CN115557481A - Recycling method of iron phosphate slag recycled by ammonia water - Google Patents

Recycling method of iron phosphate slag recycled by ammonia water Download PDF

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Publication number
CN115557481A
CN115557481A CN202211303488.6A CN202211303488A CN115557481A CN 115557481 A CN115557481 A CN 115557481A CN 202211303488 A CN202211303488 A CN 202211303488A CN 115557481 A CN115557481 A CN 115557481A
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China
Prior art keywords
iron phosphate
cylinder
ammonia
recovery cylinder
pretreatment
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CN202211303488.6A
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Chinese (zh)
Inventor
姚送送
朱建楠
吴国庆
徐厚宝
王浩
秦俊
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Anhui Nandu Huabo New Material Technology Co ltd
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Anhui Nandu Huabo New Material Technology Co ltd
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Priority to CN202211303488.6A priority Critical patent/CN115557481A/en
Publication of CN115557481A publication Critical patent/CN115557481A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/26Phosphates
    • C01B25/37Phosphates of heavy metals
    • C01B25/375Phosphates of heavy metals of iron
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D29/00Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/01Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements
    • B01D29/03Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements self-supporting
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D29/00Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/76Handling the filter cake in the filter for purposes other than for regenerating
    • B01D29/86Retarding cake deposition on the filter during the filtration period, e.g. using stirrers
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00Ammonia; Compounds thereof
    • C01C1/02Preparation, purification or separation of ammonia

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention discloses a method for recycling iron phosphate slag recycled by ammonia water, and belongs to the technical field of iron phosphate recycling. The invention is used for solving the technical problems that ammonia used in the ferric phosphate recovery process can not be recycled, the consumption of ammonia water is high, the production cost is high, the volatile ammonia gas and hydrochloric acid gas can generate great threat to operators, and the operation environment for recovering ferric phosphate is poor in the prior art, and the method for recycling the ferric phosphate slag recycled by the ammonia water comprises the following operation steps: the method comprises the following steps: after the iron phosphate slag is crushed, mixing the iron phosphate slag to be recovered with water according to the mass volume ratio of 1g:10-15mL of the mixture is mixed to obtain a solid-liquid mixture of the iron phosphate slag. The invention not only can recycle the ammonia recovered from the iron phosphate slag, ensure the recovery efficiency of the ammonia and improve the heat utilization rate, but also can filter solids, reduce the volatilization of ammonia gas and hydrochloric acid gas and improve the operation environment for recovering the iron phosphate.

Description

Recycling method of iron phosphate slag recycled by ammonia water
Technical Field
The invention relates to the technical field of iron phosphate recovery, in particular to a method for recycling iron phosphate slag recycled by ammonia water.
Background
Phosphating is one of important pretreatment modes before metal coating, and has wide application in the fields of chemical industry, metallurgy, automobiles, aerospace, ships and the like. However, solid wastes containing iron phosphate and zinc phosphate as main components are inevitably generated in the phosphating process.
The iron phosphate compound is an important raw material and has good application in the fields of agriculture, antirust coating, antique ceramics, steel, surface passivation and the like. Because of the unique catalytic property, ion exchange capacity and electrochemical performance, the iron phosphate has more and more important application in the fields of catalysis, lithium battery materials and the like, and the iron phosphate used in the industrial and agricultural production is synthesized by using high-cost chemical reagents at present.
Iron phosphate among the iron phosphate slag among the prior art is retrieved and is usually after using the iron phosphate of hydrochloric acid solution in with the iron phosphate slag to dissolve, filter solution, then use aqueous ammonia to adjust solution pH, separate out the iron phosphate from the solution, in retrieving the in-process to the iron phosphate, need use a large amount of aqueous ammonia usually, and the aqueous ammonia volatilizes easily, make the consumption of aqueous ammonia great, and high in production cost, in retrieving the in-process from the iron phosphate slag to the iron phosphate, need pass through multiple filtration, and the volatility of hydrochloric acid and ammonia is all great, if direct filter under open environment, volatile ammonia and hydrochloric acid gas can produce great threat to operating personnel, the operational environment of iron phosphate recovery is relatively poor.
Disclosure of Invention
The invention aims to provide a recycling method of iron phosphate slag recycled by ammonia water, which is used for solving the technical problems that in the prior art, the consumption of ammonia water is high, the ammonia water cannot be recycled, the production cost is high, the volatility of hydrochloric acid and ammonia gas is high, the hydrochloric acid and the ammonia gas are directly filtered in an open environment, the volatile ammonia gas and the hydrochloric acid gas can generate great threat to operators, and the operation environment for recycling iron phosphate is poor.
