CN100386130C - Emulsion breaking method suitable for oil-water emulsion derived from biological desulfurization - Google Patents
Emulsion breaking method suitable for oil-water emulsion derived from biological desulfurization Download PDFInfo
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Abstract
The present invention relates to a demulsification method which is suitable for an oil-water emulsion formed after biological desulfurization, which belongs to the microbe field of the petroleum industry. The present invention has a plurality of demulsification methods for an emulsion formed after fuel oil desulphurization. Used demulsifiers are divided into three classes, such as alcohol, a lipopeptide biosurfactant and a rhodococcus somatic cell. The present invention has the working procedures that the demulsifiers are sprayed to emulsion surfaces according to certain ratio (the alcohol demulsifier and the lipopeptide biosurfactant are both added according to the ratio of 1:15 to 1:25; the rhodococcus somatic cell is added according to the ratio of 1:2 to 1:10); the mixtures are processed by standing for 1 to 2 hours at the indoor temperature; after that the mixtures are processed by centrifugation on line for 10 minutes at 5000 r/min; the upper layer oil phase is processed by shunting collection, wherein the final demulsification rate of the lipopeptide biosurfactant can reach 99%. The present invention has the advantages of simple operative method, low cost and no toxic effect or pollution on environment; the present invention can make three phases of oil, water and thallus sufficiently separate. The effects of the present invention are better than that of the traditional chemical demulsifier. Simultaneously, the present invention can not influent the hydrocarbon constituents of diesel oil, but can make the heat value of the diesel oil sufficiently reserved.
Description
Technical field
The invention belongs to petrochemical industry and industrial microorganism field, specifically at several breaking methods of the emulsion that forms after the desulfurization of fuel oil.
Background technology
Emulsion be meant one or more liquid with liquid pearl form be dispersed in its immiscible liquid in the coarse dispersion system that constitutes, be called as emulsion owing to system manifests milky.In emulsion system, be called interior phase mutually with what the pearl form existed, because its discontinuity is called discontinuous phase or decentralized photo again.And another is called the foreign minister mutually, because its continuity is called continuous phase or decentralized medium again.Common emulsion has one to be the water or the aqueous solution mutually, is called as water, and another is to be called as oil phase with the immiscible organic facies of water mutually.The type of emulsion has following several: 1. oil-in-water type (Oil in Water), represent with O/W, and be oil mutually in it, the foreign minister is a water, as human milk, cow's milk etc., the emulsion that forms behind the biological desulphurization belongs to this type more; 2. water-in-oil type (Water in Oil) is represented with W/O, and interior is water mutually, and the foreign minister is an oil.Because oil is more than water, crude oil is mainly such emulsion.3. the lasso formula is represented with O/W/O or W/O/W, i.e. water and oil phase wrapping in layer alternately, and this type is less to be seen.
Emulsifying agent is the emulsion stable key of relying, and it can be adsorbed on and form monomolecular film on the oil-water interfaces, has to reduce oil water interfacial tension and stop oil droplet and poly-effect and make emulsion stable.Emulsifying agent mainly divides four classes: surfactant-based, and polymer electrolyte, natural products class and pressed powder.Influencing the stable factor of emulsion has (Xu Yanli .2000, the function of surfactant, Chemical Industry Press, Beijing: pp.106～137 such as viscosity of character, interface charge and the decentralized medium of interface gravitation, interfacial film; Yao Yunwu, Qiu Zunan, 1988, colloid and surface chemistry, pp.165～258).
Make the phenomenon of emulsion generation water-oil separating be called breakdown of emulsion.Method commonly used has: 1., maybe can not form the original emulsifying agent of surface reactive material replacement of firm film with the very strong material of another surface-active, interfacial film is changed; 2., add some can with the material of emulsifying agent generation chemical reaction, eliminate the protective effect of emulsifying agent; 3., add the different emulsifying agent of emulsification mechanism, the electrolyte as high price adds strong mixing, centrifugation, ultrasonic wave, microwave, thereby electrophoresis etc. all can quicken the coalescent purpose that reaches breakdown of emulsion of decentralized photo.
