CN210795800U - Device for preparing magnetic nano ferroferric oxide - Google Patents
Device for preparing magnetic nano ferroferric oxide Download PDFInfo
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- CN210795800U CN210795800U CN201920893210.6U CN201920893210U CN210795800U CN 210795800 U CN210795800 U CN 210795800U CN 201920893210 U CN201920893210 U CN 201920893210U CN 210795800 U CN210795800 U CN 210795800U
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Abstract
The utility model relates to a device for preparing magnetic nano ferroferric oxide, which comprises a reaction unit, a separation unit and a cleaning and drying unit; wherein the reaction unit comprises a reaction kettle,A feeding unit and a temperature control unit; the separation unit is connected with the reaction unit and comprises a high-gradient magnetic separator for separating the starch wastewater after reaction; the cleaning unit is connected with the separation unit and is used for cleaning the separated magnetic nano particles; the drying unit is connected with the separation unit and used for drying the cleaned magnetic nano material. The device can be used for preparing high-quality nano Fe3O4 products with controllable particle size distribution, crystallinity and particle composition in batches, and can remarkably reduce nano Fe while realizing resource utilization of starch wastewater3O4The preparation cost can also realize the resource utilization of the wastewater, and promote the clean production and sustainable development of the corn deep processing industry.
Description
Technical Field
The utility model belongs to the technical field of waste water treatment and nano-material preparation, especially, relate to an use device of magnetism nanometer ferroferric oxide of starch waste water as solvent preparation.
Background
Magnetic nano ferroferric oxide (Fe)3O4) The magnetic nano-composite material has the characteristics of superparamagnetism, large specific surface area, high catalytic activity, easy surface modification, no toxic or side effect on a human body and the like, and can be widely applied to the aspects of coloring agents, plastics, leather, automobile finishing coat, high-magnetic recording materials, adsorbents, catalysts, biosensing, cell tracking, tissue engineering, magnetic resonance imaging, targeted drug delivery, cancer treatment and the like. In recent years, magnetic nano-Fe3O4The metal oxide has become a hot point of academic research as an adsorption material and a catalytic material, and shows great application prospects in various fields of environmental protection, chemical industry, energy and the like.
Magnetic nano Fe3O4The preparation method of (2) is more, but the nano Fe can be prepared in batches3O4The method mainly comprises two methods, namely a mechanical ball milling method and a coprecipitation method. The mechanical ball milling method is simple and convenient to operate, but the prepared particles have the defects of wide size distribution, long preparation time, high energy consumption, easy introduction of impurities and the like, so that the method is not suitable for preparing uniform magnetic nano materials. Preparation of Fe by coprecipitation3O4Nanoparticles are very convenient, but the product generally has the defect of wide size distribution, and the surface structure of the product is often a mixture of iron oxide and iron hydroxide, so that the purity is low. Therefore, the magnetic nano Fe with controllable granularity, granularity distribution, crystallinity and particle composition is prepared in batches at low cost3O4Becomes the key to the large-scale practical application.
In recent years, the solvothermal method is widely used in the laboratory for the synthesis of nanomaterials, and Fe prepared by the method3O4The nano-crystal has the advantages of high purity, complete crystal grain development, controllable particle size and the like. However, the solvothermal method requires ethylene glycol, polyethylene glycol, sodium acetate and the like as a solvent, a stabilizer and a charge stabilizer, so that the preparation cost is high; and the lack of process and equipment for batch preparation of nanomaterials by solvothermal methods limits the scale-up of the process.
China is a large country for starch production and consumption, and the starch industry is one of important industries in national economy. However, the starch industry is also a large waste water discharge household; according to investigation, the average discharged wastewater amount of each ton of corn starch is 5-10 tons, and the wastewater has the characteristics of high Chemical Oxygen Demand (COD), high Suspended Solid (SS), high Total Nitrogen (TN), high Total Phosphorus (TP), low pH and higher difficulty in treating the tail end of the wastewater, wherein the wastewater is 4-1-low. On the other hand, the starch wastewater belongs to high-concentration acidic organic wastewater, mainly contains starch, protein and saccharide, and is rich in nutrient substances such as nitrogen, phosphorus and the like, so that the difficulty of end treatment can be reduced and the utilization efficiency of resources can be improved if the starch wastewater is effectively utilized.
