CN115636429A - Preparation process of lithium hexafluorophosphate - Google Patents
Preparation process of lithium hexafluorophosphate Download PDFInfo
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- CN115636429A CN115636429A CN202211566370.2A CN202211566370A CN115636429A CN 115636429 A CN115636429 A CN 115636429A CN 202211566370 A CN202211566370 A CN 202211566370A CN 115636429 A CN115636429 A CN 115636429A
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Abstract
The invention relates to a preparation process of lithium hexafluorophosphate, which comprises the following steps of S1, injecting anhydrous hydrogen fluoride into a vaporization chamber, and vaporizing the hydrogen fluoride by a heating unit arranged at the bottom of the vaporization chamber to obtain pure hydrogen fluoride gas; s2, injecting pure hydrogen fluoride gas into the reaction chamber, cooling and filtering the generated mixed gas of phosphorus pentafluoride and hydrogen chloride through a nitrogen temperature control area, and injecting the mixed gas into a first generation chamber; s3, reacting the mixed gas with the LiF-HF mother liquor in the first generation chamber to produce a lithium hexafluorophosphate solution, and injecting tail gas of the first generation chamber into the second generation chamber to react with the LiF-HF mother liquor in the second generation chamber to produce the lithium hexafluorophosphate solution; and S4, filtering the lithium hexafluorophosphate solutions in the first generation chamber and the second generation chamber through a 5 mu filter and a 2 mu filter in sequence, and injecting the filtered lithium hexafluorophosphate solutions into a crystallization kettle for crystallization to generate lithium hexafluorophosphate crystals.
Description
Technical Field
The invention relates to the field of preparation of lithium hexafluorophosphate, in particular to a preparation process of lithium hexafluorophosphate.
Background
LiPF6 is an important component of the lithium ion battery electrolyte, and mainly has the function of ensuring that sufficient lithium ions realize charge-discharge circulation in the charge-discharge process of the battery. The solubility, electrochemical stability, conductivity, high and low temperature performance, cycle life and other performance indexes of the composite material are balanced, so that the composite material is widely applied commercially. The LiPF6 synthesis method comprises a gas-solid method, a hydrogen fluoride solvent method, an organic solvent method and an ion exchange method, wherein the hydrogen fluoride solvent method is widely used in industry, the process flow is that phosphorus pentachloride and anhydrous hydrogen fluoride react to generate phosphorus pentafluoride gas, solid lithium fluoride is dissolved in a stainless steel container filled with hydrofluoric acid solution to prepare suspension, and then the phosphorus pentafluoride gas is introduced into a synthesis container to react to obtain the LiPF6 product. However, in the actual production process of LiPF6, the requirement on the purity of raw materials is very high, hydrogen fluoride has strong corrosivity, and the preparation process has the problems of difficult safe production control, anhydrous environment, high requirements on the content of free acid and insoluble substances and the like. Therefore, how to remove impurities and improve the product purity becomes a process difficulty.
Chinese patent CN 101570326B discloses a method for preparing lithium hexafluorophosphate, which comprises the steps of reacting anhydrous hydrogen fluoride with concentrated phosphoric acid under the protection of inert gas to prepare hexafluorophosphoric acid, and adding oleum into the prepared hexafluorophosphoric acid under cooling and stirring to prepare phosphorus pentafluoride gas; dissolving high-purity lithium fluoride in an anhydrous hydrogen fluoride solution to form the anhydrous hydrogen fluoride solution of lithium fluoride; cooling the phosphorus pentafluoride gas, then introducing the phosphorus pentafluoride gas into an anhydrous hydrogen fluoride solution containing lithium fluoride, and reacting, crystallizing, separating and drying to obtain a pure lithium hexafluorophosphate product; and continuously introducing the unreacted cooled phosphorus pentafluoride gas into the anhydrous hydrogen fluoride solution containing the lithium fluoride, and continuously reacting to obtain a lithium hexafluorophosphate finished product. But the technical problem of how to improve the production efficiency and the utilization rate of raw materials of lithium hexafluorophosphate is still not solved.
Disclosure of Invention
Therefore, the invention provides a preparation process of lithium hexafluorophosphate, which can solve the technical problem that the produced lithium hexafluorophosphate meets the standard by purifying hydrogen fluoride and optimizing the preparation process according to the production efficiency and the raw material utilization efficiency of the lithium hexafluorophosphate.
In order to achieve the above object, the present invention provides a preparation process of lithium hexafluorophosphate, comprising:
step S1, anhydrous hydrogen fluoride is injected into a vaporization chamber and is vaporized by a heating unit arranged at the bottom of the vaporization chamber, an interception net is driven by a sliding unit to move from the top to the bottom of the vaporization chamber, so that the vaporized hydrogen fluoride is fully contacted with oxides on the interception net to obtain pure hydrogen fluoride gas;
s2, injecting pure hydrogen fluoride gas into the reaction chamber, adjusting the injection position of the injection pipe through the supporting unit, then contacting with a phosphorus pentachloride loading net of the reaction chamber, cooling and filtering the generated mixed gas of phosphorus pentafluoride and hydrogen chloride through a nitrogen temperature control area, and then injecting into the first generation chamber;
s3, reacting the mixed gas with the LiF-HF mother liquor in the first generation chamber to produce a lithium hexafluorophosphate solution, and injecting tail gas of the first generation chamber into the second generation chamber to react with the LiF-HF mother liquor in the second generation chamber to produce the lithium hexafluorophosphate solution;
and S4, filtering the lithium hexafluorophosphate solutions in the first generation chamber and the second generation chamber through a 5 mu filter and a 2 mu filter in sequence, and then injecting the filtered lithium hexafluorophosphate solutions into a crystallization kettle for crystallization to generate lithium hexafluorophosphate crystals.
