CN107673409A - The system and method for MgZn ferrite is prepared using pickling sludge and pickle liquor - Google Patents
The system and method for MgZn ferrite is prepared using pickling sludge and pickle liquor Download PDFInfo
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- CN107673409A CN107673409A CN201711164519.3A CN201711164519A CN107673409A CN 107673409 A CN107673409 A CN 107673409A CN 201711164519 A CN201711164519 A CN 201711164519A CN 107673409 A CN107673409 A CN 107673409A
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- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or hydroxides
- C01G49/0063—Mixed oxides or hydroxides containing zinc
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention discloses the system and method that MgZn ferrite is prepared using pickling sludge and pickle liquor, belongs 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 by water pump, the first feed pump, the second feed pump with ferrite hydro-thermal preparation facilities respectively, the discharging opening 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 prepare predecessor, hydro-thermal prepares ferrite, separation of solid and liquid and dry ferrite.The present invention realizes that the recycling coexistence of pickling sludge and pickle liquor is put, and prepares MgZn ferrite.
Description
Technical field
The invention belongs to danger wastes recycling field, is related to one kind and prepares magnesium zinc using pickling sludge and pickle liquor
Ferritic system and method, MgZn ferrite is prepared more specifically to a kind of pickling sludge and pickle liquor hydro-thermal
System and method is put in coexistence, and industrial products --- the magnesium with compared with high added value is prepared as raw material using pickling sludge and pickle liquor
Zn ferrite.
Background technology
A large amount of pickling sludge and pickle liquor can be produced 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, contain 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.Alkaline precipitating agent is used as using calcium hydroxide or sodium hydroxide
Add in waste water, heavy metal is generated hydroxide not soluble in water by neutralization and precipitate to separate, the sediment of formation
As pickling sludge.According to Jiangsu Province's pickling sludge on-site investigation result, the enterprise of the pickling waste waters of the whole province's different industries generation at present
Industry totally 1047, produces 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 has certain economic benefit, and product can be used as smelting industry raw material, state
Interior most enterprise all carries out comprehensive utilization disposal using this method, but this method to energy resource consumption and invests all too high, operability
It is low, control improper easily generation sulfur dioxide, containing secondary pollutions such as heavy metal dusts.Hydrometallurgic recovery producing level is high, equipment letter
List, small, the easy to operate management of occupation of land, but current technique are simultaneously immature, and 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,
Need 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 advantageous to later processing operation, the main side for using pickling
Method removes iron scale.Mild steel enterprise typically uses chlorohydric acid pickling, steel rolling mill's acid-washing stainless steel typically using nitric acid, sulfuric acid,
Hydrofluoric acid etc..Because hydrochloric acid compared with other acid solutions has the characteristics of consumption is few, cost is low, pickling is quick, cleaning performance is good, from previous generation
Discipline progressively substitutes other acid to apply in acid cleaning process from the sixties.Concentrated hydrochloric acid is typically diluted to 18% or so and entered by pickling process
Row pickling, when concentration of hydrochloric acid is down to below 10%, because metal ion reaches finite concentration in acid solution, under pickling effect is notable
Drop, it is difficult to reach requirement, be now regarded as spent acid (i.e. pickle liquor) 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, design, management, control and corrosion resistant to equipment
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 separated out in concentration process, easily causes equipment blocking, therefore have necessarily
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
Fill 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.
And for example Application No. 201110110999.1, Publication No. CN102219493A Chinese invention patent disclose one
The method that kind prepares MnZn ferrite feed powders using pickle liquor and zinc coated slag, this application case is that zinc coated slag is dissolved in into acid
Wash waste liquid and obtain mixed solution, then the pH value for adjusting mixed solution with ammoniacal liquor adds fluoride and reacted to 3-6
Liquid, flocculant is added thereto, filter removing precipitation and obtain filtrate, filtrate and manganese chloride are pressed into Fe in ferrite composition2O3/
MnO/ZnO mol ratio is configured to precipitation solution, adds the precipitating reagent that ammonium hydrogen carbonate and ammoniacal liquor are prepared thereto, and reaction is starched
Material, by slurry oxidation, washing and filtering, the drying after ageing.Raw material is used in this application case 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, and it is manganese-zinc ferrite to obtain product.
