CN212356551U - Defluorination system of wet process phosphoric acid - Google Patents
Defluorination system of wet process phosphoric acid Download PDFInfo
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- CN212356551U CN212356551U CN202021469959.7U CN202021469959U CN212356551U CN 212356551 U CN212356551 U CN 212356551U CN 202021469959 U CN202021469959 U CN 202021469959U CN 212356551 U CN212356551 U CN 212356551U
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Abstract
The embodiment of the utility model provides a defluorination system of phosphoric acid by wet process belongs to phosphoric acid production technical field. The system comprises a reaction kettle, an absorption tower and a reaction tower; the reaction tower is positioned above the reaction kettle, defluorination filler is arranged in the reaction tower, a sulfuric acid spray nozzle and a reaction liquid spray nozzle are arranged in the reaction tower and above the defluorination filler, a liquid outlet at the bottom of the reaction tower is communicated with the reaction kettle, an air inlet on the reaction tower and below the defluorination filler is connected with the reaction kettle through an exhaust pipe and used for receiving tail gas of the reaction kettle, and an air outlet at the top of the reaction tower is connected with an air inlet of the absorption tower through a pipeline; the reaction liquid nozzle is connected with the reaction kettle through a pipeline and is used for spraying reaction liquid. The utility model discloses with reaction liquid and sulphuric acid mixed reaction on defluorination filler surface, make surface reaction area greatly increased, sulphuric acid and fluorine-containing reaction liquid reaction generate heat, the fluorine-containing steam of production hardly with reation kettle in the liquid contact, the high temperature vapor that reation kettle produced simultaneously also does benefit to fluorine with reaction liquid and contact against current on defluorination filler and spills over.
Description
Technical Field
The utility model belongs to the technical field of phosphoric acid production, in particular to defluorination system of phosphoric acid by wet process.
Background
Fluorine is an extremely reactive element and is known as "recalcitrant chemical". However, once combined with other elements, fluorine becomes a compound having "high safety" that is resistant to heat and difficult to be attacked by drugs and solvents, and fluorine compounds are chemically stable and fluorine has strong non-metallic properties. Fluorine only appears in the form of minerals, and the main fluorine-containing minerals in industry are fluorite and fluorapatite. Fluorite has the chemical formula of (CaF)2) Various colors, which are distributed in large quantities around the world, are the main source of fluorine; the exploitation of fluorite ore is the biggest source of global fluorine, and the reserves of the fluorite ore in China are gradually reduced due to the long-term exploitation, which means that people mustThe problem of resource shortage of fluorite ore must be considered. The resource reserve of phosphorus ore associated with fluorine in China is 13.67-16.71 times of the reserve of fluorite which has been proved in China, the quantity of the phosphorus ore mined per year reaches 5000 million tons, the associated fluorine is 150 million tons, most of the phosphorus ore is not recycled, the loss of the fluorine is far more than the total quantity of the fluorine in the fluorite demand in China in the current year, the phosphorus ore and the fluorite are non-renewable resources, and the effective utilization of the fluorine resource is a necessary choice for the sustainable development of fluorine chemical industry. The fluorine phosphorus ore is mainly used for producing phosphoric acid, a large amount of fluorine-containing gas is generated in the process of producing the phosphoric acid by using the phosphorus ore, the most common method at present is to absorb the fluorine-containing gas by using water to generate fluosilicic acid, then the fluosilicic acid is used for producing other products, and the associated fluorine resource of the phosphorus ore is recovered.
The existing defluorination process is as follows: phosphorus ore pulp and sulfuric acid react in a reaction kettle, tail gas generated by the reaction is sent to an absorption tower to recover fluorine, and spray water is usually used in the absorption tower to recover the fluorine in the form of fluosilicic acid.