The purpose of the invention can be realized by the following technical scheme:
the recycling method of the iron phosphate slag recycled by the ammonia water comprises the following operation steps:
the method comprises the following steps: after crushing the iron phosphate slag, mixing the iron phosphate slag to be recovered with water according to a mass-volume ratio of 1g: mixing 10-15mL to obtain a solid-liquid mixture of the iron phosphate slag, putting the solid-liquid mixture of the iron phosphate slag into a pretreatment cylinder in a recovery device, adding 15wt% hydrochloric acid into the pretreatment cylinder, and adjusting the pH value of the solid-liquid mixture of the iron phosphate slag to 1 to obtain an acidic solid-liquid mixture;
step two: uniformly stirring the acidic solid-liquid mixture by a stirring assembly, introducing steam into a heating coil, heating the solution in the pretreatment cylinder to 50-60 ℃, keeping the temperature and stirring for 30-50min, lifting a top plate, driving a storage cylinder to synchronously lift, filtering by using a screen, filtering the acidic solid-liquid mixture to obtain an acidic iron phosphate solution, collecting insoluble substances in the storage cylinder, remaining the iron phosphate solution in the pretreatment cylinder, pumping the acidic iron phosphate solution into an iron phosphate recovery cylinder by using a second transfer pump, regulating the pH value of the system to 7 by using ammonia water, cooling to room temperature, continuously stirring for 30-50min, and fully separating out iron phosphate to obtain an iron phosphate solid-liquid mixture;
step three: filtering the iron phosphate solid-liquid mixture by using a screen in an iron phosphate recovery cylinder to obtain iron phosphate crystals and a solution to be recovered, collecting the iron phosphate crystals in a storage cylinder, adding NaOH into the solution to be recovered in the iron phosphate recovery cylinder, adjusting the pH value of a solution system to 12-14 to obtain an ammonia solution to be recovered, and pumping the ammonia solution to be recovered into the ammonia recovery cylinder by using a first transfer pump;
step four: making NH of ammonia solution to be recovered according to reaction mechanism of strong base to prepare weak base 4 Conversion of OH to NH 4 Cl,Under heating, NH 4 Cl to NH 3 ,NH 3 And the ammonia enters the iron phosphate recovery cylinder through the air duct, and the ammonia in the ammonia water is recycled.
Further, recovery unit includes the bottom plate, the top rigid coupling of bottom plate has ammonia recovery cylinder and iron phosphate recovery cylinder, and heating coil is installed to the inboard of ammonia recovery cylinder, install on the bottom plate and be arranged in solution to iron phosphate recovery cylinder and iron phosphate recovery cylinder in solution to the pumping module of ammonia recovery cylinder pumping, during the ammonia recovery cylinder carries the iron phosphate recovery cylinder with the ammonia of retrieving through gas transmission subassembly, the pretreatment cylinder has been cup jointed at the top of ammonia recovery cylinder, and the bottom of pretreatment cylinder extends to the inboard of ammonia recovery cylinder, the storage section of thick bamboo is all installed with the inboard of pretreatment cylinder to the iron phosphate recovery cylinder, and the screen cloth is installed to the inboard of storage section of thick bamboo, the apron is installed with the top surface of iron phosphate recovery cylinder to the pretreatment cylinder, install on the apron and correspond the stirring subassembly that sets up with iron phosphate recovery cylinder and pretreatment cylinder.
Further, the equal rigid coupling in outside top of the outside of ammonia recycling bin and iron phosphate recycling bin has a plurality of electric telescopic handle, and is a plurality of electric telescopic handle's extension end all with the bottom rigid coupling of apron, the cavity intermediate layer has been seted up to the lateral wall of iron phosphate recycling bin, the feed liquor pipe and the drain pipe that are linked together with the cavity intermediate layer have been cup jointed respectively to the outside bottom and the outside top of iron phosphate recycling bin.
Further, the pumping module is including installing first defeated pump and the second defeated pump of transferring at the bottom plate top, the connecting pipe is all installed with the output to the input of second defeated pump to first defeated pump, wherein, install the connecting pipe of first defeated pump input end and keep away from the one end of first defeated pump and extend to the inboard bottom of iron phosphate recovery section of thick bamboo, the one end of keeping away from first defeated pump at the connecting pipe of first defeated pump output end extends to the inboard top of ammonia recovery section of thick bamboo, the one end of keeping away from the second defeated pump at the connecting pipe of second defeated pump input end extends to the inboard bottom of pretreatment section of thick bamboo, the one end of keeping away from the second defeated pump at the connecting pipe of second defeated pump output end extends to the inboard top of iron phosphate recovery section of thick bamboo.
Further, the gas transmission subassembly is including seting up cavity and the air duct of rigid coupling at ammonia recovery cylinder outside top on the inner wall of iron phosphate recovery cylinder bottom, and the one end that ammonia recovery cylinder was kept away from to the air duct extends to the inboard of cavity, a plurality of gas pockets that are linked together with the iron phosphate recovery cylinder are seted up at the top of cavity, all install the check valve of giving vent to anger on a plurality of gas pockets.
Further, the stirring subassembly includes a plurality of second electric telescopic handle of rigid coupling at the apron top, a plurality of second electric telescopic handle's top rigid coupling has the roof, two driving motor are installed to the top surface of roof, two driving motor are located a pretreatment section of thick bamboo and ferric phosphate recovery cylinder directly over respectively, the (mixing) shaft is all installed to two driving motor's output, the bottom of two (mixing) shafts extends to the inboard of a pretreatment section of thick bamboo and ferric phosphate recovery cylinder respectively, and the stirring paddle leaf has all been cup jointed to the bottom of two (mixing) shafts.
Further, a plurality of perpendicular grooves have all been seted up with the inside wall of iron phosphate recovery cylinder to the preliminary treatment section of thick bamboo, and the top in perpendicular groove extends to the top of preliminary treatment section of thick bamboo or iron phosphate recovery cylinder, and the inboard sliding connection in perpendicular groove has the stopper, and the one end of a plurality of stoppers all extends to the outside in perpendicular groove and respectively with the outside top rigid coupling of two storage barrels, the concave section down rather than coaxial setting has been cup jointed at the bottom center of preliminary treatment section of thick bamboo, and the screen cloth all is located the inboard of concave section down with stirring paddle leaf, and wherein, stirring paddle leaf's a plurality of blades all incline the setting, and stirring paddle leaf's bottom and the top surface laminating of screen cloth, stirring paddle leaf's top surface flushes top surface with the top surface of concave section down, and the (mixing) shaft is connected with the storage barrel through coupling mechanism.
