CN117534047A - Method for separating potassium and sodium in phosphate mother liquor - Google Patents
Method for separating potassium and sodium in phosphate mother liquor Download PDFInfo
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- CN117534047A CN117534047A CN202311429566.1A CN202311429566A CN117534047A CN 117534047 A CN117534047 A CN 117534047A CN 202311429566 A CN202311429566 A CN 202311429566A CN 117534047 A CN117534047 A CN 117534047A
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- potassium
- sodium
- mother liquor
- phosphate
- separating
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- 239000012452 mother liquor Substances 0.000 title claims abstract description 71
- 239000011734 sodium Substances 0.000 title claims abstract description 60
- 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 title claims abstract description 58
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 58
- 229910019142 PO4 Inorganic materials 0.000 title claims abstract description 55
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 title claims abstract description 55
- 239000010452 phosphate Substances 0.000 title claims abstract description 55
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 229910052700 potassium Inorganic materials 0.000 title claims abstract description 50
- 239000011591 potassium Substances 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000000926 separation method Methods 0.000 claims abstract description 36
- 238000001816 cooling Methods 0.000 claims abstract description 31
- 239000010413 mother solution Substances 0.000 claims abstract description 26
- 239000013078 crystal Substances 0.000 claims abstract description 25
- 238000002425 crystallisation Methods 0.000 claims abstract description 14
- 230000008025 crystallization Effects 0.000 claims abstract description 14
- CUXQLKLUPGTTKL-UHFFFAOYSA-M microcosmic salt Chemical compound [NH4+].[Na+].OP([O-])([O-])=O CUXQLKLUPGTTKL-UHFFFAOYSA-M 0.000 claims abstract description 10
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims abstract description 10
- 235000019796 monopotassium phosphate Nutrition 0.000 claims abstract description 10
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000001105 regulatory effect Effects 0.000 claims abstract description 8
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 20
- 239000012535 impurity Substances 0.000 abstract description 5
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 18
- 239000002002 slurry Substances 0.000 description 3
- 239000001488 sodium phosphate Substances 0.000 description 3
- 229910000162 sodium phosphate Inorganic materials 0.000 description 3
- 235000011008 sodium phosphates Nutrition 0.000 description 3
- UPDATVKGFTVGQJ-UHFFFAOYSA-N sodium;azane Chemical compound N.[Na+] UPDATVKGFTVGQJ-UHFFFAOYSA-N 0.000 description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 3
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 1
- 235000019799 monosodium phosphate Nutrition 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
- 235000011009 potassium phosphates Nutrition 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/30—Alkali metal phosphates
- C01B25/308—Methods for converting an alkali metal orthophosphate into another one; Purification; Decolorasing; Dehydrating; Drying
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
- C01B25/451—Phosphates containing plural metal, or metal and ammonium containing metal and ammonium
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Fertilizers (AREA)
Abstract
The invention provides a method for separating potassium and sodium in phosphate mother liquor, which comprises the following steps: firstly, separating out potassium in a potassium-sodium-containing phosphate mother solution from the phosphate mother solution in a potassium dihydrogen phosphate mode to obtain a potassium-removed mother solution; then, carrying out crystallization separation on sodium in the potassium-removed mother solution, so as to realize separation of potassium and sodium; specifically, the method comprises the following steps: s1, removing potassium: regulating the pH value of the phosphate mother liquor to 4.0-5.0, cooling and crystallizing, and separating out potassium dihydrogen phosphate crystals by centrifugal separation to obtain a potassium-removed mother liquor; s2, removing sodium: regulating the pH value of the potassium-removed mother solution to 7.5-8.5, cooling and crystallizing, and separating out sodium ammonium phosphate crystals by centrifugal separation to obtain a sodium-removed mother solution; the separation method provided by the invention is used for separating potassium and sodium in the mother liquor, removing sodium impurities in the system, purifying the mother liquor, improving the quality of the circulating mother liquor, ensuring the normal operation of the production system, and achieving the purposes of improving the quality of products and improving the production capacity.
Description
Technical Field
The invention relates to the technical field of phosphate mother liquor treatment, in particular to a method for separating potassium and sodium in phosphate mother liquor.
Background
In the production process of a large number of enterprises in the chemical industry, a large amount of phosphate mother liquor is generated, sodium is continuously enriched in the mother liquor as an impurity element in the production process of potassium phosphate, and the production process is seriously influenced when the sodium is enriched to a certain amount. The potassium salt and the sodium salt are soluble salts, and always coexist in nature. The separation of sodium and potassium in the chemical industry is mainly realized by utilizing the different solubilities of the sodium and potassium at different temperatures, and with the development of production and economy, the complete separation of sodium and potassium is difficult to realize by using a common recrystallization method.
The technology related to sodium-potassium separation in the prior art comprises the following steps: the Chinese patent with publication number of CN102448885A discloses a separation and extraction device and a separation and extraction method for sodium and potassium, which adopts a mode of combining multistage cooling crystallization and conversion absorption to separate potassium chloride and sodium bicarbonate.
Disclosure of Invention
The invention aims to provide a method for separating potassium and sodium in phosphate mother liquor, which is used for separating potassium and sodium in the mother liquor, removing sodium impurities in a system, purifying the mother liquor, improving the quality of circulating mother liquor, ensuring the normal operation of a production system and achieving the purposes of improving the quality of products and improving the production capacity.
