measuring devices can generally be used to measure the turbidity of emulsions or suspensions. These can either measure the intensity of the transmitted light or the intensity of the scattered light and derive a relative turbidity value in%. These gauges are usually pre-set to show the turbidity directly as a relative% value. Since it does not depend on absolute values of the turbidity in the context of the inventive method, but on the relative change in the turbidity, it is not necessary to determine absolute values of the turbidity. This presupposes that the measurement of the turbidity during the entire process sequence always takes place with the same measuring arrangement using the same light path.
- the method according to the invention differs from previously described methods in that, in sub-step c), the integral of the turbidity profile is calculated as a function of the added amount of the organic emulsion breaker. Since the amount of emulsion breaker added increases and correlates with time, this is equivalent to calculating the integral of the turbidity curve as a function of time elapsed since the beginning of the addition of the emulsion splitter. If the concentration of the emulsion breaker solution added is known, which can be assumed in practice, the amount of emulsion breaker added up to a selected point in time ti is also known.
- Sub-step d) calculates auxiliary values at arbitrary times ti, which contain the integral of the turbidity profile at the same time ti as a variable parameter.
- the optimal amount of splitting agents is determined. This is the amount of splitting agent that must be added to the emulsion sample until 2 different conditions are met simultaneously.
- the first condition relates to the course of turbidity itself, while the second condition relates to the auxiliary value which is related to the latter via the integral of the turbidity profile. How these two conditions must be in each case in order to give the optimum amount of emulsion breakers depends on the nature of the emulsion to be split on the one hand and on the emulsion breaker used on the other hand and can be determined empirically in preliminary experiments.
- the first preselected condition is that the relative haze value increases with further addition of the organic emulsion breaker.
- the second preselected condition for the auxiliary value depends on how the auxiliary value is defined or calculated.
- the auxiliary values are calculated by dividing the value of the integral of the turbidity profile as a function of the added amount of the organic emulsion breaker at different times ti after the addition of the organic emulsion breaker by a variable V, is the value t x or contains this, where t x is the time since the beginning of the addition of the organic emulsion breaker until the respective time ti.
- the time t x can be expressed in seconds.
- the auxiliary values are calculated in step d) by dividing the integral of the turbidity profile at time U by the time t x in seconds, which has elapsed since the beginning of the addition of the emulsion separator until time ti.
- the fulfillment of the second preselected condition can be determined more clearly if one adds an empirically determined number y to calculate the auxiliary values at t x .
- this is preferably in the range of 0.5 to 50 and in particular in the range of 1 to 20.
- y 10 can be set.
- the value of y can be adjusted so that the fulfillment of the second condition correlates particularly well with the optimum amount of emulsion breaker. This can be optimized by practical splitting tests. The once empirically determined optimum value of y is then maintained as long as the same emulsion breaker is used and the nature of the emulsion to be cleaved does not change too much.
- the second preselected condition can be chosen differently, whereby it is possible to check in preliminary tests which choice yields the better cleavage results with lower consumption of chemicals.
- the second preselected condition is that the turbidity value at a time ti is smaller than the auxiliary value at the same time ti.
- the slope of the turbidity curve must be positive, but secondly the absolute value of the turbidity must be so small that it is smaller than the auxiliary value.
- the turbidity of the emulsion generally increases, so that the first condition is generally fulfilled here.
- the integral of the turbidity curve is still comparatively small, so that the auxiliary value also represents a small number. Therefore, the said second preselected condition is generally not fulfilled here.
- the turbidity curve usually reaches a maximum, according to which the turbidity values drop with further addition of splitting agent, ie the gradient of the curve is negative.
- the integral of the turbidity curve continues to increase, so that the auxiliary value also increases and eventually becomes larger than the turbidity value itself. Then, the said second preselected condition is satisfied, but not the first preselected condition, since at this stage the turbidity values remove with further addition of splitting agent.
- turbidity values either reach a minimum at further splitting agent addition, after which they increase again, or at least a plateau at which they vary by a low absolute value.
- a state is reached in which the turbidity values continue to increase systematically or at least as a consequence of statistical fluctuations, given continued addition of splitting agent.
- the first preselected condition is fulfilled anew, so that the time added amount of emulsion breaker is determined as the optimum amount.
- the second preselected condition such that the difference: (turbidity value at a time ti minus auxiliary value at the same time t-i) is less than a predetermined and / or empirically determined threshold value.
