CN104785164A - Device for preparing colloidal particles through electrostatic spraying and control method of device - Google Patents
Device for preparing colloidal particles through electrostatic spraying and control method of device Download PDFInfo
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- CN104785164A CN104785164A CN201510177757.2A CN201510177757A CN104785164A CN 104785164 A CN104785164 A CN 104785164A CN 201510177757 A CN201510177757 A CN 201510177757A CN 104785164 A CN104785164 A CN 104785164A
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Abstract
The invention discloses a device for preparing colloidal particles through electrostatic spraying and a control method of the device. Evaluating and measuring devices used by the invention include a spraying liquid storage tank, a high-pressure liquid spraying chamber, a metal spray head for electrostatic spraying, a leading-out pole, an inter-pole electric field distribution modulation structure and a powder collection box. According to the device for preparing colloidal particles through electrostatic spraying and the control method of the device, a grounded collector is moved forwards, and a small hole is formed right opposite to the spraying opening of the metal spray head for electrostatic spraying as the leading-out pole, so that the inter-pole distance is greatly shortened, and only a smaller voltage needs to be added to realize the same electric field intensity; meanwhile, the inter-pole anti-electromagnetic interference capability is improved, and the safety of using equipment is further improved; the inter-pole electric field distribution modulation structure is further added at the spraying opening end of a high-voltage pole, so that the electric field distribution between the two poles can be better gathered, a power line in the electric field near the inter-pole spraying opening can penetrate through the small hole in the leading-out pole, and accordingly all the electrified atomized liquid drops can penetrate through the small hole in the leading-out pole and enter the powder collection box at the rear end of the leading-out pole; in addition, particle in-situ observation and analysis equipment can be mounted.
Description
Technical field
The present invention relates to colloidal solid technology of preparing, be specifically related to a kind of electrostatic spray and prepare colloidal solid device and control method thereof.
Background technology
Electrostatic spray refers to and makes to need ejecting fluid to form droplet by high pressure, electrostatic equipment and charged, and charged drop surface forms the atomization droplet of escaping due to high electrostatic field.Can by various fluid by electrostatic spray, comprise Polymer Solution, biomolecule, protein solution, be suspended mixed liquor, the even liquid electrolyte of melting, be atomized by high-pressure electrostatic, and by the control measures such as electric field, temperature humidity of periphery, prepare uniform coating, spray paint film, and granular deposit.The early stage research of electrostatic Spraying technique starts from the beginning of eighties of last century, first Lord Rayleigh establishes to electrostatic spray the quantity of electric charge that preliminary theory model carrys out quantification drop, i.e. " the Rayleigh limit ", and the Hydrodynamics Mechanism of this system has been further developed by Zeleny, establish droplet charged leave nozzle formed drippage, fall apart from, pulse, and convergent cone spray, until the 1970's, the theoretical research of this problem is still constantly perfect, the wherein what is called " Taylor cone " of Taylor proposition, and developed the dielectric model for conductor fluid.After this, analytic theory model also there is development, but definite prediction atomized drop size, carried charge is still a challenge.In recent years, researcher, by experiment for multiple fluid and mixed system, proposes some empirical equations to predict the parameter such as size, shape, carried charge of drop.
Along with the fast development of 20th century nanometer science and technology, electrostatic spray have also been obtained very big concern as a kind of important technology of preparing, and electrostatic spray is progressively applied to the preparation of micron and nano particle.The electrostatic atomizer adding receiving pole with traditional shower nozzle is preparing micron and nano particle, because device is too simple, be difficult to preparation requirement, such as, particle size uniformity controls, the requirement of spout low-voltage, and powder collection pre-treatment etc. is all subject to great restriction.Especially in pharmaceuticals industry, friendly Polymer Solution medicine carrying is used, dry through electrostatic spray, variation, controlled medicine carrying model can be prepared, thus electrostatic Spraying technique is greatly paid close attention to.And other industry is as in the spraying industrial production of the shells such as automobile, household electrical appliances, instrument, the preparation of milk powder, food, drug powder particles, and to numerous areas such as crops pesticide sprayings, also make electrostatic Spraying technique extensively be researched and developed as a kind of technology of key.Due to the demand that it is important, researcher has expanded large quantity research for several main parameter, as found controlled empirical equation to describe viscosity, conductance, surface tension, density, the dielectric parameter that each parameter comprises fluid, the shape of nozzle, size, material, the rate of flow of fluid sprayed, electric field level etc.But the regulation and control for electric field itself have but been left in the basket with design, especially how to regulate and control the spatial distribution of drop surrounding electric field, spray droplet size and later stage are controlled there is important effect.