Breakdown of emulsion is the process of a complexity, and at present still the fixing rule of neither one can be used, therefore the also omnipotent demulsifier of neither one.More to the research of breakdown of emulsion both at home and abroad in recent years, all be to carry out the composite of demulsifier according to emulsion specific formation characteristics and ionic strength, or bacterium or its metabolite have been utilized, as (Chang Je Hwan such as organic acid and surfactants, YoonJung Kim, Bum Hawn Lee, et al.2001, Biotechnol Prog.17:876～880; Xiali is new, Cao Guoying .2002 such as Lu Shiwei, chemical research and application .14 (6), 623～627; Madhusweta D.2001, Bioresource Technology.79:15～22; Lee Jae-Chan, Ki-Young Lee.2000, Biotechnol.Prog.22:1157～1163).External a lot of to the research of breakdown of emulsion, successfully developed multiple breaking method, comprise method (Dunning H N such as heating, forceful electric power, ultrasonic wave, microwave, chemical demulsification, Moore J W, Denekas M O.1953, Ind.Eng.Chem., 45:1759～1765; Lee C J, WangS S, Chan C C.1995, J.Chinese Institute Chem.Eng., 26 (4): 263～275; Fang C S, Lai PMC, ChangBKL.1980, Environ.Prog.8 (4): 235～238; Li K L, Xia L X, Li J, et al.2001, CarbohydrateResearch, 331:9～12; Gabriel G, Gabriel S, Grant E H, et al.1998, Chem.Soc.Rev.27:213～223).Graduate doctor Guo Donghong of petroleum exploration and development selects a kind of biological demulsifying agent for use, it and three kinds of composite crude oil demulsifications that carry out of polyether type demulsifying agent are tested, the result shows that the introducing of biological demulsifying agent can significantly improve the speed and the effect of crude oil emulsion breaking emulsion and dewatering.Pass through electrochemical method, the trend that the adding of discovery biological demulsifying agent makes the interfacial film electric capacity of chemical demulsification solution increase in time is obvious, the breakdown time of interfacial film shortens, and the also corresponding enhancing of interfacial film resistance decline degree in time, this proves absolutely that biological demulsifying agent and chemical demulsifier have " cooperative effect " (Guo Donghong etc., 1999, synergistic mechanism research of MICROBIAL SURFACTANT and demulsifier, oilfield chemistry information, 1:17-19).People such as Nalina find that from filtered out one group of mixed bacterial by the oil pollution place they have good demulsification activity, can make kerosene-water model emulsion reach demulsification efficiency 96% in one hour.Freeze thawing and autoclaving do not influence its demulsification activity.The back confirms it is that the surfactant that thalline particle and thalline produce plays demulsification (Nalina Nadarajah, Ajay Singh, Owen P.Ward, 2002a, Process Biochemistry, 37:1135～1141; Nalina Nadarajah, Ajay Singh, Owen P.Ward, 2002b, World Journal of Microbiology﹠amp; Biotechnology, 18:435～440; ).
The biological desulphurization of diesel oil reaction (biodesulfurization is hereinafter to be referred as BDS) is carried out in heterogeneous (oil/water/thalline) system, and the hydrophobicity of thalline self makes it can touch organic facies better to carry out desulphurization reaction.The surfactant that thalline produces can be emulsified into droplet with oil phase, heterogeneous system reaction under emulsifying agent and strong ventilation stirring action can produce a kind of stable emulsion, this has brought difficulty for the water-oil separating in BDS later stage, and seriously influenced process of industrialization (the Abhijeet P B of BDS, Eric N K, Matthew J G, et al.2002, Biotechnol.Prog., 18:88～93).At present, the breaking method that BDS uses is centrifugal process and hydrocyclone (hydrocyclone) method (Yu L, Meyer T, Folsom B.1998, USPatent No.5772901), it is with a kind of about long 1m, the conical pipe alternative reaction jar of diameter 5～10cm, liquid is from a big inflow and begin rotation, the part that density is big (water) is thrown to the lateral wall of pipe, and light in the centre, separated portions flows in the continuous device, the application of this method has very big potentiality, because it does not have drive unit, separating oil-aqueous mixtures can separate the thalline that is positioned at the oil-water interface place simultaneously at low cost.If in the oil water is arranged, thalline will be isolated pure oil from thalline-aqueous phase on the water droplet surface.As a little oil dripping being added in the surplus solution, becoming oil is arranged in the water, thalline is in oil droplets.This reacts reusable edible, mixes the composition of phase by control, can not consume too many energy and obtain pure relatively water or oil, has reduced manufacturing cost.But the shortcoming of the method is a breakdown of emulsion fully, and the diesel oil rate of recovery is still very limited.
The DBT group is vital to intracellular transport process for whole sweetening process, but this transhipment effect can step up " intimate contact " between profit, thereby causes emulsus structure closely, therefore will reclaim sweet oil, separating by-products just must be broken up this emulsification structure; Make the BDS technology to the industrialization transition, just must develop various simple to operate, expense is cheap, make oil/water/the thalline three-phase is able to abundant separation, nonhazardous, free of contamination breaking method.
Summary of the invention:
Main purpose of the present invention is to overcome the above-mentioned shortcoming that existing demulsification technology exists, and several breakdown of emulsion new methods that are used for forming behind the fuel oil biological desulphurization emulsion are provided.It is to utilize microorganism to reach the breakdown of emulsion purpose jointly with method chemistry.