Further, coupling mechanism is including the adapter sleeve that is located the screen cloth bottom, and the outside of adapter sleeve is equipped with a plurality of one ends and its outer wall fixed connection's connecting rod, and the other end of a plurality of connecting rods all with the lower concave section inside wall rigid coupling of storage cylinder, the inboard movable sleeve of adapter sleeve is equipped with the connector, and the connector is connected with the adapter sleeve through the round pin axle, and the top of connector extends to the top of adapter sleeve and rotates with the bottom of (mixing) shaft to be connected.
Further, be equipped with the clamp plate in the iron phosphate recovery section of thick bamboo, the clamp plate slip cap is established outside the (mixing) shaft, and clamp plate top rigid coupling has the guide bar of a plurality of vertical settings, and the outside movable sleeve of guide bar is equipped with the spring, and the top of a plurality of guide bars all extends to the top of apron, and the equal rigid coupling in top of a plurality of guide bars has the limiting plate.
The invention has the following beneficial effects:
1. through the ammonia recovery section of thick bamboo, the preliminary treatment section of thick bamboo on the ammonia recovery section of thick bamboo is established to the cover, can heat the intensification to the liquid in the ammonia recovery section of thick bamboo when heating the intensification, the effectual heat utilization ratio that has improved, the iron phosphate is retrieved and is extracted the aqueous ammonia that uses and can carry out recycle to the ammonia through the ammonia recovery section of thick bamboo, reduces the consumption of aqueous ammonia, saves manufacturing cost.
2. Can collect insoluble solid in the ferric phosphate crystal that separates out and the preliminary treatment section of thick bamboo in the ferric phosphate recovery cylinder through the storage section of thick bamboo, and in the roof rises, the storage section of thick bamboo rises in step and removes liquid drop, avoid volatile ammonia and hydrochloric acid gas can produce great threat to operating personnel, stirring paddle leaf rises with the storage section of thick bamboo in step, can prevent that the screen cloth from taking place to block up, improve the filter effect, the clamp plate that sets up on the ferric phosphate recovery cylinder, can pass through relative motion, carry out the filter-pressing to the ferric phosphate of collecting in the storage section of thick bamboo, guarantee the ferric phosphate and filter drying nature.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic perspective view of the present invention;
FIG. 2 is a front cross-sectional structural view of the present invention;
FIG. 3 is a schematic view of the overall structure of the storage cartridge of the present invention;
FIG. 4 is a schematic view of the overall structure of the stirring blade of the present invention;
FIG. 5 is an enlarged view of the portion A in FIG. 2;
FIG. 6 is an enlarged view of the structure at B in FIG. 2 according to the present invention.
In the figure: 1. a base plate; 2. an ammonia recovery cylinder; 201. a heating coil; 3. an iron phosphate recovery cylinder; 301. a hollow interlayer; 302. a liquid inlet pipe; 303. a liquid outlet pipe; 4. a pretreatment cartridge; 5. a storage cylinder; 501. a vertical slot; 502. A limiting block; 503. screening a screen; 6. a cover plate; 601. a first electric telescopic rod; 7. a stirring assembly; 701. a second electric telescopic rod; 702. a top plate; 703. a drive motor; 704. a stirring shaft; 705. a stirring paddle; 706. A connector; 707. connecting sleeves; 708. a connecting rod; 8. a gas delivery assembly; 801. a gas-guide tube; 802. a cavity; 803. air holes; 804. an air outlet one-way valve; 9. a pumping assembly; 901. a first transfer pump; 902. a connecting pipe; 903. a second transfer pump; 10. pressing a plate; 1001. a guide bar; 1002. a spring; 1003. and a limiting plate.
Detailed Description
The technical solutions of the present invention will be described below clearly and completely in conjunction with the embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
This embodiment is arranged in solving among the prior art ferric phosphate recovery process aqueous ammonia consumption and is big, and the aqueous ammonia can not recycle, leads to the higher problem of manufacturing cost.
Referring to fig. 1-3, the recycling method of iron phosphate slag recycled by ammonia water according to this embodiment includes a bottom plate 1, an ammonia recovery cylinder 2 and an iron phosphate recovery cylinder 3 are fixedly connected to the top of the bottom plate 1, a heating coil 201 is installed inside the ammonia recovery cylinder 2, a pumping assembly 9 for pumping the solution in the pretreatment cylinder 4 to the iron phosphate recovery cylinder 3 and the iron phosphate recovery cylinder 2 is installed on the bottom plate 1, the ammonia recovery cylinder 2 conveys the recovered ammonia gas to the iron phosphate recovery cylinder 3 through a gas conveying assembly 8, the pretreatment cylinder 4 is sleeved on the top of the ammonia recovery cylinder 2, the bottom of the pretreatment cylinder 4 extends to the inside of the ammonia recovery cylinder 2, storage cylinders 5 are installed on the insides of the iron phosphate recovery cylinder 3 and the pretreatment cylinder 4, a screen 503 is installed on the insides of the storage cylinders 5, iron phosphate covers 6 are installed on the top surfaces of the pretreatment cylinder 4 and the recovery cylinder 3, and a stirring assembly 7 corresponding to the iron phosphate recovery cylinder 3 and the pretreatment cylinder 4 is installed on the cover plate 6.