And for example Application No. 2009100503423, Publication No. CN101565304A Chinese invention patent disclose one
The processing method of kind electroplating sludge and pickle liquor cooperative with hydrothermal ferrite.This application case using industrial waste electroplating sludge and
Pickle liquor is raw material, and with water as solvent, ammoniacal liquor obtains corresponding heavy metal hydroxide under certain condition as pH adjusting agent
Thing 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 form different growth units, and according to certain bind mode nucleating growth, crystallize into stable compound iron
Oxysome.It is electroplating sludge to be dealt with objects in the program, 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 the inventive technique scheme 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 present invention provides a kind of using sour
Wash sludge and pickle liquor prepares the system and method for MgZn ferrite.Pickling can both be realized using technical scheme
The minimizing disposal of sludge and pickle liquor, while industrial products-MgZn ferrite with compared with high added value can be prepared, it is real
The recycling of existing danger wastes, so as to bring certain benefit to enterprise.
2nd, technical scheme
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 discharging opening 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 reactor and the stirring of acid and alkali-resistance high-temperature-resistant high-pressure-resistant
Device, the agitator are located in the reactor, and the bottom longitudinal section of the reactor is ellipse, and bottom is to recessed structure
Be advantageous to the discharge of ferrite mixed liquor, the agitator uses polytetrafluoroethylene (PTFE) material and for U-shape structure.
Further, the separation of solid and liquid filter-pressing device is plate and frame filter press, plate compression technique can realize solid with
Liquid is efficiently separated, and moisture content is down into 70% by the technique most multipotency at present.
Further, the discharging opening of the separation of solid and liquid filter-pressing device passes through conveyer belt and the ferrite drying device
Charging aperture is connected.
Further, in addition to ferrite collection device, the discharging opening of the ferrite drying device and the ferrite
Collection device connects, and ferrite drying device exports low structure design, described ferrite drying device bag using entrance is high
Entrance, cylinder and outlet are included, drying process middle cylinder body rotates, the rotation of cylinder, while plays a part of transmission and uniformly heat.
A kind of method that MgZn ferrite is prepared using pickling sludge and pickle liquor, pickling sludge and acid are utilized described
Wash waste liquid and prepare 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 stirred, and alkali 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, 2-4atm bar
Under part, it is stirred in ferrite hydro-thermal preparation facilities, hydro-thermal reaction obtains ferrite mixed liquor after terminating, treat that ferrite mixes
Close after liquid naturally cools to room temperature and drive kettle；
C, separation of solid and liquid：Ferrite mixed liquor drains into separation of solid and liquid filter-pressing device by discharging pump, press filtration separation liquid, obtains
To ferrite solid；
D, ferrite is dried：Ferrite solid is sent to ferrite drying device and dried, and by dried iron oxygen
Body discharge is collected.
Further, the dosage of pickling sludge is the 1/5-1/ of the ferrite hydro-thermal preparation facilities volume in step A
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 alkali 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, particle diameter 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 scheme：The present invention adopts
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 needed, therefore there is more preferable economic benefit.
The technical scheme announced with Publication No. CN102219493A Chinese invention patent except that, it is of the invention
Product is MgZn ferrite, does not need input cost to supplement other metals in preparation process, technique is simple, has good economy
Benefit.
The technical scheme announced with Publication No. CN101565304A Chinese invention patent except 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
In technical scheme there is larger difference in sludge components composition, 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, both are prepared
Product it is also different, the product that the invention is prepared is nickel-zinc ferrite, and the product that is prepared of the present invention is magnesium zinc-iron
Oxysome.
