CN112062235B - Oil-water separation device based on composite magnet - Google Patents
Oil-water separation device based on composite magnet Download PDFInfo
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- CN112062235B CN112062235B CN202010941307.7A CN202010941307A CN112062235B CN 112062235 B CN112062235 B CN 112062235B CN 202010941307 A CN202010941307 A CN 202010941307A CN 112062235 B CN112062235 B CN 112062235B
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
Abstract
The invention discloses an oil-water separation device based on a composite magnet, which comprises a magnetic separation tank, wherein the magnetic separation tank is provided with a stirring device, the stirring device comprises a stirring paddle, the stirring paddle extends into the magnetic separation tank, an electromagnet is arranged in the stirring paddle, the magnetic separation tank is also connected with a mixed liquid inlet device and a suction device, the magnetic separation tank or the stirring device is connected with a lifting device, the lifting device is used for adjusting the height of the stirring paddle from the bottom of the magnetic separation tank, and magnetic particles with lipophilicity on the surface are contained in the magnetic separation tank.
Description
Technical Field
The invention belongs to the field of water treatment devices, and particularly relates to an oil-water separation device based on a composite magnet.
Background
In the fields of chemical production, sewage treatment and the like, oil-water separation treatment needs to be carried out on an oil-containing water body under a large number of scenes so as to achieve the purposes of resource recovery, pollution reduction, economic benefit improvement and the like. At present, two main methods for separating oil from water are mechanical separation and physical adsorption. The mechanical separation generally utilizes the density difference of oil and water phases and relies on gravity or a centrifugal mode to carry out separation treatment, although the oily wastewater treated in unit time has larger amount, the separation is not thorough and the effect is poor; the physical adsorption mode mainly depends on the performance of the adsorption material, common adsorption materials comprise activated carbon, porous foam and the like, but the problems of small oil absorption and low oil-water selectivity exist, the separation efficiency is low, and the adsorption material is difficult to treat subsequently. The two separation modes are combined, so that the effect and efficiency of oil-water separation are expected to be improved. Patent document CN101215060A discloses an apparatus for treating oilfield wastewater, which uses modified magnetic particles for adsorption filtration. However, the problems of incomplete separation, low separation efficiency and the like still exist, and the characteristics of complicated device, troublesome operation and the like exist.
Disclosure of Invention
In view of this, the present invention provides an oil-water separator based on a composite magnet.
The technical scheme is as follows:
the oil-water separation device based on the composite magnet comprises a magnetic separation tank and is characterized in that a stirring device is arranged in the magnetic separation tank, the stirring device comprises a stirring paddle, the stirring paddle extends into the magnetic separation tank, and an electromagnet is arranged in the stirring paddle;
the magnetic separation tank is also connected with a mixed liquid inlet device and a suction device;
the magnetic separation tank or the stirring device is connected with a lifting device, and the lifting device is used for adjusting the height of the stirring blade pitch from the bottom of the magnetic separation tank;
magnetic particles are contained in the magnetic separation tank, and the surfaces of the magnetic particles are lipophilic.
By adopting the design, an oil-water mixture is added into the magnetic separation tank, the electromagnet in the stirring paddle is not electrified, the stirring paddle enables the magnetic particles with oleophylic surfaces to fully adsorb the oil phase, the stirring paddle is adjusted to be positioned at a proper position in the magnetic separation tank according to the density of the oil phase relative to the water phase, the electromagnet is electrified to attract the magnetic particles, so that the oil phase is gathered, the water phase and the oil phase are sequentially extracted and separated by using the suction device, the whole oil-water separation device is ingenious in design, after the electromagnet is powered off, the magnetic particles are dispersed in liquid again under the centrifugal force action when the stirring paddle rotates, and the oil-water separation device can be repeatedly used for many times.
According to a preferable technical scheme, the stirring device further comprises a stirring support, wherein a stirring shaft is arranged on the stirring support through a bearing, the stirring shaft is vertically arranged, the upper end of the stirring shaft is in transmission connection with a driving device for driving the stirring shaft to rotate, the lower end of the stirring shaft is connected with the stirring paddle, and the stirring shaft is in a hollow rod shape;
the stirring paddle comprises a stirring head with an internal cavity, the outer wall of the stirring head is fixedly connected with a blade, the inner cavity of the stirring head is communicated with the inner cavity of the stirring shaft, the electromagnet is arranged in the stirring head, and a lead of the electromagnet is connected with a power supply after being led out through the inner cavity of the stirring shaft;
the electromagnet is coated by the stirring head in a liquid seal mode, and the shell of the stirring head is made of plastics.
By adopting the design, the electromagnet is reliably installed, does not interfere with the stirring paddle, and is separated from the magnetic particles and the liquid to be separated.