Crushing iron phosphate slag, mixing 1 part of iron phosphate slag to be recovered with 10-15 parts of water according to the volume ratio to obtain an iron phosphate slag solid-liquid mixture, adjusting acid and heating the iron phosphate slag solid-liquid mixture through a pretreatment cylinder 4, dissolving iron phosphate into liquid to obtain a solution containing the iron phosphate, adjusting the temperature through an iron phosphate recovery cylinder 3 to be neutral, separating out the iron phosphate in the solution, filtering to obtain an iron phosphate hydrate, adjusting alkali to obtain an aqueous solution generated by filtering, and generating NH (NH) after the aqueous solution is subjected to alkali adjustment 4 Mixed solution of Cl, naCl and NaOH, injecting the mixed solution into an ammonia recovery cylinder 2 for heating, and NH 4 Cl is decomposed to generate ammonia gas, the ammonia gas is input into the iron phosphate recovery cylinder 3 through the gas transmission assembly 8 for recovery, so that the consumption of ammonia water is reduced, and NH in the mixed solution 4 After the Cl is decomposed, the mixed solution becomes strong alkali, and can be used as a solvent for alkali adjustment.
Specifically, the gas transmission assembly 8 comprises a cavity 802 formed in the inner wall of the bottom of the iron phosphate recovery cylinder 3 and a gas guide tube 801 fixedly connected to the top of the outer side of the ammonia recovery cylinder 2, one end, away from the ammonia recovery cylinder 2, of the gas guide tube 801 extends to the inner side of the cavity 802, a plurality of air holes 803 communicated with the iron phosphate recovery cylinder 3 are formed in the top of the cavity 802, and an air outlet check valve 804 is installed on each of the air holes 803.
The ammonia gas that the ammonia recovery section of thick bamboo 2 heating produced, gas thermal expansion, the safety that obtains of retrieving discharges from ammonia recovery section of thick bamboo 2 through air duct 801 and enters into cavity 802, dredges through the check valve 804 that gives vent to anger and pours into the iron phosphate recovery section of thick bamboo 3 into from the bottom of phosphoric acid recovery section of thick bamboo 3 into, and the ammonia is vertical upwards to drift and fully contacts with the solution in the iron phosphate recovery section of thick bamboo 3, carries out abundant absorption and utilization to the ammonia that obtains of retrieving.
Further, the equal rigid coupling in outside top of the outside of ammonia recovery section of thick bamboo 2 and iron phosphate recovery section of thick bamboo 3 has a plurality of electric telescopic handle 601, and the extension end of a plurality of electric telescopic handle 601 all with the bottom rigid coupling of apron 6, cavity intermediate layer 301 has been seted up to the lateral wall of iron phosphate recovery section of thick bamboo 3, and the feed liquor pipe 302 and the drain pipe 303 that are linked together with cavity intermediate layer 301 have been cup jointed respectively to the outside bottom and the outside top of iron phosphate recovery section of thick bamboo 3.
The drain pipe has been cup jointed to one side bottom of ammonia recovery cylinder 2, install the valve on the drain pipe, thereby the outside of ammonia recovery cylinder 2 is discharged to the solution in the convenient ammonia recovery cylinder 2, a plurality of electric telescopic handle 601 synchronous extension, promote the vertical upward movement of apron 6, thereby open pretreatment cylinder 4 and iron phosphate recovery cylinder 3, the solid that collects in the convenient storage cylinder 5 clears up and collects, enter into cavity intermediate layer 301 through heat transfer medium through feed liquor pipe 302, discharge from drain pipe 303 again, cool down iron phosphate recovery cylinder 3, guarantee that the iron phosphate in the solution can fully separate out, all install at pretreatment cylinder 4 and iron phosphate recovery cylinder 3's outside top and annotate the liquid mouth (not shown), thereby the solution pH in convenient pretreatment cylinder 4 or the iron phosphate recovery cylinder 3 adjusts.
Specifically, the pumping assembly 9 includes a first transport pump 901 and a second transport pump 903 installed on the top of the base plate 1, the input ends and the output ends of the first transport pump 901 and the second transport pump 903 are both installed with a connecting pipe 902, wherein one end of the connecting pipe 902 installed at the input end of the first transport pump 901, which is far away from the first transport pump 901, extends to the inside bottom of the iron phosphate recovery cylinder 3, one end of the connecting pipe 902 installed at the output end of the first transport pump 901, which is far away from the first transport pump 901, extends to the inside top of the ammonia recovery cylinder 2, one end of the connecting pipe 902 installed at the input end of the second transport pump 903, which is far away from the second transport pump 903, extends to the inside bottom of the pretreatment cylinder 4, and one end of the connecting pipe 902 installed at the output end of the second transport pump 903, which is far away from the second transport pump 903, extends to the inside top of the iron phosphate recovery cylinder 3.
First defeated pump 901 starts, can with the solution pump in the iron phosphate recovery cylinder 3 send ammonia recovery cylinder 2, second defeated pump 903 starts, can with the solution pump in the pretreatment barrel 4 send iron phosphate recovery cylinder 3 in, in shifting the solution, the iron phosphate cartridge filter 3 keeps airtight state with pretreatment barrel 4, can reduce the volatilization of ammonia or hydrochloric acid to reduce the harm of volatile ammonia or hydrochloric acid gas to operating personnel.
