CN114870589A - Method for comprehensively utilizing lithium hexafluorophosphate tail gas - Google Patents
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Abstract
The invention discloses a method for comprehensively utilizing lithium hexafluorophosphate tail gas, which comprises the following steps: (1) and (3) recovering phosphorus pentafluoride: introducing lithium hexafluorophosphate process tail gas into a washing tower to be washed by using an organic solvent, heating and desorbing the obtained washing liquid, condensing and removing impurities from the desorbed gaseous substance to obtain phosphorus pentafluoride gas for recycling, and mixing the desorbed organic solvent with the condensed organic solvent for tail gas washing; the organic solvent is carbon tetrachloride or benzene; (2) and (3) fluorine recovery: introducing the washed tail gas in the step (1) into a chloride solution for reaction and fluorine removal, so that hydrogen fluoride in the tail gas reacts with chloride in the solution to generate fluoride salt precipitate, then filtering, washing and drying to obtain fluoride salt, and supplementing chloride to the filtrate for recycling in tail gas fluorine removal; (3) and (3) hydrogen chloride recovery: and (3) performing multistage absorption on the tail gas in the step (2) by using water to obtain industrial concentrated hydrochloric acid.
Description
Technical Field
The invention relates to the field of fluorine chemical preparation, and particularly relates to a method for comprehensively utilizing lithium hexafluorophosphate tail gas.
Background
At present, a hydrofluoric acid solvent method is mainly used for industrially producing lithium hexafluorophosphate, and the method comprises the steps of reacting phosphorus pentachloride with anhydrous hydrogen fluoride to generate phosphorus pentafluoride gas, introducing lithium fluoride to dissolve in LiF ∙ HF solution formed by the anhydrous hydrogen fluoride to react to obtain synthetic liquid, and cooling, crystallizing, separating and drying to obtain the product. In the process, in the process of preparing phosphorus pentafluoride by reacting phosphorus pentachloride and anhydrous hydrogen fluoride, heat is violently released to cause the anhydrous hydrogen fluoride to volatilize, a gas mixture after reaction passes through a filter and a condenser and then enters a hydrofluoric acid solution containing lithium fluoride to react, a large amount of phosphorus pentafluoride and lithium fluoride react and are consumed in the process, a large amount of hydrogen chloride gas, inert protective gas nitrogen and unreacted hydrogen fluoride and phosphorus pentafluoride gas generated by the reaction overflow together to form process tail gas, and the tail gas contains about 30-35% of HCl and 1-4% of PF 5 8-12% of HF, and the balance of nitrogen.
Most of hydrogen fluoride gas is removed by condensation at present, and then hydrogen chloride and phosphorus pentafluoride which are difficult to condense under normal pressure are removed by water absorption, and fluorine-containing dilute hydrochloric acid is a byproduct.
To this patent provide a lithium hexafluorophosphate tail gas comprehensive utilization's method, promote separation efficiency, realize the high-efficient utilization of fluorine, phosphorus, chlorine resource.
Disclosure of Invention
The invention provides a method for comprehensively utilizing lithium hexafluorophosphate tail gas, which is simple in process and high in separation efficiency, and realizes efficient cyclic utilization of fluorine, chlorine and phosphorus resources.
Based on the purpose, the invention adopts the following technical scheme:
a method for comprehensively utilizing lithium hexafluorophosphate tail gas comprises the following steps:
(1) and (3) recovering phosphorus pentafluoride: introducing lithium hexafluorophosphate process tail gas into a washing tower to be washed by using an organic solvent, heating and desorbing the obtained washing liquid, condensing and removing impurities from the desorbed gaseous substance to obtain phosphorus pentafluoride gas for recycling, and mixing the desorbed organic solvent with the condensed organic solvent for tail gas washing; the organic solvent is carbon tetrachloride or benzene;
(2) and (3) fluorine recovery: introducing the washed tail gas in the step (1) into a chloride solution for reaction and fluorine removal, so that hydrogen fluoride in the tail gas reacts with chloride in the solution to generate fluoride salt precipitate, then filtering, washing and drying to obtain fluoride salt, and supplementing chloride to the filtrate for recycling in tail gas fluorine removal;
(3) and (3) hydrogen chloride recovery: and (3) performing multistage absorption on the tail gas in the step (2) by using water to obtain industrial concentrated hydrochloric acid which can be directly sold.