As a preferred technical scheme, the upper end of the stirring shaft is in threaded connection with a buckle cover, the upper surface of the buckle cover is provided with two floating electrodes, and the distance from one floating electrode to the central line of the buckle cover is greater than the distance from the other floating electrode to the central line of the buckle cover;
and a butt joint disc is arranged right above the stirring shaft, the lower surface of the butt joint disc corresponds to two floating electrodes, the two floating electrodes are respectively provided with an annular electrode, the two floating electrodes are respectively floated and abutted against the corresponding annular electrodes, and the two annular electrodes are respectively connected with the two poles of the power supply through leads.
Design more than adopting, two floating electrodes and two annular electrode mutually support for when the stirring rake rotates, still can be to the electro-magnet circular telegram, can be like this with the stirring head of its adsorbed oil phase attraction of magnetic particle intercommunication in the low-speed stirring, be convenient for fully assemble the oil phase in the oil water mixture.
As a preferred technical scheme, the driving device is a speed regulating motor, the speed regulating motor is installed on the stirring support, a driving wheel is arranged on an output shaft of the speed regulating motor, a driven wheel is arranged on the stirring shaft, and the driven wheel is in transmission connection with the driving wheel through a belt.
By adopting the design, the rotating speed of the stirring paddle is convenient to adjust, and the rotating speed requirements of different stages are met.
As a preferred technical scheme, the mixed liquid inlet device comprises a high-position liquid storage tank, and the high-position liquid storage tank is connected with the magnetic separation tank through a suction pipe.
By adopting the design, the oil-water mixture to be separated is conveniently led into the magnetic separation tank.
As preferred technical scheme, above-mentioned suction device includes the liquid pump, the inlet of this liquid pump pass through the suction tube with the magnetism separating tank is connected, and the liquid outlet of this liquid pump is connected with first parting liquid storage tank.
By adopting the design, when oil and water are separated, one phase is extracted by the suction device, and the position of the suction pipe extending into the magnetic separation tank can be adjusted, so that the device is suitable for the suction of the oil and water phases with different densities and different interface heights.
As a preferred technical solution, a liquid outlet with a sealing valve is provided at the bottom of the magnetic separation tank, and a second separation liquid storage tank is provided below the liquid outlet.
By adopting the design, when one of the oil phase and the water phase is extracted, the other phase can be discharged from the liquid outlet and collected.
As a preferred technical scheme, the lifting device is arranged below the magnetic separation groove, the lifting device is a hydraulic cylinder, the hydraulic cylinder is vertically arranged, the cylinder body of the hydraulic cylinder is fixed, a support frame is arranged at the upper end of a piston rod of the hydraulic cylinder, and the magnetic separation groove is arranged on the support frame.
By adopting the design, the stirring head is adjusted to the oil phase subjected to phase separation through the lifting adjustment magnetic separation tank.
Preferably, the magnetic particles are Fe 3 O 4 @Co 3 O 4 Composite magnetic particles of Fe 3 O 4 @Co 3 O 4 The composite magnetic particles are made of Fe 3 O 4 Core and Co coated on the surface thereof 3 O 4 Shell composition of Fe 3 O 4 @Co 3 O 4 The surface of the composite magnetic particle is grafted with polyethyleneimine.
By adopting the design, the composite magnetic particles have good lipophilicity and enhanced structural stability through grafting of the polyethyleneimine, and are not easy to agglomerate.
Preferably, fe is used as the main component 3 O 4 @Co 3 O 4 The surface of the composite magnetic particle is coated with a substrate polymer, the substrate polymer layer is provided with a catechol group, and the substrate polymer is used for grafting polyethyleneimine on the surface of the substrate polymer layer through the reaction of the catechol group and the amino group of the polyethyleneimine.
By adopting the design, the Fe is conveniently realized 3 O 4 @Co 3 O 4 And (3) grafting modification of the surface of the composite magnetic particle.
Compared with the prior art, the invention has the following beneficial effects: the oil-water mixture is added into the magnetic separation tank, the oil phase is adsorbed by the magnetic particles after being stirred at a low speed, then the stirring paddle is adjusted to be positioned at a proper position in the magnetic separation tank, the electromagnet attracts the magnetic particles after being electrified, so that the oil phase is gathered, the water phase and the oil phase are extracted and separated by the suction device, and the device is ingenious in design and easy to operate.
