CN212758536U - Preparation facilities of ferrous liquid for ferric phosphate - Google Patents

Preparation facilities of ferrous liquid for ferric phosphate Download PDF

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Publication number
CN212758536U
CN212758536U CN202021227116.6U CN202021227116U CN212758536U CN 212758536 U CN212758536 U CN 212758536U CN 202021227116 U CN202021227116 U CN 202021227116U CN 212758536 U CN212758536 U CN 212758536U
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liquid
iron
solid
reaction tower
port
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CN202021227116.6U
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柯君雄
王镖
王红强
崔振庭
刘伟
张洪星
张吉晔
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Cangzhou Caike Lithium Energy Co ltd
Shandong Caike New Material Co ltd
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Hebei Caike Chemical Co ltd
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Abstract

The utility model provides a preparation facilities of ferrous liquid for ferric phosphate is including the solid-liquid reaction tower and the reation kettle that the series connection set up, the solid-liquid reaction tower includes the iron fixed area, add the iron notch, the liquid overflow mouth, gas collection mouth and inlet, the iron fixed area sets up in the solid-liquid reaction tower main part, it sets up on the solid-liquid reaction tower lateral wall to add the iron notch, the liquid overflow mouth sets up in solid-liquid reaction tower upper end, be higher than iron fixed area top, gas collection mouth and inlet set up respectively on the top and the bottom of solid-liquid reaction tower, reation kettle includes the liquid backward flow mouth, add sour mouth and liquid outlet, liquid overflow mouth and liquid backward flow mouth intercommunication, the liquid outlet communicates with the inlet through first pipeline, set up first ooff valve and first flow pump on the pipeline. The utility model discloses can directly add the scrap iron piece of solid-state bulky in the reation kettle with phosphoric acid reaction, the reaction liquid flows at reaction tower and reation kettle inner loop, reaches the oxidation reaction of discharging behind the concentration requirement and obtains the iron phosphate, and reaction efficiency is high.