SUMMERY OF THE UTILITY MODEL
Technical problem to be solved by the utility model
The utility model aims at providing a based on solvothermal method to amino acid, protein and saccharide in the starch waste water replace chemical reagent such as ethylene glycol, polyethylene glycol, sodium acetate as solvent and stabilizer, add alkali and ferric salt preparation nanometer Fe3O 4's process units in the starch waste water.
Means for solving the technical problem
In order to solve the problems, the utility model provides a device for preparing magnetic nano ferroferric oxide.
According to one embodiment of the utility model, the device for preparing the magnetic nano ferroferric oxide is characterized by comprising a reaction module, a separation module, a cleaning module and a drying module;
the reaction module comprises a reaction unit, a feeding unit and a temperature control unit, wherein the feeding unit is used for providing reaction raw materials for the reaction unit, and the temperature control unit is used for controlling the reaction temperature of the reaction unit;
the separation module is connected with the reaction module and is used for separating the starch wastewater after reaction;
the cleaning module is connected with the separation module and is used for cleaning the separated magnetic nano particles;
the drying module is connected with the separation module and used for drying the cleaned magnetic nano material.
In one embodiment, the feeding unit comprises a starch wastewater providing unit, an alkali providing unit and a ferric salt providing unit.
In one embodiment, the separation module comprises a high gradient magnetic separator.
In one embodiment, the high gradient magnetic separator comprises a yoke, an electromagnetic coil, and a separation vessel filled with stainless steel wool.
One embodiment is that, the cleaning module includes washing unit and mellow wine washing unit, and mellow wine washing unit includes mellow wine supply unit and high-pressure inert gas provides the unit, and mellow wine supply unit and inert gas provide the unit and cooperate each other and provide high-pressure aqueous vapor.
The beneficial effects of the utility model
The utility model discloses an aspect can be with low costs, prepare high-quality nanometer Fe that particle size distribution, crystallinity and particle composition are controllable in batches3O4And (5) producing the product. On the other hand, Fe is formed in the reduction of trivalent iron3O4In the process of nanocrystalline, partial organic matters and proteins in the wastewater can be oxidized and decomposed; prepared nano Fe3O4Can adsorb trace heavy metals in wastewater on the surface of the wastewater and magnetically separate nano Fe3O4Heavy metals are removed from the wastewater while the product is produced; the pathogenic bacteria in the wastewater can be killed in the high-temperature and high-pressure environment in the preparation process. Thus, the nano Fe is prepared by the solvothermal method3O4The starch wastewater does not contain heavy metal and pathogenic bacteria, is rich in organic matters, nitrogen and potassium (such as potassium hydroxide added in the preparation process), and part of the organic matters and proteins are effectively decomposed and can be used as a soil conditioner or a high-quality raw material for producing organic fertilizers, so that the resource utilization of the wastewater is realized, and the clearing of the corn deep processing industry is promotedClean production and sustainable development.
Further features of the present invention will become apparent from the following description of exemplary embodiments.
Drawings
FIG. 1 is a process flow chart of the utility model for synthesizing and collecting magnetic ferroferric oxide by using corn starch wastewater based on a hydrothermal method.
FIG. 2 is a schematic diagram of an apparatus for synthesizing and collecting magnetic ferroferric oxide by using corn starch wastewater based on a hydrothermal method.
Fig. 3 is a sectional view of the magnetic separator 31 in a front view.
Fig. 4 is a sectional view of the magnetic separator 31 in a plan view.
Fig. 5 is a sectional view of the structure of the magnetic separator 31 viewed from below.
FIGS. 6 and 7 are scanning electron micrographs of nano magnetic ferroferric oxide synthesized by using corn starch wastewater.