Further, the central control unit selects the injection rate Z of the anhydrous hydrogen fluoride in the step S1 according to the target single generation amount m0 of the lithium hexafluorophosphate crystal, wherein,
when M0 is less than or equal to M1, the central control unit selects a first preset hydrogen fluoride injection rate Z1 as the injection rate of anhydrous hydrogen fluoride;
when M1 is more than M0 and more than M2, the central control unit selects a second preset hydrogen fluoride injection rate Z2 as the injection rate of anhydrous hydrogen fluoride;
when M0 is larger than or equal to M2, the central control unit selects a third preset hydrogen fluoride injection rate Z3 as the injection rate of anhydrous hydrogen fluoride;
the hydrogen fluoride injection rate Z is preset by the central control unit, the first hydrogen fluoride injection rate Z1 is preset, the second hydrogen fluoride injection rate Z2 is preset, the third hydrogen fluoride injection rate Z3 is preset, the lithium hexafluorophosphate generation amount M is preset by the central control unit, the first lithium hexafluorophosphate generation amount M1, the second lithium hexafluorophosphate generation amount M2 and the third lithium hexafluorophosphate generation amount M3 are set.
Further, under a first preset condition, the central control unit adjusts the injection rate of the anhydrous hydrogen fluoride according to the bubble amount u1 on the liquid surface of the second generation chamber within the first preset reaction time t1 in the step S3, wherein,
when U1 is less than or equal to U1, the central control unit increases the injection rate Zi to Zi1 of the anhydrous hydrogen fluoride, and sets Zi1= Zi × k1, wherein k1 is a first adjusting parameter;
when U1 is more than U1 and less than U2, the central control unit does not adjust the injection rate of the current anhydrous hydrogen fluoride;
when U1 is larger than or equal to U2, the central control unit reduces the injection rate Zi to Zi2 of the anhydrous hydrogen fluoride, zi2= Zi × k2 is set, and k2 is a second adjusting parameter;
the central control unit presets a bubble amount U, sets a first preset bubble amount U1 and a second preset bubble amount U2, the first preset condition is that the target single generation amount m0 of lithium hexafluorophosphate crystals is smaller than the second preset lithium hexafluorophosphate generation amount, and the injection rate of the tail gas recovered from the second generation chamber to the first generation chamber is smaller than or equal to the second preset tail gas injection rate, wherein i =1,2.
Further, when the bubble amount U1 on the liquid surface of the second generation chamber is less than or equal to the first preset bubble amount within the first preset reaction time t1, the central control unit obtains a first adjustment parameter k1, and sets k1= (1 + (U1-U1)/U1) × M0/M2.
Further, when the bubble amount U1 on the liquid surface of the second generation chamber is greater than or equal to a second preset bubble amount within the first preset reaction time t1, the central control unit obtains a second adjustment parameter k2, and sets k2= (1- (U1-U2)/U2) × M0/M2.
Further, under a second preset condition, the central control unit compares the injection rate Zij of the real-time anhydrous hydrogen fluoride with a preset injection rate standard value Z0 of the anhydrous hydrogen fluoride to regulate the movement rate of the intercepting net, wherein,
when Zij is less than or equal to Z0, the central control unit does not adjust the movement rate of the interception network;
when Zij is larger than Z0, the central control unit reduces the moving speed of the interception network;
j =1,2, and the second preset condition is that the injection rate of the tail gas recovered from the second generation chamber to the first generation chamber is greater than a second preset injection rate of the tail gas, and the amount of bubbles on the liquid surface of the second generation chamber is greater than or equal to a second preset amount of bubbles.
Further, after the second preset reaction time t2 after the injection rate of the anhydrous hydrogen fluoride is adjusted, the central control unit obtains the liquid level bubble amount u2 of the second generation chamber in the first preset reaction time t1, and adjusts the injection angle of the injection pipe in the step S2 according to the liquid level bubble amount change value delta u, and sets delta u = u1-u2, wherein,
when the delta U is less than or equal to the delta U1, the central control unit judges that the injection rate of the anhydrous hydrogen fluoride is reduced, and simultaneously, the injection angle of the injection pipe is increased according to the bubble amount U2 of the liquid surface of the second generation chamber after the second preset reaction time t 2;
when the delta U1 is less than delta U and less than or equal to delta U2, the central control unit judges that the current preparation process meets the standard;
when Deltau > DeltaU2, the central control unit judges that the injection rate of the anhydrous hydrogen fluoride is increased;
the central control unit is preset with a bubble quantity variation standard value delta U, a first preset bubble quantity variation standard value delta U1 and a second preset bubble quantity variation standard value delta U2.
Further, when the central control unit determines that the amount u2 of bubbles is present on the liquid surface of the second generation chamber after the second preset reaction time t2, the injection angle theta of the injection pipe is increased to theta 1, the central control unit compares the adjusted injection angle of the injection pipe with a preset angle W0, and adjusts the support height of the support unit, wherein,
when the theta 1 is less than or equal to W0, the central control unit reduces the supporting height of the supporting unit;
when theta 1 is larger than W0, the central control unit increases the supporting height of the supporting unit.
Further, in the step S1, the central control unit controls an injection rate of nitrogen gas into the vaporizing chamber through the second pump body according to a moving rate v1 of the intercepting net while anhydrous hydrogen fluoride is injected into the vaporizing chamber, wherein,
when V1 is less than or equal to V0, the central control unit judges that the injection rate of the nitrogen in the vaporizing chamber is increased;
when V1 is greater than V0, the central control unit does not adjust the injection rate of the nitrogen in the vaporization chamber.
