CN220788065U - Device system for preparing ferric phosphate - Google Patents

Device system for preparing ferric phosphate Download PDF

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Publication number
CN220788065U
CN220788065U CN202322578190.2U CN202322578190U CN220788065U CN 220788065 U CN220788065 U CN 220788065U CN 202322578190 U CN202322578190 U CN 202322578190U CN 220788065 U CN220788065 U CN 220788065U
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gas
roasting furnace
furnace
ferric phosphate
tower
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CN202322578190.2U
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张博远
苏宗华
王红梅
汪洪
万文
刘超
严季春
黄燕
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Chengdu Yizhi Technology Co ltd
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Chengdu Yizhi Technology Co ltd
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Abstract

The utility model discloses a device system for preparing ferric phosphate, which relates to the technical field of ferric phosphate, and comprises a mixing tower, a filter, a venturi type preconcentrator, a roasting furnace and a cooling conveyor, wherein the mixing tower is used for preparing raw material liquid, the filter is used for filtering particulate matters in the raw material liquid, the venturi type preconcentrator is used for evaporating water in the raw material liquid to obtain concentrated liquid, the roasting furnace is used for decomposing the concentrated liquid at high temperature, and the cooling conveyor is used for cooling and conveying solid products in the roasting furnace; the roasting furnace is connected with the upper end of the pre-concentrator through a furnace gas pipeline; the preconcentrator is also connected with a tail gas treatment device through a pipeline. The device provided by the utility model prepares the ferric phosphate by a roasting method, opens up a new method for preparing the ferric phosphate, can recycle waste gas and save energy consumption.

