CN1648058A - Microwave demulsifying and purifying method for emulsifying liquid waste water - Google Patents
Microwave demulsifying and purifying method for emulsifying liquid waste water Download PDFInfo
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- CN1648058A CN1648058A CN 200510045630 CN200510045630A CN1648058A CN 1648058 A CN1648058 A CN 1648058A CN 200510045630 CN200510045630 CN 200510045630 CN 200510045630 A CN200510045630 A CN 200510045630A CN 1648058 A CN1648058 A CN 1648058A
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Abstract
The microwave method of demulsifying and purifying emulsifying liquid waste water in water processing field features that microwave irradiation is adopted in processing emulsifying liquid waste water. The flocculating demulsifier solution is compounded with calcium chloride, aluminum chloride, ferric chloride, aluminum sulfate, ferric sulfate, polyaluminum sulfate, polyferric sulfate and polyacrylamide and the added amount is 0.5-25.0 g/L. The microwave has frequency 2450 MHz or 915 MHz, power 0.4-64 kw, and irradiation time 1-5 min. The microwave demulsifying reactor consists of mainly microwave generator and demulsifying reactor. The present invention has the advantages of oil content lowering rate over 95 %, CODCr lowering rate of about 80 %, short reaction time, low reaction power consumption and easy oil-water separation.
Description
Technical field
The microwave demulsifying and purifying method of emulsifying liquid waste water of the present invention, emulsifying liquid waste water is cut in the emulsifying liquid waste water, the especially industry of floorboard with high oil content high stable difficult degradation that relate to the processing machine processing industry, belongs to water treatment field.
Background technology
All can produce the oil-water emulsion phenomenon in many commercial runs, promptly be a kind of phenomenon that oil molecule and water molecules all contain mutually with liquid state.Therefore the demulsification technology field that has a wide range of applications: the existence of water-oil emulsion in petroleum industry, will increase the burden of accumulating, in the work-ing life of reducing pipeline, must make oily water separation; Emulsion that forms in liquid liquid contacts as extraction process or solution are carried secretly in these application all needs to carry out breakdown of emulsion, could guarantee carrying out smoothly of these Industrial processes.So the research of demulsification technology is one of important topic of chemical separation technology research always.
The emulsifying liquid waste water processing of mechanical processing industry is the difficult problem in the environmental engineering all the time.Industrial emulsion liquid waste water especially mainly contains a large amount of oils and tensio-active agent etc., its oil-contg and chemical oxygen demand (COD) (COD in the cutting fluid waste water
CrDesired value) very high, if not treated just discharging, not only severe contamination surface water body and underground water source destroy ecotope, and the restriction Economic development, cause serious economy loss.Owing to the surfactivity effect of exhibiting high surface promoting agent, make that emulsifying liquid waste water stability is very high and survivable, in the emulsifying liquid waste water so intractability is bigger.The waste water that is the emulsification attitude need carry out breakdown of emulsion, to reach the purpose of oily water separation and purification.
The tradition demulsification technology mainly contains chemical demulsification method, heating demulsification type method, electric demulsification method and physics breakdown of emulsion method.
The heating demulsification type method is the temperature by traditional heating rising emulsion, and along with the rising of temperature, the viscosity of oil phase and density descend, and emulsifying agent increases in the solubleness of water and oil phase simultaneously, makes the coalescent aggravation of emulsion, and liquid-sheet disintegration reaches the purpose of breakdown of emulsion.The deficiency that the heating demulsification type method exists has: (1) breakdown of emulsion liquid temp raises slow, causes the industrial cycle of operation of whole breakdown of emulsion process long; (2) capacity usage ratio is low, causes a large amount of energy wastages, deficiency in economic performance.
The electric demulsification technology is meant that w/o type (water-in-oil-type) emulsion is under the effect of high-voltage electric field (direct current or interchange), fine droplet in drop polarization distortion (expansions, elongation etc.) or the emulsion collides mutually in the high-speed motion process and to cause liquid-sheet disintegration, small droplets to be agglomerated into big drop and realize breakdown of emulsion.Electric demulsification method breakdown of emulsion is mainly used in and separates salt solution, emulsion liquid membrane breakdown of emulsion etc. from crude oil completely.The deficiency that the electric demulsification technology exists has: (1) can only act on the w/o type emulsion, is difficult to reach the effect of breakdown of emulsion for bigger O/W type (oil-in-water-type) emulsion of water content; (2) need plus high-voltage field, energy consumption is very big, and security is low.
Physics breakdown of emulsion method mainly contains two kinds of gravity settling and centrifugal breakdown of emulsion methods.Gravity settling and centrifugal breakdown of emulsion method are to utilize the biphase density difference to carry out breakdown of emulsion.Under gravity and action of centrifugal force, because the density difference, oil phase rises in the milk sap, and water descends, drop generation polymerization, thus realized the biphase separation.The deficiency that physics breakdown of emulsion method exists has: (1) generally speaking, particularly for microemulsion, the speed of polymerization of fluid drops is slower, if there is tensio-active agent, drop substantially can polymerization or speed extremely slow; (2) because speed is slower, and gravity settling equipment is huge, and centrifugal breakdown of emulsion energy consumption is big, economic benefit and demulsification are poor.
Chemical demulsification method is present the most traditional demulsification technology, and it is meant that the pH value of using chemical demulsifier or regulating emulsion makes the method for emulsion fragmentation.The emulsion splitter molecule infiltrates and sticks on the interface of emulsion droplet, displaces emulsifying agent, and the failure surface film, disperse phase is discharged and coalescent, phase-splitting, reaches the purpose of breakdown of emulsion.The chemical demulsification effect is better, and can prevent the formation of emulsion by adding emulsion splitter in advance.The deficiency that chemical demulsification method exists has: (1) must be studied for different emulsion systems and adopt different emulsion splitters, otherwise can not reach good effect; (2) adding emulsion splitter dosage is big in the system, and a lot of emulsion splitters may bring some adverse influences for handled system, so the application of chemical demulsification method has been subjected to very big restriction.