Further, in the step S2, the reaction chamber is provided with a nitrogen temperature control region for cooling the generated mixed gas, and the central control unit reduces the temperature of the nitrogen injected into the reaction chamber according to the injection angle of the injection pipe.
Compared with the prior art, the method has the advantages that the method removes impurities from hydrogen fluoride, filters phosphorus pentafluoride gas, and enables the generated lithium hexafluorophosphate solution to pass through the primary filter and the secondary filter, so that the impurity content in lithium hexafluorophosphate crystal products for preparing lithium batteries is effectively reduced, the product purity is improved, the operation is easy, and the production efficiency is high. Excessive HF can be recycled by condensation, the utilization efficiency of raw materials is improved, the production process of the product is carried out in equipment with good sealing performance, and the moisture content in the product is reduced under the protection of high-purity nitrogen in the whole process. Meanwhile, in the crystallization process, the formed crystal is dried twice, so that the content of free acid in the product is effectively reduced, the HF mixed with the free acid is removed, and the product quality is improved. Two-stage synthesis reaction is set in the synthesis process of lithium hexafluorophosphate, a phosphorus pentafluoride intermediate product can be 100% utilized, the production efficiency is improved, the emission of pollutants is reduced, and the effects of energy conservation, consumption reduction and environmental protection are achieved.
In particular, the control unit of the present invention divides the amount of lithium hexafluorophosphate generated into two standard values and compares the set standard values of the amount of lithium hexafluorophosphate crystal single generation with the set two standard values, respectively, to determine the injection rate of anhydrous hydrogen fluoride for generating lithium hexafluorophosphate crystals, wherein the larger the target amount of lithium hexafluorophosphate single generation is, the larger the injection rate of anhydrous hydrogen fluoride is, and at the same time, the control unit determines that the target amount of lithium hexafluorophosphate crystals single generation is smaller than the second preset amount of lithium hexafluorophosphate generated and the injection rate of phosphorus pentafluoride not reacted with the LiF-HF mother liquor in the second generation chamber to be recovered to the first generation chamber is equal to or less than the second preset rate of tail gas injection, that is, the production efficiency of lithium hexafluorophosphate meets the standards for each raw material utilization rate, the central control unit obtains the preset reaction time in the second generation chamber, the bubble amount generated by the liquid level is compared with the preset bubble amount, and the injection rate of the anhydrous hydrogen fluoride is adjusted to ensure the production efficiency and the raw material utilization rate of the lithium hexafluorophosphate.
Particularly, in the invention, when the injection rate of the tail gas recovered from the first generation chamber by the second generation chamber is determined to be greater than the second preset injection rate of the tail gas, and the bubble amount on the liquid surface of the second generation chamber is greater than or equal to the second preset bubble amount, the characteristic is that in the current lithium hexafluorophosphate preparation process, the impurity removal of anhydrous hydrogen fluoride is insufficient, and the reason for poor impurity removal of anhydrous hydrogen fluoride is that the injection rate of anhydrous hydrogen fluoride is too high, so that the injection rate of the current anhydrous hydrogen fluoride obtained by the central control unit is greater than the preset standard value of the anhydrous hydrogen fluoride injection rate, and the moving rate of the intercepting net for impurity removal is reduced, so that oxides on the intercepting net are in full contact with the anhydrous hydrogen fluoride, and pure hydrogen fluoride injected into the reaction chamber is ensured.
In particular, the present invention determines whether the adjusted indicator solves the problems of poor lithium hexafluorophosphate production efficiency and poor raw material utilization efficiency by re-acquiring the difference between the amount of bubbles generated by the liquid surface of the second generation chamber within the preset time and the amount of bubbles before the adjustment after a period of time after the adjustment of the injection rate of anhydrous hydrogen fluoride, wherein when the difference between the amount of bubbles acquired by the central control unit and the amount of bubbles before the adjustment is less than or equal to the first preset bubble amount variation criterion value, it indicates that the adjusted indicator does not solve the problems of poor raw material utilization rate and even worsens the problems, and therefore, when the central control unit determines that the injection angle of the injection pipe is adjusted, the central control unit compares the adjusted injection angle with the preset angle to improve the contact range of anhydrous hydrogen fluoride and phosphorus chloride to improve the amount of phosphorus fluoride produced, further improves the production efficiency and raw material utilization efficiency of lithium hexafluorophosphate, and when the central control unit determines that the injection angle of the injection pipe is adjusted, the central control unit compares the adjusted injection angle with the preset angle, and when the support angle of the support unit is lower than the preset angle, it improves the production efficiency of lithium hexafluorophosphate, and thus it indicates that the injection rate of the adjusted indicator is less than the amount of bubbles acquired by the first preset bubble amount of bubbles, and thus it solves the problems of bubbles after the adjusted indicator.
Particularly, the invention injects inert gas nitrogen into the vaporizing chamber to protect the stability of hydrogen fluoride and reduce the risk in the process of preparing lithium hexafluorophosphate, and simultaneously, when the vaporizing chamber removes impurities from the hydrogen fluoride, the stability of the hydrogen fluoride is improved by injecting the nitrogen, and simultaneously, the contact time of the hydrogen fluoride and the interception net is adjusted by controlling the injection rate of the nitrogen so as to achieve the effect of effective impurity removal, wherein when the central control unit judges that the movement rate of the interception net is adjusted, if the movement rate is too low, the central control unit increases the injection rate of the nitrogen so as to ensure that the hydrogen fluoride is fully contacted with oxides on the interception net, and thus the contact time of the hydrogen fluoride and the oxides on the interception net is prolonged.