Description

Preparation facilities of ferrous liquid for ferric phosphate
Technical Field
The utility model relates to a preparation facilities of ferrous liquid for iron phosphate belongs to chemical industry technical field.
Background
The iron phosphate serving as the lithium battery positive electrode material has the advantages of stable structure, good cycle performance, low cost and the like. At present, iron phosphate is prepared by reacting iron salt with phosphate, the iron needs to be prepared into the iron salt firstly, the process is complex, the cost is high, various reagents are needed, and a large amount of wastewater and waste gas are generated in the process. Or after the ferrous iron liquid is prepared from an iron source, the ferrous iron liquid is subjected to operations such as oxidation and crystal transformation to prepare the iron phosphate, the preparation efficiency of the ferrous iron liquid directly influences the preparation efficiency of the iron phosphate, and the uniformity of the concentration of the ferrous iron liquid influences the quality of subsequent iron phosphate.
SUMMERY OF THE UTILITY MODEL
The utility model discloses an overcome prior art drawback, provide a preparation facilities of ferrous liquid for iron phosphate, can with the reaction with phosphoric acid in the solid-state bulky scrap iron piece direct addition reation kettle, practice thrift the cost, the ferrous liquid of reaction flows at reaction tower and reation kettle inner loop, and the further oxidation reaction of discharging obtains the iron phosphate after reaching the concentration requirement, and reaction efficiency is high.
The utility model provides a technical scheme that its technical problem adopted is:
a preparation device of ferrous liquid for ferric phosphate comprises a solid-liquid reaction tower and a reaction kettle which are arranged in series, wherein the solid-liquid reaction tower comprises an iron fixing area, an iron adding port, a liquid overflow port, a gas collecting port and a liquid inlet, the iron fixing area is arranged at an intermediate position in a main body of the solid-liquid reaction tower, the iron adding port is arranged on a side wall of the solid-liquid reaction tower, the liquid overflow port is arranged at the upper end of the solid-liquid reaction tower and higher than the top end of the iron fixing area, the gas collecting port and the liquid inlet are respectively arranged at the top end and the bottom end of the solid-liquid reaction tower, the top end of the reaction kettle is provided with a liquid reflux port and an acid adding port, the bottom end of the reaction kettle is provided with a liquid outlet, the liquid overflow port is communicated with the liquid inlet through a first pipeline, a first switch valve and a first flow pump are arranged on the pipeline of the reaction kettle, the liquid outlet is connected with, and a second switching valve and a second flow pump are arranged on the second pipeline.
Above-mentioned preparation facilities of ferrous liquid for iron phosphate, the mouth of adding iron of solid-liquid reaction tower still is provided with leads to the nitrogen pipe, lead to the nitrogen pipe with add the iron mouth intercommunication.
According to the device for preparing the ferrous liquid for the iron phosphate, the monitoring sight glass is fixedly arranged at the lower part of the iron fixing area.
According to the device for preparing the ferrous liquid for the iron phosphate, the bottom of the iron fixing area is provided with the quick cleaning opening.
According to the device for preparing the ferrous liquid for the iron phosphate, the main pipeline communicated with the gas collecting port is provided with the third switch valve, and the hydrogen recovery pipeline communicated with the main pipeline is provided with the fourth switch valve.
The utility model has the advantages that:
the utility model adopts the series connection mode of the solid-liquid reaction tower and the reaction kettle, the iron sheet with fixed quantity is added in the solid-liquid reaction tower, the phosphoric acid with fixed quantity and certain concentration is added in the reaction kettle, the phosphoric acid flows circularly from the reaction kettle to the solid-liquid reaction tower and continuously reacts with the iron sheet in the solid-liquid reaction tower until the concentration of the ferrous iron liquid in the reaction kettle reaches the production requirement, the ferrous iron liquid is input into the next procedure, the reaction of the iron sheet is thorough, the residue is less, the concentration of the ferrous iron liquid is controllable, the reaction can be continuously carried out, and the production efficiency is high; introducing nitrogen at the first iron adding port simultaneously, replacing oxygen in the reaction kettle by using the nitrogen, and forming nitrogen seal at the iron adding port by using the nitrogen to prevent hydrogen generated in the reaction kettle from overflowing from the iron adding port; the sight glass is arranged in the iron fixing area, and the residual amount of iron sheets in the solid-liquid reaction tower is monitored through the sight glass, so that iron can be supplemented conveniently and timely; the quick cleaning port can discharge the reaction residue in time.