Summary of the invention
Purpose of the present invention overcomes in the chemical demulsification technology with task and exists: (1) must be studied for different emulsion systems and adopt different emulsion splitters, has bigger limitation; (2) add the big deficiency of emulsion splitter dosage in the system, and propose a kind of system is required low, flexible operation, demulsification efficiency and COD
CrThe reduced rate height, oily water separation is easy, and the reaction times is short, the microwave demulsifying and purifying method of the emulsifying liquid waste water that energy consumption is low, special proposition technical solution of the present invention.
Basic design of the present invention is to make full use of microwave exposure to cause advantage and the bridge connection flocculation breakdown of emulsion of flocculation agent and the characteristics of charge neutrality flocculation breakdown of emulsion synergy breakdown of emulsion that polar molecule rotates activating effect and quick internal heating effect; Microwave radiation causes the semipolar water molecules high speed rotating of emulsifying liquid waste water, and oil molecule and other non-polar molecules are difficult for causing rotation, thereby reduced the original high stability of emulsion, promoted the gathering of water molecules, the emulsion temperature raises rapidly in the following short period of time of heating effect at internal loss simultaneously, viscosity significantly reduces, and viscosity reduces and promotes the thermal effect of emulsion in microwave field again, and the disengaging time of oil and water shortens greatly; Flocculating demulsifier can be by bridging effect between the liquid pearl or liquid bead surface charge neutralization causing flocculation breakdown of emulsion; It is collaborative with microwave and flocculation agent breakdown of emulsion to the present invention is based on this mechanism, places microwave field irradiation when making emulsifying liquid waste water add flocculation agent, makes the reaction times of breakdown of emulsion and effect obviously strengthen.
The microwave demulsifying and purifying method of emulsifying liquid waste water proposed by the invention is separated after comprising power control, time control, temperature control and reaction, and it is characterized in that: emulsifying liquid waste water is handled and adopted microwave exposure to carry out; Microwave demulsifying should add flocculating demulsifier before purifying in emulsifying liquid waste water, the flocculating demulsifier that is adopted comprises, calcium chloride, aluminum chloride, iron(ic) chloride, Tai-Ace S 150, ferric sulfate, polymerize aluminum chloride (PAC), bodied ferric sulfate (PFS), polyacrylamide (PAM) and composite flocculating demulsifier thereof, and to prepare the form interpolation of liquid, making its final concn is 0.5-25.0g/L; The processing step of the microwave demulsifying and purifying method of emulsifying liquid waste water is:
The first step is opened the by-pass valve control [5] of inlet channel [7], and emulsifying liquid waste water is injected in the breakdown of emulsion reactor [19], and its volumetric quantity is 2/5 to 2/3 of a reactor volume;
Second step, open flocculating demulsifier and add pipeline [15], the flocculating demulsifier preparation liquid of having prepared is added in the breakdown of emulsion reactor [19];
The 3rd step, close flocculating demulsifier and add pipeline [15], start microwave generator [13], the microwave frequency that is adopted in the processing is 2450MHz or 915MHz, power is 0.4-64kW, and the emulsifying liquid waste water temperature is elevated to 70-110 ℃ gradually from room temperature in the treating processes, keeps 0.5-2min under this temperature, adopt K-type armoured thermocouple [9] and electronic temp indicator [8] indicated temperature, microwave exposure total time is 1-5min;
The 4th step, to shut down, the power supply of closing microwave generator [13] should leave standstill 1-24h with the emulsifying liquid waste water after the microwave exposure processing, and its oil phase, water, solid phase are separated;
The 5th step, oil, water and solid phase after discharging separates, its order is, at first, open outflow of separation of oil pipeline [16] oil phase and collection, after this, the pipeline [17] that is separated of fetching boiling water again gives off water, at last, open settling discharge tube [18], microwave demulsifying is purified the settling removing that is produced and carries out subsequent processes.
The microwave demulsifying and purifying method of emulsifying liquid waste water proposed by the invention, it is further characterized in that: described emulsifying liquid waste water is the emulsifying liquid waste water that mechanical processing industry produces; Described flocculating demulsifier should be mixed with solution morphology during for solid and add in the waste water, can be directly during for liquid or the dilution back add in the waste water, and composite flocculating demulsifier mixes in back adding waste water with two or more flocculating demulsifiers preparation liquid forms.
Use the microwave demulsifying reactor [24] of the microwave demulsifying and purifying method of emulsifying liquid waste water proposed by the invention, it is characterized in that: this reactor mainly is to be made of microwave generator [13] and breakdown of emulsion reactor [19] two parts, multi resonant in the microwave generator [13] magnetron [10] that shakes directly links to each other with an end of microwave catheter [14], the other end of microwave catheter [14] is inserted and secured on centre in it from breakdown of emulsion reactor [19] top center position, breakdown of emulsion reactor [19] is that a top is normal cone platform shape, the bottom is the rounding taper type, and the middle part is cylindrical tubular article, its top is provided with two and leaks energy suppressor [6] and emulsifying liquid waste water inlet channel [7], vapour outlet [20] pipeline is communicated with, adopt K-type armoured thermocouple [9] and electronic temp indicator [8] indicated temperature, K-type armoured thermocouple [9] is in position with microwave catheter [14] sustained height from fixing the insertion until its end of breakdown of emulsion reactor [19] top frustum of a cone sidewall, the sidewall of breakdown of emulsion reactor [19] is by adding pipeline [15] with flocculating demulsifier solution by suppressor [6] by leaking in proper order respectively up and down, separation of oil pipeline [16] and aqueous phase separation pipeline [17] are communicated with, and the bottom of breakdown of emulsion reactor [19] can be communicated with settling discharge tube [17] by suppressor [6] by leaking; These connecting pipelines are equipped with by-pass valve control [7], the gas that produces in the breakdown of emulsion reactor [19], and through vapour outlet [20], alkali lye tourie [21], gas adsorption post [22], last residual exhaust [23] emptying.
