CN207451636U - The system that MgZn ferrite is prepared using pickling sludge and pickle liquor - Google Patents
The system that MgZn ferrite is prepared using pickling sludge and pickle liquor Download PDFInfo
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- CN207451636U CN207451636U CN201721563162.1U CN201721563162U CN207451636U CN 207451636 U CN207451636 U CN 207451636U CN 201721563162 U CN201721563162 U CN 201721563162U CN 207451636 U CN207451636 U CN 207451636U
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Abstract
The utility model discloses the systems that MgZn ferrite is prepared using pickling sludge and pickle liquor, belong to danger wastes recycling field.System includes water tank, water pump, ferrite hydro-thermal preparation facilities, the first feed pump, the second feed pump, acid storage tank, storage alkali tank, discharging pump, separation of solid and liquid filter-pressing device, ferrite drying device and ferrite collection device, water tank, acid storage tank, storage alkali tank are connected respectively by water pump, the first feed pump, the second feed pump with ferrite hydro-thermal preparation facilities, the discharge port of ferrite hydro-thermal preparation facilities is connected by discharging pump with separation of solid and liquid filter-pressing device, and separation of solid and liquid filter-pressing device is connected with ferrite drying device.Using pickling sludge and pickle liquor prepare MgZn ferrite method include preparing predecessor, hydro-thermal prepares ferrite, separation of solid and liquid and dry ferrite.The utility model realizes that the recycling coexistence of pickling sludge and pickle liquor is put, and prepares MgZn ferrite.
Description
Technical field
The utility model belongs to danger wastes recycling field, is related to a kind of utilization pickling sludge and is prepared by pickle liquor
The system of MgZn ferrite prepares being total to for MgZn ferrite more specifically to a kind of pickling sludge with pickle liquor hydro-thermal
Disposal system prepares industrial products --- the magnesium zinc-iron oxygen with compared with high added value using pickling sludge and pickle liquor as raw material
Body.
Background technology
A large amount of pickling sludge and pickle liquor can be generated in metallurgy industry production process, wherein containing plurality of heavy metal from
Son, intractability is big, and cost of disposal is high, does not find economical and effective method of disposal all the time, and it is special to cause serious region
The environmental pollution of sign property, seriously constrains the development of metallurgy industry.
Pickling sludge source is in the processing procedure of acid waste water, pickling and phosphatization production of the waste water in metallurgy
Process contains substantial amounts of metallic element.Essential element content is in pickling sludge：Fe30 ± 5%, Ca20 ± 5%, Cl5 ±
2%th, S5 ± 2%, P5 ± 1%, Zn4 ± 1%, Mg4 ± 1%, Si2 ± 1%, Al1 ± 0.5% and other trace elements.Mesh
Before, it is hydroxide precipitation method to handle the most important method of the waste water.Using calcium hydroxide or sodium hydroxide as alkaline precipitating agent
It adds in waste water, by neutralization heavy metal is made to generate hydroxide not soluble in water and precipitate to separate, the sediment of formation
As pickling sludge.According to the on-site investigation of Jiangsu Province's pickling sludge as a result, the whole province's different industries generate the enterprise of pickling waste waters at present
Industry totally 1047, generates 17,870,000 tons of pickling waste waters year, and waste water year processing sludge reaches 16.5 ten thousand tons.Wherein Taizhou Xinghua, wear
The pickling sludge yield in the area such as south, Nantong economic development zone, Wuxi Huishan District, Beitang District is larger, accounts for the 63.7% of the whole province.
In general, the main resource disposal options of pickling sludge include pyrometallurgical smelting, hydrometallurgic recovery and stabilize skill
Art.Pyrometallurgical smelting method comprehensive utilization degree is high, and with certain economic benefit, product can be as smelting industry raw material, state
Interior most enterprise all carries out comprehensive utilization disposal using this method, but this method to energy consumption and invests all excessively high, operability
It is low, control improper easy generation sulfur dioxide, containing secondary pollutions such as heavy metal dusts.Hydrometallurgic recovery producing level is high, equipment letter
It is single, take up little area, easy to operate management, but technique and immature at present, the economic benefit is not high, and leaching agent can be caused in practical application
The problems such as dosage is big, efficiency is low, phase analysis is difficult.Although stabilization technology can by harmful substance and environment relative insulation,
It needs to occupy substantial amounts of soil and space resources, Heavy Metal Level In Sludge is not reduced, however it remains the risk of secondary pollution,
It is also a kind of waste of heavy metal resources simultaneously.