- either the first or second alternative for the second preselected condition may result in a better cleavage result.
- only one of these two embodiments is even successful, since possibly only one of the two variants for the second preselected condition leads to this selected second preselected condition being fulfilled simultaneously with the first preselected condition.
- the supplier of emulsion breakers can determine in preliminary tests which process variant and optionally which choice of threshold or size y for a given emulsion breaker leads to the most unambiguous and technically most meaningful values for the optimum amount of emulsion breaker. This may additionally depend on the type of emulsion.
- the type of the emulsion to be cleaved and the emulsion breaker used are constant over long periods of time, while the amount of oil in the emulsion and hence the optimal amount of cleavers can vary.
- the method according to the invention In order to determine the optimum amount of emulsion breaker, the method according to the invention with fixed preset values for the second condition to be selected on the one hand and for the threshold value or the number y on the other hand can then be maintained. The optimal criteria are thus determined once by preliminary tests and are then retained for productive operation. If an electronic control and evaluation unit is used for the method according to the invention, these pre-determined values of this electronic unit can be permanently entered.
- the emulsion breaker may be expedient not to check after the first addition or after a few addition steps whether the first and second preselected conditions have already been fulfilled.
- statistical or at least uncharacteristic fluctuations of the haze values can occur, before the turbidity values assume a significant course on further addition of the emulsion breaker.
- the process of the invention is characterized by adding the organic emulsion breaker to the emulsion sample for a preselected period of time before verifying that the first and second preselected conditions are simultaneously satisfied for the first time.
- This preselected period from the start of the emulsion breaker addition may be, for example, in the range from 10 to 120 seconds, in particular in the range from 15 to 60 seconds and preferably in the range from 20 to 40 seconds.
- measuring arrangements can be used which comprise radiation source and detector and which are commercially available as predefined and preset building units.
- the relative turbidity meter itm-2 from Negele Messtechnik GmbH, Raiffeisenweg 7, 87743 Egg an der Günz (Germany) is suitable for this purpose. This provides as output signal of the detector directly the relative haze values in%, which can serve as input values for the method according to the invention.
- the radiation source and the detector are close to each other. “Close to one another” may mean that the respective center points of the radiation source and the detector in the direction perpendicular to the axis of the light and / or infrared radiation emanating from the radiation source have a distance in the range of 0.5 to 5 cm ,
- the determination method according to the invention is preferably carried out with infrared radiation.
- a wavelength range of about 840 to about 880 nm is suitable for this purpose.
- a (preferably electronic) control and evaluation unit is used, in which an algorithm for carrying out steps b) to d) is stored.
- the preselected first and second conditions can be preset together with, as the case may be, the value for the number y according to claim 4 or the threshold value according to claim 6 inventive method readily human intervention with the help of the control and evaluation are carried out automatically.
- a sample is drawn from the emulsion to be cleaved, determines the optimum amount of emulsion breaker and added by automatic control of valves and / or pumps this optimum amount of emulsion breaker from a storage vessel of the emulsion to be cleaved.
- the amount of emulsion breaker to be added per liter of emulsion and per minute to the emulsion sample must be selected. This depends in particular on the oil content of the emulsion and on the amount of emulsifying components in the emulsion. Practical tests have shown that it is preferable to add the organic emulsion breaker in an amount of 0.02 to 5 g of active ingredient per liter of emulsion sample within a measuring period in the range of 0.5 to 10 minutes. In particular, the amount of emulsion breaker added per liter of emulsion sample and minute is selected such that the inventive method for determining the optimum amount of breaker agent can be completed in a time interval between 1 minute and 5 minutes.
- the composition of the emulsion changes in an unexpected manner, it may happen that the preselected process variant and the preset values within the aforementioned time window do not meet the criterion that both the first preselected condition for the turbidity course as a function of added amount of the organic emulsion breaker on the one hand and the second preselected condition for the auxiliary value on the other hand are simultaneously satisfied.
- the automatic determination of the optimum amount of emulsion breaker has then failed.
- the determination method ie the further measurement of the turbidity with further addition of emulsion breaker, then probably no longer leads to a meaningful result and should be discontinued.
- the control and evaluation unit outputs an alarm signal. Then the pre- set process parameters in the control and evaluation by manual tests and adjusted.