Further, the temperature of the organic solvent is 20-30 ℃ during washing in the step (1).
Further, when the concentration of phosphorus pentafluoride in the organic solvent in the step (1) reaches 40-60 g/L, heating washing liquid is needed, and desorbing phosphorus pentafluoride; the temperature of the cleaning solution is 50-65 ℃ during heating, and the heating time is 30-60 min.
Further, the condensation temperature in the step (1) is-10-20 ℃;
further, in the step (2), the reaction temperature is controlled to be 20-50 ℃, the concentration of chloride salt in the washing liquid is 50-400g/L, and the chloride salt is any one of calcium chloride, aluminum chloride, ferric chloride, magnesium chloride, sodium chloride and lithium chloride.
Further, when the concentration of the chloride salt in the chloride salt solution in the step (2) is lower than 10g/L, the solution needs to be filtered, and the filtrate is continuously recycled after the chloride salt is supplemented.
Further, the temperature of water in the absorption in the step (3) is 15-25 ℃, and industrial concentrated hydrochloric acid with the concentration of 30-38% is obtained through absorption.
Further, in the step (1), the flow speed of the tail gas in the washing tower is 1-2 m/s, and the spraying amount of the organic solvent is 0.2-0.5L/s.
Further, the tail gas after multistage absorption in the step (3) is subjected to alkali treatment and discharged after reaching the standard.
The device for realizing the method comprises a washing tower, a reaction tank, an absorption device and a desorption tank which are connected by pipelines, the device comprises a condenser, a filter and a dissolving tank, wherein an organic solvent inlet, a lithium hexafluorophosphate process tail gas inlet, a washing liquid outlet and a washed tail gas outlet are respectively arranged on a washing tower, the washing liquid outlet is connected with an desorption tank through a pipeline, the washed tail gas outlet is connected with a reaction tank through a pipeline, the reaction tank is provided with a tail gas outlet and a washing liquid outlet, the tail gas outlet is connected with an absorption device, the washing liquid outlet is connected with the filter, the filter is provided with a liquid outlet and a solid outlet, fluoride salt is discharged outside through the solid outlet, the liquid outlet of the filter is connected with the dissolving tank through a pipeline, and the dissolving tank is connected with the reaction tank through a pipeline, so that a chloride solution meeting the requirement is obtained after chloride is supplemented in the dissolving tank and then returns to the reaction tank for continuous use;
the desorption tank is provided with a gas outlet and a liquid outlet, the gas outlet is connected with the condenser, the condenser is provided with a gas outlet and a liquid outlet, the gas outlet is used for discharging phosphorus pentafluoride outwards, and the liquid outlet of the condenser is connected with the liquid outlet of the desorption tank in parallel through a pipeline and then connected with the organic solvent inlet of the washing tower.
Furthermore, the absorption device is formed by connecting a plurality of stages of spraying absorption towers in series, and the absorption mode is gas-liquid countercurrent contact. A stirring mechanism is arranged in the dissolving tank.
The method comprises the steps of absorbing phosphorus pentafluoride in lithium hexafluorophosphate tail gas by using an organic solvent, desorbing the phosphorus pentafluoride by heating, and removing the volatilized organic solvent by condensation so as to achieve the aim of recovering the phosphorus pentafluoride; and (2) removing fluorine from the washed tail gas by using a chloride solution, reacting hydrogen fluoride in the tail gas with chloride in the solution to generate a fluoride salt precipitate and hydrogen chloride gas, firstly dissolving the hydrogen chloride generated by the reaction and the hydrogen chloride in the tail gas into the solution, and leaving the hydrogen chloride generated by the reaction and the hydrogen chloride contained in the tail gas out of the solution in a gaseous form after the hydrogen chloride in the solution is saturated, thereby realizing the effective separation of the hydrogen fluoride and the hydrogen chloride gas in the tail gas.
