CN115959687B - Process for producing hexafluorophosphate at low cost - Google Patents
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Abstract
本发明涉及低成本生产六氟磷酸盐的工艺，属于六氟磷酸盐生产技术领域。本发明解决的技术问题是提供一种低成本生产六氟磷酸盐的新工艺。该工艺包括以下步骤：a、干燥空气、萤石、硫磺与含磷物质反应生成PF5粗品；b、PF5粗品通过冷冻纯化，通入有液态黄磷的反应釜，点燃，得到纯化后的PF5气体；c、纯化后的PF5气体与氟化盐反应，生成物通过萃取，经过静止分层过滤，得液态六氟磷酸盐。本发明通过物料替代，工艺革新实现多产品耦合的横向发展，以及实现副产品和废弃物资源化利用的立体化产业结构，减少生产过程中的资源和能源消耗。生产过程安全，避免了反应的危险性、纯化效果好，可用于制备高纯度六氟磷酸盐。
The invention relates to a process for producing hexafluorophosphate at low cost, and belongs to the technical field of hexafluorophosphate production. The technical problem solved by the invention is to provide a new process for producing hexafluorophosphate at low cost. The process comprises the following steps: a. dry air, fluorite, sulfur and phosphorus-containing substances react to generate PF5 crude product; b. PF5 crude product is purified by freezing, introduced into a reactor with liquid yellow phosphorus, ignited, and purified PF5 gas is obtained; c. purified PF5 gas reacts with fluoride salt, and the product is extracted and filtered by static stratification to obtain liquid hexafluorophosphate. The invention realizes the horizontal development of multi-product coupling through material substitution and process innovation, and realizes the three-dimensional industrial structure of resource utilization of by-products and waste, thereby reducing resource and energy consumption in the production process. The production process is safe, avoids the danger of reaction, has good purification effect, and can be used to prepare high-purity hexafluorophosphate.
Description
Technical Field
The invention relates to a process for producing hexafluorophosphate at low cost, and belongs to the technical field of hexafluorophosphate production.
Background
Hexafluorophosphates, including lithium hexafluorophosphate (LiPF) 6 ) And sodium hexafluorophosphate (NaPF) 6 ) Is a common electrolyte material for preparing lithium ion batteries or sodium ion batteries. LiPF is manufactured by increasingly steering to make all-electric or hybrid electric vehicles 6 The demand for (c) has increased dramatically over the last few years. Thus, liPF 6 The price of (2) has increased by more than 500% over the last 3 years.
The current methods for producing hexafluorophosphate mainly comprise a gas-solid reaction method, a hydrogen fluoride solution method, an organic solution method and an ion exchange method. The hydrogen fluoride solution method is the most used technology at home and abroad. The main advantages of the process are that phosphorus pentafluoride and lithium fluoride are very soluble in hydrogen fluoride, the whole reaction is easy to carry out and control, and the reaction speed is high.
The invention patent with publication number of CN114538406A discloses a preparation method of high-purity lithium hexafluorophosphate, 1) reacting phosphorus pentachloride with anhydrous hydrofluoric acid or hydrogen fluoride gas to prepare phosphorus pentafluoride; 2) Dissolving LiF in an anhydrous HF solvent, introducing the obtained phosphorus pentafluoride into the solution, and reacting to obtain an anhydrous HF solution of lithium hexafluorophosphate; 3) Distilling the anhydrous HF solution of the lithium hexafluorophosphate to remove hydrofluoric acid to obtain solid lithium hexafluorophosphate; 4) And (3) recrystallizing the lithium hexafluorophosphate solid by using supercritical carbon dioxide or liquid carbon dioxide as a solvent to obtain purified lithium hexafluorophosphate. The process adopts an HF solution method, crystallization is not easy to control, and HF remained in the product is in the form of a complex LiPF 6 The form of HF is present in the product, and it is extremely difficult for the general method to reduce the mass fraction of HF to 1X 10 -5 The purity of the product is greatly affected; residual HF corrodes battery materials, thereby affecting battery electrical performance. The process has high requirements on equipment materials, corrosion prevention measures and production safety measures, increases capital investment and has high production cost.
Disclosure of Invention
Aiming at the defects, the invention solves the technical problem of providing a novel process for producing hexafluorophosphate with low cost.