Drawings
FIG. 1 shows the solvothermal preparation of Fe 3 O 4 @Co 3 O 4 A flow chart of composite magnetic particles;
FIG. 2 is a surface functionalization grafting technology for preparing Fe 3 O 4 @Co 3 O 4 -a flow diagram of PEI composite magnetic particles;
FIG. 3 shows Fe obtained by the method of example 1 3 O 4 @Co 3 O 4 Composite magnetic particles and Fe 3 O 4 @Co 3 O 4 -an X-ray diffraction pattern of PEI composite magnetic particles;
FIG. 4 is a scanning electron microscope photograph of a composite magnetic particle prepared by the method of example 1, in which (a) Fe 3 O 4 @Co 3 O 4 Composite magnetic particles, (b, c, d) Fe 3 O 4 @Co 3 O 4 -PEI composite magnetic particles;
FIG. 5 shows Fe obtained by the method of example 1 3 O 4 @Co 3 O 4 、Fe 3 O 4 @Co 3 O 4 /Pdop、Fe 3 O 4 @Co 3 O 4 -infrared absorption spectrum of PEI;
FIG. 6 shows Fe obtained by the method of example 1 3 O 4 @Co 3 O 4 -PEI surface contact angle measurement picture, wherein: (a) test process schematic; (b) water contact angle test photograph; (c) photo of oil contact angle test;
FIG. 7 shows Fe 3 O 4 @Co 3 O 4 Composite magnetic particles and Fe 3 O 4 @Co 3 O 4 -magnetic property profile of the PEI composite magnetic particles;
FIG. 8 shows the use of Fe 3 O 4 @Co 3 O 4 Composite magnetic particles and Fe 3 O 4 @Co 3 O 4 -photo of oil-water separation experiment of PEI composite magnetic particles, wherein: adding composite magnetic particles, water and oil into a glass bottle, (b) carrying out ultrasonic treatment to fully mix, (c) standing for a period of time, and (d) adding a permanent magnet for adsorption separation;
FIG. 9 is a photograph showing the transmittance of the oil-water mixture after different treatments, wherein the left, middle and right sides of the photograph are respectively the emulsion containing Fe dispersed in the oil-containing emulsion 3 O 4 @Co 3 O 4 -PEI composite magnetic particles, magnet attracting Fe dispersed in oil-containing emulsion 3 O 4 @Co 3 O 4 Pictures of PEI composite magnetic particles, wherein (a) the bottle back is a text background, (b) the bottle back is a white background, (c) the bottle back is a red background, (d) Fe 3 O 4 @Co 3 O 4 -adsorption capacity of PEI composite magnetic particles for different types of oil;
FIG. 10 is Fe 3 O 4 @Co 3 O 4 -graph of adsorption capacity of PEI composite magnetic particles on gasoline as a function of adsorption time, wherein: (ii) (a) adsorption capacity, (b) adsorption efficiency;
FIG. 11 is Fe 3 O 4 @Co 3 O 4 The adsorption effect of the composite magnetic particles for oil-water separation adsorption treatment is realized by cyclic regeneration, and the transmittance of a water body after oil-water separation is taken as an evaluation index;
FIG. 12 is a schematic view of the oil-water separator;
FIG. 13 is a schematic structural view of a stirring paddle;
FIG. 14 is a schematic view of a ring electrode mounted on a docking tray.
Detailed Description
The present invention will be further described with reference to the following examples and the accompanying drawings.
(one) preparation of Fe 3 O 4 @Co 3 O 4 -PEI magnetic composite particles
Example 1
Method for preparing Fe by solvothermal method 3 O 4 @Co 3 O 4 -PEI composite magnetic particles, comprising a process for the preparation of Fe 3 O 4 @Co 3 O 4 Composite magnetic particles and Fe 3 O 4 @Co 3 O 4 The composite magnetic particle is modified in two processes, which are respectively illustrated in fig. 1 and fig. 2. The method comprises the following specific steps:
step one, deionized water, ethanol and butanol are mixed according to the weight ratio of 120:120:3 as a reaction solvent (solution A), 0.60g of FeSO was added 4 ·7H 2 O、1.20g CoCl 2 ·6H 2 O, 0.50g of Na 3 C 6 H 5 O 7 ·2H 2 O and 0.16g of CO (NH) 2 ) 2 Mixing, dissolving in water solution, stirring for 5-30 min, and adding solution A into the solution;
step two, after continuously stirring the mixed solution for 10min, adjusting the pH value of the solution to 7-10, transferring the solution to a 30ml polytetrafluoroethylene lining stainless steel high-pressure reaction kettle, and reacting for 10h at 160 ℃ to obtain brown yellow Fe 3 O 4 @ CoOOH precursor powder;
step three, collecting the obtained precursor powder by using a magnet, washing the precursor powder by using deionized water and ethanol for multiple times, and drying the precursor powder in a vacuum drying oven at the temperature of 60 ℃ for more than 12 hours;
step four, roasting the obtained precursor in a muffle furnace at the temperature of 300 ℃ for 1h to prepare the needed Fe 3 O 4 @Co 3 O 4 Composite magnetic particles;
