CN112174104B - High-temperature stripping defluorination method and device for wet-process phosphoric acid - Google Patents
High-temperature stripping defluorination method and device for wet-process phosphoric acid Download PDFInfo
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Abstract
The invention discloses a high-temperature stripping defluorination method and a device thereof for wet-process phosphoric acid, relating to the technical field of wet-process phosphoric acid defluorination. The method comprises the steps of firstly removing heavy metals from raw material phosphoric acid, then clarifying and filter-pressing to remove solid impurities in the phosphoric acid, and obtaining clarified concentrated phosphoric acid with low solid content; uniformly mixing a defluorinating agent and clarified concentrated phosphoric acid, heating the mixture to 70-90 ℃, pumping the phosphoric acid into a defluorinating tower through a pump for steam stripping defluorination, keeping phosphoric acid in a liquid storage tank at the lower part of the defluorinating tower in a boiling state, and recovering fluorine-containing gas through water washing to obtain a phosphorus-fluorine ratio P2O5A low fluorine content defluorinated phosphoric acid with a F of 380 or more. Under the boiling state of phosphoric acid, the escape efficiency of the gas containing fluorine in the phosphoric acid can be improved, the fluorine content in the acid can be effectively reduced, and the defluorination efficiency and the yield of defluorinated phosphoric acid are improved. The defluorinated phosphoric acid produced by the method has good quality and high yield, and can be directly used for producing feed-grade calcium phosphate salt and also can be applied to the field with higher requirements on the quality of phosphoric acid.
Description
Technical Field
The invention relates to the technical field of wet-process phosphoric acid defluorination, in particular to a high-temperature stripping defluorination method and a device thereof for wet-process phosphoric acid.
Background
Since the 50 s in the 20 th century, the world countries use wet-process phosphoric acid as a raw material to produce calcium phosphate as a feed additive, wherein the feed-grade calcium phosphate mainly comprises DCP (calcium hydrogen phosphate), MCP (monocalcium phosphate) and MDCP (calcium monohydrogen phosphate).
The source of phosphorus in feed-grade calcium hydrophosphate is mainly wet-process phosphoric acid, and the key technology for producing feed phosphate by adopting the wet-process phosphoric acid is the purification of the wet-process phosphoric acid, namely, the fluorine content and the content of other impurities in the wet-process phosphoric acid reach the requirement of producing the feed-grade phosphate through purification. The quality of the defluorination technology directly affects the yield and quality of the final product.
The technology of wet phosphoric acid defluorination mainly comprises two technologies: chemical precipitation and gas stripping defluorination. The chemical precipitation method is based on the principle that sodium salt or potassium salt is added to convert fluosilicic acid in phosphoric acid into sodium fluosilicate or potassium fluosilicate precipitate, so as to achieve the aim of defluorination. But the defluorination efficiency is not high, lime milk is required to be added for secondary precipitation defluorination, the process operation is more complicated, and the phosphorus loss is larger. The principle of the gas stripping defluorination method is to add active SiO into phosphoric acid2After phosphoric acid is heated by a heat medium, HF and H in the acid2SiF6With SiO2Conversion by reaction to SiF4Escape, thereby achieving the aim of defluorination. The gas stripping defluorination method is divided into a groove type defluorination process and a tower type defluorination process according to different phosphoric acid heating modes.
The principle of the groove type defluorination process is to add active SiO into the concentrated phosphoric acid2Blowing hot air, HF and H in acid into storage tank filled with concentrated phosphoric acid2SiF6In SiF at about 80 ℃4Air is blown in to escape from the acid. The phosphoric acid is a continuous phase, the air is a dispersed phase, the phosphoric acid is not fully contacted with the air, and the defluorination effect is poor. And the defects of high equipment investment and high energy consumption exist, and the current industrial application is less.
The principle of the tower defluorination process is that concentrated phosphoric acid and active SiO2Mixing the raw materials in proportion, circularly heating by an acid heater, spraying into an empty tower, introducing normal temperature air into the bottom of the empty tower to make concentrated acid liquidThe drops are in countercurrent contact with normal temperature air to remove HF and H in acid2SiF6With SiF4The morphology of (2) escapes. The tower defluorination process features that the continuous phase is air and the dispersed phase is phosphoric acid capable of contacting with air fully. Therefore, the defluorination effect is better than that of the slot type defluorination, and the defluorination effect is more used in industrial production. However, the tower-type defluorination process has the disadvantages of high control temperature, high requirement on equipment material, and easy leakage and shutdown caused by corrosion problems in the operation process of the equipment. Meanwhile, the tower-type defluorination process has high requirements on the quality of the raw material phosphoric acid, the defluorination efficiency is low, the device productivity is low, and the production requirements of large-scale calcium feeding devices cannot be met.