In particular, the reaction chamber of the present invention is provided with a nitrogen temperature control region, and the generated mixed gas is cooled by controlling the temperature of the nitrogen injected into the nitrogen temperature control region, but when the central control unit determines that the injection angle of the injection pipe is increased, the central control unit determines to decrease the temperature of the nitrogen injected into the reaction chamber in order to ensure sufficient cooling of the generated mixed gas.
Drawings
FIG. 1 is a schematic structural diagram of a lithium hexafluorophosphate production facility according to an embodiment of the present invention;
FIG. 2 is a schematic view of a vaporization chamber according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of a reaction chamber according to an embodiment of the present invention;
FIG. 4 is a schematic diagram of the first and second chambers in accordance with an embodiment of the present invention.
Detailed Description
In order that the objects and advantages of the invention will be more clearly understood, the invention is further described in conjunction with the following examples; it should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only for explaining the technical principles of the present invention, and do not limit the scope of the present invention.
It should be noted that in the description of the present invention, the terms of direction or positional relationship indicated by the terms "upper", "lower", "left", "right", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, which are only for convenience of description, and do not indicate or imply that the device or element must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
Furthermore, it should be noted that, in the description of the present invention, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Fig. 1 is a schematic structural view of a lithium hexafluorophosphate production apparatus according to an embodiment of the present invention, which includes a vaporizer 1 for vaporizing anhydrous hydrogen fluoride; the reaction chamber 2 is connected with the vaporizing chamber and is used for reacting the vaporized anhydrous hydrogen fluoride with phosphorus pentachloride to generate phosphorus pentafluoride; the first generation chamber 3 is connected with the reaction chamber and is used for reacting phosphorus pentafluoride with LiF-HF mother liquor to generate lithium hexafluorophosphate; and the second generation chamber 4 is connected with the first generation chamber and is used for reacting the unreacted phosphorus pentafluoride and the LiF-HF mother liquor in the second generation chamber to generate lithium hexafluorophosphate after the reaction in the first generation chamber.
Please refer to fig. 2, which is a schematic structural diagram of a vaporization chamber according to an embodiment of the present invention, including a first pump 11 disposed at the bottom of the vaporization chamber and used for controlling an injection rate of anhydrous hydrogen fluoride, a sliding unit disposed inside the vaporization chamber and used for controlling a moving rate of an interception net 19, a second pump 12 used for controlling an injection rate of nitrogen gas into the vaporization chamber, and a first pipeline 13 used for injecting vaporized and decontaminated hydrogen fluoride into a reaction chamber, where the sliding unit includes a first slide bar 17 disposed at one side of the vaporization chamber, a first loop 16 disposed on the first slide bar, and a first motor 18 used for controlling a moving rate of the first loop on the first slide bar, the sliding unit further includes a second slide bar 14 disposed at an opposite side of the first slide bar, and a second loop 15 disposed on the second slide bar, and the interception net is connected between the first loop and the second loop, and an oxidant used for decontaminating is disposed on the interception net.
Please refer to fig. 3, which is a schematic diagram of a reaction chamber according to an embodiment of the present invention, including a phosphorus pentafluoride carrier net 22 disposed inside the reaction chamber, a filter net 24 disposed on one side of the phosphorus pentafluoride carrier net, and a nitrogen temperature control region disposed between the filter net and the phosphorus pentafluoride carrier net, wherein the nitrogen temperature control region is provided with a third pump 23 for controlling an injection rate of nitrogen into the reaction chamber, the other side of the phosphorus pentafluoride carrier net is provided with an injection pipe 25 capable of adjusting an injection angle through a supporting unit, the injection pipe is provided with a sleeve 26 for fixing the injection pipe on an inner wall of the reaction chamber to avoid movement, the supporting unit includes a second motor 27 for controlling a telescopic height of the telescopic rod, and the generated phosphorus pentafluoride is injected into the first generation chamber from the second pipe 21.
Referring to fig. 4, a schematic structural diagram of the first generation chamber and the second generation chamber according to the embodiment of the present invention includes a third pipe 42 for injecting the phosphorus pentafluoride gas that does not participate in the reaction in the first generation chamber into the second generation chamber, and a fourth pump 32 for controlling the injection rate of the tail gas that is recovered from the phosphorus pentafluoride gas that does not participate in the reaction in the second generation chamber into the first generation chamber.
Specifically, the preparation process of the lithium hexafluorophosphate comprises the following steps of S1, injecting anhydrous hydrogen fluoride into a vaporizing chamber, vaporizing the hydrogen fluoride by a heating unit arranged at the bottom of the vaporizing chamber, and moving an intercepting net from the top of the vaporizing chamber to the bottom of the vaporizing chamber under the driving of a sliding unit so that the vaporized hydrogen fluoride is fully contacted with oxides on the intercepting net to obtain pure hydrogen fluoride gas; s2, injecting pure hydrogen fluoride gas into the reaction chamber, adjusting the injection position of the injection pipe through the supporting unit, then contacting with a phosphorus pentachloride loading net of the reaction chamber, cooling and filtering the generated mixed gas of phosphorus pentafluoride and hydrogen chloride through a nitrogen temperature control area, and then injecting into the first generation chamber; s3, reacting the mixed gas with the LiF-HF mother liquor in the first generation chamber to produce a lithium hexafluorophosphate solution, and injecting tail gas of the first generation chamber into the second generation chamber to react with the LiF-HF mother liquor in the second generation chamber to produce the lithium hexafluorophosphate solution; and S4, filtering the lithium hexafluorophosphate solutions in the first generation chamber and the second generation chamber through a 5 mu filter and a 2 mu filter in sequence, and injecting the filtered lithium hexafluorophosphate solutions into a crystallization kettle for crystallization to generate lithium hexafluorophosphate crystals.