Description

Device system for preparing ferric phosphate
Technical Field
The utility model relates to the technical field of ferric phosphate, in particular to a device system for preparing ferric phosphate.
Background
The ferric phosphate is widely applied to manufacturing of lithium iron phosphate batteries, and has the characteristics of safety and reliability. Iron phosphate is a precursor material for preparing lithium iron phosphate, and the demand is very large. The preparation method of the ferric phosphate comprises a chemical precipitation method, a hydrothermal synthesis method, a sol-gel method, a fluoride ion system synthesis method, a biological template method, a microwave auxiliary method, a flame spray drying method and the like.
Since the electrochemical activity of the FePO 4 material directly affects the electrochemical properties of the finally prepared lithium iron phosphate material, how to prepare high-performance iron phosphate materials by using a method commonly used in industry is a significant problem. Currently, the method for industrially synthesizing iron phosphate materials is mainly a precipitation method. The precipitation method has wide application due to the advantages of low requirements on equipment, low energy consumption, easy industrialization, adjustable preparation process and the like, fePO 4 materials with uniform granularity, large specific surface area and high electrochemical activity can be prepared by the method, but certain limitations exist, the preparation process is complicated, the preparation process usually comprises the processes of pulp mixing, aging, filtering, washing, drying and the like, the accuracy requirement of the pulp mixing process is high, the requirements on raw materials are strict, and the preparation processes of the preparation process are completely different by adopting different raw materials; in addition, the water consumption in the washing process is extremely high, and the sewage treatment cost is extremely high; the filter cake of the FePO 4 material is thick, and the traditional drying technology is uneven in drying and high in energy consumption, so that a vacuum drying technology is needed in most cases, and the local temperature is prevented from being too high.
Disclosure of utility model
The utility model aims to overcome the defects of the prior art, provides a device system for preparing ferric phosphate, and aims to provide a novel method for preparing ferric phosphate by dissolving Fe 2O3 powder in an acid solution formed by mixing hydrochloric acid and phosphoric acid to form turbid liquid, burning the turbid liquid to produce ferric phosphate and recycling tail gas, so that energy consumption is saved.
In order to achieve the above purpose, the technical scheme adopted by the utility model is as follows:
A device system for preparing ferric phosphate comprises a mixing tower, a filter, a venturi type preconcentrator, a roasting furnace and a cooling conveyor, wherein the mixing tower is sequentially connected and used for preparing raw material liquid, the filter can filter particulate matters in the raw material liquid, the venturi type preconcentrator can evaporate water in the raw material liquid to obtain concentrated liquid, the roasting furnace can decompose the concentrated liquid at high temperature, and the cooling conveyor can cool and convey solid products in the roasting furnace;
The roasting furnace is connected with the upper end of the pre-concentrator through a furnace gas pipeline; the preconcentrator is also connected with a tail gas treatment device through a pipeline.
Further, the mixing tower and the filter are made of glass fiber reinforced plastic, and a filter barrel wrapped by a PVDF filter screen is arranged in the filter; the flow rate of the materials conveyed by the cooling conveyor is 0.0065m/s, the throughput is 100-10000 Kg/h, the cooling area is 50-600 square meters, and the temperature of the cooled materials is 30-100 ℃.
Further, the roasting furnace is in a vertical cylinder shape and comprises an upper cone and a lower cone; the shell of the roasting furnace is of a steel plate welding structure, the inner side of the shell is lined with refractory acid-resistant bricks, and the outer side of the shell is wrapped with an insulating layer; a plurality of burners are arranged in the roasting furnace and are arranged on the furnace body in a tangential direction; the furnace top of the roasting furnace is provided with a dual-fluid atomizing spray gun made of niobium materials.
Further, the tail gas treatment device comprises an exhaust gas fan which is connected with the preconcentrator and can extract the tail gas, a first washing tower which is used for washing HCl gas in the tail gas by desalted water, and a second washing tower which is used for washing the tail gas again by desalted water added with alkali liquor.
Further, an absorption tower capable of absorbing HCl gas, a third washing tower for carrying out primary washing on the HCl gas in the tail gas and a graphite heat exchanger capable of reducing the temperature of the tail gas to below 40 ℃ are arranged between the pre-concentrator and the waste gas fan.
Further, the absorption tower is made of FRP or PPH materials; the inside of the absorption tower is filled with PP structured packing, and the upper part of the absorption tower is provided with a spray head made of PTFE material; the first washing tower and the second washing tower are both filled towers, made of FRP or PPH materials, are internally provided with PP corrugated fillers, and are provided with spray heads made of PTFE materials at the upper parts; the washing water outlet of the first washing tower is connected with the absorption tower, and the second washing tower is connected with a chimney for discharging waste gas.
Further, the third scrubber is a rear venturi.
Compared with the prior art, the utility model has the following beneficial effects:
