阅读说明：本技术 基于磁性颗粒动态床的乳化液连续破乳分离方法 (Emulsion continuous demulsification separation method based on magnetic particle dynamic bed ) 是由 薛佳 杨文新 贺梦凡 彭开铭 黄翔峰 吴宝强 熊永娇 王宇 于 2021-07-05 设计创作，主要内容包括：本发明涉及废乳化液处理的技术领域,尤其涉及一种基于磁性颗粒动态床的乳化液连续破乳分离方法。包括一套基于磁性颗粒动态床的乳化液连续破乳分离装置,通过磁性颗粒操控系统产生交变磁场,使磁性颗粒被束缚于乳化液流路中特定区域并产生往复运动,形成磁性颗粒动态床；乳化液以垂直于颗粒往复运动的方向通过动态床,磁性颗粒与乳化液中的油滴碰撞,捕集油滴、破坏油水界面膜并促进油滴聚并,完成粗粒化破乳和油水分离过程,并具有连续出水和排出浮油的作用。可将乳化液透光率由5%以下提升至95%以上,具有出水水质良好,运行稳定的特点,解决了磁性颗粒破乳研究中较难实现连续破乳、磁场作用单一、颗粒需特定修饰、破乳效能低等问题。(The invention relates to the technical field of waste emulsion treatment, in particular to a continuous emulsion breaking and separating method for emulsion based on a magnetic particle dynamic bed. The device comprises a set of emulsion continuous demulsification separation device based on a magnetic particle dynamic bed, wherein an alternating magnetic field is generated by a magnetic particle control system, so that magnetic particles are bound in a specific area in an emulsion flow path and reciprocate to form the magnetic particle dynamic bed; the emulsion passes through the dynamic bed in a direction perpendicular to the reciprocating motion of the particles, the magnetic particles collide with oil drops in the emulsion, the oil drops are trapped, an oil-water interfacial film is damaged, coalescence of the oil drops is promoted, coarse-grained demulsification and oil-water separation processes are completed, and the device has the effects of continuously discharging water and floating oil. The method can improve the light transmittance of the emulsion from below 5% to above 95%, has the characteristics of good effluent quality and stable operation, and solves the problems that continuous emulsion breaking is difficult to realize in the emulsion breaking research of magnetic particles, the magnetic field effect is single, the particles need specific modification, the emulsion breaking efficiency is low, and the like.)

1. The continuous emulsion breaking and separating method of the emulsion based on the magnetic particle dynamic bed is characterized by comprising a set of continuous emulsion breaking and separating device based on the magnetic particle dynamic bed, wherein the device consists of a magnetic particle control system, an emulsion flow path and an emulsion breaking and separating operation platform, and the separating method comprises the following steps:

s1, constructing an alternating magnetic field capable of enabling magnetic particles to reciprocate, wherein the alternating magnetic field is generated by a pair of sucker type electromagnets which are symmetrically arranged, the action surfaces of the sucker type electromagnets capable of generating attraction force face inwards oppositely, and the sucker type electromagnets are fixed on the demulsification separation operation platform;

s2, adjusting parameters of the magnetic particle control system to generate a specific current signal to act on the sucker type electromagnets, so that the two sucker type electromagnets are alternately electrified to realize the effect that the two electromagnets alternately generate attraction force, and magnetic substances can generate reciprocating motion between the two sucker type electromagnets;

s3, placing a part of the emulsion flow path between the two sucker-type electromagnets, adding a certain amount of magnetic particles into the emulsion flow path, wherein under the action of the two sucker-type electromagnets, the magnetic particles are bound in a magnetic field action area between the two sucker-type electromagnets by a magnetic field and do not flow with the flow phase;

s4, enabling the emulsion to continuously flow into the emulsion flow path, enabling the emulsion to flow through the dynamic bed layer in a direction perpendicular to the reciprocating motion direction of the magnetic particles, capturing the liquid drops by the particles in the process, enabling the liquid drops to reciprocate along with the particles, enabling the liquid drops to continuously collide and coalesce, and enabling coarse granulation to occur;

s5, after the large-particle-size liquid drops formed by coarse granulation are separated from the bed layer, a floating oil layer is gradually formed in the emulsion flow path and can be discharged from the emulsion flow path periodically to realize oil recovery;

s6, closing the magnetic particle control system, introducing distilled water into the emulsion flow path, discharging the magnetic particles in the emulsion flow path, cleaning the flow path, and repeating the steps S1-S5 to repeatedly treat the emulsion for multiple times.

