CN117776129A - Method for producing high-purity battery grade monoammonium phosphate by using purified phosphoric acid byproduct washing residual acid - Google Patents
Method for producing high-purity battery grade monoammonium phosphate by using purified phosphoric acid byproduct washing residual acid Download PDFInfo
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- CN117776129A CN117776129A CN202311844511.7A CN202311844511A CN117776129A CN 117776129 A CN117776129 A CN 117776129A CN 202311844511 A CN202311844511 A CN 202311844511A CN 117776129 A CN117776129 A CN 117776129A
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- phosphoric acid
- concentration
- monoammonium phosphate
- neutralized
- battery grade
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 35
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 title claims abstract description 33
- 235000019837 monoammonium phosphate Nutrition 0.000 title claims abstract description 33
- 239000006012 monoammonium phosphate Substances 0.000 title claims abstract description 31
- 238000005406 washing Methods 0.000 title claims abstract description 31
- 239000002253 acid Substances 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 239000006227 byproduct Substances 0.000 title claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000004176 ammonification Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- 150000003839 salts Chemical class 0.000 claims abstract description 9
- 239000002002 slurry Substances 0.000 claims abstract description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001953 recrystallisation Methods 0.000 claims abstract description 5
- 238000007865 diluting Methods 0.000 claims abstract description 3
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 3
- 238000001816 cooling Methods 0.000 claims description 14
- 230000032683 aging Effects 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 230000005484 gravity Effects 0.000 claims description 5
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 17
- 239000011574 phosphorus Substances 0.000 abstract description 17
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 17
- 239000012535 impurity Substances 0.000 abstract description 16
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000006477 desulfuration reaction Methods 0.000 abstract description 4
- 230000023556 desulfurization Effects 0.000 abstract description 4
- 238000003825 pressing Methods 0.000 abstract description 4
- 238000006115 defluorination reaction Methods 0.000 abstract description 3
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 2
- 238000002425 crystallisation Methods 0.000 description 18
- 230000008025 crystallization Effects 0.000 description 18
- 239000013078 crystal Substances 0.000 description 14
- 239000000706 filtrate Substances 0.000 description 12
- 239000003337 fertilizer Substances 0.000 description 7
- 239000012065 filter cake Substances 0.000 description 6
- 239000012528 membrane Substances 0.000 description 6
- 239000011575 calcium Substances 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 239000004254 Ammonium phosphate Substances 0.000 description 3
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 3
- 235000019289 ammonium phosphates Nutrition 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 235000015097 nutrients Nutrition 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000001694 spray drying Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052785 arsenic Inorganic materials 0.000 description 2
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 239000002686 phosphate fertilizer Substances 0.000 description 2
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- Fertilizers (AREA)
Abstract
The invention discloses a method for producing high-purity battery grade monoammonium phosphate by utilizing purified phosphoric acid byproduct washing residual acid, which comprises the following steps: desorbing purified phosphoric acid byproduct washing residual acid in a concentration tower, adding desalted water, and diluting to P 2 O 5 The concentration is 25% -28%, the neutralization reaction is carried out with liquid ammonia in an ammonification reactor, the pH of the reaction end point is controlled to be 3.8-4.7, neutralized slurry is obtained, neutralized clear liquid obtained by filter pressing of the neutralized slurry is kept stand and aged for 8-16 hours at the temperature of 45-60 ℃, concentrated, cooled and crystallized at the end point temperature of 35-45 ℃, and high-purity battery grade monoammonium phosphate is obtained through salt washing, recrystallization treatment and fluidized bed drying. The invention uses purified phosphoric acid byproduct spent acid as raw material to pass through the industrial production method of ammonification reaction, impurity removal, concentration and drying, the production process does not need procedures of desulfurization, defluorination, heavy metal removal and the like, the process is simple, the production cost is low, the impurity removal rate is high, the phosphorus yield is high, and a new way for efficiently utilizing phosphorus resources is provided for the spent acid of wet purification phosphoric acid production enterprises.
Description
Technical Field
The invention belongs to the technical field of comprehensive utilization of phosphoric acid chemical washing residual acid, and particularly relates to a method for producing high-purity battery grade monoammonium phosphate by utilizing purified phosphoric acid byproduct washing residual acid.
Background
The yield of wet purified phosphoric acid increases to 300 ten thousand tons for 2023 years, 500 ten thousand tons for 2025 years is expected, and the yield of spent acid will reach 100 ten thousand tons. The concentration of the residual acid after desorption and concentration is high, the impurity content is low, the residual acid is currently used for producing phosphate fertilizer, feed additives and the like, and the utilization value of a phosphorus source is low.