The invention relates to a process for producing hexafluorophosphate at low cost, which comprises the following steps:
a. the dry air, fluorite, sulfur and phosphor-containing material react to generate PF 5 Crude products; the phosphorus-containing material is wet concentrated phosphoric acid, polyphosphoric acid and P 2 O 5 Solid yellow phosphorus or liquid yellow phosphorus;
b、PF 5 the crude product is frozen and purified, and then is introduced into a reaction kettle with liquid yellow phosphorus for reaction, thus obtaining the purified PF 5 A gas;
c. purified PF 5 The gas reacts with fluoride salt, the temperature is controlled below 15 ℃ in the reaction process, the product is extracted by adding a solvent of lithium battery electrolyte, and the rest separation is carried outFiltering the layer to obtain liquid hexafluorophosphate, wherein the fluoride salt is LiF or NaF.
In one embodiment of the invention, in step a, the moisture content of the dry air is below 20wt%.
In one embodiment of the present invention, in the step b, the freezing temperature of the freeze purification is-40 to 15 ℃ and the pressure is 0.0 to 0.5MPa.
In one embodiment of the invention, in step b, the reaction is carried out at 30 ℃.
In one embodiment of the invention, in step b, the P produced is reacted 2 O 3 And returning to the step a.
In one embodiment of the invention, in the step c, the fluoride salt is in the form of particles, the particles with the particle size of 250-380 mu m account for 25-35 wt% and the rest are particles with the particle size of 100-200 mu m; in a preferred embodiment of the invention, the particles having a particle size of 250 to 380 μm account for 30wt%.
In one embodiment of the present invention, in the step c, the solvent of the lithium battery electrolyte is at least one of ethylene glycol dimethyl ether, isopropyl ether, anisole, propylene carbonate, methyl ethyl carbonate, ethylene carbonate, vinylene carbonate and methyl propionate.
In one embodiment of the invention, in step c, the liquid hexafluorophosphate is concentrated and crystallized and filtered to give solid hexafluorophosphate.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, through material substitution and process innovation, the transverse development of multi-product coupling is realized, a three-dimensional industrial structure for recycling byproducts and wastes is realized, and the resource and energy consumption in the production process is reduced.
2. The production process is safe, avoids the danger of reaction, has good purification effect, and can be used for preparing high-purity LiPF 6 Or NaPF 6 。
3. The hexafluorophosphate obtained by the process has the purity of 99.99 percent, the moisture content of less than 2ppm and the free acid (calculated by HF) content of less than 6ppm.
Drawings
FIG. 1 is a flow chart of a process for low cost production of hexafluorophosphate in an embodiment of the present invention.
Detailed Description
The invention relates to a process for producing hexafluorophosphate at low cost, which comprises the following steps:
a. the dry air, fluorite, sulfur and phosphor-containing material react to generate PF 5 Crude products; the phosphorus-containing material is wet concentrated phosphoric acid, polyphosphoric acid and P 2 O 5 Solid yellow phosphorus or liquid yellow phosphorus;
b、PF 5 the crude product is frozen and purified, then the reaction kettle with liquid yellow phosphorus is introduced, excessive oxygen reacts with the yellow phosphorus, and oxygen is removed, thus obtaining the purified PF 5 A gas;
c. purified PF 5 The gas reacts with fluoride salt, the temperature is controlled below 15 ℃ in the reaction process, the product is extracted by adding a solvent of lithium battery electrolyte, and liquid hexafluorophosphate is obtained through static layering and filtering, wherein the fluoride salt is LiF or NaF.
The invention realizes the transverse development of multi-product coupling through material replacement and process innovation, has safe production process, avoids the danger of reaction, has good purification effect, and can be used for preparing high-purity LiPF 6 Or NaPF 6 . The hexafluorophosphate obtained by the process has the purity of 99.99 percent, the moisture content of less than 2ppm and the free acid (calculated by HF) content of less than 6ppm.
In one embodiment of the invention, in step a, the moisture content of the dry air is below 20wt%.