2. The continuous emulsion breaking and separating method of the emulsion based on the dynamic bed of the magnetic particles as claimed in claim 1, wherein: and in the S2, the magnetic particle control system provides current signals for the two sucker type electromagnets through a double-channel function generator respectively, the function generator generates the same waveforms through double channels, and the waveforms are square waves, rectangular waves, pulse waves or CMOS waves.

3. The continuous emulsion breaking and separating method of the emulsion based on the dynamic bed of the magnetic particles as claimed in claim 2, characterized in that: the function generator has the same dual-channel output amplitude and frequency, the frequency range is 1-5 Hz, and the dual-channel phase difference is 150-210 degrees.

4. The continuous emulsion breaking and separating method of the emulsion based on the dynamic bed of the magnetic particles as claimed in claim 2, characterized in that: the output signals of the function generator are amplified by a pair of power amplifiers and then act on the sucker type electromagnets, the voltage acting on the two sucker type electromagnets after amplification is 12-24V, and correspondingly, the surface magnetic field intensity of the two sucker type electromagnets is above 400Gs when the two sucker type electromagnets are electrified.

5. The continuous emulsion breaking and separating method of the emulsion based on the dynamic bed of the magnetic particles as claimed in claim 1, wherein: the part of the emulsion flow path between the two sucker-type electromagnets is flat in design, and the distance between action surfaces of the two sucker-type electromagnets is less than 3 cm.

6. The continuous emulsion breaking and separating method of the emulsion based on the dynamic bed of the magnetic particles as claimed in claim 1, wherein: and the hydraulic retention time of the emulsion in the S4 in the magnetic field action area is 30-120S.

7. The continuous emulsion breaking and separating method of the emulsion based on the dynamic bed of the magnetic particles as claimed in claim 1, wherein: the magnetic particles in S3 are Fe₃O₄The hydrated particle size of the particles is micron-sized and can reach 200 meshes at most.

8. The continuous emulsion breaking and separating method of the emulsion based on the dynamic bed of the magnetic particles as claimed in claim 1, wherein: and in the S3, the magnetic particles are added into the emulsion flow path in a dry feeding mode, and the feeding amount of the particles is 1-5g each time.

9. The continuous emulsion breaking and separating method of the emulsion based on the dynamic bed of the magnetic particles as claimed in claim 1, wherein: the emulsion in the S4 is an oil-in-water model emulsion and an emulsion stabilized by an anionic surfactant, the oil phase of the oil-in-water model emulsion comprises low-viscosity short-chain alkane and hydrocarbon and high-viscosity mineral oil, and the concentration of the surfactant is in the range of 0-20 mg/L.

10. The continuous emulsion breaking and separating method of the emulsion based on the dynamic bed of magnetic particles as claimed in claim 9, wherein: the oil phase of the model emulsion comprises dichloromethane, trichloromethane, carbon tetrachloride, petroleum ether, hexadecane, soybean oil, liquid paraffin, vacuum pump oil and engine oil, the concentration range of the oil is 1-20 g/L, and the particle size of droplets of the emulsion is mainly distributed in the range of 1-10 microns.

Technical Field

The invention relates to a method for continuously demulsifying and separating emulsion based on a magnetic particle dynamic bed.

Background

Under the drive of the action compendium of 'Chinese manufacturing 2025', the dosage of high-quality metal working fluid is increased along with the rapid development of the precision machining industry in China, the metal working fluid becomes waste emulsion after being recycled until being invalid, and the waste emulsion has extremely high environmental pollution and ecological risk and belongs to dangerous waste (code HW 09). The waste emulsion contains a large amount of mineral oil and surfactant, emulsion droplets are stably dispersed in a water phase in a micro/nano droplet mode under the wrapping of an oil-water interface film formed by the surfactant, the stability is high, and the demulsification and oil-water separation difficulty is high.