Monoammonium phosphate (also known as monoammonium phosphate) is one of the phosphorus sources for synthesizing lithium iron phosphate cathode materials. Most of monoammonium phosphate in the market is in industrial grade, and the impurity content is difficult to meet the requirement of preparing battery grade. In order to improve the purity, most enterprises adopt wet crude phosphoric acid or industrial monoammonium phosphate as raw materials, and because arsenic and sulfate radical contents are high, arsenic removal and desulfurization process treatment are required, so that the cost is increased, the phosphorus yield is low, and the purity is difficult to meet the requirements. At present, high-purity hot phosphoric acid or wet purification industrial phosphoric acid is utilized to produce battery grade monoammonium phosphate, but the production cost is high; for cost reduction, the following publication numbers are: CN106629644 a, a patent entitled a method for producing industrial primary and battery grade monoammonium phosphate from chemical fertilizer grade monoammonium phosphate, is high in raw material acid impurity, and needs to be subjected to impurity removal for many times, so that the cost is increased; for example, the publication number is CN 116425132A, the name is a patent of a preparation method of high-quality industrial grade monoammonium phosphate, wet phosphoric acid is adopted, and because of high impurity, desulfurization, defluorination and heavy metal removal are needed, and the flow is complicated; the method for preparing battery grade monoammonium phosphate by using phosphate fertilizer has the publication number of CN 116588908A and the application thereof, and has long production flow and complex process, and is difficult to realize industrialization.
Disclosure of Invention
The invention aims to solve the defects of the prior art, and provides a method for producing high-purity battery grade monoammonium phosphate by ammonification reaction, impurity removal, concentration, drying and the like by taking the purified phosphoric acid byproduct washing acid as a raw material, adopting the process without the procedures of desulfurization, defluorination, heavy metal removal and the like, and realizing industrial production.
The technical scheme adopted by the invention is as follows:
the method for producing the high-purity battery grade monoammonium phosphate by utilizing the byproduct of purified phosphoric acid and the surplus acid comprises the following steps:
step 1, desorbing the purified phosphoric acid byproduct washing residual acid by a concentration tower, adding desalted water and diluting to P 2 O 5 The concentration is 25-28%, and the reaction product is neutralized with liquid ammonia in an ammonification reactor, and the pH of the reaction end point is controlled to be 3.8-4.7, thus obtaining neutralized slurry;
step 2, press-filtering the neutralized slurry in the step 1 to obtain a neutralized clear liquid;
and step 3, standing and aging the neutralized clear liquid in the step 2 at 45-60 ℃ for 8-16 hours, concentrating, cooling and crystallizing to a final temperature of 35-45 ℃, and carrying out salt washing, recrystallization treatment and fluidized bed drying to obtain the high-purity battery grade monoammonium phosphate.
Further, the purifying phosphoric acid by-product is P in the washing residual acid 2 O 5 The concentration is more than or equal to 50 percent, the MER value is 2 percent, and the MER in the concentrated phosphoric acid refers to the sesquioxide in the phosphoric acidAnd->The ratio of the contents, i.e. mer= (-je)>+/>++/>+silica+manganese oxide)/phosphorus pentoxide content.
Further, the neutralization reaction is carried out at a temperature of 85-95 ℃ for 60-120min.
Further, the concentration temperature is 70-90 ℃, and the specific gravity of the end point is 1.36-1.42; salt washing is as follows: washing with a clear liquid, and salt washing with a nearly saturated solution to remove soluble impurities on the surface of the crystal and obtain purer crystal.
Further, the end point temperature of the recrystallization is 25 to 30 ℃.
Further, the drying temperature of the fluidized bed is 85-125 ℃ and the drying time is 10-15min.
The invention has the beneficial effects that:
1. the invention adopts wet method to purify phosphoric acid pickling residual acid as raw material, removes a large amount of impurities such as iron, aluminum and the like to obtain neutralized clear liquid containing ammonium dihydrogen phosphate by controlling pH at 3.8-4.7 through an ammoniation reaction end point of phosphoric acid and liquid ammonia, then stands still and ages the neutralized clear liquid to remove supersaturation degree of the impurities in the solution so as to remove calcium and magnesium impurities in the neutralized clear liquid, and effectively controls crystallization rate at 35-45 ℃ at a crystallization end point temperature so as to lead crystals to complete growth, and introduces salt washing to wash out the impurities attached to the surfaces of the crystals at the crystallization stage to obtain high-purity battery grade ammonium dihydrogen phosphate.
2. The invention has high impurity removal rate and high phosphorus yield in industrial production, and the produced battery grade monoammonium phosphate provides a new way for efficiently utilizing phosphorus resources for the washing residual acid of a production enterprise for purifying phosphoric acid by a wet method.
