CN115594198A - Method for preparing battery-grade sodium fluoride by one-step method and obtained product - Google Patents
Method for preparing battery-grade sodium fluoride by one-step method and obtained product Download PDFInfo
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- CN115594198A CN115594198A CN202211286914.XA CN202211286914A CN115594198A CN 115594198 A CN115594198 A CN 115594198A CN 202211286914 A CN202211286914 A CN 202211286914A CN 115594198 A CN115594198 A CN 115594198A
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- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 title claims abstract description 104
- 235000013024 sodium fluoride Nutrition 0.000 title claims abstract description 51
- 239000011775 sodium fluoride Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 47
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000003513 alkali Substances 0.000 claims abstract description 17
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 8
- 230000000694 effects Effects 0.000 claims abstract description 4
- 238000005728 strengthening Methods 0.000 claims abstract description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 239000000047 product Substances 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 11
- -1 polytetrafluoroethylene Polymers 0.000 claims description 10
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 10
- 239000000706 filtrate Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- 238000010907 mechanical stirring Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 238000003828 vacuum filtration Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims 1
- 238000000746 purification Methods 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 235000017550 sodium carbonate Nutrition 0.000 description 9
- 235000011121 sodium hydroxide Nutrition 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 230000002572 peristaltic effect Effects 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 235000012239 silicon dioxide Nutrition 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000005188 flotation Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000002000 Electrolyte additive Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000013094 purity test Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/02—Fluorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Secondary Cells (AREA)
Abstract
The invention provides a method for preparing battery-grade sodium fluoride by a one-step method and an obtained product, belonging to the technical field of battery materials. The battery-grade sodium fluoride product is prepared by introducing the strengthening effect of an ultrasonic field in the neutralization reaction process of high-purity hydrofluoric acid and high-purity alkali. The method can prepare the battery-grade sodium fluoride product in one step by improving a hydrofluoric acid neutralization method, not only has the product purity as high as 99.99 percent, but also omits a complicated purification process, and is easy for industrial production.
Description
Technical Field
The invention belongs to the technical field of battery materials, and particularly relates to a method for preparing battery-grade sodium fluoride by a one-step method and an obtained product.
Background
With the development of new energy technology, the application of lithium ion batteries is explosively increased, and the problems of lithium ore resource shortage and rapid cost rise are simultaneously caused, while sodium ore resources are rich and relatively low in cost, the sodium ion batteries can perfectly make up the dilemma faced by lithium batteries in the fields of energy storage and low-speed electric vehicles, partial or even complete substitution is realized, sodium hexafluorophosphate in sodium salt is similar to lithium hexafluorophosphate in lithium salt and occupies an important position, battery-grade sodium fluoride can be used as a raw material of sodium hexafluorophosphate, the application prospect is wide, but few existing battery-grade sodium fluoride enterprises in the market exist, and the industrial-grade sodium fluoride purification process faces numerous problems of complex technical route, high cost and the like.
At present, sodium fluoride is prepared most commonly and widely by a sodium fluosilicate soda ash method, and a method for preparing sodium fluoride by the sodium fluosilicate soda ash method is reported in patent CN 106517246B, wherein a sodium fluosilicate solution soda ash solution is sequentially and continuously added into a tubular reactor to generate sodium fluoride and silicon dioxide slurry, the sodium fluoride and the silicon dioxide slurry enter a multi-stage flotation device for flotation, the slurry containing the sodium fluoride and the slurry containing the silicon dioxide are respectively obtained after the flotation, and the sodium fluoride product and the silicon dioxide product are respectively obtained by centrifugation, washing and drying, wherein the purity of the sodium fluoride prepared by the method is only about 98.5 percent, and the problem that the silicon dioxide and the sodium fluoride are not completely separated exists; in the inorganic salt industry handbook, a method for preparing sodium fluoride by a hydrofluoric acid neutralization method is recorded, wherein hydrofluoric acid with the mass fraction of 40% is added into a lead-making reaction kettle, then soda ash or caustic soda solution is slowly added for neutralization, and a sodium fluoride product is obtained through crystallization, centrifugal dehydration and drying, so that the problems of low product purity and high cost exist; the method for preparing sodium fluoride from high-purity sodium carbonate and hydrofluoric acid in a water phase is recorded in high-purity reagent purification and preparation, and the sodium fluoride prepared by the method has the problems of anions and cations and multiphase micro-inclusion, and cannot meet the requirement of a battery-grade electrolyte additive on raw materials. Therefore, the preparation method of the battery-grade sodium fluoride, which is simple and convenient and is easy for industrial production and has high product purity, is very important.