The chemical agent demulsification is widely applied to the treatment of waste emulsion due to mature technology, simplicity and practicability and low construction and operation cost, but has the problems of high adding amount of the chemical agent, high floc yield, low separation speed, high secondary waste yield and the like. The magnetic particles have the advantages of easy control of surface properties, easy control by a magnetic field, quick magnetic responsiveness, recyclability and the like, and are widely concerned in emulsion breaking research. The research of utilizing magnetic particle demulsification begins in 2012, in recent years, various functional magnetic particles with special surface wettability, chargeability and morphology structures are developed by researchers, the particles can be adsorbed on an oil-water interface based on hydrophobic effect, electrostatic effect, size effect and special morphology structures, the stability of an oil-water interface film is further influenced, the magnetic responsiveness of emulsified liquid droplets is endowed, the rapid separation of the magnetic response liquid droplets and a continuous phase is realized under the action of a magnetic field, and the demulsification is realized.

At the present stage, the magnetic particle demulsification mostly adopts functionalized modified nano-scale magnetic particles, and is limited by higher cost and complicated modification work, related researches are mostly limited to a laboratory sequencing batch processing scale, direct engineering application is difficult, continuous demulsification cannot be realized, and researches of directly demulsifying micron-scale magnetic particles which are low in cost and do not need specific modification work are rarely reported. On the other hand, the magnetic field acts only in the process of separating droplets from the continuous phase as a key force for demulsification of magnetic particles, and does not act in key steps of trapping droplets, promoting coalescence and coarse granulation of droplets, breaking an oil-water interface film, and the like.

Disclosure of Invention

The invention aims to solve the defects and provides a method for continuously demulsifying and separating emulsion based on a magnetic particle dynamic bed.

In order to overcome the defects in the background technology, the invention is based on the basic principle of demulsification of alternating magnetic field and magnetic particles, micron-sized magnetic particles are directly utilized, the alternating electromagnetic field is utilized to restrain the magnetic particles in a flow path and make the magnetic particles generate transverse reciprocating motion to form a dynamic bed of the magnetic particles, liquid drops can be trapped by the particles in the process that emulsion flows through the bed layer from bottom to top, further collision and coalescence are carried out, and a coarse-grained demulsification process is generated. The continuous emulsion breaking and separating method based on the magnetic particle dynamic bed comprises a set of continuous emulsion breaking and separating device based on the magnetic particle dynamic bed, and the device consists of a magnetic particle control system, an emulsion flow path and an emulsion breaking and separating operation platform, and the separating method comprises the following steps:

s1, constructing an alternating magnetic field capable of enabling magnetic particles to reciprocate, wherein the alternating magnetic field is generated by a pair of sucker type electromagnets which are symmetrically arranged, the action surfaces of the sucker type electromagnets capable of generating attraction force face inwards oppositely, and the sucker type electromagnets are fixed on the demulsification separation operation platform;

s2, adjusting parameters of the magnetic particle control system to generate a specific current signal to act on the sucker type electromagnets, so that the two sucker type electromagnets are alternately electrified to realize the effect that the two electromagnets alternately generate attraction force, and magnetic substances can generate reciprocating motion between the two sucker type electromagnets;

s3, placing a part of the emulsion flow path between the two sucker-type electromagnets, adding a certain amount of magnetic particles into the emulsion flow path, wherein under the action of the two sucker-type electromagnets, the magnetic particles are bound in a magnetic field action area between the two sucker-type electromagnets by a magnetic field and do not flow with the flow phase;

s4, enabling the emulsion to continuously flow into the emulsion flow path, enabling the emulsion to flow through the dynamic bed layer in a direction perpendicular to the reciprocating motion direction of the magnetic particles, capturing the liquid drops by the particles in the process, enabling the liquid drops to reciprocate along with the particles, enabling the liquid drops to continuously collide and coalesce, and enabling coarse granulation to occur;

s5, after the large-particle-size liquid drops formed by coarse granulation are separated from the bed layer, a floating oil layer is gradually formed in the emulsion flow path and can be discharged from the emulsion flow path periodically to realize oil recovery;

s6, closing the magnetic particle control system, introducing distilled water into the emulsion flow path, discharging the magnetic particles in the emulsion flow path, cleaning the flow path, and repeating the steps S1-S5 to repeatedly treat the emulsion for multiple times.