Pickle liquor derives from the acid cleaning process of Steel material.Pickle liquor essential element content is：Fe2+50±5g/L、Fe3 +30 ± 5g/L and Ca, Mg, Zn are micro.During the storage of rerolled steel material or after heat treatment, surface can generate one layer
Fine and close iron oxide cortex, to ensure that steel material surface chemical property is conducive to later processing operation, the main side for using pickling
Method removes iron scale.Mild steel enterprise generally using chlorohydric acid pickling, steel rolling mill's acid-washing stainless steel generally using nitric acid, sulfuric acid,
Hydrofluoric acid etc..Because hydrochloric acid compared with other acid solutions has the characteristics that consumption is few, at low cost, pickling is quick, cleaning performance is good, from previous generation
Discipline progressively substitutes other acid to apply in acid cleaning process from the sixties.Pickling process generally by concentrated hydrochloric acid be diluted to 18% or so into
Row pickling, when concentration of hydrochloric acid is down to below 10%, because metal ion reaches a certain concentration in acid solution, under pickling effect is notable
Drop, it is difficult to reach requirement, be regarded as spent acid (i.e. pickle liquor) at this time and dispose.At present, national pickle liquor discharge
Measure 1 × 106m of ＞3/a。
At present, the main method of pickle liquor disposal has membrane processing method, high-temperature roasting method, evaporation absorption method.Membrane processing method
Can high efficiente callback acid and metal salt, acid recovering rate is high, purity is high, but treating capacity is small, and pre-processing requirements are high, and membrane module is easy
Pollution, cost of disposal are high.High-temperature roasting method investment is big, and occupation area of equipment is big, to the design of equipment, management, control and corrosion resistant
The requirement of erosion is high, and operating cost is high, consumes a large amount of cooling waters, electricity, fuel, therefore is appropriate only for large enterprise, in being not suitable for
Small business.Evaporation absorption method equipment requirement is higher, and regular maintenance is frequent, and operating cost is higher, while pickle liquor evaporates back
The concentration of hydrochloric acid of receipts is relatively low, and frerrous chloride crystallization can be precipitated in concentration process, be easy to cause equipment blocking, therefore has centainly
Limitation.
Through retrieval, prepare ferritic research respectively with pickle liquor on pickling sludge at present and be disclosed, such as document
《Pickling sludge prepares ferrite absorption Pb2+Waste water is studied》In analyze pickling sludge physicochemical characteristics, additional iron chloride is mended
It fills source of iron and complex ferrite is synthesized with pickling sludge, research magnesium Ni ferrite is to Pb2+Adsorption.Chlorination is used in the research
Iron supplements source of iron, it is necessary to put into certain cost, and economy is relatively low, and magnesium Ni ferrite is obtained by handling single danger wastes.
For another example Application No. 201110110999.1, the Chinese invention patent of Publication No. CN102219493A disclose one
The method that kind prepares MnZn ferrite feed powders using pickle liquor and zinc coated slag, this application is that zinc coated slag is dissolved in acid
It washes waste liquid and obtains mixed solution, then the pH value for adjusting mixed solution with ammonium hydroxide adds in fluoride and reaction is obtained by the reaction to 3-6
Liquid adds flocculant thereto, filters removing precipitation and obtains filtrate, by filtrate and manganese chloride by Fe in ferrite ingredient2O3/
The molar ratio of MnO/ZnO is configured to precipitation solution, adds in the precipitating reagent that ammonium hydrogen carbonate and ammonium hydroxide are prepared thereto, slurry is obtained by the reaction
Material, by slurry oxidation, washing filtering, the drying after ageing.Raw material is used in this application as zinc coated slag, it is dirty with pickling
Mud composition is different.Because zinc coated slag main component is zinc, manganese chloride, technique are required supplementation with when preparing ferrite using zinc coated slag
Complex, economy is relatively low, obtains product as manganese-zinc ferrite.
For another example Application No. 2009100503423, the Chinese invention patent of Publication No. CN101565304A disclose one
The processing method of kind electroplating sludge and pickle liquor cooperative with hydrothermal ferrite.This application using industrial waste electroplating sludge and
Pickle liquor is raw material, and with water as solvent, ammonium hydroxide obtains corresponding heavy metal hydroxide under certain condition as pH adjusting agent
Object undergoes the specific physical chemistry ring that can not be realized under a normal temperature and pressure as predecessor, then these metal hydroxides
Border, fully dissolving forms different growth units, and according to certain bind mode nucleating growth, crystallizes into stable compound iron
Oxysome.It is dealt with objects in the program as electroplating sludge, essential element constituent：Fe65 ± 5%, Ca20 ± 5%, Zn2.0 ±
0.5%th, Ni0.4 ± 0.05%, Cr0.5 ± 0.05% and Cu, Cd, Pb are micro, and every gram of electroplating sludge needs to add in the program
The volume of pickle liquor is 0.82~2.82ml, and the difference of pickle liquor dosage can influence containing for the metallic elements such as nickel magnesium zinc
Amount, what which was prepared is the nickel-zinc ferrite with suitable nickel zinc content.
The content of the invention
1st, to solve the problems, such as
For current metallurgy industry pickling sludge and the reluctant problem of pickle liquor, the utility model provides a kind of profit
The system that MgZn ferrite is prepared with pickling sludge and pickle liquor.Acid can both be realized using the technical solution of the utility model
The minimizing disposal of sludge and pickle liquor is washed, while industrial products-MgZn ferrite with compared with high added value can be prepared,
The recycling of danger wastes is realized, so as to bring certain benefit to enterprise.
2nd, technical solution
To solve the above problems, the present invention adopts the following technical scheme that.
A kind of system that MgZn ferrite is prepared using pickling sludge and pickle liquor, including water tank, water pump, ferrite
Hydro-thermal preparation facilities, the first feed pump, the second feed pump, acid storage tank, storage alkali tank, discharging pump, separation of solid and liquid filter-pressing device and iron
Oxysome drying device, the water tank, the acid storage tank, the storage alkali tank respectively by the water pump, first feed pump,
Second feed pump is connected with the ferrite hydro-thermal preparation facilities, and the discharge port of the ferrite hydro-thermal preparation facilities passes through
The discharging pump is connected with the separation of solid and liquid filter-pressing device, the separation of solid and liquid filter-pressing device and the ferrite drying device
Connection.