Specifically, in the embodiment of the present invention, in the step S4, the synthetic liquid in the crystallization kettle is subjected to fractional cooling crystallization. And after the temperature reduction is finished, carrying out solid-liquid separation, putting the mother liquor into a mother liquor tank for treatment and then recycling, blowing and drying the crystal by using high-purity nitrogen, then feeding the crystal into a crusher to uniformly form particles, then feeding the crystal into a secondary dryer for high-temperature drying, and using high-purity nitrogen for protection in the whole process. And finally, carrying out grading packaging operation to obtain the required finished product.
Specifically, the method removes impurities from hydrogen fluoride, filters phosphorus pentafluoride gas, and passes the generated lithium hexafluorophosphate solution through a primary filter and a secondary filter, so that the impurity content in a lithium hexafluorophosphate crystal product for preparing a lithium battery is effectively reduced, the product purity is improved, the operation is easy, and the production efficiency is high. Excessive HF can be recycled by condensation, the utilization efficiency of raw materials is improved, the production process of the product is carried out in equipment with good sealing performance, and the moisture content in the product is reduced under the protection of high-purity nitrogen in the whole process. Meanwhile, in the crystallization process, the formed crystal is dried twice, so that the content of free acid in the product is effectively reduced, the HF mixed with the free acid is removed, and the product quality is improved. Two-stage synthesis reaction is set in the synthesis process of lithium hexafluorophosphate, a phosphorus pentafluoride intermediate product can be 100% utilized, the production efficiency is improved, the emission of pollutants is reduced, and the effects of energy conservation, consumption reduction and environmental protection are achieved.
Specifically, the central control unit selects the injection rate Z of the anhydrous hydrogen fluoride in the step S1 according to the target single generation amount m0 of the lithium hexafluorophosphate crystal,
when M0 is less than or equal to M1, the central control unit selects a first preset hydrogen fluoride injection rate Z1 as the injection rate of anhydrous hydrogen fluoride;
when M1 is larger than M0 and smaller than M2, the central control unit selects a second preset hydrogen fluoride injection rate Z2 as the injection rate of anhydrous hydrogen fluoride;
when M0 is larger than or equal to M2, the central control unit selects a third preset hydrogen fluoride injection rate Z3 as the injection rate of anhydrous hydrogen fluoride;
the central control unit presets a hydrogen fluoride injection rate Z, a first preset hydrogen fluoride injection rate Z1, a second preset hydrogen fluoride injection rate Z2 and a third preset hydrogen fluoride injection rate Z3, and simultaneously presets a lithium hexafluorophosphate generation amount M, a first preset lithium hexafluorophosphate generation amount M1, a second preset lithium hexafluorophosphate generation amount M2 and a third preset lithium hexafluorophosphate generation amount M3.
Specifically, under a first preset condition, the central control unit adjusts the injection rate of the anhydrous hydrogen fluoride according to the bubble amount u1 on the liquid surface of the second generation chamber within the first preset reaction time t1 in the step S3, wherein,
when U1 is less than or equal to U1, the central control unit increases the injection rate Zi to Zi1 of the anhydrous hydrogen fluoride, and sets Zi1= Zi × k1, wherein k1 is a first adjusting parameter;
when U1 is more than U1 and less than U2, the central control unit does not adjust the injection rate of the current anhydrous hydrogen fluoride;
when U1 is larger than or equal to U2, the central control unit reduces the injection rate Zi to Zi2 of the anhydrous hydrogen fluoride, zi2= Zi × k2 is set, and k2 is a second adjusting parameter;
the central control unit presets a bubble amount U, sets a first preset bubble amount U1 and a second preset bubble amount U2, the first preset condition is that the target single generation amount m0 of lithium hexafluorophosphate crystals is smaller than the second preset lithium hexafluorophosphate generation amount, and the injection rate of the tail gas recovered from the second generation chamber to the first generation chamber is smaller than or equal to the second preset tail gas injection rate, wherein i =1,2.
Specifically, the present embodiment does not limit the preset amount of bubbles as long as it can evaluate the lithium hexafluorophosphate production efficiency and the raw material utilization efficiency, and provides a preferred embodiment in which the amount of bubbles produced per unit area is preferably 5 to 10 per unit time, that is, the first preset amount of bubbles is 5 and the second preset amount of bubbles is 10.
When the bubble amount U1 on the liquid surface of the second generation chamber is less than or equal to the first preset bubble amount within the first preset reaction time t1, the central control unit obtains a first adjusting parameter k, and sets k = (1 + (U1-U1)/U1) × M0/M2.
When the bubble amount U1 on the liquid surface of the second generation chamber is greater than or equal to a second preset bubble amount within the first preset reaction time t1, the central control unit obtains a second adjusting parameter k, and sets k = (1- (U1-U2)/U2) × M0/M2.