Use the microwave demulsifying reactor [24] of the microwave demulsifying and purifying method of emulsifying liquid waste water proposed by the invention, it is characterized in that: the breakdown of emulsion reactor [19] of the microwave demulsifying and purifying method of emulsifying liquid waste water, can adopt its one or more place side by side the industrial flow chart of the microwave demulsifying and purifying method of emulsifying liquid waste water, when adopting many, can use side by side with many breakdown of emulsion reactors [19] by a shared microwave generator [13], its influent waste water pipeline [7] and alkali lye tourie [the 2 stingy body adsorption columns [22] that are equipped with, residual exhaust [23] discharging, and the discharging of oil water phase and solid phase is all by by-pass valve control [5], pipeline uses side by side, in the less emulsifying liquid waste water industrial treatment of flooding quantity, can be equipped with a waste liquid storage pool [1] deposit and be in the emulsifying liquid waste water that standing separation produced in the cycle, adopt a microwave generator [13] to connect a breakdown of emulsion reactor [19] and carry out the microwave demulsifying reaction; And big when the emulsifying liquid waste water quantum of output, when microwave demulsifying industrial equipments flooding quantity is big, when a breakdown of emulsion reactor [19] enters the standing separation cycle, then control mobile microwave producer [13] or regulate waveguide commentaries on classics road device [25] another or other several the microwave demulsifyings purifications that still can carry out emulsifying liquid waste water are in turn reacted and discharging by automatization.
The microwave demulsifying producer of emulsifying liquid waste water that the present invention adopts is further characterized in that: microwave generator [13] is made up of shake magnetron [10] and cooling system [12] of high-voltage regulator [11], multi resonant, the multi resonant magnetron [10] that shakes is provided with an equally distributed 1-32 (PCC) power, and the power of each (PCC) power is 0.4-2.0kW; Cooling system [12] is blower fan cooling or the cooling of sealing recirculated water, the heat that produces when shaking magnetron [10] work in order to cooling high-voltage regulator [11] and multi resonant; Microwave catheter [14], should be to make by microwave reflection is good, high temperature resistant, physical strength is high and cheap hydronalium or rolled copper material, adopt the square-section microwave catheter, its form is the vast sky heart metal tube of square-section, the interior empty size of microwave catheter need be designed to should be able to guarantee to transmit high-order type microwave, promptly by the cutoff wavelength of its definite high-order type microwave of being propagated, the smooth no crator cusp of microwave catheter internal surface palpus is in case major structure becomes the electromagnetic field skewness; Breakdown of emulsion reactor [19] side is cylindrical, top and bottom are truncated cone, its internal surface should be smooth, and its inside does not have outstanding wedge angle or screw, and should be by be difficult for inhaling ripple, being difficult for that burn into is high temperature resistant, physical strength good and be easy to the material processed making, be good with cold rolled stainless steel sheet.
Microwave conductive process in the microwave demulsifying reactor is: the multi resonant of microwave by microwave generator [13] magnetron [10] that shakes produces, passing through microwave catheter [14] again is conducted in the breakdown of emulsion reactor [19], microwave radiation and be reflected into pending emulsifying liquid waste water, and microwave is then fully reacted with emulsifying liquid waste water through repeatedly reflection and refraction at breakdown of emulsion reactor [19] wall; Abundant reacted microwave is absorbed by absorbing material when process is leaked energy suppressor [6] and can therefore not produce leakage.
Definite principle about microwave demulsifying reactor operating parameter is as follows: the scope of flocculating demulsifier dosage is 0.5-25.0g/L, as emulsifying liquid waste water COD
CrIndex and oleaginousness all when low, are got its lower value, work as COD
CrWhen index and oleaginousness are all higher, get its higher limit; For preventing that its volume of packing breakdown of emulsion reactor [19] into should be breakdown of emulsion reactor [19] volumetrical 2/5-2/3 because of the emulsifying liquid waste water boiling causes stopping up each pipeline; The emulsifying liquid waste water temperature is elevated to 70-110 ℃ gradually from room temperature in the treating processes, as emulsifying liquid waste water COD
CrIndex and oleaginousness all when low, are got its lower value, work as COD
CrWhen index and oleaginousness are all higher, get its higher limit; For guaranteeing to obtain good breakdown of emulsion decontamination effect improving, temperature hold-time should be 0.5-2.0min in the reaction, when the flocculating demulsifier dosage more after a little while, get its lower value, when the flocculating demulsifier dosage more for a long time, get its higher limit; Microwave exposure total time is 1-5min, when emulsifying liquid waste water when heat-up rate is fast under microwave exposure, gets its lower value, when heat-up rate is slow, gets its higher limit; Reaction back time of repose is 1-24h, as emulsifying liquid waste water COD
CrWhen all lower the and flocculating demulsifier settling property of index and oleaginousness is better, get its lower value; Otherwise, get its higher limit.
Use the microwave demulsifying reactor of the microwave demulsifying and purifying method of emulsifying liquid waste water, should note: answer the integrity of inspection apparatus, equipment and pipeline and each junction that ne-leakage is arranged before (1) device starts; (2) check being connected and security of power supply system and power unit; (3) leak case of inspection microwave source; (4) after guaranteeing that above-mentioned three check results are qualified, can start the microwave demulsifying reactor, start cooling system simultaneously to guarantee that magnetron does not heat up; (5) to note being used for the permission upper limit of thermometric thermopair, avoid causing its damage; (6) before reaction finishes, must close microwave power supply earlier, and cooling system works on and cools off fully until the multi resonant magnetron that shakes.