Further, the ferrite hydro-thermal preparation facilities includes reaction kettle and the stirring of acid and alkali-resistance high-temperature-resistant high-pressure-resistant
Device, the blender are located in the reaction kettle, and the bottom longitudinal section of the reaction kettle is ellipse, and bottom is to recessed structure
Be conducive to the discharge of ferrite mixed liquor, the blender uses polytetrafluoroethylene (PTFE) material and for U-shaped structure.
Further, the separation of solid and liquid filter-pressing device be plate and frame filter press, plate compression technique can realize solid with
Liquid efficiently separates, and moisture content is down to 70% by the technique most multipotency at present.
Further, the discharge port of the separation of solid and liquid filter-pressing device passes through conveyer belt and the ferrite drying device
Feed inlet is connected.
Further, ferrite collection device, discharge port and the ferrite of the ferrite drying device are further included
Collection device connects, and ferrite drying device exports low structure design, the ferrite drying device bag using entrance is high
Include entrance, cylinder and outlet, drying process middle cylinder body rotates, the rotation of cylinder, while plays the role of transmission and uniformly heated.
A kind of method that MgZn ferrite is prepared using pickling sludge and pickle liquor utilizes pickling sludge and acid described
It washes waste liquid and prepares and followed the steps below in the system of MgZn ferrite：
A, predecessor is prepared：Pending pickling sludge is added in ferrite hydro-thermal preparation facilities, from water tank to
Water and stirring and dissolving are added in ferrite hydro-thermal preparation facilities, pickling is added into ferrite hydro-thermal preparation facilities from acid storage tank and gives up
Liquid supplements source of iron and stirs evenly, and lye is added as precipitating reagent into ferrite hydro-thermal preparation facilities from storage alkali tank；
B, hydro-thermal prepares ferrite：Ensure hydrothermal temperature and vapour pressure be respectively 150-250 DEG C, the item of 2-4atm
Under part, it is stirred in ferrite hydro-thermal preparation facilities, ferrite mixed liquor is obtained after hydro-thermal reaction, treat that ferrite mixes
Kettle is opened after closing liquid cooled to room temperature；
C, separation of solid and liquid：Ferrite mixed liquor drains into separation of solid and liquid filter-pressing device by discharging pump, and press filtration separation liquid obtains
To ferrite solid；
D, dry ferrite：Ferrite solid is sent to ferrite drying device and is dried, and by dried iron oxygen
Body discharge is collected.
Further, in step A pickling sludge dosage be the ferrite hydro-thermal preparation facilities volume 1/5-1/
3, the quality of water, the quality of pickling sludge, the quality of pickle liquor added into ferrite hydro-thermal preparation facilities meets m respectively
(water)：M (pickling sludge)=(1-3)：1, m (pickle liquor)：M (pickling sludge)=(0.3-1)：1, and will by adding lye
The pH value of solution is adjusted to 8-11 in the ferrite hydro-thermal preparation facilities, stirring and dissolving in the ferrite hydro-thermal preparation facilities
Rotating speed be 200-500r/min, mixing time 0.5-2h.
Further, the rotating speed stirred in step B is 200-500r/min, mixing time 5-10h.Vapour pressure, temperature,
Mixing speed, mixing time, which reach requirement, could realize that hydro-thermal reaction is complete, and so as to be prepared, grain size is tiny, uniform iron oxygen
Body.
Further, the product ferrite that separation of solid and liquid filter-pressing device press filtration separation ferrite mixed liquor obtains in step C
Solid aqueous rate is 70-90%.
Further, drying temperature is 100-150 DEG C in ferrite drying device in step D.
With《Pickling sludge prepares ferrite absorption Pb2+Waste water is studied》Unlike disclosed technical solution：The present invention adopts
It is prepared jointly with pickling sludge and pickle liquor, product is MgZn ferrite, can be reached while two kinds of danger of disposal of resources
The purpose of discarded object, and input cost supplement source of iron is not required, therefore with better economic benefit.
The technical solution announced with the Chinese invention patent of Publication No. CN102219493A is the difference is that the present invention
Product is MgZn ferrite, in preparation process input cost is not required to supplement other metals, simple for process, has good economy
Benefit.
The technical solution announced with the Chinese invention patent of Publication No. CN101565304A is the difference is that in this programme
In the pickling sludge used essential element content for：Fe30 ± 5%, Ca20 ± 5%, Cl5 ± 2%, S5 ± 2%, P5 ± 1%,
Zn4 ± 1%, Mg4 ± 1%, Si2 ± 1%, Al1 ± 0.5% and other trace elements, technical solution of the present invention and the invention
Sludge components composition is there are larger difference in technical solution, therefore process conditions are also different, and every gram of pickling sludge needs in the present invention
The volume of the pickle liquor of addition is 0.3~1ml, and what the present invention obtained is suitable magnesium Zn content, in addition, the two is prepared
Product it is also different, the product which is prepared is nickel-zinc ferrite, and the product that is prepared of the present invention is magnesium zinc-iron
Oxysome.