Wherein: valves 7, 10, 14, 15, 21, 24, 25, 29, 30, 33, 34, a water tank 1, a rapid detector 2, a fiber rotary disc type filter 3, a starch waste liquid storage unit 5, a circulating pump 6, 11, a circulating oil heating container 8, a circulating oil heating container 9, an alkali medicine storage tank 12, a ferric salt medicine storage tank 13, a stirrer motor 16, an exhaust hole 17, a flushing nozzle 18, a stirrer 19, a centrifugal pump 22, a gas storage tank (nitrogen gas), 23, a backflushing water tank 26, an ultrasonic generator 27, a water level probe 28, a high gradient magnetic separator 31, a cleaning liquid tank (methanol) 32, a vacuum drier 35, a residual material recovery tank 36, a central control table 37, a temperature induction probe 38, an automatic pressure regulator 39, a reaction kettle interlayer 40, nano particle sewage inlet 3-1 clear water, a methanol inlet 3-2, a high pressure nozzle 3- An acoustic generator 3-7 excitation coil 3-8 south pole 3-9 sewage outlet 3-10 methanol mixed nanoparticle outlet 3-11 yoke iron 3-12 matrix 3-13
Detailed Description
One embodiment of the present disclosure will be specifically described below, but the present disclosure is not limited thereto.
The starch wastewater is mainly obtained from the drainage after protein recovery in working sections of corn soaking, germ separation and washing, fiber washing, flotation concentration, protein filter pressing and the like and the mixed wastewater of evaporation condensate water generated in the recovery of corn soaking water resources when corn is used as a raw material for producing starch. Starch is deeply processed into other products, and the wastewater mainly comes from the total wastewater generated by ion exchange column washing water, washing water of various devices, washing water and the like.
The alkali is not particularly limited, and an alkali which is inexpensive, easily available, harmless to animals and plants, and capable of neutralizing organic acids well is preferable if the added element can be absorbed by plants.
The trivalent ferric salt is not particularly limited, and the trivalent ferric salt which is low in price, easy to obtain, harmless to animals and plants and capable of oxidizing organic matters in the wastewater is preferred; other options, for example: and (3) iron oxide.
COD is a representation method of chemical oxygen demand, and the lower the COD is, the lower the content of organic matters is represented; tests show that when the dosage is lower than 2800, the organic matter is insufficient, the smooth reaction cannot be guaranteed, and when the dosage is higher than 20000, the dosage is too much, the reaction is insufficient, and waste is caused. COD is 2800-20000, and COD and the dosage are in a linear and direct proportional relationship.
According to an embodiment of the utility model, the utility model discloses a preparation magnetism nanometer ferroferric oxide's device, including reaction module, separation module, washing module and drying module. A control module may also be further included.
FIG. 1 and FIG. 2 show a process and equipment for synthesizing and collecting magnetic ferroferric oxide by using corn starch wastewater based on a hydrothermal method. The console 37 will control the automatic detection of COD, water injection, dosing, stirring, heating, cooling and cleaning. All annotate powder waste liquid memory cell 5 before equipment work at every turn, when equipment work once more, annotate powder waste liquid memory cell 5 again, the value that detects COD is carried out again to fast detector 2 simultaneously.
[ control Module ]
The component parts and the connection mode of the control module can be realized by selecting a conventional control device in the prior art without special limitation, as long as the functions of the utility model can be realized. It is used for controlling the steps of automatic COD detection, addition and proportion of reaction raw materials, stirring, heating, cooling, cleaning and the like. For example, as shown in fig. 1 and 2, the control module is a console 37, and the console 37 controls automatic COD detection, water injection, dosing, stirring, heating, temperature reduction, and cleaning. All annotate powder waste liquid memory cell 5 before equipment work at every turn, when equipment work once more, annotate powder waste liquid memory cell 5 again, the value that detects COD is carried out again to fast detector 2 simultaneously.
[ reaction Module ]
The reaction module comprises a reaction unit, a feeding unit and a temperature control unit, the structure and the connection mode are not particularly limited as long as the functions of the utility model can be realized, the feeding unit is used for providing starch wastewater, alkali and ferric salt for the reaction kettle, and the temperature control module is used for controlling the reaction temperature of the reaction kettle;
as shown in fig. 1 and 2, the feeding unit comprises a starch waste liquid storage unit 5 and an alkali medicine storage tank 12 and a ferric salt medicine storage tank 13, which are communicated with a reaction kettle 20.