Major advantage of the present invention is: control is convenient in (1) microwave heating, starts microwave device, and heating begins immediately; Device is closed, and stops heating at once, does not have the heating lag-effect; (2) since microwave heating be internal heating, rate of heating is fast, thus the reaction times be no more than 5 minutes, energy consumption of reaction is low; (3) microwave transmits by microwave catheter, and security is higher; (4) the oil-contg reduced rate is more than 95%, COD
CrAbout reduced rate 80%, the oily water separation phenomenon is remarkable, is applicable to the elementary or second-stage treatment of emulsifying liquid waste water; (5) device is easy to carry out automatization control in the big factory of emulsifying liquid waste water treatment capacity.
Description of drawings
Further specify details of the present invention below in conjunction with accompanying drawing:
The present invention establishes 4 accompanying drawings altogether, and Fig. 1 is a microwave demulsifying and purifying method process flow diagram synoptic diagram of the present invention; Fig. 2 is the cross-sectional view of facing of the microwave demulsifying reactor that proposes of the present invention; Fig. 3 is the cross-sectional view of facing that is in microwave demulsifying reactor in the technical process; Fig. 4 is in the technical process to adopt the be connected in parallel microwave demulsifying reactor of a microwave generator of two breakdown of emulsion reactors to face cross-sectional view, now is respectively described below:
Fig. 1 is the process flow diagram synoptic diagram of microwave demulsifying and purifying method of the present invention.
Be stored in emulsifying liquid waste water in the waste water storage pool [1] by pipeline, enter in the breakdown of emulsion reactor [19] via the by-pass valve control of strainer [2], lift pump [3], under meter and inlet channel.When emulsifying liquid waste water injection volume is breakdown of emulsion reactor [19] volumetrical 2/5-2/3, should close the by-pass valve control of inlet channel, and the unlatching flocculating demulsifier adds pipeline [15] injection flocculating demulsifier solution.When treating that the flocculating demulsifier dosage reaches industrial breakdown of emulsion requirement, close flocculating demulsifier and add pipeline [15], start microwave generator [13] and startup cooling system wherein, emulsifying liquid waste water is finished the breakdown of emulsion reaction under the combined action of microwave exposure and flocculating demulsifier.Steam waste gas in its reaction process is through vapour outlet [20], alkali lye tourie [21] and gas adsorption column [22], last residual exhaust [23] emptying.Fine line arrow express liquid flow direction among the figure, the heavy line arrow is represented the solid phase emission direction, dotted arrow is represented exhaust gas flow direction.Symbol [16], [17] and [18] are respectively separation of oil pipeline, aqueous phase separation pipeline and settling discharge tube, and empty frame is depicted as microwave demulsifying reactor [24].
Fig. 2 is the cross-sectional view of facing of the microwave demulsifying reactor that proposes of the present invention.
The microwave demulsifying reactor mainly is to be made of microwave generator [13] and breakdown of emulsion reactor [19], microwave generator [13] links to each other with microwave catheter [14], breakdown of emulsion reactor [19] is that a top is normal cone platform shape, the bottom is the rounding taper type, and the middle part is cylindrical tubular article, its top is by leaking energy suppressor [6] and emulsifying liquid waste water inlet channel [7], vapour outlet [20] pipeline is communicated with, adopt K-type armoured thermocouple [9] and electronic temp indicator [8] indicated temperature, the sidewall of breakdown of emulsion reactor [19] is by adding pipeline [15] with flocculating demulsifier by suppressor [6] by leaking in proper order respectively up and down, separation of oil pipeline [16] and aqueous phase separation pipeline [17] are communicated with, and the bottom of breakdown of emulsion reactor [19] can be communicated with settling discharge tube [18] by suppressor [6] by leaking; These connecting pipelines are equipped with by-pass valve control [5], so that the enforcement of the carrying out of breakdown of emulsion reaction and oily water separation operation.Be provided with multi resonant shake magnetron [10], high-voltage regulator [11] and cooling system [12] in the microwave generator [13].Fine line arrow express liquid flow direction among the figure, the heavy line arrow is represented the solid phase emission direction, dotted arrow is represented exhaust gas flow direction.
Fig. 3 is the cross-sectional view of facing that is in microwave demulsifying reactor in the technical process.
Emulsifying liquid waste water is collected in the waste water storage pool [1] of factory, waste water can inject breakdown of emulsion reactor [19] by suppressor [6] through strainer [2], lift pump [3] and under meter [4] by-pass valve control [5] through inlet channel [7] from the top of breakdown of emulsion reactor and through leaking, when the amount of pending emulsifying liquid waste water injection is about the 2/5-2/3 of breakdown of emulsion reactor [19] cubic capacity, stop to inject the by-pass valve control [5] of closing inlet channel [7].Adding by the opening and closing flocculating demulsifier of flocculating demulsifier adds pipeline [15] realization, opening flocculating demulsifier adds pipeline [15] and just injects and prepared the flocculating demulsifier solution of finishing, close flocculating demulsifier and add pipeline [15], flocculating demulsifier solution adds and finishes.After this, open microwave generator [13] and produce microwave, enter in the breakdown of emulsion reactor [19] by microwave catheter [14], microwave is subjected to breakdown of emulsion reactor [19] inwall multiple reflection and refraction, makes emulsifying liquid waste water finish the microwave demulsifying reaction process.After reaction finishes, leave standstill breakdown of emulsion reactor [19], when reaching when leaving standstill the cycle, oil phase, water and solid phase will reach tangible the separation, open separation of oil pipeline [16], aqueous phase separation pipeline [17] and the settling discharge tube [18] that is positioned on breakdown of emulsion reactor [19] side wall surface this moment successively, thereby separate oil phase, water and bottom precipitation, collect oil phase, subsequent processes water and bottom precipitation.The mensuration of the emulsifying liquid waste water temperature of reaction in the breakdown of emulsion reactor [19] adopts K-type armoured thermocouple [9] and electronic temp indicator [8], the gas that emulsifying liquid waste water produces in the microwave demulsifying reaction process and moisture by with vapour outlet [20], alkali lye tourie [21] and the gas adsorption column gas exhaust duct of [22] connection mutually, be residual exhaust [23] emptying then.The fine line direction of arrow that enters breakdown of emulsion reactor [19] among the figure represents to enter the flow direction of emulsifying liquid waste water and flocculating demulsifier solution, flow out the dotted arrow direction indication steam tail gas flow direction of breakdown of emulsion reactor [19], and the flow direction of oil phase, aqueous phase separation is represented with the fine line arrow, and the flow direction that solid deposits is separated is then represented with the heavy line arrow.What empty frame was represented among the figure is microwave demulsifying reactor [24].