3rd, advantageous effect
Compared with the prior art, beneficial effects of the present invention are：
(1) system provided by the invention that MgZn ferrite is prepared using pickling sludge and pickle liquor, realizes pickling
The minimizing disposal of sludge and pickle liquor, while the MgZn ferrite with compared with high added value is prepared, it realizes dangerous useless
The recycling of gurry, so as to bring certain benefit to enterprise；
(2) system provided by the invention that MgZn ferrite is prepared using pickling sludge and pickle liquor, the bottom of reaction kettle
Portion longitudinal section is ellipse, which is conducive to the discharge of ferrite mixed liquor；
(3) system provided by the invention that MgZn ferrite is prepared using pickling sludge and pickle liquor, separation of solid and liquid pressure
Filter device can realize the solid of ferrite mixed liquor and efficiently separating for liquid, be conducive to the progress of follow-up drying process, especially
When it is by plate compression technique, most moisture content is down to 70% by multipotency；
(4) system provided by the invention that MgZn ferrite is prepared using pickling sludge and pickle liquor, ferrite drying
When device exports low design using entrance is high, with the rotation of cylinder, while play the role of transmission and uniformly heated；
(5) system provided by the invention that MgZn ferrite is prepared using pickling sludge and pickle liquor, ferrite hydro-thermal
It is connected between preparation facilities and separation of solid and liquid filter-pressing device using discharging pump, separation of solid and liquid filter-pressing device and ferrite drying device
Between be placed in using transmission band connection, ferrite collection device below ferrite drying device discharge port, can so reach company
The purpose of continuous metaplasia production, so as to improve production efficiency, realizes the maximization of the performance of enterprises；
(6) method provided by the invention that MgZn ferrite is prepared using pickling sludge and pickle liquor, pickling sludge and
Pickle liquor prepares ferrite jointly, has not only realized the minimizing disposal of danger wastes, but also realizes the mesh of recycling
, increase the profit of enterprise；
(7) method provided by the invention that MgZn ferrite is prepared using pickling sludge and pickle liquor, ferrite hydro-thermal
The high vapour pressure condition of preparation facilities high temperature realizes the complete progress of reaction, so as to prepare the higher ferrite of quality；
(8) method provided by the invention that MgZn ferrite is prepared using pickling sludge and pickle liquor, using hydro-thermal method
It can synthesize that grain size is tiny, uniform powder, be conducive to low-temperature sintering, pure Spinel is directly obtained under relatively lower temp
Ferrite.
Description of the drawings
Fig. 1 is the structure diagram for the system that MgZn ferrite is prepared using pickling sludge and pickle liquor；
Fig. 2 is the flow chart for the method that MgZn ferrite is prepared using pickling sludge and pickle liquor.
Label declaration in schematic diagram：1st, water tank；2nd, water pump；3rd, ferrite hydro-thermal preparation facilities；4th, the first feed pump；
5th, the second feed pump；6th, acid storage tank；7th, alkali tank is stored up；8th, discharging pump；9th, separation of solid and liquid filter-pressing device；10th, conveyer belt；11st, iron oxygen
Body drying device；12nd, ferrite collection device.
Specific embodiment
The present invention will be described in detail below in conjunction with the accompanying drawings.
As shown in Figure 1, a kind of system that MgZn ferrite is prepared using pickling sludge and pickle liquor, including water tank 1,
It is water pump 2, ferrite hydro-thermal preparation facilities 3, the first feed pump 4, the second feed pump 5, acid storage tank 6, storage alkali tank 7, discharging pump 8, solid
Liquid separates filter-pressing device 9 and ferrite drying device 11, and the water tank 1, the acid storage tank 6, the storage alkali tank 7 pass through respectively
The water pump 2, first feed pump 4, second feed pump 5 are connected with the ferrite hydro-thermal preparation facilities 3, the iron
The discharge port of oxysome hydro-thermal preparation facilities 3 is connected by the discharging pump 8 with the separation of solid and liquid filter-pressing device 9, the solid-liquid
Separation filter-pressing device 9 is connected with the ferrite drying device 11.Ferrite hydro-thermal preparation facilities 3 has agitating function, water pump
2nd, the first feed pump 4, the second feed pump 5 use acid-alkali-corrosive-resisting elevator pump.
The ferrite hydro-thermal preparation facilities 3 includes reaction kettle and blender, and the blender is located in the reaction kettle,
The bottom longitudinal section of the reaction kettle is ellipse, and bottom is conducive to the discharge of ferrite mixed liquor to recessed structure, described
Blender uses polytetrafluoroethylene (PTFE) material and for U-shaped structure.
The separation of solid and liquid filter-pressing device 9 is plate and frame filter press, is down to moisture content by plate compression technique most multipotency
70%.
The charging that the discharge port of the separation of solid and liquid filter-pressing device 9 passes through conveyer belt 10 and the ferrite drying device 11
Mouth is connected.
Ferrite collection device 12 is further included, the discharge port of the ferrite drying device 11 is collected with the ferrite to be filled
12 connections are put, and the ferrite drying device exports low structure design using entrance is high.