According to another embodiment of the invention, the magnetic particle control system in S2 provides current signals to the two sucker electromagnets through two-channel function generators, wherein the function generators generate the same waveforms by two channels, and the waveforms are selected from square waves, rectangular waves, pulse waves or CMOS waves.

According to another embodiment of the invention, the method further comprises that the dual-channel output amplitude and frequency of the function generator are the same, the frequency range is 1-5 Hz, and the dual-channel phase difference is 150- & ltwbr/& gt210 °.

According to another embodiment of the present invention, the output signal of the function generator is amplified by a pair of power amplifiers and then applied to the sucker-type electromagnets, the voltage applied to the two sucker-type electromagnets after amplification is 12-24V, and accordingly, when the two sucker-type electromagnets are energized, the surface magnetic field strength is above 400 Gs.

According to another embodiment of the invention, the part of the emulsion flow path between the two sucker-type electromagnets is flat, so that the distance between the action surfaces of the two sucker-type electromagnets is ensured to be less than 3cm, the magnetic field intensity is prevented from being attenuated due to the overlarge distance between the two sucker-type electromagnets, and further sufficient driving force can be provided for magnetic particles to generate reciprocating motion between the two sucker-type electromagnets.

According to another embodiment of the invention, the hydraulic retention time of the emulsion in the action area of the magnetic field in the S4 is further 30-120S, so as to ensure that emulsion droplets are fully contacted with the magnetic particles, and the droplets are fully collided and coalesced.

According to another embodiment of the invention, the magnetic particles in the S3 are Fe3O4 particles, and the hydrated particle size of the particles is micron-sized and can reach 200 meshes at most and is less than or equal to 74 microns.

According to another embodiment of the present invention, the method further comprises the step of adding the magnetic particles in S3 into the emulsion flow path in a dry feeding manner, wherein the feeding amount of the magnetic particles is 1-5g per time.

According to another embodiment of the present invention, the emulsion in S4 is an oil-in-water model emulsion, the emulsion is stabilized by an anionic surfactant, the oil phase of the oil-in-water model emulsion comprises low-viscosity short-chain alkane and hydrocarbon and high-viscosity mineral oil, and the concentration of the surfactant is in the range of 0-20 mg/L.

According to another embodiment of the present invention, further comprising that the oil phase of the model emulsion comprises dichloromethane, chloroform, carbon tetrachloride, petroleum ether, hexadecane, soybean oil, liquid paraffin, vacuum pump oil and engine oil, the oil concentration is in the range of 1-20 g/L, and the emulsion droplet size is mainly distributed in the range of 1-10 μm.

The invention has the beneficial effects that:

(1) from the aspect of a demulsification method, the invention couples the traditional magnetic particle demulsification method and research means such as alternating electromagnetic field droplet control and the like, and provides a magnetic particle dynamic bed demulsification separation technology and a device. A small amount of magnetic particle dry powder is added into the oil-water separation chamber, particles reciprocate between the two electromagnets under the action of a magnetic field to form a magnetic particle dynamic bed, and oil drops are captured by the bed layer and collide and coalesce with each other in the process that emulsion flows through the bed layer along the direction perpendicular to the reciprocating motion direction of the particles, so that emulsion breaking and oil-water separation are realized. The reciprocating motion of the magnetic particles also strengthens the shearing and friction between the particles and the fluid and the mutual collision between the particles, which is beneficial to the falling of oil stains adsorbed on the surfaces of the particles and the floating to the liquid surface, thereby effectively improving the effluent quality, improving the demulsification efficiency of the magnetic particles and reducing the particle adding amount.