Patent CN1196332A discloses a high-temperature hydrolysis defluorination method and device for producing feed-grade calcium hydrophosphate by wet-process phosphoric acid, wherein a pure high-temperature defluorination method is disclosed, which uses heat-conducting oil as a heating medium to indirectly heat phosphoric acid, simultaneously introduces overheated or saturated steam into phosphoric acid for bubbling, and then takes away fluorine-containing gas by dry hot air, and the temperature of an acid medium is 120-125 ℃. The phosphoric acid product obtained by the method has high heavy metal and solid contents, and the fluorine content is high after one-time defluorination, so that the production efficiency is low if multiple defluorination is required for production of feed-grade calcium phosphate.
Disclosure of Invention
The invention aims to provide a high-temperature stripping defluorination method and a device thereof for wet-process phosphoric acid, which solve the problems of low efficiency and low productivity and high requirement on equipment of the existing defluorination process.
In order to solve the technical problems, the invention adopts the following technical scheme: the high-temperature stripping defluorination method of wet-process phosphoric acid is characterized by comprising the following steps:
(1) carrying out heavy metal removal treatment on raw material phosphoric acid, and then clarifying and filter-pressing to remove solid impurities in the phosphoric acid to obtain clarified concentrated phosphoric acid with low solid content;
(2) uniformly mixing a defluorinating agent and clarified concentrated phosphoric acid, heating the mixture to 70-90 ℃, pumping the phosphoric acid into a defluorinating tower through a pump for steam stripping defluorination, keeping phosphoric acid in a liquid storage tank at the lower part of the defluorinating tower in a boiling state, and recovering fluorine-containing gas through water washing to obtain phosphorus and fluorineRatio P2O5Defluorinated phosphoric acid with low fluorine content and over 380F.
The further technical proposal is that the solid content of the raw material phosphoric acid in the step (1) is less than or equal to 0.4 percent, and P is2O5The concentration is 41-50%.
The further technical proposal is that the defluorinating agent in the step (2) is white carbon black or active SiO2The addition amount of the defluorinating agent is 1.0-1.5 times of the theoretical dosage, and the mass concentration of the defluorinating agent slurry is 8-20%.
A further technical scheme is that the phosphoric acid heating mode in the step (2) is indirect heating, a tube type or coil heat exchanger is adopted to heat phosphoric acid, and a heating medium is low-pressure steam or heat conducting oil.
The further technical proposal is that the boiling state temperature in the step (2) is controlled to be 120-150 ℃.
A further technical scheme is that the defluorination tower in the step (2) is a hollow cavity, and the side wall of the defluorination tower is sequentially provided with a raw material phosphoric acid inlet, a steam inlet and a finished product acid outlet from top to bottom, wherein the raw material phosphoric acid inlet is connected with a phosphoric acid spray head which is uniformly distributed in the tower body; the steam inlet is connected with a steam spray pipe, the steam spray pipe is arranged in the tower body, and the top of the tower body is provided with an exhaust port.
The further technical scheme is that more than three steam inlets are arranged in parallel, and the number of the steam spray pipes is consistent with that of the steam inlets.
The further technical scheme is that the bottom of the defluorination tower is obliquely arranged, and the inclination angle is 3-8 degrees.
The reaction mechanism is as follows: the main reactions in the defluorination process are as follows:
6HF+SiO2→H2SiF6+2H2O
H2SiF6→SiF4↓ +2HF ↓ (heating)
2H2SiF6+SiO2→3SiF4↑+2H2O
Compared with the prior art, the invention has the beneficial effects that: clarifying and purifying phosphoric acid by removing heavy substances and filter pressing, and adding into a reactorThe fluorinating agents are mixed and preheated by an indirect heating mode, preheated phosphoric acid is pumped into a defluorination tower and sprayed out from a spray head, one part of phosphoric acid is in countercurrent with steam at the lower part to realize steam stripping defluorination, the other part of phosphoric acid is stored at the bottom of the defluorination tower and is kept in a boiling state by steam heating, the temperature is controlled at 120-150 ℃, defluorination and purification are realized, and the phosphorus-fluorine ratio (P) is obtained2O5/F) defluorinated phosphoric acids above 380. Under the boiling state of phosphoric acid, the escape efficiency of the gas containing fluorine in the phosphoric acid can be improved, the fluorine content in the acid can be effectively reduced, and the defluorination efficiency and the yield of defluorinated phosphoric acid are improved. The defluorinated phosphoric acid produced by the method has good quality and high yield, and can be directly used for producing feed-grade calcium phosphate salt and also can be applied to the field with higher requirements on the quality of phosphoric acid.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is a schematic view of the structure of the defluorination column of the present invention.