[ separation Unit ]
The separation unit is connected with the reaction module, the structure and the connection mode are not particularly limited as long as the functions of the utility model can be realized, and the high gradient magnetic separator 31 is adopted in the utility model; the high gradient magnetic separator 31 is communicated with the reaction kettle 20 and used for separating starch wastewater (also called nano particle wastewater) after reaction.
The high gradient magnetic separator 31 comprises 3-12 parts of yoke iron, 3-8 parts of exciting coil, a separating container filled with stainless steel wool, 3-1 parts of nano particle sewage inlet, 3-2 parts of clear water and methanol inlet, 3-11 parts of methanol mixed nano particle outlet and 3-10 parts of sewage outlet. The upper half part of the external device is a cylinder, and the lower half part is a bowl with an upward opening. The inner machine type upper half part is a cylinder, the lower half part is a circular truncated cone, the outer diameter a of the circular truncated cone at the upper part is provided with the inner diameter b and the height h1, the diameter of a water inlet is d1, d2, b/a is 0.98-0.99, h1/a is 0.29-0.39, and d1/b is 0.08-0.1. The diameter of the bottom of the lower half circular truncated cone is b, the diameter of the top of the lower half circular truncated cone is b, the height of the lower half circular truncated cone is h2, the diameter of effluent is d3, d4, d3/b and d4/b are 0.08-0.1. The volume V ═ pi h1b2/4+ pi h2[ (d3+ d4)2+ b2+ (d3+ d4) b ]/3. The substrates 3-13 are both cylinders with the diameter c, and the c/b is 0.75-0.8. The inner diameter magnetic field gradient can be as high as 1000G/mum, and a plurality of magnetic separators can be connected.
[ cleaning Module ]
The component parts and the connection mode of the cleaning module can be realized by selecting conventional devices in the prior art without special limitation as long as the functions of the utility model can be realized. The cleaning module is connected with the separation unit and used for cleaning the separated magnetic nano particles; the device comprises a water washing unit and an alcohol washing unit, wherein the alcohol washing unit comprises an alcohol supply unit and a high-pressure inert gas supply unit, and the alcohol supply unit and the inert gas supply unit are matched with each other to supply high-pressure water vapor;
the utility model discloses in, adopted gas holder (nitrogen gas) 23, recoil basin 26, washing fluid reservoir (methyl alcohol) 32, it is linked together with high gradient magnetic separator 31, and gas holder (nitrogen gas) 23 and washing fluid reservoir (methyl alcohol) 32 link to each other, can form the air water mixture (or refer to the air water mixture) and let in high gradient magnetic separator 31.
When cleaning, firstly washing with water and then washing with alcohol, wherein the washing with water and the washing with alcohol can be repeated, and after the washing with alcohol again, the washing with alcohol again can be carried out by adopting a high-pressure water-gas mixture formed by inert gas and alcohol.
[ drying Module ]
The conventional device in the existing technology can be selected to realize the component parts, the connection mode and the like of the drying module without special limitation as long as the functions of the utility model can be realized. The drying module is connected with the separation unit and used for drying the cleaned magnetic nano material. In the utility model, a vacuum drier 15 is adopted.
Examples
The present invention will be described in more detail by way of examples, but the present invention is not limited to the following examples.