In one embodiment of the present invention, in the step b, the freezing temperature of the freeze purification is-40 to 15 ℃ and the pressure is 0.0 to 0.5MPa. H can be isolated by deep freeze purification 2 O。
To remove coarse PF 5 Adding liquid yellow phosphorus into the reaction kettle, and then reacting to generate P 2 O 3 In one embodiment of the invention, in step b, the reaction is carried out at 30 ℃.
To save forAbout the cost, realizing the recycling of materials, in one embodiment of the invention, in the step b, the P generated by the reaction 2 O 3 And (c) returning to the step a to replace yellow phosphorus as a reaction raw material.
In one embodiment of the invention, step c is carried out in a fluidized bed reactor or a jacketed reactor. Preferably, in the step c, the fluoride salt is granular, the proportion of the granules with the grain diameter of 250-380 mu m is 25-35 wt%, and the rest is the granules with the grain diameter of 100-200 mu m; preferably, the particles having a particle size of 250 to 380 μm account for 30wt%. The coarse particles can play a role in crushing the fine particles, so that acting force among the fine particles is reduced. Through the configuration of different particles, the agglomeration of fluoride salt particles is effectively reduced, good fluidization is realized, and the generated hexafluorophosphate is prevented from completely coating solid particles, so that the further progress of the reaction is prevented, and the yield and purity are improved.
In the step c, the solvent of the lithium battery electrolyte which is commonly used in the art and can dissolve hexafluorophosphate is adopted for extraction, and in one embodiment of the invention, the solvent of the lithium battery electrolyte in the step c is at least one of ethylene glycol dimethyl ether diethyl ether, isopropyl ether, anisole, propylene carbonate, methyl ethyl carbonate, ethylene carbonate, vinylene carbonate and methyl propionate.
In one embodiment of the invention, in step c, the liquid hexafluorophosphate is concentrated and crystallized and filtered to give solid hexafluorophosphate.
The following describes the invention in more detail with reference to examples, which are not intended to limit the invention thereto.
Example 1
As shown in fig. 1, a process for producing lithium hexafluorophosphate at low cost comprises the following steps:
(1) Drying air in fluidized bed or reactor, concentrating phosphoric acid, fluorite and sulfur to obtain PF at temperature lower than 150deg.C 5 、H 2 O, etc.
(2) Introducing the crude phosphorus pentafluoride into a freezing bubble tower, and operating at the temperature of-40 ℃ to 15 ℃ to operate the freezing bubble towerSeparating H by freezing under 0.0-0.5MPa 2 O. To remove coarse PF 5 Adding liquid yellow phosphorus into a reaction kettle, and igniting at 30deg.C to generate P 2 O 3 Returning to the first fluidized bed or the reaction kettle.
(3) Purified PF 5 The gas reacts with LiF in a fluidized bed reactor.
To the fluidized bed reactor, 30wt% of coarse LiF particles of 250 to 380 μm and the balance of fine LiF particles of 100 to 200 μm were added. The coarse particles can break up the fine particles, and reduce the acting force among the fine particles. The addition of coarse particles can effectively reduce the agglomeration of LiF particles and realize good reaction.
The temperature is controlled below 15 ℃ in the reaction process. Extracting the product with ethylene glycol dimethyl ether (DME), standing, and filtering to obtain liquid LiPF 6 Recovering heat generated by yellow phosphorus combustion, concentrating and crystallizing to obtain solid LiPF 6 The product, insoluble LiF, is returned to the fluidized bed reactor of step (3).
The purity of the purified lithium hexafluorophosphate product obtained by crystallization in this example was 99.99%, the moisture content was less than 2ppm, and the free acid (calculated as HF) content was less than 6ppm.
Example 2
As shown in fig. 1, a process for producing sodium hexafluorophosphate at low cost comprises the following steps:
(1) Drying air in fluidized bed or reactor to obtain excessive polyphosphoric acid, fluorite and sulfur at a temperature lower than 150deg.C to obtain PF 5 、H 2 O, etc.
(2) Introducing the crude phosphorus pentafluoride into a freezing bubble column with the operating temperature of-40 ℃ to 15 ℃ and the operating pressure of the freezing bubble column of 0.0-0.5MPa, and separating H by freezing 2 O. To remove coarse PF 5 Adding liquid yellow phosphorus into a reaction kettle, and igniting at 30deg.C to generate P 2 O 3 Returning to the first fluidized bed or the reaction kettle.