Pickling sludge agitation is dissolved in the water by the present invention by ferrite hydro-thermal preparation facilities 3, adds in pickling thereto
Waste liquid supplements source of iron, adds alkaline precipitating agent and adjusts pH value, and hydro-thermal reaction is carried out under the conditions of certain temperature and vapour pressure and is obtained
To ferrite mixed liquor, the ferrite mixed liquor of generation is drained by discharging pump in separation of solid and liquid filter-pressing device 9, separates liquid
Solid is obtained, ferrite solid is transported in ferrite drying device 11 by conveyer belt 10 and is dried, the iron oxygen after drying
Body is collected into ferrite collection device 12.System using the present invention can effectively realize the money of pickling sludge and pickle liquor
Sourceization is disposed, and is reduced environmental pollution, and operating procedure is simple, can realize automation continuous production.
As shown in Fig. 2, a kind of method that MgZn ferrite is prepared using pickling sludge and pickle liquor, in the utilization
Prepared by pickling sludge and pickle liquor follows the steps below in the system of MgZn ferrite：
A, predecessor is prepared：Pending pickling sludge is added in ferrite hydro-thermal preparation facilities 3, by water tank 1
Water and stirring and dissolving are added into ferrite hydro-thermal preparation facilities 3, is added from acid storage tank 6 into ferrite hydro-thermal preparation facilities 3
Pickle liquor supplements source of iron and stirs evenly, and lye is added as precipitation into ferrite hydro-thermal preparation facilities 3 from storage alkali tank 7
Agent, the dosage of pickling sludge are the 1/5-1/3 of 3 volume of ferrite hydro-thermal preparation facilities, prepare and fill to ferrite hydro-thermal
It puts the quality of the water added in 3, the quality of pickling sludge, the quality of pickle liquor and meets m (water) respectively：M (pickling sludge)=
(1-3)：1, m (pickle liquor)：M (pickling sludge)=(0.3-1)：1, and prepared the ferrite hydro-thermal by adding lye
The pH value of solution is adjusted to 8-11 in device (3), and the rotating speed of stirring and dissolving is 200- in the ferrite hydro-thermal preparation facilities (3)
500r/min, the time stirred every time are 0.5-2h；
B, hydro-thermal prepares ferrite：Under conditions of 150-250 DEG C of temperature, vapour pressure 2-4atm, in ferrite hydro-thermal system
It is at the uniform velocity stirred in standby device 3, speed of agitator 200-500r/min, mixing time 5-10h, after hydro-thermal reaction
To ferrite mixed liquor, kettle is opened after ferrite mixed liquor cooled to room temperature；
C, separation of solid and liquid：Ferrite mixed liquor drains into separation of solid and liquid filter-pressing device 9 by discharging pump 8, and press filtration separates liquid,
Ferrite solid is obtained, ferrite solid aqueous rate is 70-90%；
D, dry ferrite：Ferrite solid is sent to ferrite drying device 11 and is dried, drying temperature 100-
150 DEG C, dried ferrite is discharged and is collected.
The techniques such as the present invention is by preparing predecessor, hydro-thermal prepares ferrite, separation of solid and liquid and dry ferrite, are realized
The disposal of resources of pickling sludge and pickle liquor, and carried out by the process to more than each process and technological parameter excellent
Change design, so as to ensure the effect of pickling sludge and pickle liquor disposal of resources, effectively reduce the pollution to environment.
The present invention is further described below with reference to specific embodiment.
Embodiment 1
As shown in Figure 1, a kind of system that MgZn ferrite is prepared using pickling sludge and pickle liquor, including water tank 1,
It is water pump 2, ferrite hydro-thermal preparation facilities 3, the first feed pump 4, the second feed pump 5, acid storage tank 6, storage alkali tank 7, discharging pump 8, solid
Liquid separates filter-pressing device 9 and ferrite drying device 11, and the water tank 1, the acid storage tank 6, the storage alkali tank 7 pass through respectively
The water pump 2, first feed pump 4, second feed pump 5 are connected with the ferrite hydro-thermal preparation facilities 3, the iron
The discharge port of oxysome hydro-thermal preparation facilities 3 is connected by the discharging pump 8 with the separation of solid and liquid filter-pressing device 9, the solid-liquid
Separation filter-pressing device 9 is connected with the ferrite drying device 11.Ferrite hydro-thermal preparation facilities 3 has agitating function, water pump
2nd, the first feed pump 4, the second feed pump 5 use acid-alkali-corrosive-resisting elevator pump.
The present apparatus carries out hydro-thermal reaction and provides reacting environment for pickling sludge and pickle liquor mixing, realizes pickling dirt
The minimizing disposal of mud and pickle liquor, achievees the purpose that continuous production, while the magnesium with compared with high added value is prepared
Zn ferrite realizes the recycling of danger wastes, so as to bring certain benefit to enterprise.
Embodiment 2
As shown in Figure 1, a kind of system that MgZn ferrite is prepared using pickling sludge and pickle liquor, structure is with implementing
Example 1 is compared, except that：The ferrite hydro-thermal preparation facilities 3 includes reaction kettle and blender, and the blender is located at
In the reaction kettle, the bottom longitudinal section of the reaction kettle is ellipse, and bottom is conducive to ferrite mixing to recessed structure
The discharge of liquid, to reach the high-temperature and high-presure resistent purpose of acid-fast alkali-proof, the blender uses polytetrafluoroethylene (PTFE) material and for U-shaped knot
Structure.