The method has simple process flow, solves the problem that the phosphorus pentafluoride is difficult to recover in the traditional lithium hexafluorophosphate tail gas treatment process, and solves the technical problems of fluorine resource waste, poor quality of byproduct hydrochloric acid and the like caused by incomplete separation of hydrogen fluoride and hydrogen chloride gas in the process tail gas. The whole treatment process has no discharge of three wastes, and the inorganic fluoride and the industrial concentrated hydrochloric acid are prepared, so that the high-efficiency utilization of resources is realized, new economic benefits are created, and the production cost is further reduced.
Drawings
FIG. 1 is a process flow diagram of the present invention; the legend in FIG. 1 is as follows:
1. a washing tower; 2. a reaction tank; 3. an absorption device; 4. a filter; 5. a desorption tank; 6. a condenser; 7. a dissolving tank.
Detailed Description
The invention is further illustrated below with reference to the figures and examples.
A device for comprehensively utilizing lithium hexafluorophosphate tail gas, which comprises a washing tower 1, a reaction tank 2, an absorption device 3 and a desorption tank 5 which are connected by pipelines, the device comprises a condenser 6, a filter 4 and a dissolving tank 7, wherein the washing tower 1 is respectively provided with an organic solvent inlet, a lithium hexafluorophosphate process tail gas inlet, a washing liquid outlet and a washed tail gas outlet, the washing liquid outlet is connected with a desorption tank 5 through a pipeline, the washed tail gas outlet is connected with a reaction tank 2 through a pipeline, the reaction tank 2 is provided with a tail gas outlet and a washing liquid outlet, the tail gas outlet is connected with an absorption device 3, the washing liquid outlet is connected with the filter 4, the filter 4 is provided with a liquid outlet and a solid outlet, fluoride salt is discharged outside through the solid outlet, the liquid outlet of the filter 4 is connected with the dissolving tank 7 through a pipeline, and the dissolving tank 7 is connected with the reaction tank 2 through a pipeline, so that after chloride salt is supplemented in the dissolving tank 7, a chloride solution meeting the requirement is obtained and then returned to the reaction tank 2 for continuous use;
the desorption tank 5 is provided with a gas outlet and a liquid outlet, the gas outlet is connected with the condenser 6, the condenser 6 is provided with a gas outlet and a liquid outlet, the gas outlet is used for discharging phosphorus pentafluoride outwards, and the liquid outlet of the condenser 6 is connected with the liquid outlet of the desorption tank 5 in parallel through a pipeline and then is connected with the organic solvent inlet of the washing tower 1.
The absorption device 3 is formed by connecting a plurality of stages of spraying absorption towers in series, the absorption mode is gas-liquid countercurrent contact, and a stirring mechanism is arranged in the dissolving tank 7.