- the overall process according to the invention for the splitting of oil / water emulsions and its control thus preferably proceeds automatically under program control. It has proven to be advantageous in practice, that before the measurement of turbidity, the sample chamber is pre-rinsed with the emulsion to be split, then the actual emulsion sample is filled into the sample chamber and homogenized, followed by the addition of organic emulsion breaker and measurement of turbidity starts. This can be done completely automatically if the control and evaluation unit is programmed accordingly and the device to be used has the required valves and pumps.
- a second aspect of the present invention relates to a method for splitting an oil / water emulsion in a slit container by adding organic emulsion breakers, wherein the required amount of organic emulsion breakers determined by a method according to one or more of claims 1 to 13 and programmatically controlled an emulsion sample is transferred to the sample chamber, hereby carries out the method according to one or more of claims 1 to 13 and manually or automatically determined by this determined amount of splitting agent in the splitting container and mixed with the oil / water emulsion.
- This process for splitting an oil / water emulsion can be carried out by determining the optimum amount of emulsion breakers per liter of emulsion to be broken by the method described above and adding the appropriate amount directly to the splitting container manually or by switching on corresponding metering devices.
- the further course of the process then corresponds to the state of the art: waiting for the phase separation, separating the oil phase from the water phase and separate disposal or reprocessing of the two separate phases.
- the addition of the optimally determined amount of splitting agent into the splitting container takes place automatically without human intervention.
- the control and evaluation unit for the method described above for determining the optimum amount of splitting agent then independently controls corresponding pumps and / or metering valves in order to give the amount of splitting agent determined to be optimal in the splitting agent container.
- the process for splitting an oil / water emulsion can be carried out batchwise or continuously.
- the slit container is filled with the oil / water emulsion, determined by the process according to the invention, the optimum amount of splitting agent, this is in the slit container, waits for the separation into an oil phase and a water phase and separates the two phases from each other.
- continuous addition of the emulsion breaker is meant here that the complete separation of the emulsion is not awaited before emulsion breaker is added again to the fresh emulsion. Rather, “continuous” here means that new emulsion breaker is added while the cleavage is still going on and while new emulsion is entering the cleavage vessel. H. in a constant stream without interruption. However, “continuous” may also mean that the amount of emulsion breaker recognized as optimal may be added in a timed manner, with a preselected waiting time after each addition.
- this continuous cleavage method is checked at pre-selected intervals, which may for example be in the range of 5 minutes to 2 hours, whether the intended amount of emulsion breakers nor the optimum amount corresponds or whether this is to be adapted. This is done by the method described above for determining the required amount of emulsion breaker. If it should appear during the check that the current amount of emulsion breaker no longer corresponds to the optimum amount, which can be attributed, for example, to a change in the oil content of the emulsion, then the amount of emulsion breaker to be added can be adapted accordingly automatically.
- an improved method for determining the optimum amounts of organic emulsion breaker is provided, with the aid of which, in the industrial production process, the emulsion splitting can be carried out reliably and fully automatically. If the method for determining the optimum amount of emulsion breaker fail, it can be provided that operating personnel is notified by an alarm message.
- the emulsions cleaved by the process according to the invention are without exception oil-in-water emulsions, as obtained, for example, in the processing of metallic materials. These emulsions are used to cool the workpieces and tools in metal cutting, for example, cutting, drilling and turning, or to improve the sliding and separating behavior in non-cutting metal processing, such as deep drawing. Emulsions in this sense are thus processed or for experimental purposes also synthetically produced cooling lubricant, thermoforming, cutting and / or Bohremulsionen, whereby emulsion mixtures fall under the above term.
- the oil-in-water emulsions described are aqueous systems which may contain up to 10% of oil; These are usually created by external entry.
- emulsions in the above-mentioned sense also mean the classical alkaline neutral or acid degreasing and cleaning baths which are obtained, for example, in the automobile industry in the degreasing or cleaning of metal sheets.
- the compounds used as organic breakers are known in the art.
- cleavers demulsifiers
- cationic polymers are used. These preferably have a molecular weight in the range of 50,000 to 500,000.
- compounds based on polyamines, polyamidoamines, polyimines, condensation products of o-toluidine and formaldehyde, quaternary ammonium compounds and ionic surfactants are advantageously used, ie with good cleavage results even at low Demulgatorkonzentrationen.
- polyamines having an average molecular weight in the range of 75,000 to 200,000 or condensation products of o-toluidine and formaldehyde are particularly preferred even at low cleavage concentrations due to the good cleavage results.