Be used for the breaking method of the water-oil emulsion that forms behind the biological desulphurization, one of used demulsifier is the alcohols demulsifier;
The method that adopts is: the water-oil emulsion that biological desulphurization forms, by the ratio of 1: 15 to 1: 25 (v/v) to this demulsifier of emulsion surface sprinkling, room temperature effect 1～2h, the online centrifugal 10min of 5000r/min, shunting collection upper oil phase;
Two of used demulsifier is lipopeptid type biological surfactant classes;
The method that adopts is: the water-oil emulsion that biological desulphurization forms adds this demulsifier to the emulsus surface, room temperature effect 1～2h, the online centrifugal 10min of 5000r/min, shunting collection upper oil phase by the ratio of 1: 15 to 1: 25 (v/v);
Three of used demulsifier is red coccus somatic cells classes;
The method that adopts is: the water-oil emulsion that biological desulphurization forms adds this demulsifier to the emulsion surface, room temperature effect 1～2h, the online centrifugal 10min of 5000r/min, shunting collection upper oil phase by the ratio of 1: 2 to 1: 10 (v/v);
Used alcohols is: ethanol, propyl alcohol, isopropyl alcohol, butanols, isobutanol or isoamyl alcohol.
Used lipopeptid type biological surfactant is at NB culture medium (peptone 1% from bacillus subtilis, beef extract 0.5%, sodium chloride 0.5%) extraction obtains in the zymotic fluid after top fermentation is cultivated, this strain name is Bacillus subtilisNK-LRL068, be preserved in " China Committee for Culture Collection of Microorganisms's common micro-organisms " center ", preserving number CGMCCNO.1080.
Used NB culture medium (peptone 1%, beef extract 0.5%, sodium chloride 0.5%) the Rhodococcus strain name of Pei Yanging is called Rhodococcus erythropolis PR-1, is preserved in " China Committee for Culture Collection of Microorganisms's common micro-organisms " center ", preserving number CGMCC NO.1465.The thalline itself that is used for breakdown of emulsion is exactly the somatic cells that is used for biological desulphurization, and thalline itself has the effect of emulsification oil phase and water formation emulsion simultaneously.
More than these methods can carry out application in the breakdown of emulsion to the emulsion that forms behind the biological desulphurization.
Technical scheme of the present invention is as follows:
1, the preparation of biological desulphurization emulsion:
(horse very with Rhodococcus erythropolis DS-3 thalline, Liu Jian, Tong Mingyou etc., microorganism journal, 2002,42:126～131) be suspended from the bacteria suspension of making 20mg/mL in the DBT culture medium, and mix with diesel oil (4: 1, v/v), 30 ℃, can produce the upper strata behind the 300r/min shaken cultivation 24h is that stable three-phase (thalline, diesel oil, water) emulsion, lower floor is the mixed liquor of water, and upper strata emulsion can be stablized one month.
The evaluation of 2, emulsification type:
Oil red O (Oil Red) is the dyestuff that is dissolved in organic facies, and oil red O solution (2%, the hexadecane preparation) 50 μ L join in the freshly prepared emulsion, and mixing if emulsion is dyed redness fully, then is a w/o type emulsion; If have only punctation in the emulsion, and do not dyed redness fully, then be O/W type emulsion.
3, the selection of demulsifier and demulsification evaluation:
Add the emulsion of vibration mixing in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that should contain 1mL in theory), different water-soluble demulsifiers (because of emulsion is the O/W type) are added in the emulsion with certain proportion, vibration mixing (alcohols adopts the not mode of mixing that slowly adds), room temperature is placed 1-2h or the centrifugal 20min of 4000r/min, scale method measures the diesel oil amount (XmL) that every pipe is separated out, and the contrast water replaces.Every kind of bacterium liquid or to complying 3 groups of parallel laboratory tests.Demulsification efficiency %=XmL/1mL * 100%.
4, the analysis of diesel component:
HP GC 6890, PONA chromatographic column (50m * 0.20mm id * 0.50 μ m), HP AED chem workstation, U.S. Agilent company.HP2 heated getter type helium clarifier, U.S. Valco instrument company.
HP GC 6890 is furnished with the split sampling system of shunting/not, in the experiment with the shunting mode sample introduction.All gas flow among the GC and pressure all use electron pressure control (EPC), and an aux. pressure control device on HP 6890 GC is in order to control AED reaction gas pressure.With HP G1916A automated fluid injector (ALS) sample introduction.Main operating condition and parameter: 280 ℃ of injector temperatures; Carrier gas is a helium; 120 ℃ of post heating schedules keep 5min; Rise to 270 ℃ with 1.5 ℃/min speed; Press 12psi before the post; Split ratio 100/1; The volume 1 μ L of sample introduction.