(3) Purified PF 5 The gas reacts with the NaF in a fluidized bed reactor.
30wt% of NaF coarse particles of 250-380 mu m and the balance of fine particles of 100-200 mu m are added into a fluidized bed reactor. The coarse particles can break up the fine particles, and reduce the acting force among the fine particles. The addition of the coarse particles can effectively reduce the agglomeration of NaF particles and realize good reaction.
The temperature is controlled below 15 ℃ in the reaction process. Extracting the product with ethylene glycol dimethyl ether (DME), standing, and filtering to obtain liquid NaPF 6 Recovering heat generated by yellow phosphorus combustion, concentrating and crystallizing to obtain solid NaFPF 6 The product, insoluble NaF, is returned to the fluidized bed reactor of step (3).
The purity of the purified lithium hexafluorophosphate product obtained by crystallization in this example was 99.99%, the moisture content was less than 2ppm, and the free acid (calculated as HF) content was less than 6ppm.
Example 3
As shown in fig. 1, a process for producing lithium hexafluorophosphate at low cost comprises the following steps:
(1) Passing dry air, excess P in a fluidized bed or reactor 2 O 5 Generating PF with fluorite and sulfur at a temperature lower than 150deg.C 5 、H 2 O, etc.
(2) Introducing the crude phosphorus pentafluoride into a freezing bubble column with the operating temperature of-40 ℃ to 15 ℃ and the operating pressure of the freezing bubble column of 0.0-0.5MPa, and separating H by freezing 2 O. To remove coarse PF 5 Adding liquid yellow phosphorus into a reaction kettle, and igniting at 30deg.C to generate P 2 O 3 Returning to the first fluidized bed or the reaction kettle.
(3) Purified PF 5 The gas reacts with LiF in a fluidized bed reactor.
To the fluidized bed reactor, 30wt% of coarse LiF particles of 250 to 380 μm and the balance of fine LiF particles of 100 to 200 μm were added. The coarse particles can break up the fine particles, and reduce the acting force among the fine particles. The addition of coarse particles can effectively reduce the agglomeration of LiF particles and realize good reaction.
The temperature is controlled below 15 ℃ in the reaction process. The product is extracted by adding ethylene glycol dimethyl ether (DME) and is processed byFiltering by static layering to obtain liquid LiPF 6 Recovering heat generated by yellow phosphorus combustion, concentrating and crystallizing to obtain solid LiPF 6 The product, insoluble LiF, is returned to the fluidized bed reactor of step (3).
The purity of the purified lithium hexafluorophosphate product obtained by crystallization in this example was 99.99%, the moisture content was less than 2ppm, and the free acid (calculated as HF) content was less than 6ppm.
Example 4
As shown in fig. 1, a process for producing sodium hexafluorophosphate at low cost comprises the following steps:
(1) Drying air in fluidized bed or reactor to obtain excessive solid yellow phosphorus, fluorite and sulfur at temperature lower than 150deg.C to obtain PF 5 、H 2 O, etc.
(2) Introducing the crude phosphorus pentafluoride into a freezing bubble column with the operating temperature of-40 ℃ to 15 ℃ and the operating pressure of the freezing bubble column of 0.0-0.5MPa, and separating H by freezing 2 O. To remove coarse PF 5 Adding liquid yellow phosphorus into a reaction kettle, and igniting at 30deg.C to generate P 2 O 3 Returning to the first fluidized bed or the reaction kettle.
(3) Purified PF 5 The gas reacts with the NaF in a fluidized bed reactor.
30wt% of NaF coarse particles of 250-380 mu m and the balance of fine particles of 100-200 mu m are added into a fluidized bed reactor. The coarse particles can break up the fine particles, and reduce the acting force among the fine particles. The addition of the coarse particles can effectively reduce the agglomeration of NaF particles and realize good reaction.
The temperature is controlled below 15 ℃ in the reaction process. Extracting the product with ethylene glycol dimethyl ether (DME), standing, and filtering to obtain liquid NaPF 6 Recovering heat generated by yellow phosphorus combustion, concentrating and crystallizing to obtain solid NaFPF 6 The product, insoluble NaF, is returned to the fluidized bed reactor of step (3).