Example 2
This embodiment is arranged in solving among the prior art ferric phosphate sediment and water and mixes the effect relatively poor, when retrieving the ferric phosphate, need pass through a lot of filtration, and the volatility of hydrochloric acid and ammonia is all great, if direct filters under open environment, volatile ammonia and hydrochloric acid gas can produce great threat, the lower problem of security to operating personnel.
Referring to fig. 2-6, in the method for recycling iron phosphate slag recycled by ammonia water according to the present embodiment, the stirring assembly 7 includes a plurality of second electric telescopic rods 701 fixedly connected to the top of the cover plate 6, a top plate 702 is fixedly connected to the tops of the plurality of second electric telescopic rods 701, two driving motors 703 are installed on the top surface of the top plate 702, the two driving motors 703 are respectively located right above the pretreatment cylinder 4 and the iron phosphate recovery cylinder 3, stirring shafts 704 are installed at output ends of the two driving motors 703, bottoms of the two stirring shafts 704 respectively extend to inner sides of the pretreatment cylinder 4 and the iron phosphate recovery cylinder 3, and stirring blades 705 are respectively sleeved at bottoms of the two stirring shafts 704.
Driving motor 704 drive (mixing) shaft 704 rotates, drives stirring paddle leaf 705 and rotates to solution to in the pretreatment cartridge 4 or the ferric phosphate recovery cylinder 3 stirs, makes the solid in the solution and the abundant misce bene of liquid, and then guarantees the recovery efficiency of ferric phosphate, and a plurality of second electric telescopic handle 701 extend in step, promote roof 702 upward movement, drive the (mixing) shaft 704 and the synchronous upward movement of stirring paddle leaf 705.
Specifically, a plurality of perpendicular grooves 501 have all been seted up with the inside wall of iron phosphate recovery cylinder 3 to a pretreatment section of thick bamboo 4, the top of perpendicular groove 501 extends to the top of a pretreatment section of thick bamboo 4 or iron phosphate recovery cylinder 3, the inboard sliding connection of perpendicular groove 501 has stopper 502, the one end of a plurality of stoppers 502 all extends to the outside of perpendicular groove 501 and respectively with the outside top rigid coupling of two storage barrels 5, the concave section rather than coaxial setting has been cup jointed at the bottom center of a pretreatment section of thick bamboo 4, screen cloth 503 all is located the inboard of concave section down with stirring paddle leaf 705, wherein, a plurality of blades of stirring paddle leaf 705 all incline the setting, stirring paddle leaf 705's bottom and screen cloth 503's top surface laminating, stirring paddle leaf 705's top surface flushes with the top surface of concave section down, stirring shaft 704 is connected with storage barrels 5 through coupling mechanism.
One end of the storage cylinder 5, which is located at the inner side of the pretreatment cylinder 4 and the iron phosphate recovery cylinder 3, is matched with the pretreatment cylinder 4 or the iron phosphate recovery cylinder 3, the storage cylinder 5 is limited by a plurality of limiting blocks 502, the storage cylinder 5 is prevented from moving upwards, the storage cylinder 5 rotates per se, the storage cylinder 5 ascends synchronously along with the stirring shaft 704, the stirring shaft 704 ascends simultaneously, the bottom of the stirring paddle 705 is always attached to the top surface of the screen 503, the screen 503 can be prevented from being blocked, it is ensured that the solution can be filtered out quickly, when the storage cylinder 5 ascends, solids existing in the liquid can be filtered, the filtering operation is synchronously carried out along with the ascending of the top plate 702, and the filtering operation is always located at the inner side of the cylinder body, so that the harm to operators caused by the large amount of volatilization of ammonia gas and hydrochloric acid gas due to the exposed operation is avoided.
Specifically, coupling mechanism is including being located the adapter sleeve 707 of screen cloth 503 bottom, and the outside of adapter sleeve 707 is equipped with a plurality of one end and its outer wall fixed connection's connecting rod 708, and the other end of a plurality of connecting rods 708 all with the lower concave section inside wall rigid coupling of storage cylinder 5, and the inboard movable sleeve of adapter sleeve 707 is equipped with connector 706, and connector 706 is connected with adapter sleeve 707 through the round pin axle, and the top of connector 706 extends to the top of adapter sleeve 707 and is connected with the bottom rotation of (mixing) shaft 704.
Connector 706 is true polygon structure, and connector 706 is connected with adapter sleeve 707 through the round pin axle, conveniently dismantles storage cylinder 5 and (mixing) shaft 704, conveniently takes out the solids of storing in the storage cylinder 5, a plurality of connecting rods 708 level set up and with screen cloth 503's bottom butt, and then support screen cloth 503, prevent that screen cloth 503 from warping with the inner wall component force of storage cylinder 5.
Further, be equipped with clamp plate 10 in the iron phosphate recycling bin 3, clamp plate 10 slip cap is established outside (mixing) shaft 704, and clamp plate 10 top rigid coupling has the guide bar 1001 of a plurality of vertical settings, and the outside activity cover of guide bar 1001 is equipped with spring 1002, and the top of a plurality of guide bars 1001 all extends to the top of apron 6, and the equal rigid coupling in top of a plurality of guide bars 1001 has limiting plate 1003.