Embodiment 3
As shown in Figure 1, a kind of system that MgZn ferrite is prepared using pickling sludge and pickle liquor, structure is with implementing
Example 1 is compared, except that：The separation of solid and liquid filter-pressing device 9 is plate and frame filter press, and plate compression technique can realize solid
With efficiently separating for liquid, moisture content is down to 70% by the technique most multipotency at present.
Embodiment 4
As shown in Figure 1, a kind of system that MgZn ferrite is prepared using pickling sludge and pickle liquor, structure is with implementing
Example 1 is compared, except that：The discharge port of the separation of solid and liquid filter-pressing device 9 is dried by conveyer belt 10 and the ferrite
The feed inlet of device 11 is connected, and is connected between ferrite hydro-thermal preparation facilities 3 and separation of solid and liquid filter-pressing device 9 using discharging pump 8,
It is connected between separation of solid and liquid filter-pressing device 9 and ferrite drying device 11 using conveyer belt 10, can so reach continuous metaplasia
The purpose of production so as to improve production efficiency, realizes the maximization of the performance of enterprises.
Embodiment 5
As shown in Figure 1, a kind of system that MgZn ferrite is prepared using pickling sludge and pickle liquor, structure is with implementing
Example 1 is compared, except that：Further include ferrite collection device 12, the discharge port of the ferrite drying device 11 with it is described
Ferrite collection device 12 connects, and the ferrite drying device 11 is using the low structure design in the high outlet of entrance, described
Ferrite drying device 11 includes entrance, cylinder and outlet, and drying process middle cylinder body is rotated, with the rotation of cylinder, risen simultaneously
To transmission and uniformly heated effect.
Embodiment 6
As shown in Figure 1, a kind of system that MgZn ferrite is prepared using pickling sludge and pickle liquor, including water tank 1,
It is water pump 2, ferrite hydro-thermal preparation facilities 3, the first feed pump 4, the second feed pump 5, acid storage tank 6, storage alkali tank 7, discharging pump 8, solid
Liquid separates filter-pressing device 9 and ferrite drying device 11, and the water tank 1, the acid storage tank 6, the storage alkali tank 7 pass through respectively
The water pump 2, first feed pump 4, second feed pump 5 are connected with the ferrite hydro-thermal preparation facilities 3, the iron
The discharge port of oxysome hydro-thermal preparation facilities 3 is connected by the discharging pump 8 with the separation of solid and liquid filter-pressing device 9, the solid-liquid
Separation filter-pressing device 9 is connected with the ferrite drying device 11.Ferrite hydro-thermal preparation facilities 3 has agitating function, water pump
2nd, the first feed pump 4, the second feed pump 5 use acid-alkali-corrosive-resisting elevator pump.
The ferrite hydro-thermal preparation facilities 3 includes reaction kettle and blender, and the blender is located in the reaction kettle,
The bottom longitudinal section of the reaction kettle is ellipse, and the blender uses polytetrafluoroethylene (PTFE) material and for U-shaped structure.
The separation of solid and liquid filter-pressing device 9 is plate and frame filter press.
The charging that the discharge port of the separation of solid and liquid filter-pressing device 9 passes through conveyer belt 10 and the ferrite drying device 11
Mouth is connected.
Ferrite collection device 12 is further included, the discharge port of the ferrite drying device 11 is collected with the ferrite to be filled
12 connections are put, and the ferrite drying device exports low structure design using entrance is high.
A kind of method that MgZn ferrite is prepared using pickling sludge and pickle liquor, as shown in Fig. 2, in the utilization
Prepared by pickling sludge and pickle liquor follows the steps below in the system of MgZn ferrite：
A, predecessor is prepared：100kg pickling sludge is added in ferrite hydro-thermal preparation facilities 3, the dosage of sludge
To add to 1/5 volume of ferrite hydro-thermal preparation facilities 3, it is that the addition of follow-up raw material retains adequate space, ensures reaction
Effective progress；Adding water stirring into ferrite hydro-thermal preparation facilities 3 by water pump 2 from water tank 1, water dosage is 300kg,
The speed of agitator of blender is 500r/min, mixing time 0.5h；From acid storage tank 6 by feed pump 4 to ferrite hydro-thermal system
Pickle liquor supplement source of iron is added in standby device 3 and is stirred evenly, the dosage of pickle liquor is 30kg, and speed of agitator is
500r/min, mixing time 0.5h；Hydroxide into ferrite hydro-thermal preparation facilities 3 is added by feed pump 5 from storage alkali tank 7
PH is adjusted to 8, speed of agitator 500r/min, mixing time 0.5h by sodium solution；
B, hydro-thermal prepares ferrite：Under conditions of 150 DEG C of temperature, vapour pressure 2atm, in ferrite hydro-thermal preparation facilities 3
Middle at the uniform velocity to be stirred, speed of agitator 200r/min, time 10h obtain ferrite mixed liquor, treat autoclave body after reaction
Kettle is opened after cooled to room temperature；
C, separation of solid and liquid：Ferrite mixed liquor drains into separation of solid and liquid filter-pressing device by discharging pump, and press filtration separation liquid obtains
To the ferrite solid that moisture content is 90%；
D, dry ferrite：Ferrite solid is sent to ferrite drying device 11 by conveyer belt 10 and is dried, and dries
Dry temperature is 100 DEG C, and dried ferrite is collected by discharge port discharge in ferrite collection device 12.