The purity of the purified lithium hexafluorophosphate product obtained by crystallization in this example was 99.99%, the moisture content was less than 2ppm, and the free acid (calculated as HF) content was less than 6ppm.
Example 5
As shown in fig. 1, a process for producing lithium hexafluorophosphate at low cost comprises the following steps:
(1) Drying air in fluidized bed or reactor to obtain excessive liquid yellow phosphorus, fluorite and sulfur at temperature lower than 150deg.C to obtain PF 5 、H 2 O, etc.
(2) Introducing the crude phosphorus pentafluoride into a freezing bubble column with the operating temperature of-40 ℃ to 15 ℃ and the operating pressure of the freezing bubble column of 0.0-0.5MPa, and separating H by freezing 2 O. To remove coarse PF 5 Adding liquid yellow phosphorus into a reaction kettle, and igniting at 30deg.C to generate P 2 O 3 Returning to the first fluidized bed or the reaction kettle.
(3) Purified PF 5 The gas reacts with LiF in a fluidized bed reactor.
To the fluidized bed reactor, 30wt% of coarse LiF particles of 250 to 380 μm and the balance of fine LiF particles of 100 to 200 μm were added. The coarse particles can break up the fine particles, and reduce the acting force among the fine particles. The addition of coarse particles can effectively reduce the agglomeration of LiF particles and realize good reaction.
The temperature is controlled below 15 ℃ in the reaction process. Extracting the product with ethylene glycol dimethyl ether (DME), standing, and filtering to obtain liquid LiPF 6 Recovering heat generated by yellow phosphorus combustion, concentrating and crystallizing to obtain solid LiPF 6 The product, insoluble LiF, is returned to the fluidized bed reactor of step (3).
The purity of the purified lithium hexafluorophosphate product obtained by crystallization in this example was 99.99%, the moisture content was less than 2ppm, and the free acid (calculated as HF) content was less than 6ppm.
Claims (9)
1. A process for the low cost production of hexafluorophosphate comprising the steps of:
a. the dry air, fluorite, sulfur and phosphor-containing material react to generate PF 5 Crude products; the phosphorus-containing material is wet concentrated phosphoric acid, polyphosphoric acid and P 2 O 5 Solid yellow phosphorus or liquid yellow phosphorus;
b、PF 5 the crude product is frozen and purified, and then is introduced into a reaction kettle with liquid yellow phosphorus for reaction, thus obtaining the purified PF 5 A gas;
c. purified PF 5 The gas reacts with fluoride salt, the temperature is controlled below 15 ℃ in the reaction process, the product is extracted by adding a solvent of lithium battery electrolyte, and liquid hexafluorophosphate is obtained through static layering and filtering, wherein the fluoride salt is LiF or NaF.
2. The process for low cost production of hexafluorophosphate according to claim 1, wherein: in step a, the moisture content of the dry air is lower than 20wt%.
3. The process for low cost production of hexafluorophosphate according to claim 1, wherein: in the step b, the freezing temperature of the freezing purification is-40-15 ℃ and the pressure is 0.0-0.5 MPa.
4. The process for low cost production of hexafluorophosphate according to claim 1, wherein: in step b, the reaction is carried out at 30 ℃.
5. The process for low cost production of hexafluorophosphate according to claim 1, wherein: in step b, P produced by the reaction 2 O 3 And returning to the step a.
6. The process for low cost production of hexafluorophosphate according to claim 1, wherein: in the step c, the fluoride salt is granular, the proportion of the granules with the grain diameter of 250-380 mu m is 25-35 wt%, and the rest is the granules with the grain diameter of 100-200 mu m.
7. The process for low-cost production of hexafluorophosphate according to claim 6, wherein: in the step c, the particle ratio of the particles with the particle size of 250-380 mu m is 30wt%.
8. The process for low cost production of hexafluorophosphate according to claim 1, wherein: in the step c, the solvent of the lithium battery electrolyte is at least one of ethylene glycol dimethyl ether, isopropyl ether, anisole, propylene carbonate, methyl ethyl carbonate, ethylene carbonate, vinylene carbonate and methyl propionate.
9. The process for low cost production of hexafluorophosphate according to claim 1, wherein: and c, concentrating and crystallizing the liquid hexafluorophosphate, and filtering to obtain the solid hexafluorophosphate.
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