- Fig. 1 illustrates the procedure of claim 5, where the second preselected condition is that the turbidity value at a time ti is less than the auxiliary value at the same time t-i.
- the auxiliary value is calculated as: (integral of turbidity) / (time in seconds + 10)
- the second preselected condition according to claim 5 is satisfied from about 25 seconds. However, between 25 seconds and 85 seconds, the first preselected condition according to claim 2 is not satisfied, that the haze value increases with further addition of the organic emulsion breaker. This is only the case again after 90 seconds, so that the determination of the optimum amount of emulsion breaker ends here.
- the amount of emulsion breaker added per liter of emulsion over 90 seconds is the amount required for optimal cleavage.
- Fig. 2 illustrates the method in the variant of claim 6, according to which the second preselected condition is that the difference: (turbidity value to a Time ti minus auxiliary value at the same time ti) is less than a selected threshold.
- the auxiliary value is calculated as: (integral of turbidity) / (time in seconds + 10)
- the second preselected condition according to claim 6 is fulfilled from about 20 seconds. However, between 20 seconds and 120 seconds, the first preselected condition according to claim 2 is not satisfied, that the haze value increases with further addition of the organic emulsion breaker. This is only the case again after 125 seconds, so that the determination of the optimum amount of emulsion breaker ends here.
- the amount of emulsion breaker added per liter of emulsion over 125 seconds is the amount required for optimal cleavage. The figure shows that the choice of the threshold is not critical within wide limits.
- Gap Test 1 Course of turbidity and auxiliary value as a function of the addition of
- Emulsion breakers are Emulsion breakers.
- Gap test 2 course of turbidity and the difference (turbidity - auxiliary value) as
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- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE200610008559 DE102006008559A1 (de) | 2006-02-22 | 2006-02-22 | Verfahren zur Spaltung von Öl/Wasser-Emulsionen und dessen Steuerung |
PCT/EP2007/000136 WO2007096024A1 (de) | 2006-02-22 | 2007-01-10 | Verfahren zur spaltung von öl/wasser-emulsionen und dessen steuerung |
Publications (1)
Publication Number | Publication Date |
---|---|
EP2035107A1 true EP2035107A1 (de) | 2009-03-18 |
Family
ID=37946137
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP07702641A Withdrawn EP2035107A1 (de) | 2006-02-22 | 2007-01-10 | Verfahren zur spaltung von öl/wasser-emulsionen und dessen steuerung |
Country Status (3)
Country | Link |
---|---|
EP (1) | EP2035107A1 (de) |
DE (1) | DE102006008559A1 (de) |
WO (1) | WO2007096024A1 (de) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102007042520A1 (de) * | 2007-09-07 | 2009-03-12 | New Environmental Technology Gmbh | Verfahren und Vorrichtung zur kontinuierlichen Aufbereitung belasteter Fluide |
AU2018334414B2 (en) * | 2017-09-13 | 2023-08-17 | Halliburton Energy Services, Inc. | Optical analysis of wellbore fluid demulsifiers |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3627199A1 (de) * | 1986-08-11 | 1988-02-25 | Henkel Kgaa | Verfahren zur steuerung der spaltung von oel-/wasseremulsionen |
DE4107643A1 (de) * | 1991-03-09 | 1992-09-10 | Bayer Ag | Verfahren zur spaltung von oel-in-wasser-emulsionen |
DE4311423C1 (de) * | 1993-04-07 | 1994-07-28 | Metron Rhewatec Gmbh Ges Fuer | Verfahren zur Steuerung der Zudosierung eines Spaltmittels zu einer Öl-Wasser-Emulsion |
DE19532476A1 (de) * | 1995-09-02 | 1997-03-06 | Winfried Prof Dr Schmidt | Verfahren und Vorrichtung zur Behandlung von ölhaltigen Abwässern, insbesondere zur Trennung von Öl-in-Wasser-Emulsionen |
-
2006
- 2006-02-22 DE DE200610008559 patent/DE102006008559A1/de not_active Withdrawn
-
2007
- 2007-01-10 WO PCT/EP2007/000136 patent/WO2007096024A1/de active Application Filing
- 2007-01-10 EP EP07702641A patent/EP2035107A1/de not_active Withdrawn
Non-Patent Citations (1)
Title |
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See references of WO2007096024A1 * |
Also Published As
Publication number | Publication date |
---|---|
DE102006008559A1 (de) | 2007-08-30 |
WO2007096024A1 (de) | 2007-08-30 |
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