Example 1:
a method for comprehensively utilizing lithium hexafluorophosphate tail gas comprises the following steps:
(1) introducing lithium hexafluorophosphate process tail gas into a washing tower 1, wherein the diameter of the washing tower 1 is 0.5m, the height of the washing tower is 5m, a metal wire mesh filler (made of C276 or Monel) is used, the height of the filler is 3m, the flow rate of the tail gas in the washing tower 1 is controlled to be 1m/s, the tail gas is washed by carbon tetrachloride at the spraying amount of 0.3L/s, and the washing temperature is controlled to be 20 ℃. When the concentration of the phosphorus pentafluoride in the washing liquid reaches 40g/L, introducing the washing liquid into a desorption tank 5, desorbing for 30min at 65 ℃, collecting the desorbed gaseous substances and introducing the gaseous substances into a condenser 6, setting the temperature of the condenser 6 to be-10 ℃, collecting uncondensed gas, namely phosphorus pentafluoride, and mixing the condensed carbon tetrachloride and the desorbed carbon tetrachloride for recycling;
(2) introducing the tail gas washed in the step (1) into a reaction tank 2, reacting aluminum chloride solution with the concentration of 400g/L with hydrogen fluoride in the tail gas, controlling the reaction temperature to be 50 ℃, introducing a washing solution into a filter 4 for filtering when the concentration of aluminum chloride in the solution is lower than 10g/L to obtain aluminum fluoride, introducing the filtrate into a dissolving tank 7, adding aluminum chloride until the concentration of aluminum chloride in the solution is 400g/L, and recycling;
(3) and (3) introducing the tail gas subjected to secondary washing in the step (2) into an absorption device 3, performing multistage countercurrent absorption by using water at 15 ℃ until the concentration of hydrogen chloride in the water reaches 38wt% to obtain concentrated hydrochloric acid, and performing alkali treatment on the unabsorbed tail gas to achieve the standard and discharge.
Example 2:
a method for comprehensively utilizing lithium hexafluorophosphate tail gas comprises the following steps:
(1) introducing lithium hexafluorophosphate process tail gas into a washing tower 1, controlling the flow rate of the tail gas in the washing tower 1 to be 1.5m/s, washing the tail gas by using carbon tetrachloride at 25 ℃ in a spraying amount of 0.4L/s, introducing washing liquid into a desorption tank 5 when the concentration of phosphorus pentafluoride in the carbon tetrachloride reaches 50g/L, desorbing for 45min at 60 ℃, collecting desorbed gaseous substances, introducing the gaseous substances into a condenser 6, keeping the temperature of the condenser 6 at 0 ℃, collecting uncondensed gas, namely phosphorus pentafluoride, and mixing the condensed carbon tetrachloride and the desorbed carbon tetrachloride for recycling;
(2) introducing the tail gas subjected to the primary washing in the step (1) into a reaction tank 2, performing secondary washing on the tail gas by using an aluminum chloride solution with the concentration of 200g/L, controlling the reaction temperature to be 35 ℃, introducing a washing solution into a filter 4 for filtering when the concentration of aluminum chloride in the solution is lower than 10g/L to obtain aluminum fluoride, introducing the filtrate into a dissolving tank 7, adding aluminum chloride until the concentration of aluminum chloride in the solution is 200g/L, and recycling;
(3) and (3) introducing the tail gas subjected to secondary washing in the step (2) into an absorption device 3, performing multi-stage countercurrent absorption by using water at the temperature of 20 ℃ until the concentration of hydrogen chloride in the water reaches 36wt% to obtain concentrated hydrochloric acid, and performing alkali treatment on the unabsorbed tail gas to achieve the standard and discharging.
Example 3:
a method for comprehensively utilizing lithium hexafluorophosphate tail gas comprises the following steps:
(1) introducing lithium hexafluorophosphate process tail gas into a washing tower 1, controlling the flow rate of the tail gas in the washing tower 1 to be 2m/s, washing the tail gas by using carbon tetrachloride at 30 ℃ in a spraying amount of 0.5L/s, introducing a washing liquid into a desorption tank 5 when the concentration of phosphorus pentafluoride in the carbon tetrachloride reaches 60g/L, desorbing for 60min at 50 ℃, collecting desorbed gaseous substances, introducing the gaseous substances into a condenser 6, keeping the temperature of the condenser 6 at 20 ℃, collecting uncondensed gas, namely phosphorus pentafluoride, and mixing the condensed carbon tetrachloride and the desorbed carbon tetrachloride for recycling;
(2) introducing the tail gas subjected to the primary washing in the step (1) into a reaction tank 2, performing secondary washing on the tail gas by using an aluminum chloride solution with the concentration of 50g/L, controlling the reaction temperature to be 20 ℃, introducing a washing solution into a filter 4 for filtering when the concentration of aluminum chloride in the washing solution is lower than 10g/L to obtain aluminum fluoride, introducing the filtrate into a dissolving tank 7, adding aluminum chloride until the concentration of aluminum chloride in the solution is 50g/L, and recycling;
(3) and (3) introducing the tail gas subjected to secondary washing in the step (2) into an absorption device 3, performing multistage countercurrent absorption by using water at the temperature of 25 ℃ until the concentration of hydrogen chloride in the water reaches 30wt% to obtain concentrated hydrochloric acid, and performing alkali treatment on the unabsorbed tail gas to achieve the standard and discharge.