The demulsifier that the present invention uses not only has better breakdown of emulsion ability (seeing Fig. 1 and Fig. 2), and it is low to have a cost, with strong points, easily be degraded, free from environmental pollution, the processing facility is not had advantages such as corrosiveness, thus it behind biological desulphurization, extract in the development and application prospect in water-oil separating field very wide.
Demulsifier among Fig. 1 is respectively:
1, water;
2, Tween 80;
3, lipopeptid type biological surfactant;
4, isopropyl alcohol;
5, red coccus somatic cells;
Two pipes are respectively among Fig. 2:
1, control tube;
2, demulsifier is handled pipe;
A: oil phase B: emulsion layer C: water
The demulsification of the different demulsifiers of table 1 under best proportion
Diesel oil mainly is made up of normal alkane and side chain isoparaffin, keeps its n-alkane proportion most important for oil quality, the variation that the two big standards of estimating diesel quality are normal paraffin component, Cetane number and the sulfur content of diesel oil.The present invention is to 0
#The centrifugal back of diesel oil and demulsifier breakdown of emulsion is reclaimed diesel oil and is carried out the GC-MS analysis, in conjunction with the shared whole peak area percentage proof of each component alcohols, lipopeptid type biological surfactant and red coccus cell breakdown of emulsion and centrifugal after, the peak area percentage of the normal paraffin component that diesel oil is main there is no obvious change, illustrates that the breakdown of emulsion process does not influence the calorific value of oil product (Fig. 3, Fig. 4, Fig. 5).
The method that the invention has the beneficial effects as follows is simple to operate, expense is cheap, to environment nonhazardous, pollution-free; Make oil/water/thalline three-phase be able to abundant separation, and effect is better than traditional chemical demulsifier; Do not influence simultaneously the hydrocarbon component of diesel oil, the calorific value of diesel oil is fully kept.
Description of drawings:
Fig. 1: the demulsification of different demulsifiers,
Fig. 2: lipopeptid type biological surfactant demulsification,
Fig. 3: 0
#The hydrocarbon component GC analysis chart of diesel oil;
Fig. 4: the hydrocarbon component GC analysis chart of diesel oil behind the breakdown of emulsion;
Fig. 5: the hydrocarbon component GC analysis chart of diesel oil behind the lipopeptid type biological surfactant breakdown of emulsion.
The specific embodiment:
Embodiment 1: ethanol is as the using method of demulsifier
1. the preparation of biological desulphurization emulsion:
(horse very with Rhodococcus erythropolis DS-3 thalline, Liu Jian, Tong Mingyou etc., microorganism journal, 2002,42:126～131) be suspended from the bacteria suspension of making 20mg/mL in the DBT culture medium, and mix with diesel oil (4: 1, v/v), 30 ℃, can produce the upper strata behind the 300r/min shaken cultivation 24h is that stable three-phase (thalline, diesel oil, water) emulsion, lower floor is the mixed liquor of water, and upper strata emulsion can be stablized one month.
2. the evaluation of emulsification type:
Oil red O (Oil Red) is the dyestuff that is dissolved in organic facies, and oil red O solution (2%, the hexadecane preparation) 50 μ L join in the freshly prepared emulsion, and mixing if emulsion is dyed redness fully, then is a w/o type emulsion; If have only punctation in the emulsion, and do not dyed redness fully, then be O/W type emulsion.
3. breakdown of emulsion and effect assessment thereof:
1). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/15 (v/v) ethanol (because of emulsion is the O/W type), room temperature is placed 2h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.97mL, demulsification efficiency %=97%.
2). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/25 (v/v) ethanol (because of emulsion is the O/W type), room temperature is placed 2h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.95mL, demulsification efficiency %=95%.
3). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/20 (v/v) ethanol (because of emulsion is the O/W type), room temperature is placed 2h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.98mL, demulsification efficiency %=98%.
4). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/15 (v/v) ethanol (because of emulsion is the O/W type), room temperature is placed 1h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.96mL, demulsification efficiency %=96%.
5). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/25 (v/v) ethanol (because of emulsion is the O/W type), room temperature is placed 1h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.94mL, demulsification efficiency %=94%.
6). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/20 (v/v) ethanol (because of emulsion is the O/W type), room temperature is placed 1h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.97mL, demulsification efficiency %=97%.
4. the analysis of diesel component:
HP GC 6890, PONA chromatographic column (50m * 0.20mm id * 0.50 μ m), HP AED chem workstation, U.S. Agilent company.HP2 heated getter type helium clarifier, U.S. Valco instrument company.