(2) From the aspect of demulsification materials, the modified magnetic emulsion is based on unmodified micron-sized magnetic particles, does not need any preparation and modification work, does not need to add chemical agents, and has higher demulsification efficiency. The amount of the emulsion which can be processed by the magnetic particles per unit mass is 0.5-1L/g, which is obviously higher than that of the emulsion which can be processed by the magnetic particles per unit mass in related researches. For example, the treatment capacity of the functionalized magnetic nanoparticles used in the published Chinese patent CN112138430A is 200 ml per gram of particle emulsion; the Chinese patent CN109354139B uses magnetic particles to cooperate with coagulant to treat waste emulsion from machining, and the treatment amount of particles per gram is 417 ml of emulsion; the disclosed Chinese invention patent CN110379577A uses the functionalized magnetic nano particles in the repeated emulsification and emulsion breaking process of emulsion, and the handling capacity of each gram of particles is about 250 ml; in an article (Demulfication of organic-Acid-Coated magnetic Nanoparticles for cyclic hexane-in-Water Nanoemulsions) published in the Energy & Fuels journal by Liang et al, Oleic Acid-Coated Fe3O4 Nanoparticles are used for treating a Cyclohexane-Water model emulsion, and the treatment amount of each gram of particles is only 33 ml in order to achieve the ideal treatment effect; wang et al, in an article published in the Environmental Science, Water Research & Technology journal (Cyclic amine-functionalized magnetic nanoparticles for Electrical evaluation of crop oil-in-Water emulsions) treated a crude oil-Water model emulsion with amino-functionalized magnetic nanoparticles at a particle throughput of about 400 ml per gram. Effectively expands the adaptability of the micron-sized magnetic particles directly used for emulsion breaking of the emulsion and reduces the treatment cost.

(3) From the aspect of treatment effect, the set of continuous emulsion breaking and separating device based on the magnetic particle dynamic bed can realize continuous and automatic treatment on the emulsion under the condition of lower particle adding amount, the light transmittance of the outlet water can be improved to more than 60% from less than 5% of the inlet water and is kept stable, the highest light transmittance can reach more than 95%, the subsequent treatment difficulty is greatly reduced, the oil phase can be effectively separated, and the device has a resource recycling function.

(4) From the aspect of treatment objects and application range, the magnetic particle dynamic bed demulsification technology provided by the invention can effectively capture emulsified oil drops, destroy an oil-water interface membrane and promote coalescence of the liquid drops, and realizes high-efficiency demulsification and oil-water separation on oil-in-water emulsions stabilized by various surfactants, wherein the concentration of the surfactant is 0-20mg/L, the concentration range of the oil is 1-20 g/L, and the particle sizes of the oil drops are mainly distributed in a micron order. The application range is expanded to the practical complex waste emulsion generated in the field of mechanical processing, and the method has important significance for the practical application and popularization of micron-sized magnetic particles and dynamic beds of the magnetic particles.

Drawings

The invention is further illustrated with reference to the following figures and examples.

FIG. 1 is a schematic overall view of a continuous emulsion breaking and separating device for emulsion based on a dynamic bed of magnetic particles, provided by the invention;

FIG. 2 is a schematic structural diagram of a front view of the oil-water separation chamber and the DC suction cup type electromagnet;

FIG. 3 is a schematic structural diagram of a side view of the oil-water separation chamber and the DC suction cup type electromagnet;

FIG. 4 is a diagram showing the effect of continuous operation in example 2 of the present invention

FIG. 5 is a diagram showing the effect of continuous operation in example 3 of the present invention.

Wherein: 1. the device comprises a magnetic particle control system, 2, an emulsion flow path, 3, a demulsification separation operation platform, 1-1, a function generator, 1-2, a power amplifier, 1-3, a transformer, 1-4, a direct current sucker type electromagnet, 2-1, a water inlet tank, 2-2, a water outlet tank, 2-3, a waste oil tank, 2-4, a peristaltic pump, 2-5, an oil-water separation chamber, 3-1, a platform, 3-2, a slide rail, 3-3, an electromagnet fixer, 3-3 and an electromagnet fixer.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

According to the invention, micron-sized magnetic particles are utilized, and under the premise of not adding other chemical agents and smaller particle adding amount, a magnetic particle dynamic bed is formed under the action of an external alternating magnetic field, emulsion droplets are captured, an oil-water interface film is damaged, the droplets are aggregated and coarsely granulated, and continuous demulsification and oil-water separation are realized. Has the advantages of high demulsification and separation efficiency, small particle adding amount, stable operation and the like.