A reaction stage:
firstly, filling a starch waste liquid storage unit 5 for deep processing of starch waste water, feeding back a COD value of the starch waste water detected by a rapid detector 2 to a central console 37, driving a metering pump 3 by the central console 37 to inject (1/3-5/8) volume of waste water into a reaction kettle 20, and then preheating circulating oil (controlling the temperature at 180-220 ℃) by a circulating oil heating container 8The circulating oil cooling container 9 also starts cooling the circulating oil (the temperature of the circulating oil cooling container 9 is controlled to be-10 to 0 ℃). The ratio of the amounts of the materials added into the reaction kettle 20 is Fe3+/OH—1/3.0-1/3.5, Fe3+ (ferric sulfate or ferric chloride can be used), and OH- (potassium hydroxide, sodium hydroxide or ammonia water can be used). When the COD of the wastewater is 2800, the amount of Fe3+ substance added is 1.3mmol (millimole) to 2.0mmol per 40ml of wastewater. When the COD of the wastewater is 2800-20000, the amount of the added Fe3+ is in direct proportion to the COD. The central control unit 37 calculates the amount of alkali and ferric salt to be added according to the value of COD and the volume of the water injected into the reaction kettle 20, and when the amount of the water is set, the metering pump 4 stops working (the water outlet speed of the pump is controlled to be 2.0 m/s-2.5 m/s). Next, console 37 controls valve 14 to open and inject the required amount of base, and agitator 19 is stopped after 5 minutes of rotation. After standing for 15 minutes, the center console 37 controls the dosing valve 15 to open the trivalent iron salt stirrer 19 with the required injection amount, and stops stirring after 5 minutes (the rotation speed is controlled to be 40r/min-60 r/min). Then the central console 37 controls the three- way valves 7 and 10 to communicate the circulating pump 6, the circulating oil heating container 8 and the circulating pump 11, and starts the circulating pumps 6 and 11 to inject hot oil in the circulating oil heating container 8 into the reaction kettle 20 for heating (the central console 37 controls the temperature of the hot oil to be stable at 180-220 ℃ and lasts for 10 hours), after the 10 hours of reaction time, the circulating pump 6 stops working, the circulating pump 11 pumps all hot oil in the interlayer of the reaction kettle into the circulating oil heating container 8 and stops working (the circulating oil heating container 8 keeps the temperature at 180-220 ℃, heat loss is reduced, and heating time is saved for the next reaction), the central console 37 controls the three-way valves 7 and 10 (communicates the circulating pump 6 and the circulating oil cooling container 9 with the circulating pump 11) and starts the circulating pumps 6 and 11 to inject cold oil in the circulating oil cooling container 9 into the reaction kettle; the reaction vessel was cooled.
A magnetic separation stage:
the central console 37 controls the temperature of the temperature sensing probe 38 to be 20-30 ℃; the circulation pump 6 stops working, and the circulation pump 11 pumps all cold oil in the interlayer of the reaction kettle into the circulation oil cooling container 9 and stops working; ball valve 21 and kettle vent 17 are opened and the kettle begins to drain and high gradient magnetic separator 31 (see fig. 2) is activated. After the wastewater after reaction completely enters the separator 31; the rinsing spout 18 is opened; after the stirrer 19 starts rotating and spraying for 20-30 s; the rinsing spout 18 and the stirrer 19 are stopped. (30-60S), closing the valve 21 (closing and simultaneously controlling each reaction kettle 20 to perform the next reaction by the central console 37); the sewage containing magnetic nano material is pumped into the high gradient magnetic separator tank 31 by the centrifugal pump 22, the water level reaches the water level probe 28, the lower valve 34 is opened (the valve 34 is shown in detail in figure 3), the particles in the wastewater flowing through the separator 31 are acted by magnetic force in the magnetic field and captured by the matrix-steel wool, the wastewater flows out through the lower pipeline of the separator 31, and the wastewater is treated further. And in the working process of the separator 31, cooling water is continuously introduced for cooling, so that the normal operation of the machine is ensured. After the high gradient magnetic separator 31 is emptied of sewage, the valve 34(34 valve is shown in detail in FIG. 3) is closed.