The applicant has found that by adopting the method, the recovery rate of fluorine in the process of reacting the phosphorite pulp with the sulfuric acid to generate the phosphoric acid is only about 10%. Therefore, in the synthesis of phosphoric acid, we will face how to reduce the fluorine or other compounds of fluorine into phosphoric acid and phosphogypsum, and recycle a large amount of fluorine in the form of fluosilicic acid.
SUMMERY OF THE UTILITY MODEL
The embodiment of the utility model provides a defluorination system of phosphoric acid by wet process, this technology with reaction liquid and sulphuric acid earlier at defluorination filler mixed reaction on the surface, then flow into in the reation kettle and continue to react, the steam that produces and be rich in the fluoride among the reaction process sends elution defluorination as early as possible, gets the fluosilicic acid product, tail gas emission after up to standard. The technical scheme is as follows:
the embodiment of the utility model provides a defluorination system of wet-process phosphoric acid, which comprises a reaction kettle 5, an absorption tower 17 and a reaction tower 10; the reaction tower 10 is positioned above the reaction kettle 5, defluorination filler 11 is arranged in the reaction tower, a sulfuric acid spray head 18 and a reaction liquid spray head 12 are arranged in the reaction tower and above the defluorination filler 11, a liquid outlet at the bottom of the reaction tower is communicated with the reaction kettle 5, a gas inlet on the reaction tower and below the defluorination filler 11 is connected with the reaction kettle 5 through a gas exhaust pipe 1 and used for receiving tail gas of the reaction kettle 5, and a gas outlet at the top of the reaction tower is connected with a gas inlet of an absorption tower 17 through a pipeline; the sulfuric acid spray head 18 is connected with the sulfuric acid storage tank 15 through a pipeline and used for spraying sulfuric acid, and the reaction liquid spray head 12 is connected with the reaction kettle 5 through a pipeline and used for spraying reaction liquid.
Wherein, the embodiment of the utility model provides an in the gas vent that takes off 5 tops of reation kettle pass through blast pipe 1 and be connected with reaction tower 10 lower part lateral wall, be equipped with agitator 8 in it, its bottom is equipped with phosphoric acid discharge gate 6, and it is connected with reaction liquid shower nozzle 12 through taking reaction liquid conveying pipeline 7 of pump 9.
Wherein, the embodiment of the utility model provides an in take off absorption tower 17 intussuseption and be filled with absorption filler 16, its upper portion just is located the absorption filler 16 top and is equipped with lotion shower nozzle 19, and its lower part just is located the air inlet that absorbs the filler 16 below and is connected with the gas vent of reaction tower 10 through the pipeline that has fan 13, and its top is equipped with the tail gas export, and its bottom is equipped with fluorine recovery liquid export 4.
Wherein, the embodiment of the utility model provides an in take off reaction tower 10 and be located reation kettle 5 directly over, its liquid outlet lets in reation kettle 5 in and to the reaction liquid level top through back flow 2, the flow of back flow 2 is greater than the volume of spraying of reaction liquid shower nozzle 12 and the volume sum that sprays of sulphuric acid shower nozzle 18.
Specifically, the volume of the reaction tower 10 in the embodiment of the utility model is 0.5-2.0 times of the volume of the reaction kettle 5, and the height of the filler in the reaction tower is 3-10 m; the defluorination filling material 11 is formed by piling acid-proof bricks or plates with the side length of 100-.