step five, weighing a proper amount of Fe 3 O 4 @Co 3 O 4 The composite magnetic particles are placed in ethanol, deionized water and NH with a certain volume ratio 4 Continuously stirring for 30min at room temperature in OH mixed solution, slowly dripping dopamine hydrochloride aqueous solution into the mixed solution, reacting for 6h at room temperature, recovering the obtained precipitate with magnet, washing for 3 times with deionized water, and drying for 24h to obtain the required Fe 3 O 4 @Co 3 O 4 a/Pdap composite magnet;
step six, mixing the obtained Fe 3 O 4 @Co 3 O 4 the/Pdap composite magnet was added to 30mL of a mixed solution of linear polyethyleneimine ((PEI, 0.9mg/mL, mw =25,000)/Tris-HCl (10 mM, pH = 7-10), and after a reflux reaction at 60 ℃ for 3 hours, the mixture was stirred at room temperature for 16 hours or more to uniformly graft PEI onto Fe 3 O 4 @Co 3 O 4 A surface;
step seven, washing the obtained composite magnet for multiple times by deionized water and ethanol solution, and then placing the magnet in a drying oven at 50 ℃ for drying for 24 hours to obtain the needed Fe 3 O 4 @Co 3 O 4 -a PEI composite magnet.
Example 2
The difference from example 1 is that in step one, the ratio of deionized water, ethanol and butanol in the solution a is 120:100:3, said Na 3 C 6 H 5 O 7 ·2H 2 The addition amount of O is 0.50g; in the second step, the mixed solution is transferred into a high-pressure reaction kettle and then reacts for 2 hours at 160 ℃; and in the sixth step, refluxing and reacting for 6h.
Example 3
The difference from example 1 is that in step one, the solution a is prepared from deionized water and butanol in a ratio of 120:3, without adding ethanol or Na 3 C 6 H 5 O 7 ·2H 2 O; in the second step, the mixed solution is transferred into a high-pressure reaction kettle and then reacts for 15 hours at 160 ℃; and step five, reacting for 10 hours at room temperature.
(II) characterization of the materials
Fe prepared by the method of example 1 3 O 4 @Co 3 O 4 Composite magnetic particles and Fe 3 O 4 @Co 3 O 4 And (4) the PEI composite magnetic particles are used for researching the magnetic particle performances before and after modification by means of X-ray diffraction analysis (XRD-2700), infrared spectrum analysis (FT-IR-6000), surface contact angle test (SDC-200S), VSM magnetic performance (JDAW-2000) and the like. The test was performed according to the conventional procedure.
As shown in FIG. 3, according to Fe 3 O 4 @Co 3 O 4 Composite magnetic particles and Fe 3 O 4 @Co 3 O 4 X-ray diffraction pattern of PEI, characteristic diffraction peaks indicating Fe 3 O 4 And Co 3 O 4 Two phases exist, and diffraction peaks before and after grafting modification are not obviously changed, which indicates that the grafting modification does not influence the crystal structure.
As shown in fig. 4, there is a great difference in the micro-morphology of the two materials before (a) and after (b, c, d) modification. The materials before and after modification all have three-dimensional porous structures which are interconnected, but Fe 3 O 4 @Co 3 O 4 The microscopic morphology of the composite magnetic particles is relatively coarse. Fe 3 O 4 @Co 3 O 4 The surfaces of the composite magnetic particles are provided with flaky bulges to form a specific petal-shaped appearance structure. Modification of PEI results in Fe 3 O 4 @Co 3 O 4 Many thin layers are formed, creating many new channels. Thus, the resulting Fe was modified 3 O 4 @Co 3 O 4 PEI composite magnetic particles have more folds, more abundant pore structures and thinner pore walls, and have large specific surface area. The magnet particles have a particle size of 0.5 to 10 μm.
As shown in FIG. 5, fe is determined by several related characteristic peaks in the spectrum 3 O 4 @Co 3 O 4 PEI composite magnets have abundant oxygen-containing functional groups. The approximate position of the absorption peak and the corresponding functional group were 589cm each -1 (Fe-O)、649cm -1 (Co-O)、1735cm -1 (-C＝O)、1495cm -1 (NH-)、1375cm -1 (phenol-OH) in Fe 3 O 4 @Co 3 O 4 After PEI grafting is carried out on the surface of the composite magnet, the thickness of the PEI grafted composite magnet is 2921cm -1 And 2851cm -1 Where the CH bond functionality appears. The FT-IR analysis showed that Fe 3 O 4 @Co 3 O 4 The poly-dopamine attached to the surface of the composite magnet successfully grafts the PEI to the Fe through an addition reaction of an ortho-catechol group and an amine group on the PEI 3 O 4 @Co 3 O 4 A composite magnet surface. This indicates that Fe 3 O 4 @Co 3 O 4 And the PEI is well combined, so that the PEI can be an effective modifier.