Specifically, the control unit divides the lithium hexafluorophosphate generation amount into two standard values, and compares the set lithium hexafluorophosphate crystal single generation amount standard value with the two set standard values respectively to determine the injection rate of the anhydrous hydrogen fluoride for generating the lithium hexafluorophosphate crystals, wherein the larger the target single generation amount of the lithium hexafluorophosphate is, the larger the injection rate of the anhydrous hydrogen fluoride is, and at the same time, when the control unit determines that the target single generation amount of the lithium hexafluorophosphate crystals is smaller than the second preset lithium hexafluorophosphate generation amount and the injection rate of the phosphorus pentafluoride which is not reacted with the LiF-HF mother liquor in the second generation chamber to be recovered to the first generation chamber is equal to or less than the second preset tail gas injection rate, that is, the production efficiency of the lithium hexafluorophosphate meets the standards with the respective raw material utilization rates, the central control unit obtains the amount of bubbles generated on the liquid level in the preset reaction time in the second generation chamber, compares the amount of the bubbles with the preset amount of the bubbles, and adjusts the injection rate of the anhydrous hydrogen fluoride to ensure the production efficiency of the lithium hexafluorophosphate and the utilization rate of each raw material.
Wherein under a second preset condition, the central control unit adjusts the movement rate of the interception net according to the comparison between the injection rate Zij of the real-time anhydrous hydrogen fluoride and a preset injection rate standard value Z0 of the anhydrous hydrogen fluoride, wherein,
when Zij is less than or equal to Z0, the central control unit does not adjust the movement rate of the interception network;
when Zij is larger than Z0, the central control unit reduces the moving speed v to v1 of the intercepting net, and sets v1= v x (1- (Zij-Z0)/Z0);
j =1,2, and the second preset condition is that the injection rate of the tail gas recovered from the second generation chamber to the first generation chamber is greater than a second preset injection rate of the tail gas, and the amount of bubbles on the liquid surface of the second generation chamber is greater than or equal to a second preset amount of bubbles.
Specifically, according to the invention, the injection rate of the tail gas recovered from the first generation chamber by the second generation chamber is determined to be greater than the second preset injection rate of the tail gas, and the bubble amount on the liquid surface of the second generation chamber is greater than or equal to the second preset bubble amount, which represents that in the current lithium hexafluorophosphate preparation process, impurity removal of anhydrous hydrogen fluoride is insufficient, and the reason for poor impurity removal of the anhydrous hydrogen fluoride is that the injection rate of the anhydrous hydrogen fluoride is too fast, so that the movement rate of the interception net for impurity removal is reduced when the central control unit obtains that the current injection rate of the anhydrous hydrogen fluoride is greater than the preset standard value of the anhydrous hydrogen fluoride injection rate, so that oxides on the interception net are in full contact with the anhydrous hydrogen fluoride, and pure hydrogen fluoride injected into the reaction chamber is ensured.
Wherein, after the second preset reaction time t2 after the adjustment of the injection rate of the anhydrous hydrogen fluoride, the central control unit obtains the liquid level bubble amount u2 of the second generation chamber within the first preset reaction time t1, and adjusts the injection angle of the injection pipe in the step S2 according to the liquid level bubble amount change value Deltau, and sets Deltau = u1-u2, wherein,
when the delta U is not more than the delta U1, the central control unit judges that the injection rate Zij to Zij1 of the anhydrous hydrogen fluoride is reduced, sets Zij1= Zij x (1- (. DELTA.U 1-. DELTA.u)/. DELTA.U 1), and simultaneously improves the injection angle of the injection pipe according to the bubble amount U2 of the liquid surface of the second generation chamber after the second preset reaction time t 2;
when the delta U1 is less than the delta U and less than or equal to the delta U2, the central control unit judges that the current preparation process meets the standard;
when Δ U > Δu2, the central control unit judges that the anhydrous hydrogen fluoride injection rate Zij to Zij2 is increased, and sets Zij2= Zij x (1 + (Δu- Δ U2)/Δu 2);
the central control unit is preset with a bubble quantity variation standard value delta U, a first preset bubble quantity variation standard value delta U1 and a second preset bubble quantity variation standard value delta U2.
Specifically, when the central control unit determines that the amount U2 of bubbles is present on the liquid surface of the second generation chamber after the second preset reaction time t2, the injection angle θ of the injection pipe is increased to θ 1, θ 1= θ × (1 + (U2-1/2 × (U1 + U2)/2)/(U1 + U2)) is set, and the central control unit compares the injection angle of the injection pipe after adjustment with a preset angle W0 to adjust the support height of the support unit, wherein,
when θ 1 is not less than W0, the central control unit reduces the supporting height h0 of the supporting unit to h1, and sets h1= h × (1- (W0- θ 1)/W0);
when θ 1 > W0, the center control unit increases the support height h0 of the support unit to h2, setting h2= hx (1 + (θ 1-W0)/W0).
Specifically, the support height of the embodiment of the invention is the support distance of the support unit, namely the telescopic distance of the telescopic rod, and the injection angle of the injection pipe is the angle between the injection pipe and the horizontal plane.
Specifically, after the injection rate of the anhydrous hydrogen fluoride is adjusted, after a period of time, the difference between the amount of bubbles generated on the liquid surface of the second generation chamber in the preset time and the amount of bubbles before the adjustment is obtained again, so as to determine whether the adjusted index solves the problems of poor lithium hexafluorophosphate production efficiency and poor raw material utilization efficiency, wherein when the difference between the amounts of bubbles obtained by the central control unit is less than or equal to the first preset bubble amount change standard value, the adjusted index does not only solve the problem of poor raw material utilization rate, but even worsens the problem, therefore, the central control unit greatly reduces the injection rate of the anhydrous hydrogen fluoride again, adjusts the injection range of the injection pipe in the reaction chamber, improves the contact range of the anhydrous hydrogen fluoride and the phosphorus chloride, and improves the generation amount of the phosphorus fluoride, the production efficiency and the raw material utilization efficiency of lithium hexafluorophosphate are further improved, meanwhile, when the central control unit judges that the injection angle of the injection pipe is adjusted, the central control unit compares the adjusted injection angle with the preset angle, the support angle of the support unit lower than the preset angle is reduced, the support angle of the support unit higher than the preset angle is improved, and when the central control unit obtains a bubble quantity difference value smaller than or equal to a second preset bubble quantity change standard value, the problem that the raw material utilization efficiency is poor is solved through the adjusted index, the bubble quantity is greatly reduced, but the adjusted bubble quantity is too low, the production efficiency of lithium hexafluorophosphate is lower, therefore, the injection rate of anhydrous hydrogen fluoride is properly improved through the central control unit, and the production efficiency of lithium hexafluorophosphate is improved.