Fig. 4 is in to adopt the microwave demulsifying reactor of two breakdown of emulsion reactors microwave generator in parallel to face cross-sectional view in the technical process.
Under emulsifying liquid waste water flooding quantity situation big or water inlet continuously, can adopt many breakdown of emulsion reactors [19] use in parallel, what this figure adopted is that microwave generator two breakdown of emulsion reactors of drive [19] are connected in parallel, and in the use, two breakdown of emulsion reactors [19] branch precedence takes turns to operate.Show among the figure that two breakdown of emulsion reactors [19] in parallel all are connected with microwave generator [13] by microwave catheter [14], microwave generator [13] changes road device [25] by the waveguide in the microwave catheter [14] and determines the wherein any breakdown of emulsion reactor of irradiation [19].Its technical process is: behind emulsifying liquid waste water process strainer [2], the lift pump [3], enter two tributary under meters [4] in parallel, the by-pass valve control [5] of inlet channel [7], and inject in first breakdown of emulsion reactor [19], when injection rate is breakdown of emulsion reactor [19] volumetrical 2/5-2/3, stop to inject, close the by-pass valve control [5] of this breakdown of emulsion reactor [19] inlet channel [7], and open the by-pass valve control [5] of another branch road inlet channel [7], emulsifying liquid waste water is injected in second breakdown of emulsion reactor [19].After adding flocculating demulsifier solution in first breakdown of emulsion reactor [19], by regulating waveguide commentaries on classics road device [25] microwave generator [13] is reacted to first breakdown of emulsion reactor [19], reaction is left standstill first breakdown of emulsion reactor [19] after finishing, second breakdown of emulsion reactor this moment [19] meets the demands as injection rate, then regulates waveguide commentaries on classics road device [25] microwave generator [13] is reacted second breakdown of emulsion reactor [19].After first breakdown of emulsion reactor [19] reaches time of repose, separate oil phase, water and bottom precipitation successively, after this continue first breakdown of emulsion reactor [19] fill cycle is operated, and second breakdown of emulsion reactor [19] reaction finishes and standing separation after, also begin fill cycle operation next time, this processing step of repetitive operation so circulates.Under emulsifying liquid waste water flooding quantity situation big or water inlet continuously, then realize industrial treatment operation automatic continuous and handiness by the by-pass valve control [5] and the waveguide commentaries on classics road device [25] in robot control system(RCS) adjusting inlet channel [7] tributary.Arrow and all same Fig. 3 of other symbols.
Embodiment
Embodiment 1:
Adopt ferric sulfate as flocculating demulsifier to Dalian * * processing of the emulsifying liquid waste water that company provides
Dalian * * emulsifying liquid waste water color that company provides is an oyster white, it is neutral that the pH value is, and is all moderate emulsifying liquid waste water of oleaginousness chemistry nutritional requirement.Through Analysis Results of Water Quality be: O/W (oil-in-water) type emulsion, its pH value is 7.06, COD
CrDesired value is 24976.5mg/L, BOD
5(biochemical oxygen demand (BOD)) desired value is 4018.9mg/L, and oil-contg is 4913.0mg/L.
The microwave demulsifying cleansing operation of emulsifying liquid waste water
Utilize the microwave demulsifying and purifying method of the emulsifying liquid waste water among the present invention, adopt of the processing of a microwave demulsifying reactor, the steps include: the cutting emulsifying liquid waste water
The first step is injected pending emulsifying liquid waste water in the breakdown of emulsion reactor [19], be about breakdown of emulsion reactor [19] volumetrical 2/5 to volume till;
In second step, the interpolation of flocculating demulsifier adopts ferrum sulfuricum oxydatum solutum as flocculating demulsifier in the present embodiment, and flocculating demulsifier adds after being formulated as solution with the ferric sulfate solid chemicals, and the flocculating demulsifier concentration in the emulsifying liquid waste water is the ferric sulfate of 0.5g/L;
The 3rd step started microwave demulsifying reactor [24], and the microwave power of selecting for use is 0.4kW, and frequency is 2450MHz, and temperature rises to 100 ℃, kept temperature 2min, and the total time of microwave exposure is 5min.Shake magnetron [10] before at the unlatching multi resonant, start the cooling system [12] of microwave demulsifying device inside, multi resonant magnetron [10] Yin Wendu that shakes is too high and damage when preventing microwave demulsifying, adopt K-type armoured thermocouple [9] and electronic temp indicator [8] indicated temperature, the steam waste gas that produces in its breakdown of emulsion process is through vapour outlet [20], alkali lye tourie [21], gas adsorption post [22], last residual exhaust [23] emptying;
The 4th step, when arriving the microwave demulsifying reaction concluding time, close microwave generator [13], the multi resonant magnetron [10] that shakes will no longer be worked, cooling system [12] works on, lower the temperature with magnetron [10] that multi resonant is shaken, treat that its internal temperature is cooled to about room temperature, closes the power supply of microwave generator [13];
The 5th step, leave standstill breakdown of emulsion reactor [19] 1h after, interior the liquid layer of breakdown of emulsion reactor [19] does not have oil reservoir and occurs, but layering is obvious, the transparent liquid in upper strata is almost colourless, lower floor is that tawny precipitates, and opens each pipeline water is separated with the suspension solid phase.