Non-modified Fe 3 O 4 @Co 3 O 4 Composite magnetic particles and modified Fe 3 O 4 @Co 3 O 4 The PEI composite magnetic particles are respectively paved, and contact angle tests are carried out on 0# diesel oil and water in air, and the test process is shown in figure 6 (a). The results are shown in FIGS. 6 (b) and 6 (c). When water drops on Fe as shown in FIG. 6 (b) 3 O 4 @Co 3 O 4 The surface contact angle of the PEI composite magnet is 102.1 +/-2.7 degrees, and the PEI composite magnet is not absorbed after being placed for a long time; when oil drops on Fe 3 O 4 @Co 3 O 4 On the PEI composite magnet material, it can quickly lay flat and be absorbed. Therefore, the modified material has good hydrophobicity and good lipophilicity, and has potential application in the field of oil-water separation.
As shown in FIG. 7, fe 3 O 4 @Co 3 O 4 The saturation magnetization of the composite magnetic particles is about 70emu/g, and the modified Fe 3 O 4 @Co 3 O 4 -the saturation magnetization of the PEI composite magnetic particle is about 50emu/g.
(III) oil-Water separation experiment
As shown in FIG. 8 (a), a certain amount of Fe was added to each of two transparent glass bottles 3 O 4 @Co 3 O 4 Composite magnetic particles (left) and Fe 3 O 4 @Co 3 O 4 -PEI composite magnetic particles (right), and then adding water and light oil, respectively. After the ultrasonic treatment, as shown in fig. 8 (b), two kinds of composite magnetic particles are respectively dispersed in the liquid to form a suspension. After the mixture is kept stand for a period of time,as shown in FIG. 8 (c), fe 3 O 4 @Co 3 O 4 The composite magnetic particles are mainly distributed on the upper layer, a small amount of composite magnetic particles are distributed at the bottom of the bottle, the distribution range is wide, the rest liquid is emulsion, and Fe 3 O 4 @Co 3 O 4 The PEI composite magnetic particles are enriched on the upper layer, and the liquid on the lower layer is transparent in color. Further, two poles of the permanent magnet are respectively close to the two glass bottles, as shown in fig. 8 (d), it can be seen that the black particles in the two glass bottles are both close to the permanent magnet to a certain extent, but the left glass bottle contains Fe 3 O 4 @Co 3 O 4 The composite magnetic particles remain dispersed mainly in the upper layer, probably due to the liquid tension effect hindering Fe 3 O 4 @Co 3 O 4 Movement of composite magnetic particles in liquid, and Fe in the right vial 3 O 4 @Co 3 O 4 The PEI composite magnetic particles are clearly concentrated on the side wall of the flask near the permanent magnet and the remaining liquid is almost clear, indicating Fe 3 O 4 @Co 3 O 4 The PEI composite magnetic particles adsorb the oil phase and enrich the oil phase, and the PEI composite magnetic particles separate from the water phase.
As shown in FIG. 9 (a), the oil-containing emulsion (left) and the oil-water mixture were compared and Fe was added 3 O 4 @Co 3 O 4 -appearance of each glass bottle under post-sonication (middle) and attraction with external permanent magnet (right) conditions of PEI composite magnetic particles, as can be seen from the visibility of black pattern on background white panel, after attraction with external permanent magnet, fe was added 3 O 4 @Co 3 O 4 And (4) separating two phases in the oil-water mixture of the PEI composite magnetic particles, so that the water body becomes clear. This is further confirmed by applying a permanent magnet to attract the water body to become clear against a white background and a red background, as shown in fig. 9 (b) and 9 (c).
Further, the aqueous phase and the Fe-containing phase are mixed 3 O 4 @Co 3 O 4 Separating oil phase of PEI composite magnetic particles, extracting upper oil phase by using a syringe or a peristaltic pump, and filtering to remove oil and Fe 3 O 4 @Co 3 O 4 -PEI composite magnetic particles are separated.
If the oil in the oil-water mixture is heavy oil, adding Fe 3 O 4 @Co 3 O 4 After the magnetic particles are compounded, the adsorbed oil phase is located in the lower layer of the water phase, at this time, the water phase can be extracted, and the remaining oil phase is filtered, or the oil phase is discharged by a liquid separation device such as a separating funnel and filtered.