Drawings
The present invention will be further explained with reference to the accompanying drawings.
FIG. 1 is a schematic view of the overall structure of the reaction system of the present invention;
in the figure: 1. a solid-liquid reaction tower; 1-1, iron fixation area; 1-2, adding an iron notch; 1-3, a liquid overflow port; 1-4, a gas collection port; 1-5, liquid inlet; 1-6, introducing a nitrogen pipe; 1-7, a sight glass; 1-8, quickly cleaning mouth; 1-9, a third switch valve; 1-10, a fourth switch valve; 2. a reaction kettle; 2-1, a liquid reflux port; 2-2, adding an acid port; 2-3, a liquid outlet; 2-4, a first switch valve; 2-5, a first flow pump; 2-6, a second switch valve; 2-7 and a second flow pump.
Detailed Description
The present invention will be further described with reference to the following examples.
Referring to fig. 1, the device for preparing ferrous iron liquid for iron phosphate of the present invention comprises a solid-liquid reaction tower 1 and a reaction kettle 2 which are connected in series, wherein the solid-liquid reaction tower 1 comprises an iron fixing area 1-1, an iron adding port 1-2, a liquid overflow port 1-3, a gas collecting port 1-4 and a liquid inlet 1-5, the top end of the reaction kettle 2 is provided with a liquid reflux port 2-1 and an acid adding port 2-2, the bottom end is provided with a liquid outlet 2-3, the liquid overflow port 1-3 is communicated with the liquid reflux port 2-1 through a pipeline, the liquid inlet 1-5 is communicated with the liquid outlet 2-3 through a first pipeline, the first pipeline is provided with a first switch valve 2-4 and a first flow pump 2-5, the amount of liquid in the reaction kettle flowing back to the solid-liquid reaction tower is controlled by the first flow pump, the iron fixing area 1-1 is arranged in the main body of the solid-liquid reaction tower 1 and is a certain distance away from the bottom of the solid-liquid reaction tower, the iron adding port is arranged on the side wall of the solid-liquid reaction tower, the liquid overflow port 1-3 is arranged at the upper end of the solid-liquid reaction tower 1 and is higher than the top end of the iron fixing area 1-1, the gas collecting port 1-4 and the liquid inlet 1-5 are respectively arranged at the top end and the bottom end of the solid-liquid reaction tower 1, the liquid outlet 2-3 is connected with a subsequent reactor through a second pipeline, and the second pipeline is provided with a second switch valve 2-6 and a second flow pump 2-7. The main pipeline communicated with the gas collecting openings 1-4 is provided with third switch valves 1-9 and an oxygen detector 1-11, the hydrogen recovery pipeline communicated with the main pipeline is provided with fourth switch valves 1-10, when the oxygen content of hydrogen generated in the solid-liquid reaction tower is detected to be lower than 0.5% through the oxygen detector 1-11, the hydrogen is recovered and reused through the hydrogen recovery pipeline, and when the oxygen content is higher than 0.5%, the fourth switch valve is opened to be directly emptied.
The iron adding port 1-2 is also provided with a nitrogen introducing pipe 1-6, the nitrogen introducing pipe 1-6 is communicated with the iron adding port 1-2, oxygen in the solid-liquid reaction tower is replaced by introducing nitrogen, and nitrogen seal is formed at the iron adding port by the nitrogen, so that hydrogen generated in the reaction tower is prevented from overflowing from the iron adding port. The lower part of the iron fixing area 1-1 is fixedly provided with a sight glass 1-7, so that the residual condition of iron sheets in the solid-liquid reaction tower can be conveniently monitored, and iron can be supplemented in time; and a quick cleaning opening 1-8 is also formed in the bottom of the iron fixing area 1-1, and impurity residues left in the solid-liquid reaction tower during reaction are timely removed through the quick cleaning opening.
The reaction preparation process comprises the following steps: adding a certain amount of iron sheets into an iron fixing area of a solid-liquid reaction tower 1 through an iron adding port, adding a certain amount of phosphoric acid with a certain concentration into a reaction kettle 2, opening a first switch valve 2-4, enabling the phosphoric acid in the reaction kettle 2 to flow out from a liquid outlet 2-3, pumping the phosphoric acid into the solid-liquid reaction tower 1 through a first flow pump 2-5 from a liquid inlet 1-5, reacting with the iron sheets in the iron fixing area 1-1, enabling the phosphoric acid to enter the solid-liquid reaction tower along with the reaction, enabling the reaction to be continuously carried out, gradually raising the liquid level in the solid-liquid reaction tower to a liquid overflow port 1-3, enabling the liquid to flow into a liquid reflux port at the upper end of the reaction kettle 2 from the liquid overflow port and enter the reaction kettle 2, enabling the liquid to circulate from the reaction kettle 2 to the solid-liquid reaction tower 1, opening a second switch valve 2-6 after the concentration of ferrous liquid in the reaction kettle reaches a required concentration, inputting the ferrous liquid into, finally, the iron phosphate is prepared.