When the storage cylinder 5 in the iron phosphate recovery cylinder 3 moves upwards, the pressing plate 10 moves downwards relative to the storage cylinder 5, and the iron phosphate stored in the storage cylinder 5 is extruded, so that the iron phosphate in the storage cylinder 5 is extruded and dehydrated, the pressing plate 10 can be buffered through a plurality of springs 1002, and the iron phosphate stored in the storage cylinder 5 in different amounts can be extruded and dehydrated.
Example 3
Referring to fig. 1 to 6, the recycling method of iron phosphate slag recycled by ammonia water of the present embodiment includes the following steps:
the method comprises the following steps: after crushing the iron phosphate slag, mixing the iron phosphate slag to be recovered with water according to a mass-volume ratio of 1g: mixing 10-15mL to obtain a solid-liquid mixture of the iron phosphate slag, putting the solid-liquid mixture of the iron phosphate slag into a pretreatment cylinder 4 in a recovery device, adding 15wt% hydrochloric acid into the pretreatment cylinder 4, and adjusting the pH value of the solid-liquid mixture of the iron phosphate slag to 1 to obtain an acidic solid-liquid mixture;
the iron phosphate is easily dissolved in hydrochloric acid under the heating condition, so that the iron phosphate is extracted from the iron phosphate slag.
Step two: the stirring component 7 uniformly stirs the acidic solid-liquid mixture, steam is introduced into the heating coil 201, the solution in the pretreatment cylinder 4 is heated to 50-60 ℃, the temperature is kept and the stirring is carried out for 30-50min, the top plate 702 rises, the material storage cylinder 5 is driven to synchronously rise, the acidic solid-liquid mixture is filtered through the screen 503 to obtain an acidic iron phosphate solution, insoluble substances are collected in the material storage cylinder 5, the acidic iron phosphate solution remains in the pretreatment cylinder 4, the acidic iron phosphate solution is pumped into the iron phosphate recovery cylinder 3 through the second transfer pump 903, ammonia water is added into the iron phosphate recovery cylinder 3, the pH value of the system is adjusted to 7, the temperature is reduced to room temperature, the stirring is continued for 30-50min, and iron phosphate is fully separated out to obtain an iron phosphate solid-liquid mixture;
when the top plate 702 rises, the stirring blades 705 rotate simultaneously, the rotating stirring blades 705 can clean the screen 503 to prevent the screen 503 from being blocked, the iron phosphate solution is pumped to the iron phosphate recovery cylinder 3, the pretreatment cylinder 4 is emptied, the two storage cylinders 5 descend, and the iron phosphate slag to be recovered is added into the pretreatment cylinder 4 by repeating the steps, so that the iron phosphate slag can be continuously recovered;
step three: the top plate 702 rises to drive the storage barrel 5 to rise, the screen 503 filters the iron phosphate solid-liquid mixture to obtain iron phosphate crystals and a solution to be recovered, the iron phosphate crystals are collected in the storage barrel 5, naOH is added into the solution to be recovered in the iron phosphate recovery barrel 3, the pH value of a solution system is adjusted to 12-14 to obtain an ammonia solution to be recovered, the first transfer pump 901 is started, and the ammonia solution to be recovered is pumped into the ammonia recovery barrel 2;
when filtering iron phosphate in an iron phosphate solid-liquid mixture, a rotating stirring paddle 705 can clean the screen 503 to prevent the screen 503 from being blocked, when a pressing plate 10 enters the inner side of a storage barrel 5, a driving motor 703 positioned right above an iron phosphate recovery barrel 3 stops working, the pressing plate 10 moves downwards relative to the storage barrel 5 to perform extrusion water filtration on iron phosphate crystals in the storage barrel 5, naOH is added into the iron phosphate recovery barrel 3 to adjust the pH value of a solution system to 12-14 to obtain an ammonia solution to be recovered, a first transfer pump 901 is started to pump the ammonia solution to be recovered into an ammonia recovery barrel 2, the iron phosphate recovery barrel 3 is emptied, the two storage barrels 5 descend to conveniently transfer the acidic solid-liquid mixture in a pretreatment barrel 4 into the iron phosphate recovery barrel 3, and the process operation is kept continuous.
Step four: making NH in the ammonia solution to be recovered according to the reaction mechanism of strong base to prepare weak base 4 Conversion of OH to NH 4 Cl, in the heated state, NH 4 Cl to NH 3 ,NH 3 Form the ammonia solution in the ferric phosphate recovery cylinder 3 through air duct 801, carry out recycle to ammonia in the aqueous ammonia to the ammonia that obtains of retrieving pours into from the bottom of ferric phosphate recovery cylinder 3, can guarantee the ammonia and the solution in the ferric phosphate recovery cylinder 3 fully contacts, and then makes the solution in the ferric phosphate recovery cylinder 3 can be with ammonia make full use of, reduces ammoniaThe amount of water used.