3rd, beneficial effect
Compared to 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, realize 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 reactor
Portion longitudinal section is ellipse, and the structure is advantageous 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 advantageous 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 are dried
When device exports low design using entrance is high, with the rotation of cylinder, while play a part of transmission and uniformly heat；
(5) system provided by the invention that MgZn ferrite is prepared using pickling sludge and pickle liquor, ferrite hydro-thermal
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 discharging opening, 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 both realized the minimizing disposal of danger wastes, realizes the mesh of recycling again
, 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 particle diameter is tiny, uniform powder, be advantageous to low-temperature sintering, pure Spinel is directly obtained under relatively lower temp
Ferrite.
Brief description of the drawings
Fig. 1 is the structural representation 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.
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 discharging opening 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 reactor and agitator, and the agitator is located in the reactor,
The bottom longitudinal section of the reactor is ellipse, and bottom is advantageous to the discharge of ferrite mixed liquor to recessed structure, described
Agitator uses polytetrafluoroethylene (PTFE) material and for U-shape 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 discharging opening 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.
Also include ferrite collection device 12, the discharging opening 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 pickling thereto
Waste liquid supplements source of iron, adds alkaline precipitating agent regulation pH value, and carrying out hydro-thermal reaction under the conditions of certain temperature and vapour pressure obtains
To ferrite mixed liquor, caused ferrite mixed liquor is drained into separation of solid and liquid filter-pressing device 9 by discharging pump, separates liquid
Solid is obtained, ferrite solid is transported in ferrite drying device 11 by conveyer belt 10 and dried, the iron oxygen after drying
Body is collected into ferrite collection device 12.The money of pickling sludge and pickle liquor can be effectively realized using the system of the present invention
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 described 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 stirred, and alkali 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 the volume of ferrite hydro-thermal preparation facilities 3, prepare and fill to ferrite hydro-thermal
Put the quality of the water added in 3, the quality of pickling sludge, the quality of pickle liquor and meet 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 alkali 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
At the uniform velocity stirred in standby device 3, speed of agitator 200-500r/min, mixing time 5-10h, hydro-thermal reaction obtains after terminating
To ferrite mixed liquor, kettle is driven after ferrite mixed liquor naturally cools 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, ferrite is dried：Ferrite solid is sent to ferrite drying device 11 and dried, drying temperature 100-
150 DEG C, dried ferrite is discharged and collected.
The present invention is by preparing predecessor, hydro-thermal prepares ferrite, separation of solid and liquid and dries the technique such as ferrite, realizes
The disposal of resources of pickling sludge and pickle liquor, and carried out by the process to above each operation 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 discharging opening 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 is mixed into water-filling thermal response and provides reacting environment for pickling sludge and pickle liquor, realizes pickling dirt
The minimizing disposal of mud and pickle liquor, reaches the purpose of continuous production, while the magnesium with compared with high added value is prepared
Zn ferrite, the recycling of danger wastes is realized, 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, its structure is with implementing
Example 1 is compared, except that：Described ferrite hydro-thermal preparation facilities 3 includes reactor and agitator, and the agitator is located at
In the reactor, the bottom longitudinal section of the reactor is ellipse, and bottom is advantageous to ferrite mixing to recessed structure
The discharge of liquid, to reach the purpose of acid-fast alkali-proof high temperature high voltage resistant, the agitator 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, its 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, its structure is with implementing
Example 1 is compared, except that：The discharging opening of the separation of solid and liquid filter-pressing device 9 is dried by conveyer belt 10 and the ferrite
The charging aperture 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,
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, realize 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, its structure is with implementing
Example 1 is compared, except that：Also include ferrite collection device 12, the discharging opening 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 the effect uniformly heated.
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 discharging opening 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 reactor and agitator, and the agitator is located in the reactor,
The bottom longitudinal section of the reactor is ellipse, and the agitator uses polytetrafluoroethylene (PTFE) material and for U-shape structure.
The separation of solid and liquid filter-pressing device 9 is plate and frame filter press.
The charging that the discharging opening 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.