The continuous emulsion breaking and separating method of the emulsion based on the magnetic particle dynamic bed comprises a set of continuous emulsion breaking and separating device based on the magnetic particle dynamic bed, and the device consists of a magnetic particle control system, an emulsion flow path and an emulsion breaking and separating operation platform, and the separating method comprises the following steps:

s1, constructing an alternating magnetic field capable of enabling magnetic particles to reciprocate, wherein the alternating magnetic field is generated by a pair of sucker type electromagnets which are symmetrically arranged, the action surfaces of the sucker type electromagnets capable of generating attraction force face inwards oppositely, and the sucker type electromagnets are fixed on the demulsification separation operation platform;

s2, adjusting parameters of the magnetic particle control system to generate a specific current signal to act on the sucker type electromagnets, so that the two sucker type electromagnets are alternately electrified to realize the effect that the two electromagnets alternately generate attraction force, and magnetic substances can generate reciprocating motion between the two sucker type electromagnets;

s3, placing a part of the emulsion flow path between the two sucker-type electromagnets, adding a certain amount of magnetic particles into the emulsion flow path, wherein under the action of the two sucker-type electromagnets, the magnetic particles are bound in a magnetic field action area between the two sucker-type electromagnets by a magnetic field and do not flow with the flow phase;

s4, enabling the emulsion to continuously flow into the emulsion flow path, enabling the emulsion to flow through the dynamic bed layer in a direction perpendicular to the reciprocating motion direction of the magnetic particles, capturing the liquid drops by the particles in the process, enabling the liquid drops to reciprocate along with the particles, enabling the liquid drops to continuously collide and coalesce, and enabling coarse granulation to occur;

s5, after the large-particle-size liquid drops formed by coarse granulation are separated from the bed layer, a floating oil layer is gradually formed in the emulsion flow path and can be discharged from the emulsion flow path periodically to realize oil recovery;

s6, closing the magnetic particle control system, introducing distilled water into the emulsion flow path, discharging the magnetic particles in the emulsion flow path, cleaning the flow path, and repeating the steps S1-S5 to repeatedly treat the emulsion for multiple times.

Further, in the S2, the magnetic particle control system provides current signals to the two sucker-type electromagnets through a double-channel function generator respectively, the function generator generates the same waveforms through double channels, and the waveforms are square waves, rectangular waves, pulse waves or CMOS waves.

Further, the dual-channel output amplitude and the frequency of the function generator are the same, the frequency range is 1-5 Hz, and the dual-channel phase difference is 150-210 degrees.

Further, the output signals of the function generator are amplified by a pair of power amplifiers and then act on the sucker type electromagnets, the voltage acting on the two sucker type electromagnets after amplification is 12-24V, and correspondingly, when the two sucker type electromagnets are electrified, the surface magnetic field intensity is above 400 Gs.

Furthermore, the part of the emulsion flow path between the two sucker-type electromagnets is in a flat design, so that the distance between the action surfaces of the two sucker-type electromagnets is less than 3 cm.

Further, the hydraulic retention time of the emulsion in the S4 in the magnetic field action area is 30-120S.

Further, the magnetic particles in the S3 are Fe3O4 particles, the hydration particle size of the particles is micron-sized, and the maximum particle size can reach 200 meshes.

Further, in the step S3, the magnetic particles are added to the emulsion flow path in a dry feeding manner, and the amount of the magnetic particles added is 1 to 5g per time.

Further, the emulsion in the S4 is an oil-in-water model emulsion and an emulsion stabilized by an anionic surfactant, wherein the oil phase of the oil-in-water model emulsion comprises low-viscosity short-chain alkane and hydrocarbon and high-viscosity mineral oil, and the concentration of the surfactant is in the range of 0-20 mg/L.

Further, the oil phase of the model emulsion comprises dichloromethane, trichloromethane, carbon tetrachloride, petroleum ether, hexadecane, soybean oil, liquid paraffin, vacuum pump oil and engine oil, the concentration range of the oil is 1-20 g/L, and the particle size of the emulsion liquid drops is mainly distributed in the range of 1-10 microns.

The emulsion involved in the embodiment of the invention comprises micron-sized emulsion prepared in a laboratory, and the preparation method comprises the following steps:

(a) dispersing 2.0 g of liquid paraffin and a certain amount of Sodium Dodecyl Benzene Sulfonate (SDBS) in 198 mL of water phase, and stirring the obtained mixture at 13000 rpm for 5 min to obtain micron-sized emulsion with stable surfactants of different concentrations; the mass of the added SDBS can be 0-4 mg, and the concentration of the surfactant in the prepared emulsion is 0-20 mg/L.

(b) This step was repeated several times to prepare a model emulsion having a total amount of 2L or more.