In the 6th step, effect detection is measured the COD that handles the back water
Cr, BOD
5With the oil-contg index, water COD
CrDesired value is 6215.09mg/L, BOD
5Desired value is 382.87mg/L, and it is 5.371mg/L that ultraviolet spectrophotometry is measured oil-contg.COD
CrThe index reduced rate is 75.11%, BOD
5The index reduced rate is 96.28%, and oil-contg index reduced rate is 99.90%.
Embodiment 2:
Adopt polymerize aluminum chloride and the composite flocculating demulsifier of bodied ferric sulfate to Dalian * * processing of the emulsifying liquid waste water that company provides
Dalian * * emulsifying liquid waste water Analysis Results of Water Quality that company provides is with embodiment 1, for: O/W (oil-in-water) type emulsion, its pH value is 7.06, COD
CrDesired value is 24976.5mg/L, BOD
5Desired value is 4018.9mg/L, and oil-contg is 4913.0mg/L.
The described microwave demulsifying cleansing operation of claim according to the present invention step, adopt of the processing of a microwave demulsifying reactor to the cutting emulsifying liquid waste water, its step is with embodiment 1, wherein: till pending emulsifying liquid waste water injects in the breakdown of emulsion reactor [19] and to be about breakdown of emulsion reactor [19] volumetrical 1/2 to volume; Adopt polymeric aluminum chlorides solution to mix with polymeric ferrous sulphate solution in the present embodiment as composite flocculating demulsifier, flocculating demulsifier is 10.0% to be formulated as solution with industrial polymerize aluminum chloride solid chemicals by mass percent, the bodied ferric sulfate medicament is liquid industrial goods, dilution is 10.0% solution for mass percent, mix the back and add, make that the composite concentration of the flocculating demulsifier in the emulsifying liquid waste water is 2.0g/L polymerize aluminum chloride+1.0g/L bodied ferric sulfate; The power of microwave generator is 18kW, and frequency is 915MHz; The emulsifying liquid waste water temperature rises to 70 ℃, keeps temperature 2min, and the total time of microwave exposure is 4min; The time of repose of breakdown of emulsion reactor [19] is 16h.The interior liquid layer of breakdown of emulsion reactor [19] does not have the oil reservoir appearance behind the 16h, but layering is obvious, and the transparent liquid in upper strata is almost colourless, and lower floor is the tawny precipitation, opens each pipeline water is separated with the suspension solid phase.
Effect detection, the COD of mensuration water
CrWith oil-contg index, COD
CrDesired value is 4856.54mg/L, and it is 4.181mg/L that ultraviolet spectrophotometry is measured oil-contg.COD
CrThe index reduced rate is 80.56%, and oil-contg index reduced rate is 99.91%.
Embodiment 3:
Adopt microwave demulsifying reactor right * * machine tool plant * * processing of the industrial cutting fluid emulsifying liquid waste water of Workshop Production
This be an emulsifying liquid waste water year output be 3 tons * * machine tool plant * * workshop, emulsifying liquid waste water component stable homogeneous is milk yellow, COD
CrBe 50000-200000mg/L, the pH value is alkalescence, is oleaginousness and the higher emulsifying liquid waste water of chemical nutritional requirement.
The sampling analysis result
Water quality parameter: emulsifying liquid waste water is O/W (oil-in-water) type emulsion, and its pH value is 11.60, COD
CrDesired value is 99568.4mg/L, BOD
5Desired value is 28331.4mg/L, and oil-contg is 15301.15mg/L.
Flocculating demulsifier is selected
Select and buy the liquid industrial goods of bodied ferric sulfate commonly used in the water treatment, recording this polymeric ferrous sulphate solution all iron content with the EDTA complexometry is 2.466mol/L.
The microwave demulsifying cleansing operation of emulsifying liquid waste water
The first step is injected pending emulsifying liquid waste water in the breakdown of emulsion reactor [19] via lift pump [3] from waste water storage pool [1] and strainer [2], be about breakdown of emulsion reactor [19] volumetrical 2/3 to volume till;
Second step, open the by-pass valve control [5] that flocculating demulsifier adds pipeline [15], flocculating demulsifier solution is added in the emulsifying liquid waste water, the concentration that makes bodied ferric sulfate in the emulsifying liquid waste water is 25.0g/L;
The 3rd step, start the cooling system [12] and the microwave generator [13] of microwave demulsifying device inside according to the order of sequence, microwave exposure power is 64kW, frequency is 915MHz, temperature rises to 110 ℃, keep temperature 0.5min, the total time of microwave exposure is 1min, adopts K-type armoured thermocouple [9] and electronic temp indicator [8] indicated temperature;
The 4th step, when arriving the microwave demulsifying reaction concluding time, close microwave generator [13], cooling system [12] continues the multi resonant magnetron [10] that shakes is lowered the temperature, and treats that its internal temperature is cooled to about room temperature, closes the power supply of microwave generator [13];
In the 5th step, the microwave demulsifying method of emulsifying liquid waste water begins to leave standstill.Emulsifying liquid waste water is oleaginousness and all higher emulsifying liquid waste water of chemical nutritional requirement among this embodiment, and the selection time of repose is 24h;
The 6th step, effect detection, after the leaving standstill of reactor 24h, solution is divided into four layers, and the upper strata is the black oil reservoir, and the middle level is a Vandyke brown border solution layer, and it is the yellow solution layer down, orlop is the tawny flocks.Isolate oil phase and settling solid phase, collect reacted water, and measure its COD
Cr, BOD
5With the oil-contg index, be added into COD after the purification of waste water with the flocculating demulsifier of 25.0g/L polymeric ferrous sulphate solution
CrDesired value is 16137.92mg/L, BOD
5Desired value is 1834.79mg/L, and oil-contg only is 5.235mg/L in the waste water of ultraviolet spectrophotometry measurement purification back, COD
CrThe index reduced rate is 83.79%, BOD
5The index reduced rate is 93.52%, and oil-contg index reduced rate is 99.97%.Implement in the test exit gas have been carried out the GC/MS analysis at this in addition, do not have organic molecule to be detected.