Also include ferrite collection device 12, the discharging opening 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 described 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 agitator 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, 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
Sodium solution, pH is adjusted to 8, speed of agitator 500r/min, mixing time 0.5h；
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, reaction obtain ferrite mixed liquor after terminating, and treat kettle
Kettle is driven after naturally cooling 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, press filtration separation liquid, obtains
To the ferrite solid that moisture content is 90%；
D, ferrite is dried：Ferrite solid is sent to ferrite drying device 11 by conveyer belt 10 and dried, and dries
Dry temperature is 100 DEG C, and dried ferrite is collected into ferrite collection device 12 by discharging opening discharge.
MgZn ferrite made from this method, after testing, particle diameter 42nm, the position of each diffraction maximum and relative intensity with
Mg0.4Zn0.6Fe2O4Standard diagram coincide substantially, products therefrom is 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 agitator 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, 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, reaction obtain ferrite mixed liquor after terminating, and treat kettle
Kettle is driven after naturally cooling 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, press filtration separation liquid, obtains
To the ferrite solid that moisture content is 70%；
D, ferrite is dried：Ferrite solid is sent to ferrite drying device 11 by conveyer belt 10 and dried, and dries
Dry temperature is 150 DEG C, and dried ferrite is collected into ferrite collection device 12 by discharging opening discharge.
MgZn ferrite made from this method, after testing, particle diameter 24nm, the position of each diffraction maximum and relative intensity with
Mg0.4Zn0.6Fe2O4Standard diagram coincide substantially, products therefrom is 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 agitator 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, 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
Mixed solution, pH is adjusted to 10, speed of agitator 300r/min, time 1.5h；
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, reaction obtain ferrite mixed liquor after terminating, and treat kettle
Kettle is driven after naturally cooling 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, press filtration separation liquid, obtains
To the ferrite solid that moisture content is 80%；
D, ferrite is dried：Ferrite solid is sent to ferrite drying device 11 by conveyer belt 10 and dried, and dries
Dry temperature is 120 DEG C, and dried ferrite is collected into ferrite collection device 12 by discharging opening discharge.
MgZn ferrite made from this method, after testing, particle diameter 15nm, the position of each diffraction maximum and relative intensity with
Mg0.4Zn0.6Fe2O4Standard diagram coincide substantially, products therefrom is 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 agitator is 300r/min, time 1.5h；From acid storage tank 6 by feed pump 4 to ferrite water
Add pickle liquor supplement in equipment for heating preparing 3 source of iron and to stir, 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
Liquid, pH is adjusted to 9, speed of agitator 400r/min, time 1h；
B, hydro-thermal prepares ferrite：Under conditions of 175 DEG C of temperature, vapour pressure 2.5atm, prepare and fill in ferrite hydro-thermal
At the uniform velocity stirred in putting 3, speed of agitator 400r/min, time 8h, reaction obtains ferrite mixed liquor after terminating, and treats kettle
Body drives kettle after naturally cooling 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, press filtration separation liquid, obtains
To the ferrite solid that moisture content is 85%；
D, ferrite is dried：Ferrite solid is sent to ferrite drying device 11 by conveyer belt 10 and dried, and dries
Dry temperature is 140 DEG C, and dried ferrite is collected into ferrite collection device 12 by discharging opening discharge.
MgZn ferrite made from this method, after testing, particle diameter 28nm, the position of each diffraction maximum and relative intensity with
Mg0.4Zn0.6Fe2O4Standard diagram coincide substantially, products therefrom is 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 accompanying 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 area
Art personnel are enlightened by it, without departing from the spirit of the invention, without designing and the technical scheme for creativeness
Similar frame mode and embodiment, protection scope of the present invention all should be belonged to.
Claims (10)
- A kind of 1. 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 discharging opening 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) is dried with the ferrite and filled Put (11) connection.
- 2. the system according to claim 1 that MgZn ferrite is prepared using pickling sludge and pickle liquor, its feature are existed In：The ferrite hydro-thermal preparation facilities (3) includes reactor and agitator, and the agitator is located in the reactor, institute The bottom longitudinal section for stating reactor uses polytetrafluoroethylene (PTFE) material and for U-shape structure for ellipse, the agitator.