At present, when preparing micrometer/nanometer particle by electrostatic spray dry technology, adopt device as shown in Figure 1, the solution be stored in hydrojet storage tank 01 is transported to high pressure spray liquid chamber 02 by hydrojet carrier pipe, peristaltic pump, arrange electrostatic spray Metallic Nozzle At The Ingot 03 at the outlet end of high pressure spray liquid chamber 02, the opposite side relative with electrostatic spray Metallic Nozzle At The Ingot 03 arranges powder collection pole 04, and electrostatic spray Metallic Nozzle At The Ingot 03 connects high voltage, powder collection pole 04 ground connection, forms electric field so between.Space electric field constructed by this device exists obviously not enough when preparing micron order colloidal solid, be mainly manifested in:
1) in order to prepare micron order colloidal solid, require atomized drop particle before flying collector with regard to energy drying and moulding, this needs to make have enough distances to complete dry run between high-pressure nozzle and collector, excessive die opening defection makes two interpolar electric fields easily be subject to external interference, causes micron order colloidal solid size distribution uneven;
2) owing to needing enough spacing between shower nozzle and receiving pole, the atomization of the liquid material spray of nozzle simultaneously needs higher field intensity, and nozzle electric field is not only relevant with the physical dimension of spout, also relevant with anode-cathode distance, nozzle electric field level is directly proportional to the voltage added by interpolar, be inversely proportional to die opening, therefore, when large anode-cathode distance, in order to obtain high electric-field intensity on shower nozzle, then must add high voltage in two-stage, this just needs for shower nozzle is equipped with high voltage power supply, add the manufacturing cost of equipment undoubtedly greatly, complexity and the requirement to device security,
3) due to limited working space, be difficult to arrange the devices such as heating, drying, observation and analysis between the two poles of the earth, increasing these devices at interpolar all can cause the distribution of the space electric field between high-pressure nozzle and collector to change, and then affect the collection of grain diameter size and particle, and the observation and analysis of original position cannot be carried out;
4) collector is both as electrode, again as gathering-device, this collection efficiency is reduced, and needs periodic cleaning collector, the use of device is become and more bothers, and improve maintenance cost.
Summary of the invention
For above problems of the prior art, the present invention proposes a kind of electrostatic spray and prepares colloidal solid device and control method thereof, designs the regulation and control scheme of a set of electric field space distribution more optimized.
One object of the present invention is to provide a kind of electrostatic spray colloidal solid preparation facilities.
Electrostatic spray colloidal solid preparation facilities of the present invention comprises: hydrojet storage tank, high pressure spray liquid chamber, electrostatic spray Metallic Nozzle At The Ingot, extraction pole, interpolar Electric Field Distribution modulated structure and powder collection case; Wherein, the solution be stored in hydrojet storage tank is delivered to high pressure spray liquid chamber by peristaltic pump through hydrojet carrier pipe; On the top of high pressure spray liquid chamber, electrostatic spray Metallic Nozzle At The Ingot is set; Extraction pole is set before electrostatic spray Metallic Nozzle At The Ingot, and just aperture is arranged to the position of shower nozzle at extraction pole; Electrostatic spray Metallic Nozzle At The Ingot connects DC high voltage as high-pressure stage, and extraction pole ground connection, forms electric field therebetween; Interpolar Electric Field Distribution modulated structure is set at the spout end of electrostatic spray Metallic Nozzle At The Ingot, the Electric Field Distribution between electrostatic spray Metallic Nozzle At The Ingot and extraction pole is assembled; The charged aerosolized liquid droplets that electrostatic spray Metallic Nozzle At The Ingot place is formed is through the aperture of extraction pole, and then free flight enters the powder collection case being arranged on extraction pole rear end.