Implement in the test at this, studied by the pH value of regulating emulsifying liquid waste water also that concentration is that the 10g/L bodied ferric sulfate is to handling the COD of emulsifying liquid waste water afterwards under different pH values
CrThe influence of index, the microwave flocculation demulsifying and purifying method that draws emulsifying liquid waste water is less demanding to the pH value of emulsion system, and the pH value is in the wide spectrum scope, and the microwave of emulsifying liquid waste water flocculation demulsifying and purifying method is to its COD
CrIndex reduced rate, BOD
5Index reduced rate and oil-contg index reduced rate all can obtain good effect.
Embodiment 4:
Adopt microwave generator two breakdown of emulsion reactors in parallel right * * machine tool plant * * emulsifying liquid waste water of Workshop Production handles
This be an emulsifying liquid waste water year output be 7 tons * * machine tool plant * * workshop, emulsifying liquid waste water component stable homogeneous is newborn grey, COD
CrBe 50000-200000mg/L, it is neutral that the pH value is, and is the higher emulsifying liquid waste water of the moderate and chemical nutritional requirement of oleaginousness.
Emulsifying liquid waste water through Analysis Results of Water Quality is: O/W (oil-in-water) type emulsion, its pH value is 7.03, COD
CrDesired value is 92318.4mg/L, BOD
5Desired value is 10279.01mg/L, and oil-contg is 9820.6mg/L.
Adopt the microwave demulsifying reactor among the present invention, and place the production technique streamline, contain the microwave demulsifying purifying treatment of emulsion, step is:
The first step places the technological process of production with two breakdown of emulsion reactors [19], starts water inlet after the bug check, till first breakdown of emulsion reactor [19] is filled to volume and is about breakdown of emulsion reactor [19] volumetrical 2/3; Open the by-pass valve control [5] that flocculating demulsifier adds pipeline [15], flocculating demulsifier solution is added in the pending emulsifying liquid waste water, flocculating demulsifier adds after being formulated as solution with the ferric sulfate solid chemicals, is added to till the concentration of ferric sulfate 5g/L in the emulsifying liquid waste water; Regulate waveguide and change road device [25], guarantee to start first breakdown of emulsion reactor [19] of microwave generator [13] back and carry out breakdown of emulsion purification reaction, wherein microwave exposure power is 64kW, frequency is 915MHz, temperature rises to 85 ℃, keep temperature 1.0min, the total time of microwave exposure is 2.0min, leaves standstill 12h after the end;
Second step, when first breakdown of emulsion reactor [19] water filling finishes in the first step, turn to second breakdown of emulsion reactor [19] to inject emulsifying liquid waste water successively, add flocculating demulsifier solution, regulate waveguide commentaries on classics road device [25] and start microwave generator [13], wherein each parameter is all described with the first step;
The 3rd step, with behind the 12h first breakdown of emulsion reactor [19] oil phase, water and the solid phase after the standing separation successively separate discharge handle, after treating first breakdown of emulsion reactor [19] emptying, to first breakdown of emulsion reactor [19] water filling, after this operate described again with the first step;
The 4th step, with behind the 12h second the breakdown of emulsion reactor [19] after the standing separation be separated according to the 3rd step and carry out identical emission treatment, after treating that second breakdown of emulsion reactor [19] emptying and first breakdown of emulsion reactor [19] water filling finish, to second breakdown of emulsion reactor [19] water filling, operation after this is described with second step again;
The 5th step, effect detection, it is obvious to observe the waste water liquid layer layering of just having handled behind the 12h, and the upper strata is orange-yellow suspended particle, and lower floor is a yellow solution, and the no beds of precipitation occur, and then water can be separated water COD after this technical finesse with the suspension solid phase
CrDesired value is 11258.73mg/L, BOD
5Desired value is 1025.77mg/L, and it is 6.322mg/L that ultraviolet spectrophotometry is measured oil-contg.COD
CrThe index reduced rate is 87.80%, BOD
5The index reduced rate is 90.02%, and oil-contg index reduced rate is 99.94%.
Claims (8)
1. the microwave demulsifying and purifying method of emulsifying liquid waste water is separated after comprising power control, time control, temperature control and reaction, it is characterized in that:
A) emulsifying liquid waste water is handled and is adopted microwave exposure to carry out;
B) microwave demulsifying should add flocculating demulsifier before purifying in emulsifying liquid waste water, the flocculating demulsifier that is adopted comprises, calcium chloride, aluminum chloride, iron(ic) chloride, Tai-Ace S 150, ferric sulfate, polymerize aluminum chloride (PAC), bodied ferric sulfate (PFS), polyacrylamide (PAM) and composite flocculating demulsifier thereof, and to prepare the form interpolation of liquid, making its final concn is 0.5-25.0g/L;
C) processing step of the microwave demulsifying and purifying method of emulsifying liquid waste water is:
The first step is opened the by-pass valve control [5] of inlet channel [7], and emulsifying liquid waste water is injected in the breakdown of emulsion reactor [19], and its volumetric quantity is 2/5 to 2/3 of a reactor volume;
Second step, open flocculating demulsifier and add pipeline [15], the flocculating demulsifier preparation liquid of having prepared is added in the breakdown of emulsion reactor [19];
The 3rd step, close flocculating demulsifier and add pipeline [15], start microwave generator [13], the microwave frequency that is adopted in the processing is 2450MHz or 915MHz, power is 0.4-64kW, and the emulsifying liquid waste water temperature is elevated to 70-110 ℃ gradually from room temperature in the treating processes, keeps 0.5-2min under this temperature, adopt K-type armoured thermocouple [9] and electronic temp indicator [8] indicated temperature, microwave exposure total time is 1-5min;
The 4th step, to shut down, the power supply of closing microwave generator [13] should leave standstill 1-24h with the emulsifying liquid waste water after the microwave exposure processing, and its oil phase, water, solid phase are separated;
The 5th step, oil, water and solid phase after discharging separates, its order is, at first, open outflow of separation of oil pipeline [16] oil phase and collection, after this, the pipeline [17] that is separated of fetching boiling water again gives off water, at last, open settling discharge tube [18], microwave demulsifying is purified the settling removing that is produced and carries out subsequent processes.