MgZn ferrite made from this method, after testing, grain size 42nm, the position of each diffraction maximum and relative intensity with
Mg0.4Zn0.6Fe2O4Standard diagram coincide substantially, products therefrom be the MgZn ferrite with spinel structure, saturated magnetization
Intensity is 8emu/g, coercivity 126kA/m.
Embodiment 7
As depicted in figs. 1 and 2, a kind of method that MgZn ferrite is prepared using pickling sludge and pickle liquor, is being implemented
Being prepared using pickling sludge and pickle liquor in the system of MgZn ferrite described in example 6 is followed the steps below：
A, predecessor is prepared：167kg pickling sludge is added in ferrite hydro-thermal preparation facilities 3, the dosage of sludge
To add to 1/3 volume of ferrite hydro-thermal preparation facilities 3, it is that the addition of follow-up raw material retains adequate space, ensures reaction
Effective progress；Adding water stirring into ferrite hydro-thermal preparation facilities 3 by water pump 2 from water tank 1, water dosage is 167kg,
The speed of agitator of blender is 200r/min, time 2h；From acid storage tank 6 by feed pump 4 to ferrite hydro-thermal preparation facilities 3
In add pickle liquor supplement and source of iron and stir evenly, the dosage of pickle liquor is 167kg, speed of agitator 200r/min,
Time is 2h；Potassium hydroxide solution into ferrite hydro-thermal preparation facilities 3 is added by feed pump 5 from storage alkali tank 7, pH is adjusted
For 11, speed of agitator 200r/min, time 2h；
B, hydro-thermal prepares ferrite：Under conditions of 250 DEG C of temperature, vapour pressure 4atm, in ferrite hydro-thermal preparation facilities 3
Middle at the uniform velocity to be stirred, speed of agitator 500r/min, time 5h obtain ferrite mixed liquor, treat autoclave body after reaction
Kettle is opened after cooled to room temperature；
C, separation of solid and liquid：Ferrite mixed liquor drains into separation of solid and liquid filter-pressing device by discharging pump, and press filtration separation liquid obtains
To the ferrite solid that moisture content is 70%；
D, dry ferrite：Ferrite solid is sent to ferrite drying device 11 by conveyer belt 10 and is dried, and dries
Dry temperature is 150 DEG C, and dried ferrite is collected by discharge port discharge in ferrite collection device 12.
MgZn ferrite made from this method, after testing, grain size 24nm, the position of each diffraction maximum and relative intensity with
Mg0.4Zn0.6Fe2O4Standard diagram coincide substantially, products therefrom be the MgZn ferrite with spinel structure, saturated magnetization
Intensity is 24emu/g, coercivity 78kA/m.
Embodiment 8
As depicted in figs. 1 and 2, a kind of method that MgZn ferrite is prepared using pickling sludge and pickle liquor, is being implemented
Being prepared using pickling sludge and pickle liquor in the system of MgZn ferrite described in example 6 is followed the steps below：
A, predecessor is prepared：125kg pickling sludge is added in ferrite hydro-thermal preparation facilities 3, the dosage of sludge
To add to 1/4 volume of ferrite hydro-thermal preparation facilities 3, it is that the addition of follow-up raw material retains adequate space, ensures reaction
Effective progress；Adding water stirring into ferrite hydro-thermal preparation facilities 3 by water pump 2 from water tank 1, water dosage is 250kg,
The speed of agitator of blender is 400r/min, time 1h；From acid storage tank 6 by feed pump 4 to ferrite hydro-thermal preparation facilities 3
In add pickle liquor supplement and source of iron and stir evenly, the dosage of pickle liquor is 62.5kg, speed of agitator 300r/min,
Time is 1.5h；Sodium hydroxide and potassium hydroxide into ferrite hydro-thermal preparation facilities 3 are added by feed pump 5 from storage alkali tank 7
PH is adjusted to 10, speed of agitator 300r/min, time 1.5h by mixed solution；
B, hydro-thermal prepares ferrite：Under conditions of 200 DEG C of temperature, vapour pressure 3atm, in ferrite hydro-thermal preparation facilities 3
Middle at the uniform velocity to be stirred, speed of agitator 300r/min, time 7h obtain ferrite mixed liquor, treat autoclave body after reaction
Kettle is opened after cooled to room temperature；
C, separation of solid and liquid：Ferrite mixed liquor drains into separation of solid and liquid filter-pressing device by discharging pump, and press filtration separation liquid obtains
To the ferrite solid that moisture content is 80%；
D, dry ferrite：Ferrite solid is sent to ferrite drying device 11 by conveyer belt 10 and is dried, and dries
Dry temperature is 120 DEG C, and dried ferrite is collected by discharge port discharge in ferrite collection device 12.
MgZn ferrite made from this method, after testing, grain size 15nm, the position of each diffraction maximum and relative intensity with
Mg0.4Zn0.6Fe2O4Standard diagram coincide substantially, products therefrom be the MgZn ferrite with spinel structure, saturated magnetization
Intensity is 30emu/g, coercivity 36kA/m.