Example 4:
a method for comprehensively utilizing lithium hexafluorophosphate tail gas comprises the following steps:
(1) introducing lithium hexafluorophosphate process tail gas into a washing tower 1, controlling the flow rate of the tail gas in the washing tower 1 to be 1.5m/s, washing the tail gas by using benzene at 25 ℃ in a spraying amount of 0.4L/s, introducing a washing liquid into a desorption tank 5 when the concentration of phosphorus pentafluoride in the benzene reaches 50g/L, desorbing for 45min at 60 ℃, collecting desorbed gaseous substances, introducing the gaseous substances into a condenser 6, keeping the temperature of the condenser 6 at 0 ℃, collecting uncondensed gas, namely phosphorus pentafluoride, and mixing the condensed benzene and the desorbed benzene for recycling;
(2) introducing the tail gas subjected to the primary washing in the step (1) into a reaction tank 2, performing secondary washing on the tail gas by using an aluminum chloride solution with the concentration of 200g/L, controlling the reaction temperature to be 35 ℃, introducing a washing solution into a filter 4 for filtering when the concentration of aluminum chloride in the solution is lower than 10g/L to obtain aluminum fluoride, introducing the filtrate into a dissolving tank 7, adding aluminum chloride until the concentration of aluminum chloride in the solution is 200g/L, and recycling;
(3) and (3) introducing the tail gas subjected to secondary washing in the step (2) into an absorption device 3, performing multi-stage countercurrent absorption by using water at the temperature of 15 ℃ until the concentration of hydrogen chloride in the water reaches 36wt% to obtain concentrated hydrochloric acid, and performing alkali treatment on the unabsorbed tail gas to achieve the standard and discharging.
The contents of each component of the lithium hexafluorophosphate process tail gas and the contents (mass fractions) of each component of the unabsorbed tail gas before entering the alkali treatment apparatus in examples 1 to 4 are shown in table 1:
TABLE 1
The results in Table 1 show that the recovery rates of hydrogen chloride and hydrogen fluoride in examples 1 to 4 are estimated, and are shown in Table 2:
TABLE 2
The phosphorus pentafluoride recovery rate was estimated from the concentration of phosphorus pentafluoride in the absorbed carbon tetrachloride solution, and is shown in table 3:
TABLE 3
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for comprehensively utilizing lithium hexafluorophosphate tail gas is characterized by comprising the following steps:
(1) and (3) recovering phosphorus pentafluoride: introducing lithium hexafluorophosphate process tail gas into a washing tower to be washed by using an organic solvent, heating and desorbing the obtained washing liquid, condensing and removing impurities from the desorbed gaseous substance to obtain phosphorus pentafluoride gas for recycling, and mixing the desorbed organic solvent with the condensed organic solvent for tail gas washing; the organic solvent is carbon tetrachloride or benzene;
(2) and (3) fluorine recovery: introducing the washed tail gas in the step (1) into a chloride solution for reaction and fluorine removal, so that hydrogen fluoride in the tail gas reacts with chloride in the solution to generate fluoride salt precipitate, then filtering, washing and drying to obtain fluoride salt, and supplementing chloride to the filtrate for recycling in tail gas fluorine removal;
(3) and (3) hydrogen chloride recovery: and (3) performing multistage absorption on the tail gas in the step (2) by using water to obtain industrial concentrated hydrochloric acid.