Finally, the filtered Fe 3 O 4 @Co 3 O 4 Washing Fe with organic solvent by PEI composite magnetic particles 3 O 4 @Co 3 O 4 The PEI composite magnetic particles can wash oil stains according to a similar compatibility principle, and can be repeatedly reused after the particles adsorbed with the oil-containing emulsion are washed for many times by using organic solvents such as alcohol, ether and the like.
In another embodiment, an acid or base may be added to the miscella to adjust its pH in advance to facilitate separation of the two phases of the miscella.
Separately, commercially available diesel oil, gasoline and vegetable oil were used as oil phases, and Fe was studied under static adsorption conditions 3 O 4 @Co 3 O 4 -the adsorption capacity of PEI composite magnetic particles to the oil phase in the oil-water mixture as a function of time, as shown in fig. 9 (d). It can be seen that Fe 3 O 4 @Co 3 O 4 The adsorption capacity of PEI composite magnetic particles to gasoline and vegetable oil reaches the maximum value of about 1.4g/g in 90min, and the adsorption capacity to diesel oil reaches the maximum value of about 1.88g/g in 150 min.
Research on Fe by using diesel oil as oil phase of oil-water mixture 3 O 4 @Co 3 O 4 The adsorption capacity and adsorption efficiency of the PEI composite magnetic particles as a function of time are shown in fig. 10 (a) and 10 (b), respectively. The adsorption efficiency is calculated from the oil collection coefficient (q (%)) according to equation (1):
here, M 2 And M 1 Respectively the weight of the collected oil after separation and the originalOil weight of water-oil mixture.
Wherein, the adsorption capacity and the adsorption efficiency reach the maximum in 150min, and the adsorption efficiency is more than 90%.
Finally, cyclically regenerated Fe was examined 3 O 4 @Co 3 O 4 The PEI composite magnetic particles are used for the adsorption effect of oil-water separation, and the water phase transmittance after the oil-water separation is used as an evaluation index. As shown in FIG. 11, after 12 times of oil-water separation experiments, the transmittance is obviously reduced, which indicates that the Fe prepared by the invention 3 O 4 @Co 3 O 4 The PEI composite magnetic particle has better reusability.
The invention has the beneficial effects that: (1) The preparation method is simple, and can prevent Fe after grafting modification 3 O 4 @Co 3 O 4 The powder is agglomerated, the mechanical strength of the composite magnet is further improved, and the Fe with stable shape and structure is constructed 3 O 4 @Co 3 O 4 -PEI composite magnetic particles;
(2)Co 3 O 4 in the presence of Fe 3 O 4 The surface of the composite Fe can form a flaky porous structure, the surface area of the composite Fe can be increased, and the magnetic responsiveness of the composite magnet is improved 3 O 4 @Co 3 O 4 PEI compared with Fe 3 O 4 PEI has larger specific surface area and higher adsorption efficiency due to the existence of a porous structure;
(3)Fe 3 O 4 @Co 3 O 4 the PEI composite magnetic particles have hydrophobicity and lipophilicity, the water contact angle of the surfaces of the PEI composite magnetic particles is 102.1 +/-2.7 degrees, and the oil is in a completely wetted state on the surfaces of the PEI composite magnetic particles;
(4) The static adsorption test result shows that the maximum adsorption capacity of the adsorbent to diesel reaches 1.88g/g;
(5)Fe 3 O 4 @Co 3 O 4 after the PEI is recycled for many times, the oil-water separation efficiency can be kept above 90%.
In summary, fe 3 O 4 @Co 3 O 4 The PEI composite magnetic particle has low production costLow cost, convenient separation, high adsorption capacity, good regeneration effect, no secondary pollution and the like, and has wide application prospect in actual production.
Example 4
As shown in fig. 12, an oil-water separation device based on a composite magnet comprises a magnetic separation groove 3, a lifting device is arranged below the magnetic separation groove 3, the lifting device is a hydraulic cylinder 1, the hydraulic cylinder 1 is vertically arranged, a cylinder body of the hydraulic cylinder is fixed, a support frame 2 is arranged at the upper end of a piston rod of the hydraulic cylinder, and the magnetic separation groove 3 is arranged on the support frame 2. The magnetic separation tank 3 is also connected with a mixed liquid inlet device 6 and a suction device 7.
As shown in fig. 13, the stirring paddle includes a stirring head 41 having an inner cavity, and a blade 42 is fixedly connected to an outer wall of the stirring head 41.
The stirring shaft 43 is in a hollow rod shape, the inner cavity of the stirring shaft 43 is communicated with the inner cavity of the stirring head 41, the electromagnet 5 is arranged in the stirring head 41, and a lead of the electromagnet 5 is led out through the inner cavity of the stirring shaft 43 and then is connected with a direct current power supply.