In the figure, 1-defluorination tower, 2-raw material phosphoric acid inlet, 3-steam inlet, 4-finished acid outlet, 5-phosphoric acid spray nozzle, 6-steam spray pipe and 7-exhaust port.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
1000kg of settled phosphoric acid, P after heavy metal removal, clarification and filter pressing2O5The concentration was 48.28%, the F content was 0.82%, and the solid content was 0.31%. Adding 8.35kg of white carbon black into defluorinating agent according to the addition amount of 1.2 times of the theoretical amount, uniformly mixing, indirectly heating to 70 ℃ by adopting low-pressure steam, pumping the defluorinating agent into a defluorinating tower 1 by using a pump, spraying out from a phosphoric acid spray head 5 after entering from a raw material phosphoric acid inlet 2, defluorinating phosphoric acid liquid by convection with rising steam when the phosphoric acid liquid falls down under the action of gravity, directly introducing steam into phosphoric acid gathered at the bottom of the defluorinating tower 1 (the bottom is used as a liquid storage tank), wherein the steam is high-temperature steam, the temperature is 160 ℃, and the pressure is highThe force was 0.7 MPa. And heating the phosphoric acid in the liquid storage tank at the bottom to a boiling state by using steam, keeping the temperature at 120-135 ℃, allowing the fluorine-containing gas to escape from an exhaust port 7 at the top of the defluorination tower 1, and recovering the fluorine-containing gas by washing to obtain finished phosphoric acid discharged from a finished acid outlet 4. Production of defluorinated phosphoric acid P2O553.28% concentration, phosphorus to fluorine ratio (P)2O5and/F) is 395.
Example 2
1000kg of settled phosphoric acid, P after heavy metal removal, clarification and filter pressing2O5The concentration is 45.76%, the F content is 1.17%, and the solid content is 0.24%. The addition amount of the defluorinating agent is 1.3 times of the theoretical amount, 12.91kg of white carbon black is added and uniformly mixed, low-pressure steam is adopted for indirect heating to 80 ℃, then the defluorinating agent is pumped into a defluorinating tower 1 by a pump, the defluorinating agent enters from a raw material phosphoric acid inlet 2 and is sprayed out from a phosphoric acid spray head 5, phosphoric acid liquid falls down under the action of gravity and is defluorinated in a convection way with rising steam, the steam is directly introduced into phosphoric acid gathered at the bottom of the defluorinating tower 1 (the bottom is used as a liquid storage tank), the steam is high-temperature steam, the temperature is 165 ℃, and the pressure is 0.75 MPa. And heating the phosphoric acid in the liquid storage tank at the bottom to a boiling state by using steam, keeping the temperature at 130-145 ℃, allowing the fluorine-containing gas to escape from an exhaust port 7 at the top of the defluorination tower 1, and recovering the fluorine-containing gas by washing to obtain finished phosphoric acid discharged from a finished acid outlet 4. Production of defluorinated phosphoric acid P2O5The concentration is 52.83%, the phosphorus-fluorine ratio (P)2O5and/F) is 487.
Example 3
1000kg of settled phosphoric acid, P after heavy metal removal, clarification and filter pressing2O5The concentration was 41.84%, the F content was 1.47%, and the solid content was 0.13%. The addition amount of the defluorinating agent is 1.1 times of the theoretical amount, 13.73kg of white carbon black is added and uniformly mixed, low-pressure steam is adopted for indirect heating to 90 ℃, then the defluorinating agent is pumped into a defluorinating tower 1 by a pump, the defluorinating agent enters from a raw material phosphoric acid inlet 2 and is sprayed out from a phosphoric acid spray head 5, phosphoric acid liquid falls down under the action of gravity and is defluorinated in a convection way with rising steam, the steam is directly introduced into phosphoric acid gathered at the bottom of the defluorinating tower 1 (the bottom is used as a liquid storage tank), the steam is high-temperature steam, the temperature is 162 ℃, and the pressure is 0.8 MPa. The steam heats the phosphoric acid in the bottom liquid storage tank to a boiling state,and the temperature is kept at 140-150 ℃, the fluorine-containing gas escapes from an exhaust port 7 at the top of the defluorination tower 1 and is recovered by washing, and the finished phosphoric acid is discharged from a finished acid outlet 4. Heating, boiling, stripping and defluorinating. Production of defluorinated phosphoric acid P2O5Concentration 52.35%, phosphorus to fluorine ratio (P)2O5and/F) is 402.