The embodiment of the utility model provides a beneficial effect that technical scheme brought is: the embodiment of the utility model provides a defluorination system of wet-process phosphoric acid; in the production process, if sulfuric acid is directly injected into the bottom of the reaction kettle, the escape of fluorine is almost zero; this is because the sulfuric acid is locally overheated at the bottom of the kettle, and the generated steam dissolves fluoride in the reaction liquid during the rising process. If sulfuric acid is dripped on the liquid surface of the reaction kettle, the recovery rate of fluorine can reach 10 percent; this is due to the local superheating of the reaction at the liquid surface, the steam generated being rapidly removed from the liquid surface, wherein the fluoride has not yet dissolved in the liquid and is carried away from the liquid surface by the steam. The utility model mixes the reaction liquid and the sulfuric acid on the surface of the defluorination filler to greatly increase the surface reaction area, the sulfuric acid reacts with the fluorine-containing reaction liquid to generate heat, the generated fluorine-containing steam hardly contacts with the liquid in the reaction kettle, and meanwhile, the high-temperature steam generated by the reaction kettle contacts with the reaction liquid on the defluorination filler in a countercurrent way (the reaction liquid is dispersed and contacts with the rising high-temperature air flow) to facilitate the overflow of the fluorine; the rising air flow rapidly conveys fluorine overflowing from the defluorination filler and fluorine generated on the surface of the defluorination filler due to the local high temperature of the sulfuric acid reaction to an absorption tower for recovery, and in addition, a fan can make the interior of the system be negative pressure and is also beneficial to the removal of the fluorine; in a word, the whole process greatly improves the recovery rate of fluorine, which can reach more than 18 percent and can be improved by more than 80 percent.
Drawings
Fig. 1 is a schematic structural diagram of a defluorination system for wet-process phosphoric acid provided by an embodiment of the present invention.
In the figure: 1 exhaust pipe, 2 return pipe, 3 fluosilicic acid storage tank, 4 fluorine recovery liquid outlet, 5 reaction kettle, 6 phosphoric acid discharge port, 7 reaction liquid conveying pipeline, 8 stirrer, 9 pump, 10 reaction tower, 11 defluorination filler, 12 reaction liquid spray head, 13 blower, 14 control valve, 15 sulfuric acid storage tank, 16 absorption filler, 17 absorption tower, 18 sulfuric acid spray head and 19 washing liquid spray head.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the present invention will be described in further detail with reference to the accompanying drawings.
Example 1
Referring to fig. 1, example 1 provides a defluorination system of wet-process phosphoric acid, which comprises a reaction kettle 5, an absorption tower 17 and the like, wherein the reaction kettle 5 is used for reacting sulfuric acid with phosphate slurry to obtain phosphoric acid, the absorption tower 17 is used for treating tail gas generated in the reaction with water or alkali (preferably water) to obtain a fluorine recovery liquid (such as fluosilicic acid), and the structure is basically the same as that of the defluorination system of the existing wet-process phosphoric acid, except that: the defluorination system of this embodiment also includes a reaction column 10 for facilitating fluorine recovery. Wherein, the reaction tower 10 is located above the reaction kettle 5, and comprises a conventional tower structure, wherein defluorination filler 11 is arranged in the middle (middle part) of the tower, sulfuric acid spray nozzles 18 (at least one is arranged in the upper part of the tower and above the defluorination filler 11, so as to uniformly spray on the defluorination filler 11) and reaction liquid spray nozzles 12 (at least one is arranged as required, so as to uniformly spray on the defluorination filler 11), a liquid outlet at the bottom of the tower is communicated with the reaction kettle 5 (through a return pipe 2), an air inlet at the upper part (lower part) of the tower and below the defluorination filler 11 is connected with the reaction kettle 5 (top) through an exhaust pipe and used for receiving tail gas of the reaction kettle 5, and an air outlet at the top of the tower is connected with an air inlet of an absorption tower 17 (lower part) through. The sulfuric acid spray head 18 is connected to the sulfuric acid storage tank 15 for spraying sulfuric acid through a pipeline (a pump or/and a valve is provided as required, the sulfuric acid storage tank 15 in this embodiment is a high-level tank which is provided above the reaction tower 10 and is connected to the sulfuric acid spray head 18 through a pipeline with a control valve 14). The reaction liquid nozzle 12 is connected to the reaction kettle 5 through a pipeline (reaction liquid delivery pipeline 7) for spraying the reaction liquid.