Disclosure of Invention
The invention provides a method for preparing battery-grade sodium fluoride by a one-step method and an obtained product, the method can prepare the battery-grade sodium fluoride product by one step by improving a hydrofluoric acid neutralization method and applying an ultrasonic field effect in the preparation process, the purity of the product is up to 99.99 percent, a complex purification process is omitted, and the method is easy for industrial production.
In order to achieve the aim, the invention provides a method for preparing battery-grade sodium fluoride by a one-step method, which is prepared by introducing the strengthening effect of an ultrasonic field in the neutralization reaction process of high-purity hydrofluoric acid and high-purity alkali.
Preferably, the high-purity alkali is sodium carbonate or sodium hydroxide, and the purity is more than 99.8%; the high-purity hydrofluoric acid is electronic grade, and the purity is more than 99.99%.
Preferably, the molar ratio of the added high-purity hydrofluoric acid to the added high-purity soda is 1: (0.5-1).
Preferably, the ultrasonic power of the ultrasonic field is 50-1000w, and the time is 0.5-5h. It can be understood that the high ultrasonic power or the long ultrasonic time has no influence on the product quality, but the problems of high power and long ultrasonic time, such as high energy consumption, energy saving and the like, are involved, so that the excessively high ultrasonic power and the excessively long ultrasonic time are not needed.
Preferably, the method specifically comprises the following steps:
adding a proper amount of deionized water into the reactor, adding high-purity soda powder while stirring, and continuously stirring to obtain alkali liquor 1;
weighing high-purity hydrofluoric acid according to a proportion, slowly dripping the weighed high-purity hydrofluoric acid into the alkali liquor 1 at the speed of 3-15ml/min, and simultaneously stirring and ultrasonically treating in the dripping process;
and filtering the obtained reaction mixed liquid to obtain a sodium fluoride wet material and filtrate, and drying the obtained wet material to obtain a battery-grade sodium fluoride product.
Preferably, the obtained filtrate is saturated sodium fluoride filtrate, deionized water and high-purity alkali are supplemented, then alkali liquor 1 is continuously prepared, and the filtrate is continuously recycled according to the subsequent steps.
Preferably, the stirring mode is mechanical stirring or magnetic stirring, the rotating speed is 100-500rpm, and the stirring time is 0.5-2h; the drying temperature is 60-100 ℃, and the drying time is 3-7h. It is understood that the stirring speed may be 100, 150, 200, 250, 300, 350, 400, 450, 500rpm or any speed value in the above range according to actual conditions, and the stirring time may be 0.5, 1, 1.5, 2h or any time value in the above range; in addition, the drying temperature may be 60, 65, 70, 75, 80, 85, 90, 95, 100 ℃ or any temperature value within the above range, and the drying time may be 3, 3.5, 4, 4.5, 5, 5.5, 6, 6.5, 7h or any time value within the above range, according to actual conditions.
Preferably, the reactor used is a polytetrafluoroethylene or stainless steel reactor with a polytetrafluoroethylene liner; when filtering, a polytetrafluoroethylene filtering membrane with the aperture of 0.22-1um is adopted, the filtering mode is negative pressure vacuum filtration, and the pressure is-0.1 MPa.
The invention also provides battery-grade sodium fluoride prepared by the preparation method according to any one of the technical schemes.
Preferably, the particle size D of the battery grade sodium fluoride 50 20-100 um, high purity up to more than 99.99%, less than or equal to 10ppm of chloride ions and less than or equal to 1ppm of sulfate radicals.
Compared with the prior art, the invention has the advantages and positive effects that:
1. the invention provides a preparation method of battery-grade sodium fluoride, which is prepared by introducing an ultrasonic field strengthening effect in the neutralization reaction process of high-purity acid and high-purity alkali through an improved hydrofluoric acid neutralization preparation process. In the preparation process of the ultrasonic field, on one hand, ion micro-inclusions existing in raw materials of acid and alkali can be removed through ultra-strong penetrating force, on the other hand, the crystallization process of sodium fluoride crystals can be regulated and controlled, sodium fluoride products with small particle size and uniform size are obtained, the impurity ions are reduced to the maximum extent and enter sodium fluoride crystal grains in a wrapping manner, the content of the impurity ions is controlled from the source, the product purity can reach more than 99.99%, the chloride ions are less than or equal to 10ppm, the sulfate radicals are less than or equal to 1ppm, and the requirements of a battery-grade electrolyte additive on the raw materials are completely met.