2. The method for comprehensively utilizing the lithium hexafluorophosphate tail gas as claimed in claim 1, wherein the temperature of the organic solvent during the washing in the step (1) is 20-30 ℃; the condensation temperature is-10 to 20 ℃.
3. The method for comprehensively utilizing lithium hexafluorophosphate tail gas according to claim 1, wherein when the concentration of phosphorus pentafluoride in the organic solvent in the step (1) reaches 40-60 g/L, the washing liquid needs to be heated to desorb the phosphorus pentafluoride; the temperature of the cleaning solution is 50-65 ℃ during heating, and the heating time is 30-60 min.
4. The method for comprehensively utilizing lithium hexafluorophosphate tail gas according to claim 1, wherein in the step (2), the reaction temperature is controlled to be 20 to 50 ℃, the concentration of chloride salt in the washing liquid is 50 to 400g/L, and the chloride salt is any one of calcium chloride, aluminum chloride, ferric chloride, magnesium chloride, sodium chloride and lithium chloride.
5. The method for comprehensively utilizing lithium hexafluorophosphate tail gas as claimed in claim 1, wherein in the step (2), when the chloride concentration in the chloride solution is lower than 10g/L, the solution is required to be filtered, and the filtrate is continuously recycled after being supplemented with chloride.
6. The method for comprehensively utilizing the lithium hexafluorophosphate tail gas as claimed in claim 1, wherein the temperature of water during absorption in step (3) is 15-25 ℃, and industrial concentrated hydrochloric acid with the concentration of 30-38% is obtained through absorption.
7. The method for comprehensively utilizing the lithium hexafluorophosphate tail gas as set forth in claim 1, wherein in the step (1), the flow rate of the tail gas in the washing tower is 1m/s to 2m/s, and the spraying amount of the organic solvent is 0.2L/s to 0.5L/s.
8. An apparatus for carrying out the method of any one of claims 1 to 7, comprising a washing column, a reaction tank, an absorption apparatus, and a desorption tank connected by a pipe, the device comprises a condenser, a filter and a dissolving tank, wherein an organic solvent inlet, a lithium hexafluorophosphate process tail gas inlet, a washing liquid outlet and a washed tail gas outlet are respectively arranged on a washing tower, the washing liquid outlet is connected with an desorption tank through a pipeline, the washed tail gas outlet is connected with a reaction tank through a pipeline, the reaction tank is provided with a tail gas outlet and a washing liquid outlet, the tail gas outlet is connected with an absorption device, the washing liquid outlet is connected with the filter, the filter is provided with a liquid outlet and a solid outlet, fluoride salt is discharged outside through the solid outlet, the liquid outlet of the filter is connected with the dissolving tank through a pipeline, and the dissolving tank is connected with the reaction tank through a pipeline, so that a chloride solution meeting the requirement is obtained after chloride is supplemented in the dissolving tank and then returns to the reaction tank for continuous use;
the desorption tank is provided with a gas outlet and a liquid outlet, the gas outlet is connected with the condenser, the condenser is provided with a gas outlet and a liquid outlet, the gas outlet is used for discharging phosphorus pentafluoride outwards, and the liquid outlet of the condenser is connected with the liquid outlet of the desorption tank in parallel through a pipeline and then connected with the organic solvent inlet of the washing tower.
9. The device according to claim 8, wherein the absorption device is formed by connecting a plurality of stages of spray absorption towers in series, and the absorption mode is gas-liquid countercurrent contact.
10. The apparatus of claim 8, wherein the dissolving tank is provided with a stirring mechanism.
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| CN213976992U (en) * | 2020-12-02 | 2021-08-17 | 江苏九九久科技有限公司 | Lithium hexafluorophosphate apparatus for producing |
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