HP GC 6890 is furnished with the split sampling system of shunting/not, in the experiment with the shunting mode sample introduction.All gas flow among the GC and pressure all use electron pressure control (EPC), and an aux. pressure control device on HP 6890 GC is in order to control AED reaction gas pressure.With HP G1916A automated fluid injector (ALS) sample introduction.Main operating condition and parameter: 280 ℃ of injector temperatures; Carrier gas is a helium; 120 ℃ of post heating schedules keep 5min; Rise to 270 ℃ with 1.5 ℃/min speed; Press 12psi before the post; Split ratio 100/1; The volume 1 μ L of sample introduction.
Embodiment 2: propyl alcohol is as the using method of demulsifier
1. the preparation of biological desulphurization emulsion:
With embodiment 1.
2. the evaluation of emulsification type:
With embodiment 1.
3. breakdown of emulsion and effect assessment thereof:
1). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/15 (v/v) propyl alcohol (because of emulsion is the O/W type), room temperature is placed 2h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.9mL, demulsification efficiency %=90%.
2). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/25 (v/v) propyl alcohol (because of emulsion is the O/W type), room temperature is placed 2h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.88mL, demulsification efficiency %=88%.
3). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/20 (v/v) propyl alcohol (because of emulsion is the O/W type), room temperature is placed 2h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.91mL, demulsification efficiency %=91%.
4). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/15 (v/v) propyl alcohol (because of emulsion is the O/W type), room temperature place 1h or, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.88mL, demulsification efficiency %=88%.
5). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/25 (v/v) propyl alcohol (because of emulsion is the O/W type), room temperature is placed 1h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.86mL, demulsification efficiency %=86%.
6). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/20 (v/v) propyl alcohol (because of emulsion is the O/W type), room temperature is placed 1h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.89mL, demulsification efficiency %=89%.
4. the analysis of diesel component:
With embodiment 1.
Embodiment 3: isopropyl alcohol is as the using method of demulsifier
1. the preparation of biological desulphurization emulsion:
With embodiment 1.
2. the evaluation of emulsification type:
With embodiment 1.
3. breakdown of emulsion and effect assessment thereof:
1). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/15 (v/v) isopropyl alcohol (because of emulsion is the O/W type), room temperature is placed 2h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.97mL, demulsification efficiency %=97%.
2). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/25 (v/v) isopropyl alcohol (because of emulsion is the O/W type), room temperature is placed 2h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.95mL, demulsification efficiency %=95%.
3). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/20 (v/v) isopropyl alcohol (because of emulsion is the O/W type), room temperature is placed 2h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.97mL, demulsification efficiency %=97%.
4). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/15 (v/v) isopropyl alcohol (because of emulsion is the O/W type), room temperature is placed 1h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.96mL, demulsification efficiency %=96%.
5). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/25 (v/v) isopropyl alcohol (because of emulsion is the O/W type), room temperature is placed 1h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.95mL, demulsification efficiency %=95%.
6). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/20 (v/v) isopropyl alcohol (because of emulsion is the O/W type), room temperature is placed 1h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.97mL, demulsification efficiency %=97%.
4. the analysis of diesel component:
With embodiment 1
Embodiment 4: butanols is as the using method of demulsifier
1. the preparation of biological desulphurization emulsion:
With embodiment 1.
2. the evaluation of emulsification type:
With embodiment 1.
3. breakdown of emulsion and effect assessment thereof:
1). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/15 (v/v) butanols (because of emulsion is the O/W type), room temperature is placed 2h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.89mL, demulsification efficiency %=89%.
2). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/25 (v/v) butanols (because of emulsion is the O/W type), room temperature is placed 2h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.85mL, demulsification efficiency %=85%.
3). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/20 (v/v) butanols (because of emulsion is the O/W type), room temperature is placed 2h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.9mL, demulsification efficiency %=90%.
4). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/15 (v/v) butanols (because of emulsion is the O/W type), room temperature is placed 1h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.87mL, demulsification efficiency %=87%.
5). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/25 (v/v) butanols (because of emulsion is the O/W type), room temperature is placed 1h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.84mL, demulsification efficiency %=84%.
6). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/20 (v/v) butanols (because of emulsion is the O/W type), room temperature is placed 1h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.89mL, demulsification efficiency %=89%.
4. the analysis of diesel component:
With embodiment 1.
Embodiment 5: isobutanol is as the using method of demulsifier
1. the preparation of biological desulphurization emulsion:
With embodiment 1.
2. the evaluation of emulsification type:
With embodiment 1.
3. breakdown of emulsion and effect assessment thereof:
1). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/15 (v/v) isobutanol (because of emulsion is the O/W type), room temperature is placed 2h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.91mL, demulsification efficiency %=91%.
2). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/25 (v/v) isobutanol (because of emulsion is the O/W type), room temperature is placed 2h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.87mL, demulsification efficiency %=87%.
3). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/20 (v/v) isobutanol (because of emulsion is the O/W type), room temperature is placed 2h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.91mL, demulsification efficiency %=91%.
4). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/15 (v/v) isobutanol (because of emulsion is the O/W type), room temperature is placed 1h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.9mL, demulsification efficiency %=90%.
5). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/25 (v/v) isobutanol (because of emulsion is the O/W type), room temperature is placed 1h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.87mL, demulsification efficiency %=87%.
6). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/20 (v/v) isobutanol (because of emulsion is the O/W type), room temperature is placed 1h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.89mL, demulsification efficiency %=89%.
4. the analysis of diesel component:
With embodiment 1.
Embodiment 6: isoamyl alcohol is as the using method of demulsifier
1. the preparation of biological desulphurization emulsion:
With embodiment 1.
2. the evaluation of emulsification type:
With embodiment 1.
3. breakdown of emulsion and effect assessment thereof:
1). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/15 (v/v) isoamyl alcohol (because of emulsion is the O/W type), room temperature is placed 2h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.96mL, demulsification efficiency %=96%.
2). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/25 (v/v) isoamyl alcohol (because of emulsion is the O/W type), room temperature is placed 2h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.95mL, demulsification efficiency %=95%.
3). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/20 (v/v) isoamyl alcohol (because of emulsion is the O/W type), room temperature is placed 2h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.96mL, demulsification efficiency %=96%.
4). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/15 (v/v) isoamyl alcohol (because of emulsion is the O/W type), room temperature is placed 1h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.95mL, demulsification efficiency %=95%.
5). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/25 (v/v) isoamyl alcohol (because of emulsion is the O/W type), room temperature is placed 1h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.96mL, demulsification efficiency %=96%.
6). the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes fast, every pipe 5mL (diesel oil that contains 1mL), slowly be added in emulsion with the ratio of 1/20 (v/v) isoamyl alcohol (because of emulsion is the O/W type), room temperature is placed 1h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.96mL, demulsification efficiency %=96%.
4. the analysis of diesel component:
With embodiment 1.
Embodiment 7: the lipopeptid type biological surfactant is as the using method of demulsifier
1. the preparation of biological desulphurization emulsion:
With embodiment 1.
2. the evaluation of emulsification type:
With embodiment 1.
3. breakdown of emulsion and effect assessment thereof:
1), the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes every pipe 5mL (diesel oil that contains 1mL) fast; With Bacillus subtilis NK-LRL068 bacterial strain at NB culture medium (peptone 1%, beef extract 0.5%, sodium chloride 0.5%), 37 ℃, 200r/min fermented and cultured 72h.The emulsion of zymotic fluid and preparation is added in the emulsion fully vibration mixing in the ratio with 1/15 (v/v), and room temperature is placed 2h, and the diesel oil amount that the centrifugal 20min of 4000r/min, 3 groups of average every pipes of parallel laboratory test separate out is 0.97mL, demulsification efficiency %=97%.
2), the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes every pipe 5mL (diesel oil that contains 1mL) fast; With Bacillus subtilis NK-LR068 bacterial strain at NB culture medium (peptone 1%, beef extract 0.5%, sodium chloride 0.5%), 37 ℃, 200r/min fermented and cultured 72h.The emulsion of zymotic fluid and preparation is added in the emulsion fully vibration mixing in the ratio with 1/25 (v/v), and room temperature is placed 2h, and the diesel oil amount that the centrifugal 20min of 4000r/min, 3 groups of average every pipes of parallel laboratory test separate out is 0.96mL, demulsification efficiency %=96%.
3), the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes every pipe 5mL (diesel oil that contains 1mL) fast; With Bacillus subtilis NK-LR068 bacterial strain at NB culture medium (peptone 1%, beef extract 0.5%, sodium chloride 0.5%), 37 ℃, 200r/min fermented and cultured 72h.The emulsion of zymotic fluid and preparation is added in the emulsion fully vibration mixing in the ratio with 1/20 (v/v), and room temperature is placed 2h, and the diesel oil amount that the centrifugal 20min of 4000r/min, 3 groups of average every pipes of parallel laboratory test separate out is 0.97mL, demulsification efficiency %=97%.
4), the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes every pipe 5mL (diesel oil that contains 1mL) fast; With Bacillus subtilis NK-LR068 bacterial strain at NB culture medium (peptone 1%, beef extract 0.5%, sodium chloride 0.5%), 37 ℃, 200r/min fermented and cultured 72h.The emulsion of zymotic fluid and preparation is added in the emulsion fully vibration mixing in the ratio with 1/15 (v/v), and room temperature is placed 1h, and the diesel oil amount that the centrifugal 20min of 4000r/min, 3 groups of average every pipes of parallel laboratory test separate out is 0.97mL, demulsification efficiency %=97%.