(c) The particle size of the droplets of the model emulsion is intensively distributed in 1-10 mu m, the light transmittance of the emulsion stock solution is related to the concentration of the surfactant, the higher the concentration of the surfactant is, the lower the light transmittance of the stock solution is, and when the surfactant is not contained, the light transmittance is 2.39%.

The continuous emulsion breaking and separating device for the emulsion based on the magnetic particle dynamic bed provided by the embodiment comprises a magnetic particle control system 1, an emulsion flow path 2 and an emulsion breaking and separating operation platform 3. The magnetic particle control system 1 consists of a function generator 1-1, a power amplifier 1-2, a transformer 1-3 and a pair of direct current sucker type electromagnets 1-4; the emulsion flow path 2 consists of a water inlet groove 2-1, a water outlet groove 2-2, a waste oil groove 2-3, a pipeline, a peristaltic pump 2-4 and an oil-water separation chamber 2-5; the demulsification separation operation platform 3 consists of a platform 3-1, a slide rail 3-2, two electromagnet fixers 3-3 which are symmetrically arranged and an oil-water separation chamber fixer 3-4, and the specific implementation steps are as follows with reference to the attached figure 1:

(1) the magnetic particle control system 1, the emulsion flow path 2 and the demulsification separation operation platform 3 are respectively connected and installed. The effective action surfaces of the two sucker type electromagnets 1-4 are tightly attached to the lower parts of the left and right surfaces of the oil-water separation chamber 2-5, and the separation chamber is divided into an upper area and a lower area. The upper part of the separation chamber is not affected by the magnetic field, and the lower part is a magnetic field affected zone, see figure 2.

(2) The function generator 1-1 is adjusted to set the double-channel waveform as a CMOS wave, the output amplitude is 12V, the frequency is 2Hz, the phase difference of the double channels is 180 degrees, and the amplification factor of the power amplifier is 2 times.

(3) Starting the magnetic particle control system 1, and inputting current signals to the two sucker type electromagnets 1-4; 2 g of magnetic particles are added into the oil-water separation chamber 2-5, under the action of the magnetic particle control system 1, the magnetic particles can transversely reciprocate in a magnetic field action area at the lower part of the oil-water separation chamber 2-5 to form a magnetic particle dynamic bed, solid-liquid separation is provided at the upper part of the separation chamber, and the magnetic particles separated from the constraint of the magnetic field are settled to the magnetic field action area at the lower part and are captured by the magnetic field.

(4) Starting the peristaltic pump 2-4, pumping the emulsion into the oil-water separation chamber 2-5 at a flow rate of 10 ml/min, wherein the emulsion flows through the dynamic bed layer from bottom to top in a direction perpendicular to the reciprocating motion of the magnetic particles, and completing the demulsification and oil-water separation process. Under the flow, the hydraulic retention time of the emulsion in the magnetic field action area of the oil-water separation chamber 2-5 is 120 s.

(5) As the device operates, certain floating oil is accumulated on the liquid surface of the oil-water separation chamber 2-5, and the floating oil accumulated in the separation chamber can be skimmed off by periodically opening an oil discharge valve of the oil-water separation chamber 2-5.

(6) And sampling from the water outlet pipe every 5-20 min to test the water transmittance so as to represent the continuous operation effect of the device.

(7) After use, the whole flow path is cleaned, and the device is disassembled for standby.

In addition, perfection or optimization of the technical scheme, the emulsion continuous coarse-grained emulsion breaking device based on the magnetic particle dynamic bed provided by the invention also has the following characteristics:

preferably, the slide rail can be fixed at any position on the platform, the sucker type electromagnet can be fixed at any point along the axis of the electromagnet fixer, the oil-water separation chamber can be fixed at any point along the axis of the oil-water separation chamber fixer, the relative distance between the three fixers can be adjusted at will along the slide rail, and the demulsification separation operation platform can adapt to electromagnets and oil-water separation chambers with various sizes and shapes.

Preferably, the oil-water separation chamber 2-5 has an oil skimming function, is provided with a water inlet, a water outlet and an oil discharge port, and is of a lower-inlet and upper-outlet structure, wherein the water outlet is bent upwards to a certain height and then is bent into a horizontal pipe which can be externally connected with a water outlet pipe. The oil outlet is horizontal, the height is lower than the horizontal pipe section of the water outlet, and an oil discharge valve is arranged to discharge floating oil on the liquid surface periodically, which is shown in figure 3.