The present invention is by the powder collection pole reach in existing apparatus, make it close to shower nozzle, and just a sizeable aperture is being opened to shower nozzle place, its function is changed, be not re-used as collector, but as the extraction pole of charged aerosolized liquid droplets, device through changing like this can effectively solve Problems existing in existing apparatus: first, the introducing of extraction pole, greatly can shorten anode-cathode distance, to obtain the electric-field intensity same with existing apparatus at nozzle, only need add that at the two poles of the earth very little voltage can realize in the present invention, this greatly reduces the requirement to high voltage source undoubtedly, also improve interpolar anti-electromagnetic interference capability simultaneously, and the security of the equipment of use have also been obtained further raising, in addition, charged aerosolized liquid droplets is through can free flight after the aperture of extraction pole, increase any device in the free space of rear end, extraction pole hole and can not produce obviously impact to interpolar electric field again, temperature, powder collection case that humidity is adjustable so just can be installed in the free space of particle flight, can around powder collection case installation particle in-situ observation and analysis equipment.
But, because the jet size of the electrostatic spray Metallic Nozzle At The Ingot as high-pressure stage is less, and it is larger as the plate dimensions of extraction pole, two interpolar Electric Field Distribution can be caused to disperse, most charged aerosolized liquid droplets through the aperture of extraction pole, cannot cause wastage of material thus preparation efficiency is reduced greatly.In order to address this problem, the present invention improves further, an interpolar Electric Field Distribution modulated structure is increased at the spout end of high-pressure stage, by interpolar Electric Field Distribution modulated structure, two interpolar Electric Field Distribution can be made to be assembled preferably, make the large portion of the power line of electric field near interpolar spout can pass the aperture of extraction pole, finally make charged aerosolized liquid droplets can pass the aperture of extraction pole, then free flight enters the powder collection case of extraction pole rear end.
Bottom in powder collection case arranges powder collection plate, for collect that spray from the aperture of extraction pole, shaping after powder colloidal solid.Powder collection case is placed on warm table; Warm table is connected to warm table power supply, can temperature adjustment within the scope of 30 ~ 200 DEG C, for regulating the temperature in powder collection case, is conducive to from the charged aerosolized liquid droplets of extraction pole ejection shaping as early as possible.Position relative with aperture in powder collection case arranges window, can be taken powder collection plate by window.
The fluid speed current control of high pressure spray liquid chamber is between 0.01ml/min ~ 50ml/min.The length of electrostatic spray Metallic Nozzle At The Ingot is between 5 ~ 20mm, and the nozzle pluggage of electrostatic spray Metallic Nozzle At The Ingot is between 0.1 ~ 0.5mm, and external diameter is between 2 ~ 5mm.Extraction pole is between the dead ahead 5 ~ 20mm of electrostatic spray Metallic Nozzle At The Ingot.The aperture of the aperture of extraction pole is between 0.5 ~ 10mm.The length of side of powder collection case is between 30 ~ 100cm.
Interpolar Electric Field Distribution modulated structure is the metal cylinder of one end open, the diameter of cylinder is between 5 ~ 20mm, the other end seals, the center of sealing is provided with aperture, aperture is consistent with the external diameter of electrostatic spray Metallic Nozzle At The Ingot, the aperture of electrostatic spray Metallic Nozzle At The Ingot in the middle of interpolar Electric Field Distribution modulated structure is through stretching in metal cylinder, and the diameter of aperture, between 2 ~ 5mm, is electric connection between the two and fixes.
Another object of the present invention is the control method providing a kind of electrostatic spray colloidal solid preparation facilities.
The control method of electrostatic spray colloidal solid preparation facilities of the present invention, comprises the following steps:
1) solution be stored in hydrojet storage tank is delivered to high pressure spray liquid chamber by peristaltic pump through hydrojet carrier pipe;
2) the electrostatic spray Metallic Nozzle At The Ingot arranged on the top of high pressure spray liquid chamber is connected DC high voltage as high-pressure stage, will the extraction pole ground connection before electrostatic spray Metallic Nozzle At The Ingot be arranged on, and form electric field therebetween;
3) interpolar Electric Field Distribution modulated structure is set at the spout end of electrostatic spray Metallic Nozzle At The Ingot, Electric Field Distribution between electrostatic spray Metallic Nozzle At The Ingot and extraction pole is assembled, make the power line of electric field near interpolar spout major part to pass extraction pole aperture, thus make charged aerosolized liquid droplets can pass the aperture of extraction pole;
4) charged aerosolized liquid droplets of electrostatic spray Metallic Nozzle At The Ingot place formation is through free flight after the aperture of extraction pole, enters the powder collection case being arranged on extraction pole rear end.