Referring to fig. 1, the gas outlet at the top of the reactor 5 in the embodiment of the present invention is connected to the lower side wall (required to be located above the liquid level in the reactor 10) of the reactor 10 through a gas outlet pipe 1, and a stirrer 8 is provided therein, and the bottom of the gas outlet is provided with a phosphoric acid outlet 6 (output to a filter or a next-stage reactor (without a reactor)), which is connected to a reaction liquid nozzle 12 through a reaction liquid delivery pipe 7 with a pump 9.
Wherein, referring to fig. 1, the absorption tower 17 in the embodiment of the present invention is of a conventional structure, the absorption filler 16 (conventional filler for fluorine absorption, smaller than the defluorination filler 11) is filled in the absorption tower 17, the washing liquid nozzle 19 is disposed above the absorption filler 16 at the upper part of the absorption tower, the air inlet below the absorption filler 16 at the lower part of the absorption tower is connected with the exhaust port of the reaction tower 10 through the pipeline with the fan 13 (which simultaneously makes the whole system in negative pressure, beneficial to the removal of fluorine), the top of the absorption tower is provided with a tail gas outlet (evacuation or further processing), and the bottom of the absorption tower is provided with a fluorine recovery liquid outlet 4 (outputting to the fluosilicic acid storage tank.
Wherein, referring to fig. 1, the reaction tower 10 of the embodiment of the present invention is located directly above the reaction kettle 5, the liquid outlet of the reaction tower is introduced into the reaction kettle 5 through the return pipe 2 (specifically, it may be a vertical straight pipe, and it passes through the top of the reaction kettle 5 downward) and to the top of the reaction liquid level (the liquid of the return flow also benefits the fluorine overflow in the reaction liquid surface reaction), and the flow of the return pipe 2 is greater than the sum of the spraying amount of the reaction liquid nozzle 12 and the spraying amount of the sulfuric acid nozzle 18 to avoid the liquid gathering at the bottom of the reaction tower 10.
Specifically, the volume of the reaction tower 10 in the embodiment of the present invention is 0.5-2.0 times of the volume of the reaction kettle 5, and the height of the packing therein is 3-10 m. The defluorination filling material 11 is formed by piling acid-proof bricks or plates with the side length of 100-.
And the pipelines between the structures are provided with structures such as a fan, a pump, a valve and/or a flowmeter according to needs.
Example 2
Further, referring to fig. 1, in the embodiment of the present invention, a reaction liquid nozzle 12 and a sulfuric acid nozzle 18 are disposed at the upper portion of the reaction tower 10 above the defluorination packing 11 for spraying the reaction liquid and the sulfuric acid respectively, the exhaust gas generated by the reaction kettle 5 is sent to the air inlet at the lower portion (side wall) of the reaction tower 10 through the exhaust pipe 1 from the exhaust port at the top of the reaction tower, the reaction liquid after defluorination is sent to the reaction liquid level top of the reaction kettle 5 from the liquid outlet at the bottom of the reaction tower 10 (through the return pipe 2), and the exhaust gas of the reaction tower 10 is discharged to the absorption tower 17 from the exhaust port at the top of the reaction.
Specifically, the spraying amount of the reaction liquid nozzle 12 in the embodiment of the present invention is 0.5 to 2.0 times of the spraying amount of the sulfuric acid nozzle 18.
Wherein, the defluorination filling material 11 in the embodiment of the utility model is formed by piling acid-proof bricks or plates with the side length of 100-.
Wherein, referring to fig. 1, the absorption tower 17 in the embodiment of the present invention is filled with an absorption filler 16, the tail gas discharged from the reaction tower 10 is sent to the absorption tower 17 through a pipeline with a fan 13 and is located below the absorption filler 16, a washing liquid spray nozzle 19 (input water) is arranged in the absorption tower 17 and above the absorption filler 16, the washing liquid and the gas are in countercurrent contact on the absorption filler 16, and the fluosilicic acid is obtained at the bottom of the absorption tower 17. The fluorine recovery rate is calculated to reach more than 18 percent.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention, and any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention should be included within the protection scope of the present invention.