Drawings
FIG. 1 is a flow chart of the production process of the present invention;
fig. 2 is an XRD analysis pattern of high purity battery grade monoammonium phosphate produced in example 3 of the invention.
Detailed Description
The invention will be further elucidated with reference to the embodiments described in the accompanying drawings, it being understood that the specific embodiments described herein are only illustrative of the invention and are not intended to limit the invention.
Example 1
As shown in fig. 1, a method for producing high-purity battery grade monoammonium phosphate by using purified phosphoric acid byproduct washing residual acid comprises the following steps:
step 1, concentrating the purified phosphoric acid in a phosphoric acid concentration tower to obtain residual acid (P) 2 O 5 Concentration 50%, MER value 2%) is pumped into the reaction tank according to the diluted phosphorus concentration P 2 O 5 Adding desalted water for 28%, then conveying to an ammonification reaction tank by a pump, and introducing liquid ammonia into the ammonification reaction tank for ammonification reaction, wherein the reaction temperature is 85 ℃, and the reaction end point pH is 4.2;
step 2, conveying the neutralized slurry in the step 1 to a box type membrane filter press for filter pressing to obtain a filter cake and filtrate, washing the filter cake by hot water, and spray-drying to obtain fertilizer grade ammonium phosphate with the nutrient P+N of 52% as fertilizer, wherein the yield of the neutralized phosphorus is 96%;
step 3, aging the filtrate for 8 hours under the stirring condition of 45 ℃, filtering the filtrate by a membrane to obtain primary clear liquid, and measuring, standing and aging to reduce Ca in the filtrate from 100Mg/kg to 50Mg/kg and reduce Mg from 500Mg/kg to 300Mg/kg;
separating 1/4 of the primary clear liquid according to the volume ratio, performing salt washing, concentrating the rest 3/4 of the clear liquid in a concentration tower, concentrating the rest 3/4 of the clear liquid in a concentration end point specific gravity of 1.38, and cooling and crystallizing the concentrated clear liquid in a crystallization tank at the crystallization end point temperature of 45 ℃ at the cooling and cooling rate of 4 ℃/min to obtain primary crystals and primary mother liquid;
washing the primary crystallization with primary clear liquid to obtain washed crystals, recrystallizing the washed crystals, adding UP water for complete dissolution, heating to 90 ℃ and concentrating until microcrystalline nuclei appear, returning to a crystallization tank for cooling crystallization, centrifugally filtering, and drying at 95 ℃ under a fluidized bed to obtain high-purity battery grade monoammonium phosphate, wherein the component analysis result is shown in Table 1, and the total phosphorus yield is 60%.
Example 2
As shown in fig. 1, a method for producing high-purity battery grade monoammonium phosphate by using purified phosphoric acid byproduct washing residual acid comprises the following steps:
step 1, concentrating the purified phosphoric acid in a phosphoric acid concentration tower to obtain residual acid (P) 2 O 5 The concentration is 52%, the MER value is 2%) is pumped into the reaction tank according to the phosphorus concentration P after dilution 2 O 5 Adding desalted water to 25%, then conveying to an ammonification reaction tank by a pump, and introducing liquid ammonia into the ammonification reaction tank to carry out ammonification reaction, wherein the reaction temperature is 90 ℃, and the reaction end point pH is 4.5;
step 2, conveying the neutralized slurry in the step 1 to a box type membrane filter press for filter pressing to obtain a filter cake and filtrate, washing the filter cake by hot water, and spray-drying to obtain fertilizer grade ammonium phosphate with the nutrient P+N of 52% as fertilizer, wherein the yield of the neutralized phosphorus is 94%;
step 3, aging the filtrate for 10 hours under the stirring condition of 50 ℃, filtering the filtrate by a membrane to obtain primary clear liquid, and measuring, standing and aging to reduce Ca in the filtrate from 100Mg/kg to 20Mg/kg and reduce Mg from 500Mg/kg to 200Mg/kg;
separating 1/4 of the primary clear liquid according to the volume ratio, performing salt washing, concentrating the rest 3/4 of the clear liquid in a concentration tower, concentrating the rest 3/4 of the clear liquid in a concentration end point specific gravity of 1.4, and then cooling and crystallizing the concentrated clear liquid in a crystallization tank at the crystallization end point temperature of 40 ℃ at the cooling and cooling rate of 4 ℃/min to obtain primary crystals and primary mother liquid;
washing the primary crystallization with a primary clear solution to obtain washed crystals, recrystallizing the washed crystals, adding UP water for complete dissolution, heating to 90 ℃ and concentrating until microcrystalline nuclei appear, returning to a crystallization tank for cooling crystallization, centrifugally filtering, and drying at 120 ℃ under a fluidized bed to obtain high-purity battery grade monoammonium phosphate, wherein the component analysis result is shown in Table 1, and the total phosphorus yield is 65%.