Advantage of the present invention:
The present invention is by moving forward the collector of ground connection, and just aperture is being offered as extraction pole to the nozzle of electrostatic spray Metallic Nozzle At The Ingot, substantially reduce anode-cathode distance, only need add very little voltage just can realize same electric-field intensity, also improve interpolar anti-electromagnetic interference capability simultaneously, the security of use equipment have also been obtained further raising, in addition, temperature, powder collection case that humidity is adjustable can be installed in the free space of particle flight, also particle in-situ observation and analysis equipment can be installed around powder collection case; An interpolar Electric Field Distribution modulated structure is increased further at the spout end of high-pressure stage, two interpolar Electric Field Distribution are assembled preferably, the power line of electric field near interpolar spout is made to pass extraction pole aperture, finally make charged aerosolized liquid droplets through the aperture of extraction pole, the powder collection case of extraction pole rear end can be entered.
Accompanying drawing explanation
Fig. 1 is the structural representation that existing electrostatic spray dry technology prepares micrometer/nanometer particle device;
Fig. 2 is the schematic diagram of the embodiment one of electrostatic spray colloidal solid preparation facilities of the present invention;
Fig. 3 is 1/2 sectional view of the partial enlargement of the interpolar Electric Field Distribution modulated structure of the embodiment two of electrostatic spray colloidal solid preparation facilities of the present invention;
Fig. 4 is the schematic diagram between the spout of the electrostatic spray Metallic Nozzle At The Ingot of the embodiment one of electrostatic spray colloidal solid preparation facilities of the present invention and extraction pole, wherein, a () is the electric force lines distribution theoretical modeling calculating chart between spout and extraction pole, the actual spray effect figure between (b) spout and extraction pole;
Fig. 5 is the schematic diagram between the spout of the electrostatic spray Metallic Nozzle At The Ingot of the embodiment two of electrostatic spray colloidal solid preparation facilities of the present invention and extraction pole, wherein, a () is the electric force lines distribution theoretical modeling calculating chart between spout and extraction pole, the actual spray effect figure between (b) spout and extraction pole;
Fig. 6 is the scanning electron microscope (SEM) photograph of the micron powder colloidal solid obtained adopting electrostatic spray colloidal solid preparation facilities of the present invention.
Detailed description of the invention
Below in conjunction with accompanying drawing, by embodiment, the present invention will be further described.
Embodiment one
As shown in Figure 2, the electrostatic spray colloidal solid preparation facilities of the present embodiment comprises: hydrojet storage tank 1, high pressure spray liquid chamber 2, electrostatic spray Metallic Nozzle At The Ingot 3, extraction pole 4 and powder collection case 5; Wherein, the hydrojet be stored in hydrojet storage tank 1 is delivered to high pressure spray liquid chamber 2 by peristaltic pump through hydrojet; On the top of high pressure spray liquid chamber 2, electrostatic spray Metallic Nozzle At The Ingot 3 is set; Extraction pole 4 is set before electrostatic spray Metallic Nozzle At The Ingot 3, and just aperture 41 is being arranged to the position of shower nozzle; Electrostatic spray Metallic Nozzle At The Ingot 3 connects the high-pressure side of nozzle high-voltage power supply 9, and extraction pole 4 connects the earth terminal of nozzle high-voltage power supply 9, forms electric field therebetween; The charged aerosolized liquid droplets that electrostatic spray Metallic Nozzle At The Ingot place is formed, through free flight after the aperture 41 of extraction pole, enters the powder collection case 5 being arranged on extraction pole rear end.Bottom in powder collection case 5 arranges powder collection plate 6; Powder collection case 5 is placed on warm table 61; Warm table 61 is connected to warm table power supply 62; Position relative with aperture in powder collection case 5 arranges window 51.
In the present embodiment, the aperture of the aperture of extraction pole is 8mm, the wall thickness 0.5mm of extraction pole, electrostatic spray Metallic Nozzle At The Ingot is 8mm to the distance of the small hole center of extraction pole, the diameter of electrostatic spray Metallic Nozzle At The Ingot is 0.5mm, and the high pressure of connection is 10KV, and the area of powder collection plate is 10 × 10cm
2, heating-up temperature is 100 DEG C.By the material spray of acetone soln as liquid state that the molecular weight that concentration is 2% is the polymetylmethacrylate of 950K, prepare particle diameter at the uniform powder colloidal solid of tens micron grain sizes.