Claims (5)
1. A defluorination system of wet-process phosphoric acid, which comprises a reaction kettle (5) and an absorption tower (17); the device is characterized by also comprising a reaction tower (10); the reaction tower (10) is positioned above the reaction kettle (5), defluorination filler (11) is arranged in the reaction tower, a sulfuric acid spray head (18) and a reaction liquid spray head (12) are arranged in the reaction tower and above the defluorination filler (11), a liquid outlet at the bottom of the reaction tower is communicated with the reaction kettle (5), a gas inlet on the reaction tower and below the defluorination filler (11) is connected with the reaction kettle (5) through a gas exhaust pipe (1) and used for receiving tail gas of the reaction kettle (5), and a gas outlet at the top of the reaction tower is connected with a gas inlet of an absorption tower (17) through a pipeline; the sulfuric acid spray head (18) is connected with the sulfuric acid storage tank (15) through a pipeline and used for spraying sulfuric acid, and the reaction liquid spray head (12) is connected with the reaction kettle (5) through a pipeline and used for spraying reaction liquid.
2. The defluorination system of wet process phosphoric acid according to claim 1, wherein the exhaust port at the top of the reaction kettle (5) is connected with the lower side wall of the reaction tower (10) through an exhaust pipe (1), a stirrer (8) is arranged in the exhaust port, a phosphoric acid discharge port (6) is arranged at the bottom of the reaction kettle, and the exhaust port is connected with a reaction liquid spray head (12) through a reaction liquid conveying pipeline (7) with a pump (9).
3. The defluorination system of wet process phosphoric acid according to claim 2, characterized in that said absorption tower (17) is filled with absorption packing (16), a washing liquid spray nozzle (19) is arranged at the upper part of the absorption tower (17) and above the absorption packing (16), the air inlet at the lower part and below the absorption packing (16) is connected with the exhaust port of the reaction tower (10) through a pipeline with a fan (13), the top of the absorption tower is provided with a tail gas outlet, and the bottom of the absorption tower is provided with a fluorine recovery liquid outlet (4).
4. The defluorination system of wet-process phosphoric acid according to claim 2, wherein said reaction tower (10) is located right above the reaction kettle (5), the liquid outlet of the reaction tower is communicated into the reaction kettle (5) through the return pipe (2) and is above the reaction liquid level, the flow rate of the return pipe (2) is larger than the sum of the spraying amount of the reaction liquid nozzle (12) and the spraying amount of the sulfuric acid nozzle (18).
5. The defluorination system of wet-process phosphoric acid according to claim 1, wherein the volume of said reaction tower (10) is 0.5-2.0 times of the volume of the reaction kettle (5), and the height of the packing therein is 3-10 m; the defluorination filling material (11) is formed by piling acid-proof bricks or plates with the side length of 100-1000mm according to the requirement that the included angle between the acid-proof bricks or plates and the vertical direction is less than 10 degrees and the block distance or the plate distance is 80-150 mm.
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| CN202021469959.7U CN212356551U (en) | 2020-07-23 | 2020-07-23 | Defluorination system of wet process phosphoric acid |
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| CN202021469959.7U CN212356551U (en) | 2020-07-23 | 2020-07-23 | Defluorination system of wet process phosphoric acid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111874884A (en) * | 2020-07-23 | 2020-11-03 | 湖北祥云(集团)化工股份有限公司 | Defluorination method and system for wet-process phosphoric acid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111874884A (en) * | 2020-07-23 | 2020-11-03 | 湖北祥云(集团)化工股份有限公司 | Defluorination method and system for wet-process phosphoric acid |
| CN111874884B (en) * | 2020-07-23 | 2023-08-04 | 湖北祥云(集团)化工股份有限公司 | Defluorination method and system for wet-process phosphoric acid |
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