- 3. the system according to claim 1 that MgZn ferrite is prepared using pickling sludge and pickle liquor, its 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, its feature are existed In：The discharging opening of the separation of solid and liquid filter-pressing device (9) is entered by conveyer belt (10) and ferrite drying device (11) Material mouth is connected.
- 5. the system according to claim 1 that MgZn ferrite is prepared using pickling sludge and pickle liquor, its feature are existed In：Also include ferrite collection device (12), the discharging opening 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.
- A kind of 6. method that MgZn ferrite is prepared using pickling sludge and pickle liquor, it is characterised in that claim 1 to According to following in the system that MgZn ferrite is prepared using pickling sludge and pickle liquor in claim 5 described in any one Step is carried out：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), from acid storage tank (6) to ferrite hydro-thermal preparation facilities (3) In add pickle liquor supplement and source of iron and stir, add alkali lye into ferrite hydro-thermal preparation facilities (3) from storage alkali tank (7) As precipitating reagent；B, hydro-thermal prepares ferrite：Ensure hydrothermal temperature and vapour pressure be respectively 150-250 DEG C, 2-4atm condition Under, it is stirred in ferrite hydro-thermal preparation facilities (3), hydro-thermal reaction obtains ferrite mixed liquor after terminating, treat ferrite Mixed liquor drives kettle after naturally cooling 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, Obtain ferrite solid；D, ferrite is dried：Ferrite solid is sent to ferrite drying device (11) and dried, and by dried iron oxygen Body discharge is collected.
- 7. the method according to claim 6 that MgZn ferrite is prepared using pickling sludge and pickle liquor, its feature are existed In：The dosage of pickling sludge is the 1/5-1/3 of ferrite hydro-thermal preparation facilities (3) volume in step A, to ferrite water The quality of water, the quality of pickling sludge, the quality of pickle liquor added in equipment for heating preparing (3) meets m (water) respectively：M (acid Wash sludge)=(1-3)：1, m (pickle liquor)：M (pickling sludge)=(0.3-1)：1, and by adding alkali lye by the iron oxygen The pH value of solution is adjusted to 8-11 in body hydro-thermal preparation facilities (3), stirring and dissolving in the ferrite hydro-thermal preparation facilities (3) Rotating speed is 200-500r/min, mixing time 0.5-2h.
- 8. the method according to claim 7 that MgZn ferrite is prepared using pickling sludge and pickle liquor, its feature are existed In：The rotating speed stirred in step B is 200-500r/min, mixing time 5-10h.
- 9. the method according to claim 7 that MgZn ferrite is prepared using pickling sludge and pickle liquor, its feature are existed In：The obtained product ferrite solid aqueous rate of separation of solid and liquid filter-pressing device (9) press filtration separation ferrite mixed liquor is in step C 70-90%.
- 10. the method according to claim 7 that MgZn ferrite is prepared using pickling sludge and pickle liquor, its feature are existed In：Drying temperature is 100-150 DEG C in ferrite drying device (11) in step D.
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| CN108439479A (en) * | 2018-04-24 | 2018-08-24 | 邯郸钢铁集团有限责任公司 | Cold-rolling pickling waste liquid prepares nanometer Fe2O3The system and method for photochemical catalyst |
| CN108585056A (en) * | 2018-06-19 | 2018-09-28 | 山东大学 | A kind of tumor thermotherapy MgZn ferrite and preparation method thereof |
| 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 |
| CN110316866A (en) * | 2019-07-12 | 2019-10-11 | 北部湾大学 | The automated programming system and its technique of acid pickle are generated after a kind of pair of pickling of metal |
| CN111088412A (en) * | 2019-12-16 | 2020-05-01 | 霸州环瑞节能科技有限公司 | Acid pickling sludge resource utilization method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108439479A (en) * | 2018-04-24 | 2018-08-24 | 邯郸钢铁集团有限责任公司 | Cold-rolling pickling waste liquid prepares nanometer Fe2O3The system and method for photochemical catalyst |
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