The device of embodiment one can do another and optimize, because the jet size of the electrostatic spray Metallic Nozzle At The Ingot as high-pressure stage is less, and it is larger as the plate dimensions of extraction pole, two interpolar Electric Field Distribution can be caused to disperse, most charged aerosolized liquid droplets through the aperture of extraction pole, cannot cause wastage of material thus preparation efficiency is reduced greatly.The each electrode space position provided for the device in Fig. 2 and physical dimension, carried out analog computation by Comsol Finite Element Simulation Software to its Electric Field Distribution, the theoretical modeling of the electric force lines distribution between spout and extraction pole calculates as shown in Fig. 4 (a).Find by calculating, the power line sent from the most advanced and sophisticated 2mm of the spout of high-pressure stage is no more than 20% through the number of extraction pole aperture, that is, actual charged charged aerosolized liquid droplets is no more than 20% through the number of the aperture of extraction pole, this and actual conditions meet, and the actual spray effect between spout and extraction pole is as shown in Fig. 4 (b).Cause the basic reason of this problem to be, two interpolar Electric Field Distribution that spout and extraction pole geometry and relative position as high-pressure stage cause too are dispersed and are caused.
Embodiment two
In order to address this problem, improve further, increase an interpolar Electric Field Distribution modulated structure 7 at the spout end of the electrostatic spray Metallic Nozzle At The Ingot 3 of high-pressure stage, as shown in Figure 3.By interpolar Electric Field Distribution modulated structure, two interpolar Electric Field Distribution can be made to be assembled preferably, make the large portion of the power line of electric field near interpolar spout can pass the aperture of extraction pole, finally make charged aerosolized liquid droplets can pass the aperture of extraction pole, then free flight enters the powder collection case of extraction pole rear end.
The theoretical modeling of the electric force lines distribution between the spout of the present embodiment and extraction pole calculates as shown in Fig. 5 (a), as we know from the figure, in the present embodiment, power line within the scope of electrostatic spray Metallic Nozzle At The Ingot 2mm almost reaches 100% through the quantity of the aperture of extraction pole, that is charged aerosolized liquid droplets is almost all through the aperture of extraction pole, therefore, this is the structure that a kind of preparation efficiency is very high.Actual spray effect between spout and extraction pole is as shown in Fig. 5 (b).
In the present embodiment, interpolar Electric Field Distribution modulated structure 7 is tubular, and electrostatic spray Metallic Nozzle At The Ingot 3 stretches into about 1/2 place in metal cylinder, and the edge of metal cylinder aligns with the edge of the aperture of extraction pole.Barrel dliameter 8mm, wall thickness 0.5mm, cylinder edge is 5mm to electrostatic spray metal extraction pole vertical range, and electrostatic spray Metallic Nozzle At The Ingot 3 distance stretched in metal cylinder is 3mm, and other parameters are with embodiment one.
Fig. 6 is the scanning electron microscope (SEM) photograph of the micron powder colloidal solid obtained adopting electrostatic spray colloidal solid preparation facilities of the present invention.
It is finally noted that, the object publicizing and implementing mode is to help to understand the present invention further, but it will be appreciated by those skilled in the art that: without departing from the spirit and scope of the invention and the appended claims, various substitutions and modifications are all possible.Therefore, the present invention should not be limited to the content disclosed in embodiment, and the scope that the scope of protection of present invention defines with claims is as the criterion.