(1) When the device system provided by the utility model is used for preparing ferric phosphate, high-purity Fe 2O3 powder is dissolved in the mixed solution of hydrochloric acid and phosphoric acid to form turbid liquid, the turbid liquid is atomized by the double-fluid spray gun and then burned, the generated solid product is ferric phosphate, the ferric phosphate powder can be directly prepared, the processes of size mixing, ageing, washing, drying and the like are not needed, the preparation process is simple, and a novel method for preparing the ferric phosphate is developed.
(2) The tail gas generated by the utility model is treated by the tail gas treatment device and then discharged into the atmosphere, the tail gas treatment device can recycle the hydrochloric acid, and the waste gas is recycled while the acid is discharged into the atmosphere, so that the energy consumption is saved.
Drawings
FIG. 1 is a schematic diagram of a device system of the present utility model;
Fig. 2 is a process flow diagram of the present utility model.
Wherein, the names corresponding to the reference numerals are: the device comprises a 1-mixing tower, a 2-filter, a 3-preconcentrator, a 4-roasting furnace, a 5-absorption tower, a 6-graphite heat exchanger, a 7-third washing tower, an 8-waste gas fan, a 9-first washing tower, a 10-second washing tower, an 11-cooling conveyor and a 12-furnace gas pipeline.
Detailed Description
The utility model will be further illustrated by the following description and examples, which include but are not limited to the following examples.
As shown in fig. 1, the present embodiment provides an apparatus system for preparing iron phosphate, comprising a mixing tower 1, a filter 2, a pre-concentrator 3, a roasting furnace 4, and an exhaust gas treatment device connected to the pre-concentrator 3, which are sequentially connected.
The mixing tower 1 is made of glass fiber reinforced plastic, and is used for preparing raw material liquid, wherein Fe 2O3 powder, HCl solution with a certain proportion and H 3PO4 solution are dissolved in the mixing tower to form turbid liquid, namely the raw material liquid, and the molar ratio of H + to Fe 3+ in the raw material liquid is 3:1 to 7:1.
The filter 2 is also made of glass fiber reinforced plastic, raw material liquid in the mixing tower 1 is pumped into the filter 2 through a plastic pump, a filter barrel wrapped by a PVDF filter screen is arranged in the filter 2, and impurities such as particulate matters in the raw material liquid can be filtered out.
The filtered raw material liquid is conveyed into a pre-concentrator 3 through a circulating pump, the pre-concentrator 3 is venturi-shaped, the pre-concentrator 3 is connected with the upper end of a roasting furnace 4 through a furnace gas pipeline 12, high-temperature gas (the gas temperature is 420-850 ℃) in the roasting furnace 4 enters the pre-concentrator 3 through the furnace gas pipeline to perform heat exchange, 25-30% of water in the raw material liquid is evaporated, and concentrated liquid is obtained, and the concentrated liquid enters the roasting furnace 4 after being atomized through a spray gun.
The roasting furnace 4 is a main reaction device and is in a vertical cylinder shape and comprises an upper cone and a lower cone; the shell of the roasting furnace 4 is of a steel plate welding structure, the inner side of the shell is lined with refractory acid-resistant bricks, and the outer side of the shell is wrapped with an insulating layer; a plurality of burners are arranged in the roasting furnace 4 and are arranged on the furnace body in a tangential direction; the top of the roasting furnace 4 is provided with a dual-fluid atomizing spray gun made of niobium, concentrated solution in the pre-concentrator enters the roasting furnace 4 through the dual-fluid atomizing spray gun to be decomposed into ferric phosphate powder and HCL steam, the ferric phosphate powder and combustion hot air flow are in a countercurrent direction, the ferric phosphate powder naturally falls into a cooling conveyor 11 at the bottom of the lower furnace, the cooling conveyor 11 can cool materials while conveying the materials, the flow rate of the materials conveyed by the cooling conveyor 11 is 0.0065m/s, the treatment capacity is 100-10000 Kg/h, the cooling area is 50-600 square meters, and the temperature of the cooled materials is 30-100 ℃; tail gas consisting of HCL vapor, water vapor, natural gas combustion products, small amounts of iron phosphate powder and excess oxygen is drawn off from the top of the furnace through a furnace gas line 12 into the preconcentrator 3, where the small amounts of iron phosphate powder are absorbed.
When the roasting furnace 4 works, natural gas is used as a raw material, air is used as combustion supporting gas, the temperature at the outlet of the lower cone material is 300-600 ℃, the temperature at the burner is 1300-1450 ℃, and the temperature at the top of the furnace is 450-850 ℃; spraying the concentrated solution after atomizing in a spray gun, wherein the flowing pressure of a liquid phase is 200 kpa-400 kpa, the flow rate is 0.3m < 3 > -6 m < 3 >, and the pressure of gas phase atomization wind is 0.3 mpa-1.0 mpa; the temperature of the core reaction zone of the roasting furnace is 650-950 ℃; products with different particle sizes can be produced by adjusting the pressure ratio of the liquid phase to the gas phase and matching the sizes of the spray heads of different spray guns, and the particle size of liquid drops sprayed by the spray guns in the embodiment is 3-150 mu m.
The tail gas treatment device comprises an absorption tower 5, a graphite heat exchanger 6, a third washing tower 7, an exhaust gas fan 8, a first washing tower 9 and a second washing tower 10 which are sequentially arranged. The exhaust gas blower 8 is a main power device for gas phase flow, generates a total pressure of 5 to 20kpa, and is used for extracting tail gas generated in the roasting furnace 4, and then discharging the tail gas from a chimney after washing by the first washing tower 9 and the second washing tower 10.