2. The method provided by the invention can prepare the battery-grade sodium fluoride by one-step method, the reaction is simple and convenient, the complicated purification process is saved, the mother liquor can be recycled after the reaction, the comprehensive yield of the sodium fluoride product is more than 90%, and the industrial production is easy to realize.
Drawings
FIG. 1 is a flow diagram of the preparation of battery grade sodium fluoride;
figure 2 is an XRD spectrum of example 4, example 14 and a sodium fluoride standard.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The sodium hydroxide used in the following examples and comparative examples had a purity of 99.8% or more, and the hydrofluoric acid was of electronic grade and had a purity of 99.99% or more.
Example 1
The preparation process is shown in figure 1:
putting 200g of deionized water into a reactor A, starting mechanical stirring at the rotating speed of 300rpm, adding 50g of sodium hydroxide powder while stirring, and continuously stirring for 1 hour after the addition of the sodium hydroxide powder to obtain an alkali liquor 1;
transferring the alkali liquor 1 into a reactor B, taking 44.2ml of 49% hydrofluoric acid, and slowly dripping the hydrofluoric acid into the alkali liquor 1 by adopting a peristaltic pump at the speed of 3 ml/min;
in the dripping process, simultaneously starting a stirring device and an ultrasonic device, wherein the mechanical stirring speed is 300rpm, the ultrasonic power is 600w, and the ultrasonic stirring time is 4 hours;
filtering the obtained reaction mixed solution by adopting a 0.45-micron polytetrafluoroethylene filter membrane, wherein the pressure of a vacuum pump is-0.1 MPa during filtering, and filtering to obtain a sodium fluoride wet material and a filtrate;
drying the obtained wet material in a 90 ℃ forced air drying oven for 4 hours to obtain a battery-grade sodium fluoride product;
and transferring the filtrate into a reactor A, supplementing deionized water and sodium hydroxide powder to prepare alkali liquor 1, precipitating partial sodium fluoride crystals, and reacting and recycling the mixed liquor according to the subsequent steps.
Example 2
The preparation is as in example 1, except that the peristaltic pump speed is 6ml/min.
Example 3
The preparation process is the same as in example 1, except that the peristaltic pump speed is 9ml/min.
Example 4
The preparation process is the same as in example 1, except that the peristaltic pump speed is 12ml/min.
Example 5
The preparation process is the same as in example 1, except that the peristaltic pump speed is 15ml/min.
Example 6
The preparation method is the same as example 4, except that the ultrasonic power is 50w.
Example 7
The preparation method is the same as example 4, except that the ultrasonic power is 200w.
Example 8
The preparation method is the same as example 4, except that the ultrasonic power is 400w.
Example 9
The preparation process is the same as in example 4, except that the ultrasonic power is 800w.
Example 10
The preparation process is the same as in example 4, except that the ultrasonic power is 1000w.
Example 11
The preparation method is the same as example 4, except that the ultrasonic stirring time is 0.5h.
Example 12
The preparation method is the same as example 4, except that the ultrasonic stirring time is 2.5h.
Example 13
The preparation method is the same as example 4, except that the ultrasonic stirring time is 5h.
Example 14
The preparation method is the same as that of example 1, except that sodium carbonate is added as the soda ash, and the addition amount of hydrofluoric acid is 33.4ml (mass concentration is 49%).
Comparative example 1
The preparation method is the same as example 4, except that the ultrasonic power is 40w.
Comparative example 2
The preparation process is the same as in example 12, except that ultrasonic agitation is not performed.
Comparative example 3
The preparation process is the same as in example 3, except that the peristaltic pump speed is 16ml/min.
Performance testing
The sodium fluoride prepared in the above examples and comparative examples were subjected to a particle size test, a purity test and an ion content test, and the test results are shown in table 1 below.
TABLE 1 summary of test results for examples and comparative examples
The data in table 1 show that the hydrofluoric acid is not dripped too fast or too slow, too fast dripping can cause too violent reaction, the crystal formation speed is too fast, the product purity is influenced, and too slow dripping influences the synthesis efficiency; the ultrasonic power can not be too low or not be introduced, because the ultrasonic penetration acting force is insufficient due to too low ultrasonic penetration, micro-inclusions in product crystals are difficult to remove, the purity of the product is influenced, and the energy consumption control in the synthesis process is also not favorable when the ultrasonic power is continuously increased after reaching a certain value.