In order to enable the connection relationship between the electromagnet 5 and the power supply not to be affected when the stirring shaft 43 rotates, the upper end of the stirring shaft 43 is in threaded connection with a buckle cover 44, the upper surface of the buckle cover 44 is provided with two floating electrodes, namely a first floating electrode 52 and a second floating electrode 51, respectively, wherein the distance from the first floating electrode 52 to the center line of the buckle cover 44 is greater than the distance from the second floating electrode 51 to the center line of the buckle cover 44.
A butt joint disc 53 is arranged right above the stirring shaft 43, and the butt joint disc 53 is fixedly connected with the stirring bracket 49. As shown in fig. 14, the lower surface of the pair of pads 53 is provided with a ring electrode corresponding to the two floating electrodes, which are a first ring electrode 55 and a second ring electrode 54, respectively, and the two ring electrodes are connected to two poles of the power supply through a lead and a switch, respectively. Wherein the first floating electrode 52 floats against the first ring electrode 55 and the second floating electrode 51 floats against the second ring electrode 54. The floating electrode may be a carbon brush and the ring electrode may be a ring-shaped copper plate. In this embodiment, the second ring electrode 54 is designed to be a disk shape because it is close to the center of the docking tray 53.
The electromagnet 5 is liquid-sealed and coated by the stirring head 41, and the shell of the stirring head 41 is made of plastic, so that the shell does not influence the magnetic force transmission of the electromagnet 5. The lifting device is used for adjusting the height of the stirring paddle in the magnetic separation tank 3 to adapt to different liquid levels and oil-water separation interfaces.
The mixed liquid inlet device 6 comprises a high-level liquid storage tank 6, and the high-level liquid storage tank 6 is connected with the magnetic separation tank 3 through a suction pipe and is used for introducing an oil-water mixture into the magnetic separation tank 3.
The suction device 7 comprises a liquid pump 71, a liquid inlet of the liquid pump 71 is connected with the magnetic separation tank 3, and a liquid outlet of the liquid pump 71 is connected with a first separation liquid storage tank 72.
A liquid outlet 31 with a sealing valve is arranged at the bottom of the magnetic separation tank 3, and a second separation liquid storage tank 8 is arranged below the liquid outlet 31.
The magnetic separation tank 3 contains Fe prepared as in example 1 3 O 4 @Co 3 O 4 And (3) compounding magnetic particles.
The using method of the device comprises the following steps: after the oil-water separation device is installed, the oil-water mixture flows into the magnetic separation tank 3 from the high-position liquid storage tank 6 3 O 4 @Co 3 O 4 The composite magnetic particles can be added in advance or added later, the electromagnet 5 is kept powered off, and the stirring paddle stirs to enable Fe 3 O 4 @Co 3 O 4 Uniform distribution of composite magnetic particlesThe mixture is dispersed into the oil-water mixture to adsorb the oil phase, then the electromagnet 5 is electrified, and the rotating speed of the stirring paddle is reduced, so that the oil phase is along with Fe 3 O 4 @Co 3 O 4 The composite magnetic particles are gradually gathered near the stirring head under the magnetic attraction effect, and the height of the magnetic separation tank 3 is adjusted according to the density of the oil phase in the process. If the density of the oil phase is greater than that of the water, the stirring head 41 is close to the bottom of the magnetic separation tank 3; if the density of the oil phase is lower than that of water, the stirring head 41 is brought close to the upper part of the liquid surface. After the oil phase and the water phase are fully separated, a suction device is used for sucking the water phase or the oil phase, and the position of the liquid inlet end of the suction pipe in the liquid phase is adaptively adjusted according to the position and the volume of the two phases. Preferably, the aqueous phase is first sucked up to leave the oil phase in the magnetic separation tank 3, and then the oil phase is sucked up or discharged through the liquid outlet 31 at the bottom of the magnetic separation tank 3. Finally adding organic solvent to wash to lead Fe 3 O 4 @Co 3 O 4 And (4) regenerating the composite magnetic particles.
Finally, it should be noted that the above-mentioned description is only a preferred embodiment of the present invention, and those skilled in the art can make various similar representations without departing from the spirit and scope of the present invention.