As shown in fig. 1-6, the working process and principle of the present invention are as follows:
when the recycling agent is used, according to the volume ratio, the iron phosphate slag to be recycled and water are mixed according to the mass volume ratio of 1g:10-15mL of the iron phosphate slag solid-liquid mixture is obtained by mixing, the iron phosphate slag solution to be recovered is put into a pretreatment cylinder 4 in a recovery device, after acid adjustment and heating, iron phosphate in the iron phosphate slag solid-liquid mixture is dissolved to obtain an acidic solid-liquid mixture, the acidic solution is filtered, the filtered acidic solution is pumped into an iron phosphate recovery cylinder 3 through a second transfer pump 903, the pH of the acidic solution is adjusted by using ammonia water and ammonia gas recovered from an ammonia recovery cylinder 2, the solution in the iron phosphate recovery cylinder 3 is cooled, so that iron phosphate is separated out from the solution to obtain an iron phosphate solid-liquid mixture, the iron phosphate is filtered, the pH of the filtered solution is adjusted to 12-14 by using NaOH to obtain an ammonia solution to be recovered, the ammonia solution is pumped into an ammonia recovery cylinder 2 through a first transfer pump, steam enters a heat exchange coil 201, the ammonia solution to be recovered in the ammonia recovery cylinder 2 and the acidic solid-liquid mixture in the pretreatment cylinder 4 are simultaneously heated, and when the iron phosphate slag is recovered, operation phases are continuous, thereby ensuring that ammonia can be recovered while being recovered, and the production efficiency is improved.
The foregoing is merely exemplary and illustrative of the present invention and various modifications, additions and substitutions may be made by those skilled in the art to the specific embodiments described without departing from the scope of the invention as defined in the following claims.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise forms disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand the invention for and utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims (9)

1. The recycling method of the iron phosphate slag recycled by ammonia water is characterized by comprising the following operation steps:
the method comprises the following steps: after crushing the iron phosphate slag, mixing the iron phosphate slag to be recovered with water according to a mass-volume ratio of 1g: mixing 10-15mL to obtain a solid-liquid mixture of the iron phosphate slag, putting the solid-liquid mixture of the iron phosphate slag into a pretreatment cylinder (4) in a recovery device, adding 15wt% hydrochloric acid into the pretreatment cylinder (4), and adjusting the pH value of the solid-liquid mixture of the iron phosphate slag to 1 to obtain an acidic solid-liquid mixture;
step two: the acidic solid-liquid mixture is uniformly stirred by a stirring assembly (7), steam is introduced into a heating coil (201), the solution in the pretreatment cylinder (4) is heated to 50-60 ℃, the temperature is kept and the stirring is carried out for 30-50min, a top plate (702) rises and drives a storage cylinder (5) to rise synchronously, the acidic solid-liquid mixture is filtered by a screen (503), the acidic solid-liquid mixture is filtered to obtain an acidic iron phosphate solution, insoluble substances are collected in the storage cylinder (5), the iron phosphate solution remains in the pretreatment cylinder (4), a second transfer pump (903) pumps the acidic iron phosphate solution into an iron phosphate recovery cylinder (3), the pH of the system is adjusted to 7 by using ammonia water and is cooled to room temperature, the stirring is continued for 30-50min, and iron phosphate is fully separated out to obtain an iron phosphate solid-liquid mixture;
step three: filtering the iron phosphate solid-liquid mixture by using a screen (503) in an iron phosphate recovery cylinder (3) to obtain iron phosphate crystals and a solution to be recovered, collecting the iron phosphate crystals in a storage cylinder (5), adding NaOH into the solution to be recovered in the iron phosphate recovery cylinder (3), adjusting the pH value of a solution system to 12-14 to obtain an ammonia solution to be recovered, and pumping the ammonia solution to be recovered into an ammonia recovery cylinder (2) by using a first transfer pump (901);
step four: making NH of ammonia solution to be recovered according to reaction mechanism of strong base to prepare weak base 4 Conversion of OH to NH 4 Cl, in the heated state, NH 4 Cl to NH 3 ,NH 3 Enters the ferric phosphate recovery cylinder (3) through the air duct (801) to recycle ammonia in the ammonia water.
2. The recycling method of the iron phosphate slag recycled by the ammonia water according to claim 1, wherein the recycling device comprises a bottom plate (1), the top of the bottom plate (1) is fixedly connected with an ammonia recovery cylinder (2) and an iron phosphate recovery cylinder (3), a heating coil (201) is installed on the inner side of the ammonia recovery cylinder (2), a pumping assembly (9) used for pumping the solution in the pretreatment cylinder (4) to the iron phosphate recovery cylinder (3) and the iron phosphate recovery cylinder from the solution is installed on the bottom plate (1), the ammonia recovery cylinder (2) conveys the recovered ammonia gas to the iron phosphate recovery cylinder (3) through a gas conveying assembly (8), the top of the ammonia recovery cylinder (2) is sleeved with the pretreatment cylinder (4), the bottom of the pretreatment cylinder (4) extends to the inner side of the ammonia recovery cylinder (2), a material storage cylinder (5) is installed on the inner sides of the iron phosphate recovery cylinder (3) and the pretreatment cylinder (4), a screen (503) is installed on the inner sides of the iron phosphate recovery cylinder (3), a cover plate (6) of the pretreatment cylinder (3) and a stirring assembly (7) corresponding to the iron phosphate recovery cylinder (3) are installed on the top surface of the iron phosphate recovery cylinder (4).
3. The recycling method of iron phosphate slag recycled by ammonia water according to claim 2, wherein a plurality of first electric telescopic rods (601) are fixedly connected to the top of the outside of the ammonia recycling cylinder (2) and the top of the outside of the iron phosphate recycling cylinder (3), the extension ends of the first electric telescopic rods (601) are fixedly connected to the bottom of the cover plate (6), a hollow interlayer (301) is formed in the side wall of the iron phosphate recycling cylinder (3), and a liquid inlet pipe (302) and a liquid outlet pipe (303) communicated with the hollow interlayer (301) are respectively sleeved on the bottom of the outside and the top of the outside of the iron phosphate recycling cylinder (3).