Verification experiment
Taking the sodium fluoride products prepared by respectively adopting sodium hydroxide and sodium carbonate in the above embodiment 4 and 14 as examples, comparing the XRD peak pattern with that of the sodium fluoride standard sample, as shown in fig. 2, the two peaks have the same peak pattern and no other impurity peak, which proves that the preparation method provided by the present invention can effectively prepare the battery-grade sodium fluoride product with high purity.
Claims (10)
1. The method for preparing the battery-grade sodium fluoride by the one-step method is characterized in that the battery-grade sodium fluoride is prepared by introducing the strengthening effect of an ultrasonic field in the neutralization reaction process of high-purity hydrofluoric acid and high-purity alkali.
2. The method according to claim 1, wherein the high-purity soda is sodium carbonate or sodium hydroxide, and the purity is more than 99.8%; the high-purity hydrofluoric acid is of electronic grade, and the purity is more than 99.99%.
3. The method according to claim 1 or 2, wherein the molar ratio of the high-purity hydrofluoric acid to the high-purity soda is 1: (0.5-1).
4. Method according to claim 1 or 2, characterized in that the ultrasonic field has an ultrasonic power of 50-1000w and a time of 0.5-5h.
5. The method according to any one of claims 1 to 4, comprising in particular the steps of:
adding a proper amount of deionized water into the reactor, adding high-purity soda powder while stirring, and continuously stirring to obtain alkali liquor 1;
weighing high-purity hydrofluoric acid according to a proportion, slowly dripping the weighed high-purity hydrofluoric acid into the alkali liquor 1 at the speed of 3-15ml/min, and simultaneously stirring and carrying out ultrasound in the dripping process;
and filtering the obtained reaction mixed liquid to obtain a sodium fluoride wet material and filtrate, and drying the obtained wet material to obtain a battery-grade sodium fluoride product.
6. The method as claimed in claim 5, wherein the filtrate is saturated sodium fluoride filtrate, and after the deionized water and the high-purity soda are supplemented, the alkali liquor 1 is continuously prepared and recycled according to the subsequent steps.
7. The method according to claim 5, wherein the stirring mode is mechanical stirring or magnetic stirring, the rotating speed is 100-500rpm, and the stirring time is 0.5-2h; the drying temperature is 60-100 ℃, and the drying time is 3-7h.
8. The process according to claim 5, characterized in that the reactor used is a polytetrafluoroethylene or stainless steel reactor with polytetrafluoroethylene lining; the filtration is carried out by adopting a polytetrafluoroethylene filtration membrane with the aperture of 0.22-1um, and the filtration mode is negative pressure vacuum filtration, and the pressure is-0.1 MPa.
9. Battery grade sodium fluoride, characterized in that it is prepared according to the process of any one of claims 1 to 9.
10. The battery-grade sodium fluoride of claim 9, wherein the particle size D of the resulting battery-grade sodium fluoride 50 20-100 um, high purity up to more than 99.99%, less than or equal to 10ppm of chloride ions and less than or equal to 1ppm of sulfate radicals.
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| CN117361573A (en) * | 2023-11-13 | 2024-01-09 | 山东立中新能源材料有限公司 | Method for directly preparing battery-grade sodium fluoride from industrial-grade sodium carbonate |
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| CN103964447A (en) * | 2014-05-31 | 2014-08-06 | 苏州恒瑞生物医药科技有限公司 | Method for producing fluoride and white carbon black by accelerating hydrolysis of fluosilicate with ultrasonic waves |
| CN106517246A (en) * | 2016-11-21 | 2017-03-22 | 衡阳市锦轩化工有限公司 | Method for continuously producing sodium fluoride |
| CN108439479A (en) * | 2018-04-24 | 2018-08-24 | 邯郸钢铁集团有限责任公司 | Cold-rolling pickling waste liquid prepares nanometer Fe2O3The system and method for photochemical catalyst |
| CN111871351A (en) * | 2020-08-10 | 2020-11-03 | 邵武永太高新材料有限公司 | Lithium fluoride ultrasonic dynamic reaction crystallization process and ultrasonic dynamic reaction crystallization equipment thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117361573A (en) * | 2023-11-13 | 2024-01-09 | 山东立中新能源材料有限公司 | Method for directly preparing battery-grade sodium fluoride from industrial-grade sodium carbonate |
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