Wherein, in the step S1, the central control unit controls the injection rate of the nitrogen gas into the vaporizing chamber through the second pump body according to the moving rate v1 of the interception net while the anhydrous hydrogen fluoride is injected into the vaporizing chamber,
when V1 is not more than V0, the central control unit judges that the injection rate N to N1 of the nitrogen gas in the vaporizing chamber is increased, and sets N1= Nx (1 + (V0-V1)/V0);
when V1 is larger than V0, the central control unit does not adjust the injection rate of the nitrogen in the vaporizing chamber.
Specifically, the method comprises the steps of injecting inert gas nitrogen into a vaporizing chamber to protect the stability of hydrogen fluoride and reduce the risk in the process of preparing lithium hexafluorophosphate, and meanwhile, when the vaporizing chamber removes impurities from the hydrogen fluoride, improving the stability of the hydrogen fluoride by injecting the nitrogen, and simultaneously adjusting the contact time of the hydrogen fluoride and an interception net by controlling the injection rate of the nitrogen so as to achieve the effect of effectively removing the impurities, wherein when a central control unit judges that the movement rate of the interception net is adjusted, if the movement rate is too low, the central control unit improves the injection rate of the nitrogen so as to ensure that the hydrogen fluoride is fully contacted with oxides on the interception net, so that the contact time of the hydrogen fluoride and the oxides on the interception net is prolonged.
Wherein, in the step S2, the reaction chamber is provided with a nitrogen gas temperature control region for cooling the generated mixed gas, and the central control unit adjusts the temperature of the nitrogen gas injected into the reaction chamber according to the injection angle of the injection pipe, sets the temperature of the nitrogen gas injected into the reaction chamber NW1 to NW1, and sets NW1= NW × (1-0.35 × | [ theta ] 1-W0 |/W0)).
Specifically, the reaction chamber of the present invention is provided with a nitrogen temperature control region, and the generated mixed gas is cooled by controlling the temperature of the nitrogen injected into the nitrogen temperature control region, but when the central control unit determines that the injection angle of the injection pipe is increased, the central control unit determines to lower the temperature of the nitrogen injected into the reaction chamber to ensure sufficient cooling of the generated mixed gas in order to ensure sufficient cooling of the generated mixed gas.
So far, the technical solutions of the present invention have been described in connection with the preferred embodiments shown in the drawings, but it is easily understood by those skilled in the art that the scope of the present invention is obviously not limited to these specific embodiments. Equivalent changes or substitutions of related technical features can be made by those skilled in the art without departing from the principle of the invention, and the technical scheme after the changes or substitutions can fall into the protection scope of the invention.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention; various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation process of lithium hexafluorophosphate is characterized by comprising the following steps:
step S1, anhydrous hydrogen fluoride is injected into a vaporization chamber and is vaporized through a heating unit arranged at the bottom of the vaporization chamber, an interception net is driven by a sliding unit to move from the top to the bottom of the vaporization chamber, so that the vaporized hydrogen fluoride is fully contacted with oxides on the interception net to obtain pure hydrogen fluoride gas;
s2, injecting pure hydrogen fluoride gas into the reaction chamber, adjusting the injection position of the injection pipe through the supporting unit, then contacting with a phosphorus pentachloride carrying net of the reaction chamber, cooling and filtering the generated mixed gas of phosphorus pentafluoride and hydrogen chloride through a nitrogen temperature control area, and then injecting into the first generation chamber;
s3, reacting the mixed gas with the LiF-HF mother liquor in the first generation chamber to produce a lithium hexafluorophosphate solution, and injecting tail gas of the first generation chamber into the second generation chamber to react with the LiF-HF mother liquor in the second generation chamber to produce the lithium hexafluorophosphate solution;
and S4, filtering the lithium hexafluorophosphate solutions in the first generation chamber and the second generation chamber through a 5 mu filter and a 2 mu filter in sequence, and then injecting the filtered lithium hexafluorophosphate solutions into a crystallization kettle for crystallization to generate lithium hexafluorophosphate crystals.
2. The process for producing lithium hexafluorophosphate according to claim 1, wherein the injection rate Z of anhydrous hydrogen fluoride in said step S1 is selected by the central control unit based on the target single generation amount m0 of lithium hexafluorophosphate crystals,
when M0 is less than or equal to M1, the central control unit selects a first preset hydrogen fluoride injection rate Z1 as the injection rate of anhydrous hydrogen fluoride;
when M1 is larger than M0 and smaller than M2, the central control unit selects a second preset hydrogen fluoride injection rate Z2 as the injection rate of anhydrous hydrogen fluoride;
when M0 is larger than or equal to M2, the central control unit selects a third preset hydrogen fluoride injection rate Z3 as the injection rate of anhydrous hydrogen fluoride;
the central control unit presets a hydrogen fluoride injection rate Z, a first preset hydrogen fluoride injection rate Z1, a second preset hydrogen fluoride injection rate Z2 and a third preset hydrogen fluoride injection rate Z3, and simultaneously presets a lithium hexafluorophosphate generation amount M, a first preset lithium hexafluorophosphate generation amount M1, a second preset lithium hexafluorophosphate generation amount M2 and a third preset lithium hexafluorophosphate generation amount M3.