4. The recycling method of the iron phosphate slag recycled by the ammonia water of claim 2, wherein the pumping assembly (9) comprises a first transfer pump (901) and a second transfer pump (903) which are installed at the top of the base plate (1), the input ends and the output ends of the first transfer pump (901) and the second transfer pump (903) are both provided with a connecting pipe (902), wherein one end, far away from the first transfer pump (901), of the connecting pipe (902) installed at the input end of the first transfer pump (901) extends to the bottom inside the iron phosphate recovery cylinder (3), one end, far away from the first transfer pump (901), of the connecting pipe (902) installed at the output end of the first transfer pump (901) extends to the top inside the ammonia recovery cylinder (2), one end, far away from the second transfer pump (903), of the connecting pipe (902) installed at the input end of the second transfer pump (903) extends to the bottom inside the pretreatment cylinder (4), and one end, far away from the end of the iron phosphate recovery cylinder (3) of the connecting pipe (902) installed at the output end of the second transfer pump (903) extends to the top inside the iron phosphate recovery cylinder (3).
5. The recycling method of the phosphoric acid iron slag recycled by the ammonia water as claimed in claim 2, wherein the gas transmission assembly (8) comprises a cavity (802) formed in the inner wall of the bottom of the iron phosphate recovery cylinder (3) and a gas guide pipe (801) fixedly connected to the top of the outer side of the ammonia recovery cylinder (2), one end, away from the ammonia recovery cylinder (2), of the gas guide pipe (801) extends to the inner side of the cavity (802), the top of the cavity (802) is provided with a plurality of gas holes (803) communicated with the iron phosphate recovery cylinder (3), and the plurality of gas holes (803) are respectively provided with a gas outlet one-way valve (804).
6. The recycling method of the phosphoric acid iron slag recycled by the ammonia water of claim 2, wherein the stirring assembly (7) comprises a plurality of second electric telescopic rods (701) fixedly connected to the top of the cover plate (6), a top plate (702) is fixedly connected to the tops of the second electric telescopic rods (701), two driving motors (703) are installed on the top surface of the top plate (702), the two driving motors (703) are respectively located right above the pretreatment cylinder (4) and the iron phosphate recovery cylinder (3), the stirring shafts (704) are installed at the output ends of the two driving motors (703), the bottom parts of the two stirring shafts (704) respectively extend to the inner sides of the pretreatment cylinder (4) and the iron phosphate recovery cylinder (3), and the stirring blades (705) are sleeved at the bottom parts of the two stirring shafts (704).
7. The recycling method of the iron phosphate slag recycled by the ammonia water according to claim 6, wherein the inner side walls of the pretreatment cylinder (4) and the iron phosphate recycling cylinder (3) are provided with a plurality of vertical grooves (501), the tops of the vertical grooves (501) extend to the tops of the pretreatment cylinder (4) or the iron phosphate recycling cylinder (3), the inner side of each vertical groove (501) is connected with a limiting block (502) in a sliding manner, one ends of the limiting blocks (502) extend to the outer part of each vertical groove (501) and are fixedly connected with the top of the outer sides of the two storage cylinders (5), the center of the bottom of the pretreatment cylinder (4) is sleeved with a concave section which is coaxial with the pretreatment cylinder, the screen (503) and the stirring paddle (705) are both located on the inner side of the concave section, wherein a plurality of blades of the stirring paddle (705) are all obliquely arranged, the bottom of the stirring paddle (705) is attached to the top surface of the screen (503), the top surface of the stirring paddle (705) is flush with the top surface of the concave section, and the storage shaft (704) is connected with the storage cylinder (5) through a connecting mechanism.
8. The recycling method of iron phosphate slag recycled by ammonia water according to claim 7, wherein the connecting mechanism comprises a connecting sleeve (707) located at the bottom of the screen (503), the outside of the connecting sleeve (707) is provided with a plurality of connecting rods (708) with one ends fixedly connected with the outer wall of the connecting sleeve, the other ends of the connecting rods (708) are fixedly connected with the inner side wall of the lower concave section of the storage cylinder (5), the inner side of the connecting sleeve (707) is movably sleeved with a connecting head (706), the connecting head (706) is connected with the connecting sleeve (707) through a pin shaft, and the top of the connecting head (706) extends to the top of the connecting sleeve (707) and is rotatably connected with the bottom of the stirring shaft (704).
9. The recycling method of the iron phosphate slag recycled by the ammonia water according to claim 6, wherein a pressing plate (10) is arranged in the iron phosphate recycling cylinder (3), the pressing plate (10) is slidably sleeved outside the stirring shaft (704), a plurality of vertically arranged guide rods (1001) are fixedly connected to the top of the pressing plate (10), a spring (1002) is movably sleeved outside the guide rods (1001), the tops of the guide rods (1001) extend to the top of the cover plate (6), and a limiting plate (1003) is fixedly connected to the tops of the guide rods (1001).
CN202211303488.6A 2022-10-24 2022-10-24 Recycling method of iron phosphate slag recycled by ammonia water Withdrawn CN115557481A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116531924A (en) * 2023-05-19 2023-08-04 湖北朗润环保科技有限公司 Tail gas recovery method and system for ammonia pretreatment process of ferric phosphate wastewater

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116531924A (en) * 2023-05-19 2023-08-04 湖北朗润环保科技有限公司 Tail gas recovery method and system for ammonia pretreatment process of ferric phosphate wastewater

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Application publication date: 20230103