Claims (5)

1. The utility model provides a preparation facilities of ferrous liquid for ferric phosphate which characterized in that: the device comprises a solid-liquid reaction tower (1) and a reaction kettle (2) which are arranged in series, wherein the solid-liquid reaction tower (1) comprises an iron fixing area (1-1), an iron adding port (1-2), a liquid overflow port (1-3), a gas collecting port (1-4) and a liquid inlet (1-5), the iron fixing area (1-1) is arranged in a main body of the solid-liquid reaction tower (1), the iron adding port is arranged on the side wall of the solid-liquid reaction tower, the liquid overflow port (1-3) is arranged at the upper end of the solid-liquid reaction tower (1) and is higher than the top end of the iron fixing area (1-1), the gas collecting port (1-4) and the liquid inlet (1-5) are respectively arranged at the top end and the bottom end of the solid-liquid reaction tower (1), the top end of the reaction kettle (2) is provided with a liquid reflux port (2-1) and an acid adding port (2-2), the bottom sets up liquid outlet (2-3), liquid overflow mouth (1-3) with liquid backward flow mouth (2-1) intercommunication, the liquid outlet through first pipeline with inlet (1-5) intercommunication, set up first ooff valve (2-4) and first flow pump (2-5) on its pipeline, liquid outlet (2-3) are connected with oxidation reactor (3) through the second pipeline, set up second ooff valve (2-6) and second flow pump (2-7) on the second pipeline.
2. The apparatus for producing a ferrous liquid for iron phosphate according to claim 1, characterized in that: the iron adding port (1-2) of the solid-liquid reaction tower (1) is also provided with a nitrogen introducing pipe (1-6), and the nitrogen introducing pipe (1-6) is communicated with the iron adding port (1-2).
3. The apparatus for producing a ferrous liquid for iron phosphate according to claim 2, characterized in that: and a sight glass (1-7) is fixedly arranged at the lower part of the iron fixing area (1-1).
4. The apparatus for producing ferrous iron phosphate liquid according to claim 3, characterized in that: the bottom of the iron fixing area (1-1) is provided with a quick cleaning opening (1-8).
5. The apparatus for producing a ferrous liquid for iron phosphate according to claim 4, characterized in that: the gas collecting device is characterized in that a third switch valve (1-9) is arranged on a main pipeline communicated with the gas collecting ports (1-4), a fourth switch valve (1-10) is arranged on a hydrogen recovery pipeline communicated with the main pipeline, and an oxygen detector (1-11) is arranged on the main pipeline.
CN202021227116.6U 2020-06-29 2020-06-29 Preparation facilities of ferrous liquid for ferric phosphate Active CN212758536U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202021227116.6U CN212758536U (en) 2020-06-29 2020-06-29 Preparation facilities of ferrous liquid for ferric phosphate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202021227116.6U CN212758536U (en) 2020-06-29 2020-06-29 Preparation facilities of ferrous liquid for ferric phosphate

Publications (1)

Publication Number Publication Date
CN212758536U true CN212758536U (en) 2021-03-23

Family

ID=75087315

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202021227116.6U Active CN212758536U (en) 2020-06-29 2020-06-29 Preparation facilities of ferrous liquid for ferric phosphate

Country Status (1)

Country Link
CN (1) CN212758536U (en)

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Effective date of registration: 20221212

Address after: 257000 Hekou Blue Economic Development Zone, Dongying City, Shandong Province (east of caoqiaogou and south of Mingyuan Road)

Patentee after: Shandong caike New Material Co.,Ltd.

Patentee after: Cangzhou Caike New Energy Co.,Ltd.

Address before: 061600 east side of national highway 105, Dazhang village, Dongguang County, Cangzhou City, Hebei Province

Patentee before: HEBEI CAIKE CHEMICAL Co.,Ltd.

TR01 Transfer of patent right
CP01 Change in the name or title of a patent holder

Address after: 257000 Hekou Blue Economic Development Zone, Dongying City, Shandong Province (east of caoqiaogou and south of Mingyuan Road)

Patentee after: Shandong caike New Material Co.,Ltd.

Patentee after: Cangzhou Caike Lithium Energy Co.,Ltd.

Address before: 257000 Hekou Blue Economic Development Zone, Dongying City, Shandong Province (east of caoqiaogou and south of Mingyuan Road)

Patentee before: Shandong caike New Material Co.,Ltd.

Patentee before: Cangzhou Caike New Energy Co.,Ltd.

CP01 Change in the name or title of a patent holder