Claims (10)
1. an electrostatic spray colloidal solid preparation facilities, is characterized in that, described preparation facilities comprises: hydrojet storage tank, high pressure spray liquid chamber, electrostatic spray Metallic Nozzle At The Ingot, extraction pole, interpolar Electric Field Distribution modulated structure and powder collection case; Wherein, the solution be stored in hydrojet storage tank is delivered to high pressure spray liquid chamber by peristaltic pump through hydrojet carrier pipe; On the top of high pressure spray liquid chamber, electrostatic spray Metallic Nozzle At The Ingot is set; Extraction pole is set before electrostatic spray Metallic Nozzle At The Ingot, and just aperture is arranged to the position of shower nozzle at extraction pole; Electrostatic spray Metallic Nozzle At The Ingot connects DC high voltage as high-pressure stage, and extraction pole ground connection, forms electric field therebetween; Interpolar Electric Field Distribution modulated structure is set at the spout end of electrostatic spray Metallic Nozzle At The Ingot, the Electric Field Distribution between electrostatic spray Metallic Nozzle At The Ingot and extraction pole is assembled; The charged aerosolized liquid droplets that electrostatic spray Metallic Nozzle At The Ingot place is formed is through the aperture of extraction pole, and then free flight enters the powder collection case being arranged on extraction pole rear end.
2. preparation facilities as claimed in claim 1, it is characterized in that, described extraction pole is between the dead ahead 5 ~ 20mm of electrostatic spray Metallic Nozzle At The Ingot; The aperture of the aperture of described extraction pole is between 0.5 ~ 10mm.
3. preparation facilities as claimed in claim 1, it is characterized in that, described interpolar Electric Field Distribution modulated structure is the metal cylinder of one end open, the other end seals, the center of sealing is provided with aperture, aperture is consistent with the external diameter of electrostatic spray Metallic Nozzle At The Ingot, and the aperture of electrostatic spray Metallic Nozzle At The Ingot in the middle of interpolar Electric Field Distribution modulated structure, through stretching in metal cylinder, is electric connection between the two and fixes.
4. preparation facilities as claimed in claim 3, it is characterized in that, the diameter of the cylinder of described metal cylinder is between 5 ~ 20mm; The diameter of the aperture at the center of the sealing of the metal cylinder other end is between 2 ~ 5mm.
5. preparation facilities as claimed in claim 1, it is characterized in that, the bottom in described powder collection case arranges powder collection plate; Described powder collection case is placed on warm table; Described warm table is connected to warm table power supply.
6. preparation facilities as claimed in claim 1, is characterized in that, the fluid speed current control of described high pressure spray liquid chamber is between 0.01ml/min ~ 50ml/min.
7. preparation facilities as claimed in claim 1, it is characterized in that, the length of described electrostatic spray Metallic Nozzle At The Ingot is between 5 ~ 20mm; The nozzle pluggage of described electrostatic spray Metallic Nozzle At The Ingot is between 0.1 ~ 0.5mm; External diameter is between 2 ~ 5mm.
8. preparation facilities as claimed in claim 1, it is characterized in that, the length of side of described powder collection case is between 30 ~ 100cm.
9. preparation facilities as claimed in claim 1, it is characterized in that, in described powder collection case, the position relative with aperture arranges window.
10. a control method for electrostatic spray colloidal solid preparation facilities, is characterized in that, described control method comprises the following steps:
1) solution be stored in hydrojet storage tank is delivered to high pressure spray liquid chamber by peristaltic pump through hydrojet carrier pipe;
2) the electrostatic spray Metallic Nozzle At The Ingot arranged on the top of high pressure spray liquid chamber is connected DC high voltage as high-pressure stage, will the extraction pole ground connection before electrostatic spray Metallic Nozzle At The Ingot be arranged on, and form electric field therebetween;
3) interpolar Electric Field Distribution modulated structure is set at the spout end of electrostatic spray Metallic Nozzle At The Ingot, the Electric Field Distribution between electrostatic spray Metallic Nozzle At The Ingot and extraction pole is assembled, make the power line of electric field near interpolar spout major part to pass extraction pole aperture;
4) charged aerosolized liquid droplets of electrostatic spray Metallic Nozzle At The Ingot place formation is through free flight after the aperture of extraction pole, enters the powder collection case being arranged on extraction pole rear end.
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| CN107303538A (en) * | 2017-05-23 | 2017-10-31 | 东南大学 | A kind of biology molecule separating equipment and separation method |
| CN108883385A (en) * | 2017-10-16 | 2018-11-23 | 天津策浪生物科技有限公司 | Electrospray device, fluid unit and method for fluid unit |
| CN110404474A (en) * | 2019-07-05 | 2019-11-05 | 金华职业技术学院 | A kind of preparation method of spherical liquid particle |
| CN110570391A (en) * | 2019-07-24 | 2019-12-13 | 天津科技大学 | Image analysis method for spray freezing coating effect based on Image J |
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