2. the microwave demulsifying and purifying method of emulsifying liquid waste water according to claim 1 is characterized in that: described emulsifying liquid waste water is the emulsifying liquid waste water that mechanical processing industry produces.
3. the microwave demulsifying and purifying method of emulsifying liquid waste water according to claim 1, it is characterized in that: when described flocculating demulsifier is solid, should be mixed with solution morphology adds in the waste water, during for liquid, can directly or after the dilution add in the waste water, and composite flocculating demulsifier mixes in the back adding waste water with two or more flocculating demulsifiers preparation liquid forms.
4. use the microwave demulsifying reactor [24] of the microwave demulsifying and purifying method of emulsifying liquid waste water as claimed in claim 1, it is characterized in that: this reactor mainly is to be made of microwave generator [13] and breakdown of emulsion reactor [19] two parts, multi resonant in the microwave generator [13] magnetron [10] that shakes directly links to each other with an end of microwave catheter [14], the other end of microwave catheter [14] is inserted and secured on centre in it from breakdown of emulsion reactor [19] top center position, breakdown of emulsion reactor [19] is that a top is normal cone platform shape, the bottom is the rounding taper type, and the middle part is cylindrical tubular article, its top is provided with two and leaks energy suppressor [6] and emulsifying liquid waste water inlet channel [7], vapour outlet [20] pipeline is communicated with, adopt K-type armoured thermocouple [9] and electronic temp indicator [8] indicated temperature, K-type armoured thermocouple [9] is in position with microwave catheter [14] sustained height from fixing the insertion until its end of breakdown of emulsion reactor [19] top frustum of a cone sidewall, the sidewall of breakdown of emulsion reactor [19] is by adding pipeline [15] with flocculating demulsifier solution by suppressor [6] by leaking in proper order respectively up and down, separation of oil pipeline [16] and aqueous phase separation pipeline [17] are communicated with, and the bottom of breakdown of emulsion reactor [19] can be communicated with settling discharge tube [17] by suppressor [6] by leaking; These connecting pipelines are equipped with by-pass valve control [7], the gas that produces in the breakdown of emulsion reactor [19], and through vapour outlet [20], alkali lye tourie [21], gas adsorption post [22], last residual exhaust [23] emptying.
5. according to the microwave demulsifying reactor [24] of the microwave demulsifying and purifying method of the described emulsifying liquid waste water of claim 4, it is characterized in that: microwave generator [13] is made up of shake magnetron [10] and cooling system [12] of high-voltage regulator [11], multi resonant, the multi resonant magnetron [10] that shakes is provided with an equally distributed 1-32 (PCC) power, and the power of each (PCC) power is 0.4-2.0kW; Cooling system [12] is blower fan cooling or the cooling of sealing recirculated water, the heat that produces when shaking magnetron [10] work in order to cooling high-voltage regulator [11] and multi resonant.
6. the microwave demulsifying reactor [24] of the microwave demulsifying and purifying method of emulsifying liquid waste water according to claim 4, it is characterized in that: microwave catheter [14] should be good by microwave reflection, high temperature resistant, hydronalium that physical strength is high and cheap or rolled copper material are made, adopt the square-section microwave catheter, its form is the vast sky heart metal tube of square-section, the inner cavity size of microwave catheter need be designed to should be able to guarantee to transmit high-order type microwave, promptly determine the cutoff wavelength of the high-order type microwave propagated by it, the smooth no crator cusp of microwave catheter internal surface palpus is in case major structure becomes the electromagnetic field skewness.
7. the microwave demulsifying reactor [24] of the microwave demulsifying and purifying method of emulsifying liquid waste water according to claim 4, it is characterized in that: breakdown of emulsion reactor [19] internal surface should be smooth, and its inside does not have outstanding wedge angle or screw, and should be by be difficult for inhaling ripple, being difficult for that burn into is high temperature resistant, physical strength good and be easy to the material processed making, be good with cold rolled stainless steel sheet.
8. application rights requires the microwave demulsifying reactor [24] of the microwave demulsifying and purifying method of 4 described emulsifying liquid waste waters, it is characterized in that: the breakdown of emulsion reactor [19] of the microwave demulsifying and purifying method of emulsifying liquid waste water, can adopt its one or more place side by side the industrial flow chart of the microwave demulsifying and purifying method of emulsifying liquid waste water, when adopting many, can use side by side with many breakdown of emulsion reactors [19] by a shared microwave generator [13], its influent waste water pipeline [7] and the alkali lye tourie [21] that is equipped with, gas adsorption post [22], residual exhaust [23] discharging, and the discharging of oil water phase and solid phase is all by by-pass valve control [5], pipeline uses side by side, in the less emulsifying liquid waste water industrial treatment of flooding quantity, can be equipped with a waste liquid storage pool [1] deposit and be in standing separation and produces in the cycle and contain emulsifying liquid waste water, adopt a microwave generator [a 13] breakdown of emulsion reactor of connection [19] to carry out microwave demulsifying and react; And big when the emulsifying liquid waste water quantum of output, when microwave demulsifying industrial equipments flooding quantity is big, when a breakdown of emulsion reactor [19] enters the standing separation cycle, then control mobile microwave producer [13] or regulate waveguide commentaries on classics road device [25] another or other several the microwave demulsifyings purifications that still can carry out emulsifying liquid waste water are in turn reacted and discharging by automatization.
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