Claims (8)
1. The utility model provides an oil-water separator based on compound magnet, includes magnetic separation groove (3), its characterized in that: the magnetic separation tank (3) is provided with a stirring device (4), the stirring device (4) comprises a stirring paddle, the stirring paddle extends into the magnetic separation tank (3), and an electromagnet (5) is arranged in the stirring paddle;
the magnetic separation tank (3) is also connected with a mixed liquid inlet device and a suction device (7);
the magnetic separation tank (3) or the stirring device (4) is connected with a lifting device, and the lifting device is used for adjusting the height of the stirring blade pitch from the bottom of the magnetic separation tank (3);
magnetic particles are contained in the magnetic separation groove (3), and the surfaces of the magnetic particles are lipophilic;
the magnetic particles are Fe 3 O 4 @Co 3 O 4 Composite magnetic particles of the Fe 3 O 4 @Co 3 O 4 The composite magnetic particles are made of Fe 3 O 4 Core and Co coated on the surface thereof 3 O 4 Shell composition of Fe 3 O 4 @ Co 3 O 4 The surface of the composite magnetic particle is grafted with polyethyleneimine;
said Fe 3 O 4 @Co 3 O 4 The surface of the composite magnetic particle is coated with a substrate polymer, the substrate polymer layer is provided with a catechol group, and the substrate polymer is used for grafting polyethyleneimine on the surface of the substrate polymer layer through the reaction of the catechol group and the amino group of the polyethyleneimine;
the base polymer layer is a polydopamine layer;
the particle size of the composite magnet is 0.5-10 μm.
2. The oil-water separation device based on the composite magnet as claimed in claim 1, wherein: the stirring device (4) further comprises a stirring support (49), a stirring shaft (43) is arranged on the stirring support (49) through a bearing, the stirring shaft (43) is vertically arranged, the upper end of the stirring shaft (43) is in transmission connection with a driving device for driving the stirring shaft to rotate, the lower end of the stirring shaft (43) is connected with a stirring paddle, and the stirring shaft (43) is in a hollow rod shape;
the stirring paddle comprises a stirring head (41) with an internal cavity, the outer wall of the stirring head (41) is fixedly connected with a blade (42), the inner cavity of the stirring head (41) is communicated with the inner cavity of the stirring shaft (43), the electromagnet (5) is arranged in the stirring head (41), and a lead of the electromagnet (5) is connected with a power supply after being led out through the inner cavity of the stirring shaft (43);
the electromagnet (5) is coated by the stirring head (41) in a liquid seal mode, and the shell of the stirring head (41) is made of plastics.
3. The oil-water separation device based on the composite magnet as claimed in claim 2, wherein: the upper end of the stirring shaft (43) is in threaded connection with a buckle cover (44), the upper surface of the buckle cover (44) is provided with two floating electrodes, and the distance from one floating electrode to the center line of the buckle cover (44) is greater than the distance from the other floating electrode to the center line of the buckle cover (44);
the direct-current motor is characterized in that a butt joint disc (53) is arranged right above the stirring shaft (43), the lower surface of the butt joint disc (53) corresponds to two floating electrodes, each floating electrode is provided with an annular electrode, each floating electrode is in floating abutting contact with the corresponding annular electrode, and the two annular electrodes are connected with the two poles of the power supply through wires.
4. The oil-water separation device based on the composite magnet as claimed in claim 3, wherein: the driving device is a speed regulating motor (48), the speed regulating motor (48) is installed on the stirring support (49), a driving wheel (47) is arranged on an output shaft of the speed regulating motor (48), a driven wheel (45) is arranged on the stirring shaft (43), and the driven wheel (45) is in transmission connection with the driving wheel (47) through a belt (46).
5. The oil-water separator based on a composite magnet according to any one of claims 1 to 4, wherein: the mixed liquid inlet device comprises a high-level liquid storage tank (6), and the high-level liquid storage tank (6) is connected with the magnetic separation tank (3) through a suction pipe.
6. The oil-water separator based on a composite magnet according to any one of claims 1 to 4, wherein: the suction device (7) comprises a liquid pump (71), a liquid inlet of the liquid pump (71) is connected with the magnetic separation tank (3) through a suction pipe, and a liquid outlet of the liquid pump (71) is connected with a first separation liquid storage tank (72).
7. The oil-water separator based on a composite magnet according to any one of claims 1 to 4, wherein: a liquid outlet (31) with a sealing valve is arranged at the bottom of the magnetic separation tank (3), and a second separation liquid storage tank (8) is arranged below the liquid outlet (31).
8. The oil-water separator based on a composite magnet according to any one of claims 1 to 4, wherein: the magnetic separation groove (3) is provided with the lifting device below, the lifting device is a hydraulic cylinder (1), the hydraulic cylinder (1) is vertically arranged, the cylinder body of the hydraulic cylinder is fixed, the upper end of a piston rod of the hydraulic cylinder is provided with a support frame (2), and the magnetic separation groove (3) is arranged on the support frame (2).
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| CN113620394A (en) * | 2021-08-05 | 2021-11-09 | 天华化工机械及自动化研究设计院有限公司 | Controllable magnetic oil-water separation magnetic separator and oil-water separation method thereof |
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