Example 4
The defluorination tower 1 used in the technical scheme is a hollow cavity, and the side wall of the defluorination tower 1 is sequentially provided with a raw material phosphoric acid inlet 2, a steam inlet 3 and a finished product acid outlet 4 from top to bottom, wherein the raw material phosphoric acid inlet 2 is connected with a phosphoric acid spray head 5, and the phosphoric acid spray heads 5 are uniformly distributed in the tower body 1; the steam inlet 3 is connected with a steam spray pipe 6, the steam spray pipe 6 is arranged in the tower body 1, and the top of the tower body 1 is provided with an exhaust port 7. More than three steam inlets 3 are arranged in parallel, and the number of the steam spray pipes 6 is consistent with that of the steam inlets 3. Preheated phosphoric acid containing defluorinating agent is atomized and sprayed out from a phosphoric acid spray nozzle 5, falls under the influence of gravity, is defluorinated after being convected with rising steam, fluorine-containing gas is discharged from a top exhaust port 7, the defluorinated phosphoric acid is stored at the bottom of a defluorinating tower 1, the bottom of the defluorinating tower 1 is used as a liquid storage tank, a steam spray pipe 6 is slowly submerged along with the increase of the phosphoric acid amount, at the moment, the steam directly heats the phosphoric acid until the phosphoric acid is boiled, and the fluorine-containing gas escapes in a boiling state, so that the defluorinating efficiency is further improved, and the capacity is improved. In order to facilitate the discharge of finished phosphoric acid and the cleaning of the defluorination tower 1, the bottom of the defluorination tower 1 is obliquely arranged, and the inclination angle is 3-8 degrees.
Although the invention has been described herein with reference to a number of illustrative embodiments thereof, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this disclosure. More specifically, various variations and modifications are possible in the component parts or arrangements of the subject combination arrangement within the scope of the disclosure, the drawings and the appended claims. In addition to variations and modifications in the component parts or arrangements, other uses will also be apparent to those skilled in the art.
Claims (6)
1. The high-temperature stripping defluorination method of wet-process phosphoric acid is characterized by comprising the following steps:
(1) carrying out heavy metal removal treatment on raw material phosphoric acid, and then clarifying and filter-pressing to remove solid impurities in the phosphoric acid to obtain clarified concentrated phosphoric acid with low solid content;
(2) uniformly mixing a defluorinating agent and clarified concentrated phosphoric acid, heating the mixture to 70-90 ℃, pumping the phosphoric acid into a defluorinating tower (1) through a pump for steam stripping defluorination, wherein the defluorinating tower (1) is a hollow cavity, and the side wall of the defluorinating tower (1) is sequentially provided with a raw material phosphoric acid inlet (2), a steam inlet (3) and a finished product acid outlet (4) from top to bottom, wherein the raw material phosphoric acid inlet (2) is connected with a phosphoric acid spray nozzle (5), and the phosphoric acid spray nozzles (5) are uniformly distributed in the defluorinating tower (1); the steam inlet (3) is connected with a steam spray pipe (6), the steam spray pipe (6) is arranged in the defluorination tower (1), and the top of the defluorination tower (1) is provided with an exhaust port (7); the mixture enters from a raw material phosphoric acid inlet (2) and then is sprayed out from a phosphoric acid spray head (5), phosphoric acid drops fall under the action of gravity and are defluorinated by convection with rising steam, the steam is directly introduced into phosphoric acid at the bottom of a defluorination tower (1), the steam is high-temperature steam, and the temperature is 160-165 ℃; the phosphoric acid in a liquid storage tank at the lower part of the defluorination tower (1) is kept in a boiling state, the temperature of the boiling state is controlled to be 120-150 ℃, fluorine-containing gas is recycled by washing, and the phosphorus-fluorine ratio P is obtained2O5Defluorinated phosphoric acid with low fluorine content and over 380F.
2. The high-temperature stripping defluorination method for wet-process phosphoric acid according to claim 1, characterized in that: the solid content of the raw material phosphoric acid in the step (1) is less than or equal to 0.4 percent, and P2O5The concentration is 41-50%.
3. The high-temperature stripping defluorination method for wet-process phosphoric acid according to claim 1, characterized in that: the defluorinating agent in the step (2) is white carbon black or active SiO2The addition amount of the defluorinating agent is 1.0-1.5 times of the theoretical dosage, and the mass concentration of the defluorinating agent slurry is 8-20%.
4. The high-temperature stripping defluorination method for wet-process phosphoric acid according to claim 1, characterized in that: the heating mode of the mixture in the step (2) is indirect heating, the phosphoric acid is heated by adopting a tube type or coil pipe heat exchanger, and the heating medium is low-pressure steam or heat conducting oil.
5. The high-temperature stripping defluorination method for wet-process phosphoric acid according to claim 1, characterized in that: more than three steam inlets (3) are arranged in parallel, and the number of the steam spray pipes (6) is consistent with that of the steam inlets (3).
6. The high-temperature stripping defluorination method for wet-process phosphoric acid according to claim 1, characterized in that: the bottom of the defluorination tower (1) is obliquely arranged, and the inclination angle is 3-8 degrees.
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