And (3) a cleaning and drying stage:
after the separator stops operating, a valve 24 is opened, water is filled into a backflushing water tank 26, at the moment, a valve 29 is opened, water is filled into a separator 31, when the water level probe 28 is reached, the valves 24 and 29 are closed, an ultrasonic generator 27 (with the frequency of 3.4Hz-6.1Hz) on two sides of the inner wall of the separator is started to work for 5min and then stopped, at the moment, the separator 31 is restarted, nano particles are adsorbed on bristles again due to magnetic force, then, a valve 33 is opened (the valve 33 is shown in detail in figure 3), water flows out along with a sewage discharge pipeline, and the primary water washing process is finished. The washing process can be repeated for 2-3 times. And after the separator 31 stops operating again, opening the valve 30, introducing cleaning liquid (methanol) into the separator 31 from the cleaning tank 32, closing the valve 30 when the water level probe 28 is reached, starting the ultrasonic generator 27 again (with the frequency of 3.4Hz-6.1Hz) to work for 5min, then stopping, restarting the separator 31, adsorbing the nano particles on the bristles again, and finishing the primary alcohol washing process. The separator 31 is stopped, the valves 30 and 25 are opened, the protective gas nitrogen is filled in the gas storage tank 23, the nitrogen and methanol are mixed and then are conveyed to the top of the high-gradient magnetic separator 31, a high-pressure water-gas mixture is formed through a nozzle (the water washing process adopts a mode of filling the tank body for cleaning, water is filled into the separator 31, the first alcohol washing is the mode of filling the tank body for cleaning, the second time and the third time adopt back washing, high-pressure atomized spray formed by back washing can effectively reduce the using amount of cleaning solution methanol), the high-pressure atomized spray is sprayed on the substrate (the substrate refers to an overlapped stainless steel bristle plate, and the protruded bristles can better capture magnetic nano particles) of the high-gradient magnetic separator and the wall of the separator, through comparison, the demagnetizing back washing after the substrate is adsorbed and saturated has better back washing effect through gas-water mixing (the back washing aims, often in combination with a gas wash, the flushing pressure is increased by counter-pressurization, and the resulting water vapor mixture flushes impurities). The secondary alcohol washing process is finished. The valve 33 is opened and the magnetic nanoparticles accompanied by methanol flow into the vacuum drier 35. The total volume of the dryer is 500L, the heating area is 2.63m3, the design pressure in the tank is-0.09 Mpa to-0.096 Mpa, the device has the characteristics of obtaining higher drying speed at lower temperature, sealing and drying materials, preventing the materials and the environment from being polluted, preventing the materials from being oxidized easily, having higher heat efficiency and the like, can recover the solvent, dry the materials to very low moisture, and finally put the magnetic nano-materials after vacuum drying into the excess material recovery tank 36 for recovery.
Industrial applicability
Utilize the device of the utility model to prepare high-quality nanometer Fe with controllable particle size distribution, crystallinity and particle composition in batches3O4The product can obviously reduce the nano Fe while realizing the resource utilization of the starch wastewater3O4The preparation cost can also realize the resource utilization of the wastewater, and promote the clean production and sustainable development of the corn deep processing industry.
The present invention is not limited to the above embodiments, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are also covered by the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (6)
1. The device for preparing the magnetic nano ferroferric oxide is characterized by comprising a reaction module, a separation module, a cleaning module and a drying module;
the reaction module comprises a reaction unit, a feeding unit and a temperature control unit, wherein the feeding unit is used for providing reaction raw materials for the reaction unit, and the temperature control unit is used for controlling the reaction temperature of the reaction unit;
the separation module is connected with the reaction module and is used for separating the starch wastewater after reaction;
the cleaning module is connected with the separation module and is used for cleaning the separated magnetic nano particles;
the drying module is connected with the separation module and used for drying the cleaned magnetic nano material.
2. The apparatus of claim 1, wherein the feeding unit comprises a starch wastewater providing unit, an alkali providing unit, and a ferric salt providing unit.
3. The device of any of claims 1-2, wherein the temperature control unit comprises a heating unit and a cooling unit.
4. The apparatus of any of claims 1-2, wherein the separation module comprises a high gradient magnetic separator.
5. The apparatus of claim 4, wherein the high gradient magnetic separator comprises a yoke, a solenoid coil, a separation vessel filled with stainless steel wool.
6. The apparatus of claim 1, wherein the cleaning module comprises a water washing unit and an alcohol washing unit, the alcohol washing unit comprises an alcohol supply unit and a high pressure inert gas supply unit, and the alcohol supply unit and the inert gas supply unit cooperate with each other to supply high pressure water vapor.
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| CN110194490A (en) * | 2019-06-14 | 2019-09-03 | 长春工程学院 | A kind of method and apparatus preparing magnetic nano ferroferric oxide |
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