5), will the vibrate emulsion of mixing adds fast in several 10mL scale test tubes, every pipe 5mL (diesel oil that contains 1mL): with Bacillus subtilis NK-LR068 bacterial strain at NB culture medium (peptone 1%, beef extract 0.5%, sodium chloride 0.5%), 37 ℃, 200r/min fermented and cultured 72h.The emulsion of zymotic fluid and preparation is added in the emulsion fully vibration mixing in the ratio with 1/25 (v/v), and room temperature is placed 1h, and the diesel oil amount that the centrifugal 20min of 4000r/min, 3 groups of average every pipes of parallel laboratory test separate out is 0.96mL, demulsification efficiency %=96%.
6), the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes every pipe 5mL (diesel oil that contains 1mL) fast; With Bacillus subtilis NK-LR068 bacterial strain at NB culture medium (peptone 1%, beef extract 0.5%, sodium chloride 0.5%), 37 ℃, 200r/min fermented and cultured 72h.The emulsion of zymotic fluid and preparation is added in the emulsion fully vibration mixing in the ratio with 1/20 (v/v), and room temperature is placed 1h, and the diesel oil amount that the centrifugal 20min of 4000r/min, 3 groups of average every pipes of parallel laboratory test separate out is 0.96mL, demulsification efficiency %=96%.
4. the analysis of diesel component:
With embodiment 1.
Embodiment 8: red coccus is as the using method of demulsifier:
1. the preparation of biological desulphurization emulsion:
With embodiment 1.
2. the evaluation of emulsification type:
With embodiment 1.
3. breakdown of emulsion and effect assessment thereof:
1), the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes every pipe 5mL (diesel oil that contains 1mL) fast; With Rhodococcus sp.PR-1 bacterial strain at NB culture medium, 37 ℃, 200r/min fermented and cultured 36～72h, the centrifugal 10min of 6000r/min collects somatic cells, bacterium seed liquor and emulsion are joined in the emulsion fully vibration mixing with the ratio of 1: 2 (v/v), room temperature is placed 2h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.9mL, demulsification efficiency %=90%.
2), the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes every pipe 5mL (diesel oil that contains 1mL) fast; With Rhodococcus sp.PR-1 bacterial strain at NB culture medium, 37 ℃, 200r/min fermented and cultured 36～72h, the centrifugal 10min of 6000r/min collects somatic cells, bacterium seed liquor and emulsion are joined in the emulsion fully vibration mixing with the ratio of 1: 10 (v/v), room temperature is placed 2h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.88mL, demulsification efficiency %=88%.
3), the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes every pipe 5mL (diesel oil that contains 1mL) fast; With Rhodococcus sp.PR-1 bacterial strain at NB culture medium, 37 ℃, 200 rev/mins fermented and cultured 36～72h, the centrifugal 10min of 6000r/min collects somatic cells, bacterium seed liquor and emulsion are joined in the emulsion fully vibration mixing with the ratio of 1: 5 (v/v), room temperature is placed 2h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.9mL, demulsification efficiency %=90%.
4), the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes every pipe 5mL (diesel oil that contains 1mL) fast; With Rhodococcus sp.PR-1 bacterial strain at NB culture medium, 37 ℃, 200r/min fermented and cultured 36～72h, the centrifugal 10min of 6000r/min collects somatic cells, bacterium seed liquor and emulsion are joined in the emulsion fully vibration mixing with the ratio of 1: 2 (v/v), room temperature is placed 1h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.89mL, demulsification efficiency %=89%.
5), the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes every pipe 5mL (diesel oil that contains 1mL) fast; With Rhodococcus sp.PR-1 bacterial strain at NB culture medium, 37 ℃, 200r/min fermented and cultured 36～72h, the centrifugal 10min of 6000r/min collects somatic cells, with bacterium seed liquor and emulsion with 1: 10) (v/v) ratio joins in the emulsion fully vibration mixing, room temperature is placed 1h, the diesel oil amount that the centrifugal 20min of 4000r/min, 3 groups of average every pipes of parallel laboratory test separate out is 0.88mL. demulsification efficiency %=88%.
6), the emulsion of the mixing that will vibrate adds in several 10mL scale test tubes every pipe 5mL (diesel oil that contains 1mL) fast; With Rhodococcus sp.PR-1 bacterial strain at NB culture medium, 37 ℃, 200r/min fermented and cultured 36～72h, the centrifugal 10min of 6000r/min collects somatic cells, bacterium seed liquor and emulsion are joined in the emulsion fully vibration mixing with the ratio of 1: 5 (v/v), room temperature is placed 1h, the centrifugal 20min of 4000r/min, the diesel oil amount that 3 groups of average every pipes of parallel laboratory test are separated out is 0.88mL, demulsification efficiency %=88%.