3. The process for preparing lithium hexafluorophosphate of claim 2, wherein under the first predetermined condition, the central control unit adjusts the injection rate of anhydrous hydrogen fluoride according to the amount u1 of bubbles on the liquid surface of the second generation chamber within the first predetermined reaction time t1 in the step S3, wherein,
when U1 is less than or equal to U1, the central control unit increases the injection rate Zi to Zi1 of anhydrous hydrogen fluoride, and sets Zi1= Zi multiplied by k1, wherein k1 is a first adjusting parameter;
when U1 is more than U1 and less than U2, the central control unit does not adjust the injection rate of the current anhydrous hydrogen fluoride;
when U1 is larger than or equal to U2, the central control unit reduces the injection rate Zi to Zi2 of the anhydrous hydrogen fluoride, zi2= Zi × k2 is set, and k2 is a second adjusting parameter;
the central control unit presets a bubble amount U, sets a first preset bubble amount U1 and a second preset bubble amount U2, the first preset condition is that the target single generation amount m0 of lithium hexafluorophosphate crystals is smaller than the second preset lithium hexafluorophosphate generation amount, and the injection rate of the tail gas recovered from the second generation chamber to the first generation chamber is smaller than or equal to the second preset tail gas injection rate, wherein i =1,2.
4. The process for preparing lithium hexafluorophosphate of claim 3, wherein when the bubble amount U1 on the liquid surface of the second generation chamber within the first predetermined reaction time t1 is less than or equal to the first predetermined bubble amount, the central control unit obtains the first adjustment parameter k1, and sets k1= (1 + (U1-U1)/U1) × M0/M2.
5. The process for preparing lithium hexafluorophosphate of claim 4, wherein the central control unit obtains the second adjustment parameter k2 when the bubble amount U1 at the liquid level of the second generation chamber within the first predetermined reaction time t1 is greater than or equal to the second predetermined bubble amount, and sets k2= (1- (U1-U2)/U2) × M0/M2.
6. The preparation process of lithium hexafluorophosphate of claim 5, wherein under the second preset condition, the central control unit adjusts the movement rate of the intercepting net according to the comparison between the injection rate Zij of the real-time anhydrous hydrogen fluoride and the preset standard value Z0 of the injection rate of the anhydrous hydrogen fluoride, wherein,
when Zij is less than or equal to Z0, the central control unit does not adjust the movement rate of the interception network;
when Zij is larger than Z0, the central control unit reduces the moving speed of the interception network;
j =1,2, and the second preset condition is that the injection rate of the tail gas recovered from the second generation chamber to the first generation chamber is greater than a second preset injection rate of the tail gas, and the amount of bubbles on the liquid surface of the second generation chamber is greater than or equal to a second preset amount of bubbles.
7. The process for producing lithium hexafluorophosphate according to claim 6, wherein the central control unit obtains the bubble amount u2 at the liquid level of the second generation chamber within the first preset reaction time t1 after the second preset reaction time t2 after the adjustment of the injection rate of anhydrous hydrogen fluoride, and adjusts the injection angle of the injection pipe in the step S2 according to the change value Δ u of the bubble amount at the liquid level to set Δ u = u1-u2, wherein,
when the delta U is less than or equal to the delta U1, the central control unit judges that the injection rate of the anhydrous hydrogen fluoride is reduced, and simultaneously, the injection angle of the injection pipe is increased according to the bubble amount U2 of the liquid surface of the second generation chamber after the second preset reaction time t 2;
when the delta U1 is less than the delta U and less than or equal to the delta U2, the central control unit judges that the current preparation process meets the standard;
when Deltau > DeltaU2, the central control unit judges that the injection rate of the anhydrous hydrogen fluoride is increased;
the central control unit is preset with a bubble quantity variation standard value delta U, a first preset bubble quantity variation standard value delta U1 and a second preset bubble quantity variation standard value delta U2.
8. The process for preparing lithium hexafluorophosphate of claim 7, wherein when the central control unit determines the amount of bubbles u2 on the liquid surface of the second generation chamber after the second predetermined reaction time t2, the injection angle θ of the injection pipe is increased to θ 1, the central control unit compares the adjusted injection angle of the injection pipe with a predetermined angle W0 to adjust the supporting height of the supporting unit, wherein,
when theta 1 is not less than W0, the central control unit reduces the supporting height of the supporting unit;
when theta 1 is larger than W0, the central control unit increases the supporting height of the supporting unit.
9. The process for preparing lithium hexafluorophosphate of claim 8, wherein in the step S1, the central control unit controls an injection rate of nitrogen gas into the vaporizing chamber through the second pump body according to a moving rate v1 of the intercepting screen while anhydrous hydrogen fluoride is injected into the vaporizing chamber,
when V1 is less than or equal to V0, the central control unit judges that the injection rate of the nitrogen in the vaporizing chamber is increased;
when V1 is greater than V0, the central control unit does not adjust the injection rate of the nitrogen in the vaporization chamber.
10. The process for preparing lithium hexafluorophosphate of claim 9, wherein in the step S2, the reaction chamber is provided with a nitrogen temperature control region for cooling the generated mixed gas, and the central control unit reduces the temperature of the nitrogen gas injected into the reaction chamber according to the injection angle of the injection pipe.
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