In this embodiment, the absorption tower 5 is connected to the preconcentrator 3, and the tail gas extracted by the exhaust gas fan 8 is firstly absorbed by part of HCl gas in the absorption tower 5, then cooled to below 40 ℃ by the graphite heat exchanger 6, then washed by the third washing tower 7, and finally enters the first washing tower 9 and the second washing tower 10. The absorption tower 5 is made of FRP or PPH, PP structured packing is filled in the absorption tower, a spray head made of PTFE material is arranged on the upper portion of the absorption tower, so that spray liquid is uniformly distributed on the packing, the spray liquid flows reversely with tail gas containing HCL vapor, regenerated acid is formed by absorbing the HCL, and the operation temperature is 60-105 ℃. The water condensed by the graphite heat exchanger 6 enters the water collecting tank and flows to the absorption tower 5 for reabsorption. The third scrubber 7 is a rear venturi type, and part of HCl gas in the tail gas is scrubbed by rinsing water. The first washing tower 9 and the second washing tower 10 are filled towers, are made of FRP or PPH materials, are internally filled with PP corrugated filler, and are provided with a spray head made of PTFE material at the upper part; the washing water of the first washing tower 9 is desalted water, the water outlet of the first washing tower is connected with the absorption tower 5, the washing water sprays to absorb HCL in tail gas, and the generated weak acid solution enters the absorption tower 5 through a plastic pump; the second washing tower 10 is connected with a chimney for discharging waste gas, the washing water is desalted water added with alkali liquor, and the washed washing water is discharged into a sewage station for treatment.
The process for preparing the ferric phosphate by adopting the device is shown in fig. 2, and comprises the following steps:
S1: dissolving Fe 2O3 powder in a mixing tower by using HCl solution and H 3PO4 solution in a certain proportion to form turbid liquid (raw material liquid); the molar ratio of H + to Fe 3+ in the raw material liquid is 3:1 to 7:1, a step of;
S2: filtering the raw material liquid in a filter, conveying the filtered raw material liquid to a pre-concentrator by a circulating pump, performing heat exchange between the pre-concentrator and gas in a roasting furnace at the temperature of 420-850 ℃, evaporating 25-30% of water in the raw material liquid to form concentrated liquid, atomizing the concentrated liquid by a spray gun, and then entering the roasting furnace;
S3: decomposing the concentrated solution into ferric phosphate powder and HCL vapor in a roasting furnace, wherein the reaction equation is as follows:
FeCl3+H3PO4=FePO4↓+3HCl↑
the iron phosphate powder and the hot combustion air flow are in countercurrent direction, and naturally fall to a cooling conveyor at the bottom of the furnace to reduce the temperature to below 50 ℃ in the process of outputting the iron phosphate powder; tail gas consisting of HCL gas, steam, natural gas combustion products, a small amount of ferric phosphate powder and excessive oxygen is pumped out from the furnace top and enters a pre-concentrator through a furnace gas pipeline, and a small amount of ferric phosphate powder is absorbed in the pre-concentrator;
S4: the tail gas is pumped out by an exhaust gas fan, part of HCl gas is absorbed by an absorption tower and then is cooled to below 40 ℃ by a graphite heat exchanger, the cooled tail gas is introduced into a third washing tower to wash the HCl gas in the third washing tower for the first time by using rinsing water, then is introduced into a first washing tower to wash the HCl gas again by using desalted water, finally is introduced into a second washing tower to wash the residual HCl gas by using the desalted water added with alkali solution, and the washed tail gas is discharged from a chimney;
S5: the regenerated acid formed by absorbing HCl gas by the absorption water in the absorption tower is conveyed to a hydrochloric acid preparing station, and the prepared HCl can be mixed with Fe 2O3 powder in the step S1 to prepare raw material liquid; the water condensed by the graphite heat exchanger enters a water collecting tank and flows to an absorption tower for reabsorption; the washing water of the first washing tower and the third washing tower absorbs weak acid solution formed by HCl gas in tail gas, and the weak acid solution enters an absorption tower through a plastic pump; and the washing sewage after the second washing tower absorbs HCl gas is discharged into a sewage station for treatment.
Using the above process for preparing iron phosphate, 1000g of Fe 2O3 powder produced 1887.5g of iron phosphate.
The method dissolves the high-purity Fe 2O3 powder in the mixed solution of hydrochloric acid and phosphoric acid to form turbid liquid, and burns the turbid liquid after being atomized by a double-fluid spray gun, so that the produced solid product is ferric phosphate, and the ferric phosphate powder can be directly prepared without the processes of size mixing, aging, washing, drying and the like, and the preparation process is simple. The tail gas generated by the utility model is treated by the tail gas treatment device and then discharged into the atmosphere, and the tail gas treatment device can recycle the hydrochloric acid, so that the waste gas is recycled while the discharge of the acid into the atmosphere is reduced.
The above embodiment is only one of the preferred embodiments of the present utility model, and should not be used to limit the scope of the present utility model, but all the insubstantial modifications or color changes made in the main design concept and spirit of the present utility model are still consistent with the present utility model, and all the technical problems to be solved are included in the scope of the present utility model.