Preferably, the slide rails of the demulsification separation operation platform can be respectively fixed on the platform in the horizontal direction or the vertical direction and are respectively suitable for a transverse flow oil-water separation chamber (longitudinal reciprocating movement of particles) and a longitudinal flow oil-water separation chamber (transverse reciprocating movement of particles).

Preferably, the demulsification separation operation platform slide rail is provided with scale marks, so that the distance between the two sucker type electromagnets and the oil-water separation chamber can be conveniently measured. Handles are arranged on the two side edges of the platform 3-1, so that the whole experimental device can be conveniently moved.

Example 1

By adopting the installation and use method of the emulsion continuous demulsification and separation device based on the magnetic particle dynamic bed, a model emulsion sample with an oil phase of liquid paraffin and an oil concentration of 10 g/L is processed. The rotating speed of the emulsifying machine is 13000 r/min, and the emulsifying time is 5 min; 2 g of magnetic particles with a particle size of 1 μm, designated MP1, were added to the oil-water separation chamber.

Adjusting the magnetic particle manipulation system parameters to: channel 1: CMOS, phase 0 °, amplitude 2.4V, frequency 2 Hz; and (3) a channel 2: CMOS, amplitude 2.4V, frequency 2Hz, and two-channel phase difference 180 degrees. Amplification factor of the power amplifier: 10.

adjusting the emulsion flow path parameters as follows: the adding amount of the particles is 2 g, the rotating speed of a peristaltic pump is 2.1rpm, and the flow rate is about 10 ml/min; the hydraulic retention time of the emulsion in the magnetic field action area at the lower part of the oil-water separation chamber is 120 s, the hydraulic retention time of the emulsion in the upper part separation area of the oil-water separation chamber is 230 s, and samples are taken from the water outlet pipe every 10 min to test the water transmittance.

The demulsification separation operation platform slide rail is arranged along the horizontal direction, and the distance between the oil-water separation chamber fixer and the electromagnet fixer is 4 cm.

The effects of the continuous operation of the present invention under the above parameters are shown in table 1 and fig. 4 below.

Table 1 shows the effect of the continuous operation of example 1:

from the operation effect, the continuous emulsion breaking and separating device based on the magnetic particle dynamic bed can improve the light transmittance of the emulsion from 2.93 percent of the water inlet to more than 95 percent when MP1 with the particle size of 1 mu m is used, and has higher emulsion breaking efficiency. MP1 can make the effluent luminousness higher than 90% in the running time of 100 min, and the subsequent demulsification deoiling effect is still obvious, and the effluent luminousness is improved obviously compared with the original liquid. The handling capacity of the MP1 with unit mass for playing a high-efficiency demulsification function (the effluent transmittance is more than 90%) is more than 500 ml/g.

Example 2

By adopting the installation and use method of the emulsion continuous demulsification and separation device based on the magnetic particle dynamic bed, a model emulsion sample with an oil phase of liquid paraffin and an oil concentration of 10 g/L is processed. The rotating speed of the emulsifying machine is 13000 r/min, and the emulsifying time is 5 min; 2 g of magnetic particles (designated as MP 2) with a particle size of 1000 mesh (14 μm or less) were added to the oil-water separation chamber.

The magnetic particle control system parameters, emulsion flow path parameters and demulsification separation operation platform arrangement mode are the same as those of the test example 1.

The effects of the continuous operation of the present invention under the above parameters are shown in the following table 2 and fig. 5.

Table 2 shows the effect of the continuous operation of example 2:

from the operation effect, when the MP2 with the particle size of 1000 meshes is used, the light transmittance of the emulsion can be improved to more than 65% from 2.93% of the inflow water, the emulsion breaking and oil removing effect is obvious, and the difficulty of subsequent treatment is greatly reduced. MP2 can make the effluent luminousness higher than 60% in the operating time of 150 min, has more lasting demulsification deoiling performance, and the effluent luminousness is improved obviously compared with the stock solution. The handling capacity of the MP2 with unit mass for playing a high-efficiency demulsification function (the effluent transmittance is more than 60%) is more than 750 ml/g.

The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.