4. the analysis of diesel component:
With embodiment 1.
Claims (5)
1. be used for the breaking method of the water-oil emulsion that forms behind the biological desulphurization, it is characterized in that used demulsifier is respectively:
(1) alcohols demulsifier;
The method that is adopted is: the water-oil emulsion that biological desulphurization forms, by the ratio of 1: 15 to 1: 25 (v/v) to this demulsifier of emulsion surface sprinkling, room temperature effect 1～2h, the online centrifugal 10min of 5000r/min, shunting collection upper oil phase;
(2) lipopeptid type biological surfactant demulsifier;
The method that is adopted is: the water-oil emulsion that biological desulphurization forms adds this demulsifier to the emulsion surface, room temperature effect 1～2h, the online centrifugal 10min of 5000r/min, shunting collection upper oil phase by the ratio of 1: 15 to 1: 25 (v/v);
(3) red coccus somatic cells demulsifier;
The method that is adopted is: the water-oil emulsion that biological desulphurization forms adds this demulsifier to the emulsion surface, room temperature effect 1～2h, the online centrifugal 10min of 5000r/min, shunting collection upper oil phase by the ratio of 1: 2 to 1: 10 (v/v).
2. the breaking method that is applicable to water-oil emulsion behind the biological desulphurization according to claim 1 is characterized in that used alcohols is: ethanol, propyl alcohol, isopropyl alcohol, butanols, isobutanol or isoamyl alcohol.
3. the breaking method that is applicable to water-oil emulsion behind the biological desulphurization according to claim 1, it is characterized in that, used lipopeptid type biological surfactant is to extract to obtain from the zymotic fluid of bacillus subtilis after the top fermentation of NB culture medium is cultivated, this strain name is Bacillus subtilis NK-LRL068, be preserved in " China Committee for Culture Collection of Microorganisms's common micro-organisms " center ", preserving number CGMCC NO.1080.
4. the breaking method that is applicable to water-oil emulsion behind the biological desulphurization according to claim 1, it is characterized in that, the Rhodococcus strain name of used NB medium culture is called Rhodococcus erythropolis PR-1, be preserved in " China Committee for Culture Collection of Microorganisms's common micro-organisms " center "; preserving number CGMCC NO.1465; the thalline itself that is used for breakdown of emulsion is exactly the somatic cells that is used for biological desulphurization, and thalline itself has the effect of emulsification oil phase and water formation emulsion simultaneously.
5. according to claim 1 or 2 or the 3 or 4 described breaking methods that are applicable to water-oil emulsion behind the biological desulphurization, the emulsion that forms after to biological desulphurization carries out the application in the breakdown of emulsion.
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| CN104419519B (en) * | 2013-08-30 | 2017-08-22 | 中国石油化工股份有限公司 | A kind of method for emulsifying biodiesel demulsification |
| CN104560408B (en) * | 2013-10-23 | 2017-11-24 | 中国石油化工股份有限公司 | A kind of production method of biodiesel |
| CN105727599B (en) * | 2016-02-23 | 2017-11-07 | 同济大学 | The method that demulsifying bacteria is used to strengthen emulsion breakdown is modified using magnetic nano-particle |
| CN111876353B (en) * | 2020-07-30 | 2022-03-29 | 董丁 | Bacterial strain for producing biological demulsifier and biological demulsifier produced by bacterial strain |
| CN112742071B (en) * | 2021-01-13 | 2022-07-05 | 西南科技大学 | Low surface energy droplet oriented transportation and separation structure |
| CN113648685A (en) * | 2021-08-18 | 2021-11-16 | 唐山华油微生物科技开发有限公司 | Efficient composite microbial demulsifier and application thereof |
| CN113670914B (en) * | 2021-08-19 | 2024-03-08 | 青岛易邦生物工程有限公司 | Bacterial endotoxin detection method of oil emulsion inactivated vaccine |
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| US4961858A (en) * | 1988-07-11 | 1990-10-09 | Henkel Kommanditgesellschaft Auf Aktien | Process for the demulsification of oil/water emulsions using organic demulsifiers and the use of said process |
| CN1562791A (en) * | 2004-03-29 | 2005-01-12 | 同济大学 | Method for fabricating micropowder of lead chromate through coupling treatment of waste water of lead and chrome |
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| US4961858A (en) * | 1988-07-11 | 1990-10-09 | Henkel Kommanditgesellschaft Auf Aktien | Process for the demulsification of oil/water emulsions using organic demulsifiers and the use of said process |
| CN1562791A (en) * | 2004-03-29 | 2005-01-12 | 同济大学 | Method for fabricating micropowder of lead chromate through coupling treatment of waste water of lead and chrome |
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