Embodiment 9
As depicted in figs. 1 and 2, a kind of method that MgZn ferrite is prepared using pickling sludge and pickle liquor, is being implemented
Being prepared using pickling sludge and pickle liquor in the system of MgZn ferrite described in example 6 is followed the steps below：
A, predecessor is prepared：125kg pickling sludge is added in ferrite hydro-thermal preparation facilities 3, the dosage of sludge
To add to 1/4 volume of ferrite hydro-thermal preparation facilities 3, it is that the addition of follow-up raw material retains adequate space, ensures reaction
Effective progress；Add water stirring into ferrite hydro-thermal preparation facilities 3 by water pump 2 from water tank 1, water dosage is
312.5kg, the speed of agitator of blender is 300r/min, time 1.5h；From acid storage tank 6 by feed pump 4 to ferrite water
It adds pickle liquor supplement in equipment for heating preparing 3 source of iron and to stir evenly, the dosage of pickle liquor is 100kg, speed of agitator
For 400r/min, time 1h；It is molten that sodium hydroxide into ferrite hydro-thermal preparation facilities 3 added by feed pump 5 from storage alkali tank 7
PH is adjusted to 9, speed of agitator 400r/min, time 1h by liquid；
B, hydro-thermal prepares ferrite：Under conditions of 175 DEG C of temperature, vapour pressure 2.5atm, prepare and fill in ferrite hydro-thermal
It is at the uniform velocity stirred in putting 3, speed of agitator 400r/min, time 8h obtains ferrite mixed liquor, treats kettle after reaction
Kettle is opened after body cooled to room temperature；
C, separation of solid and liquid：Ferrite mixed liquor drains into separation of solid and liquid filter-pressing device by discharging pump, and press filtration separation liquid obtains
To the ferrite solid that moisture content is 85%；
D, dry ferrite：Ferrite solid is sent to ferrite drying device 11 by conveyer belt 10 and is dried, and dries
Dry temperature is 140 DEG C, and dried ferrite is collected by discharge port discharge in ferrite collection device 12.
MgZn ferrite made from this method, after testing, grain size 28nm, the position of each diffraction maximum and relative intensity with
Mg0.4Zn0.6Fe2O4Standard diagram coincide substantially, products therefrom be the MgZn ferrite with spinel structure, saturated magnetization
Intensity is 19emu/g, coercivity 93kA/m.
Schematically the present invention and embodiments thereof are described above, this describes no restricted, institute in attached drawing
What is shown is also one of embodiments of the present invention, and actual structure is not limited thereto.So if common skill of this field
Art personnel are enlightened by it, without departing from the spirit of the invention, are not inventively designed and the technical solution
Similar frame mode and embodiment, are within the scope of protection of the invention.
Claims (5)
1. a kind of system that MgZn ferrite is prepared using pickling sludge and pickle liquor, it is characterised in that：Including water tank
(1), water pump (2), ferrite hydro-thermal preparation facilities (3), the first feed pump (4), the second feed pump (5), acid storage tank (6), storage alkali
Tank (7), discharging pump (8), separation of solid and liquid filter-pressing device (9) and ferrite drying device (11), the water tank (1), the storage
Sour tank (6), the storage alkali tank (7) pass through the water pump (2), first feed pump (4), second feed pump (5) respectively
It is connected with the ferrite hydro-thermal preparation facilities (3), the discharge port of the ferrite hydro-thermal preparation facilities (3) passes through the discharging
Pump (8) is connected with the separation of solid and liquid filter-pressing device (9), and the separation of solid and liquid filter-pressing device (9) fills with ferrite drying
Put (11) connection.
2. the system according to claim 1 that MgZn ferrite is prepared using pickling sludge and pickle liquor, feature are existed
In：The ferrite hydro-thermal preparation facilities (3) includes reaction kettle and blender, and the blender is located in the reaction kettle, institute
The bottom longitudinal section of reaction kettle is stated as ellipse, the blender uses polytetrafluoroethylene (PTFE) material and for U-shaped structure.
3. the system according to claim 1 that MgZn ferrite is prepared using pickling sludge and pickle liquor, feature are existed
In：The separation of solid and liquid filter-pressing device (9) is plate and frame filter press.
4. the system according to claim 1 that MgZn ferrite is prepared using pickling sludge and pickle liquor, feature are existed
In：The discharge port of the separation of solid and liquid filter-pressing device (9) by conveyer belt (10) and the ferrite drying device (11) into
Material mouth is connected.
5. the system according to claim 1 that MgZn ferrite is prepared using pickling sludge and pickle liquor, feature are existed
In：Ferrite collection device (12) is further included, the discharge port of the ferrite drying device (11) is collected with the ferrite to be filled
(12) connection is put, and the ferrite drying device (11) exports low structure using entrance is high.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107673409A (en) * | 2017-11-21 | 2018-02-09 | 环境保护部南京环境科学研究所 | The system and method for MgZn ferrite is prepared using pickling sludge and pickle liquor |
| CN109399687A (en) * | 2018-12-10 | 2019-03-01 | 环境保护部南京环境科学研究所 | A method of calcirm-fluoride concentrate is prepared using highly acid fluoride wastewater treatment sludge |
-
2017
- 2017-11-21 CN CN201721563162.1U patent/CN207451636U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107673409A (en) * | 2017-11-21 | 2018-02-09 | 环境保护部南京环境科学研究所 | The system and method for MgZn ferrite is prepared using pickling sludge and pickle liquor |
| CN109399687A (en) * | 2018-12-10 | 2019-03-01 | 环境保护部南京环境科学研究所 | A method of calcirm-fluoride concentrate is prepared using highly acid fluoride wastewater treatment sludge |
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