Example 3
As shown in fig. 1, a method for producing high-purity battery grade monoammonium phosphate by using purified phosphoric acid byproduct washing residual acid comprises the following steps:
step 1, concentrating the purified phosphoric acid in a phosphoric acid concentration tower to obtain residual acid (P) 2 O 5 The concentration is 54%, the MER value is 2%) is pumped into the reaction tank, and the concentration P of the diluted phosphorus is calculated 2 O 5 Adding desalted water for 22%, then conveying to an ammonification reaction tank by a pump, and introducing liquid ammonia into the ammonification reaction tank for ammonification reaction, wherein the reaction temperature is 85 ℃, and the reaction end point pH is 4.7;
step 2, conveying the neutralized slurry in the step 1 to a box type membrane filter press for filter pressing to obtain a filter cake and filtrate, washing the filter cake by hot water, and spray-drying to obtain fertilizer grade ammonium phosphate with the nutrient P+N of 52% as fertilizer, wherein the yield of the neutralized phosphorus is 91%;
step 3, aging the filtrate for 16 hours under the stirring condition of 45 ℃, filtering the filtrate by a membrane to obtain primary clear liquid, and measuring, standing and aging to reduce Ca in the filtrate from 100Mg/kg to 30Mg/kg and reduce Mg from 500Mg/kg to 250Mg/kg;
separating 1/4 of the primary clear liquid according to the volume ratio, performing salt washing, concentrating the rest 3/4 of the clear liquid in a concentration tower, concentrating the rest 3/4 of the clear liquid in a concentration end point specific gravity of 1.36, and cooling and crystallizing the concentrated clear liquid in a crystallization tank at the crystallization end point temperature of 35 ℃ at the cooling and cooling rate of 4 ℃/min to obtain primary crystals and primary mother liquid;
washing the primary crystallization with a primary clear solution to obtain washed crystals, recrystallizing the washed crystals, adding UP water for complete dissolution, heating to 70 ℃ and concentrating until microcrystalline nuclei appear, returning to a crystallization tank for cooling crystallization, centrifugally filtering, and drying at 95 ℃ under a fluidized bed to obtain high-purity battery-grade monoammonium phosphate, wherein the component analysis result is shown in Table 1, and the total phosphorus yield is 70%.
As shown in figure 2, the XRD analysis chart of the high-purity battery grade monoammonium phosphate produced in the embodiment shows that the product crystals are well crystallized, the purity is high and no other impurity peaks exist.
Table 1 chemical compositions and standard comparisons of high purity battery grade monoammonium phosphate produced in examples 1-3
As can be seen from Table 1, the high-purity battery grade monoammonium phosphate produced industrially in the invention has high purity and low impurity content, meets the battery grade monoammonium phosphate standard, and provides a new way for efficiently utilizing phosphorus resources for purifying the surplus acid of phosphoric acid production enterprises by a wet method.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (6)
1. The method for producing the high-purity battery grade monoammonium phosphate by utilizing the purified phosphoric acid byproduct washing residual acid is characterized by comprising the following steps of:
step 1, desorbing the purified phosphoric acid byproduct washing residual acid by a concentration tower, adding desalted water and diluting to P 2 O 5 The concentration is 25-28%, and the reaction product is neutralized with liquid ammonia in an ammonification reactor, and the pH of the reaction end point is controlled to be 3.8-4.7, thus obtaining neutralized slurry;
step 2, press-filtering the neutralized slurry in the step 1 to obtain a neutralized clear liquid;
and step 3, standing and aging the neutralized clear liquid in the step 2 at 45-60 ℃ for 8-16 hours, concentrating, cooling and crystallizing to a final temperature of 35-45 ℃, and carrying out salt washing, recrystallization treatment and fluidized bed drying to obtain the high-purity battery grade monoammonium phosphate.
2. The method of claim 1, wherein the purifying phosphoric acid of step 1 produces P in the spent acid byproduct 2 O 5 The concentration is more than or equal to 50 percent, and the MER value is 2 percent.
3. The method of claim 1, wherein the neutralization reaction in step 1 is carried out at a temperature of 85 ℃ to 95 ℃ for a time of 60 to 120 minutes.
4. The method of claim 1, wherein the concentration temperature in step 3 is 70-90 ℃ and the endpoint specific gravity is 1.36-1.42.
5. The method of claim 1, wherein the recrystallization endpoint temperature in step 3 is 25-30 ℃.
6. The method according to claim 1, wherein the fluidized bed is dried at a temperature of 85-125 ℃ for 10-15min in step 3.
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