Claims (7)

1. An apparatus system for preparing ferric phosphate, characterized by comprising a mixing tower (1) for preparing raw material liquid, a filter (2) capable of filtering particulate matters in the raw material liquid, a venturi type preconcentrator (3) capable of evaporating water in the raw material liquid to obtain concentrated liquid, a roasting furnace (4) capable of decomposing the concentrated liquid at high temperature, and a cooling conveyor (11) capable of cooling and conveying solid products in the roasting furnace (4), which are connected in sequence;
The roasting furnace (4) is connected with the upper end of the pre-concentrator (3) through a furnace gas pipeline (12); the preconcentrator (3) is also connected with a tail gas treatment device through a pipeline.
2. The device system for preparing ferric phosphate according to claim 1, wherein the mixing tower (1) and the filter (2) are made of glass fiber reinforced plastic, and a filter barrel wrapped by a PVDF filter screen is arranged in the filter (2); the flow rate of the conveyed materials by the cooling conveyor (11) is 0.0065m/s, the treatment capacity is 100-10000 Kg/h, the cooling area is 50-600 square meters, and the temperature of the cooled materials is 30-100 ℃.
3. The system of apparatus for preparing iron phosphate according to claim 1, characterized in that the roasting furnace (4) is in the form of a vertical cylinder comprising an upper cone and a lower cone; the shell of the roasting furnace (4) is of a steel plate welding structure, the inner side of the shell is lined with refractory acid-resistant bricks, and the outer side of the shell is wrapped with an insulating layer; a plurality of burners are arranged in the roasting furnace (4) and are arranged on the furnace body in a tangential direction; the furnace top of the roasting furnace (4) is provided with a dual-fluid atomizing spray gun made of niobium material.
4. The plant system for the preparation of iron phosphate according to claim 1, characterized in that the off-gas treatment plant comprises an off-gas fan (8) connected to the pre-concentrator (3) and capable of withdrawing off-gas, a first scrubber (9) for scrubbing HCl gas in the off-gas with desalinated water, and a second scrubber (10) for scrubbing the off-gas again with desalinated water with lye.
5. The system for preparing ferric phosphate according to claim 4, wherein an absorber (5) capable of absorbing HCl gas, a third scrubber (7) for primarily scrubbing HCl gas in the tail gas, and a graphite heat exchanger (6) capable of reducing the temperature of the tail gas to below 40 ℃ are disposed between the preconcentrator (3) and the exhaust gas blower (8).
6. The device system for preparing ferric phosphate according to claim 5, wherein the absorption tower (5) is made of FRP or PPH material; the inside of the absorption tower (5) is filled with PP structured packing, and the upper part of the absorption tower is provided with a spray head made of PTFE material; the first washing tower (9) and the second washing tower (10) are filled towers, are made of FRP or PPH materials, are internally provided with PP corrugated fillers, and are provided with spray heads made of PTFE materials; the washing water outlet of the first washing tower (9) is connected with the absorption tower (5), and the second washing tower (10) is connected with a chimney for discharging waste gas.
7. The plant system for the preparation of iron phosphate according to claim 5, characterized in that said third scrubber (7) is of the rear venturi type.
CN202322578190.2U 2023-09-21 2023-09-21 Device system for preparing ferric phosphate Active CN220788065U (en)

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CN202322578190.2U CN220788065U (en) 2023-09-21 2023-09-21 Device system for preparing ferric phosphate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202322578190.2U CN220788065U (en) 2023-09-21 2023-09-21 Device system for preparing ferric phosphate

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CN220788065U true CN220788065U (en) 2024-04-16

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