The embodiment of the invention is realized by the following technical scheme:
a method for separating potassium and sodium in phosphate mother liquor comprises the following steps: firstly, separating out potassium in a potassium-sodium-containing phosphate mother solution from the phosphate mother solution in a potassium dihydrogen phosphate mode to obtain a potassium-removed mother solution; then, carrying out crystallization separation on sodium in the potassium-removed mother solution, so as to realize separation of potassium and sodium; specifically, the method comprises the following steps:
s1, removing potassium: regulating the pH value of the phosphate mother liquor to 4.0-5.0, cooling and crystallizing, and separating out potassium dihydrogen phosphate crystals by centrifugal separation to obtain a potassium-removed mother liquor;
s2, removing sodium: regulating the pH value of the potassium-removed mother solution to 7.5-8.5, cooling and crystallizing, and separating out sodium ammonium phosphate crystals by centrifugal separation to obtain the sodium-removed mother solution.
The technical scheme of the embodiment of the invention has at least the following advantages and beneficial effects:
the separation method can solve the problem of sodium impurity enrichment of the mother liquor in the phosphate-containing production process, and has the effects of purifying the mother liquor, improving the product quality and stabilizing the yield. And the mother solution after potassium and sodium separation can be returned to a system for use, potassium salt crystals are returned to a potassium salt production system, and ammonium sodium crystals can be used for producing sodium phosphate, so that the resource utilization of the phosphate mother solution is achieved, and greater production benefits are brought to enterprises.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The method for separating potassium and sodium in the phosphate mother liquor provided by the embodiment of the invention is specifically described below.
A method for separating potassium and sodium in phosphate mother liquor comprises the following steps: firstly, separating out potassium in a potassium-sodium-containing phosphate mother solution from the phosphate mother solution in a potassium dihydrogen phosphate mode to obtain a potassium-removed mother solution; then, carrying out crystallization separation on sodium in the potassium-removed mother solution, so as to realize separation of potassium and sodium; specifically, the method comprises the following steps:
s1, removing potassium: regulating the pH value of the phosphate mother liquor to 4.0-5.0, stirring at the speed of 50-100r/min, cooling to 15-30 ℃ at the cooling speed of 0.1-0.25 ℃/min for crystallization, separating out potassium from the phosphate mother liquor in a potassium dihydrogen phosphate mode, further realizing the separation of part of potassium, and obtaining potassium dihydrogen phosphate crystals and potassium-removed mother liquor through centrifugal separation;
s2, removing sodium: then introducing ammonia gas into the potassium-removed phosphate mother liquor, regulating the pH value of the potassium-removed phosphate mother liquor to 7.5-8.5, stirring at the speed of 150-200r/min, cooling to 5-20 ℃ at the cooling speed of 0.1-0.15 ℃/min for crystallization, and centrifugally washing and separating crystalline sodium ammonium phosphate to further realize separation of potassium and sodium, thereby finally obtaining the sodium-removed mother liquor. Finally, the obtained sodium removal mother liquor can be returned to a system for use, the potassium salt crystals are returned to a potassium salt production system, and the ammonium sodium crystals can be used for producing sodium phosphate, so that the resource utilization of the phosphate mother liquor is achieved.
In the separation process, ammonia reacts with sodium dihydrogen phosphate in phosphate mother liquor to generate ammonium sodium phosphate double salt with smaller solubility, while potassium in the phosphate mother liquor is carried out only by holding liquor during crystallization separation, and ammonium sodium phosphate with higher purity can be obtained by washing ammonium sodium phosphate crystals, thereby realizing the separation of potassium and sodium in the phosphate mother liquor containing potassium and sodium, and Na in the phosphate mother liquor is obtained by the separation method 2 O is less than or equal to 1.50 percent. The reaction formula is as follows: na (Na) + +H 2 PO 4 - +NH 3 +4H 2 O→NaNH 4 HPO 4 .4H 2 O。
The separation method can solve the problem of sodium impurity enrichment of the mother liquor in the phosphate-containing production process, and has the effects of purifying the mother liquor, improving the product quality and stabilizing the yield. And the mother solution after potassium and sodium separation can be returned to a system for use, potassium salt crystals are returned to a potassium salt production system, and ammonium sodium crystals can be used for producing sodium phosphate, so that the resource utilization of the phosphate mother solution is achieved, and greater production benefits are brought to enterprises.
Example 1
The phosphate mother liquor of this example: pH 4.8, P 2 O 5 Content 26.21%, K 2 O content 17.51%, na 2 O content 3.36%, N content 1.31%, and temperature 55 ℃.
The method for separating potassium and sodium in the phosphate mother liquor comprises the following steps:
a. and (3) potassium removal: taking 1500g of the phosphate mother liquor, stirring at a speed of 70r/min, cooling to 25 ℃ at a cooling speed of 0.2 ℃/min, and performing centrifugal separation to obtain 196g of potassium salt crystals (potassium dihydrogen phosphate crystals), wherein the potassium salt crystals have the following indexes: pH 4.7, P 2 O 5 Content 50.33%, K 2 O containsAmount of 33.62%, na 2 O content 0.21%, N content 0.19%, and returning the obtained potassium salt crystal to a potassium salt production system of the production line;
b. sodium removal process: taking 1200g of potassium-removed mother liquor obtained in the previous step, wherein the indexes are as follows: pH 4.8, P 2 O 5 Content 22.53%, K 2 O content 15.05%, na 2 3.88% of O and 1.45% of N; then introducing ammonia gas into the potassium-removed mother liquor to adjust the pH value to 8.1, and further stirring the slurry at a speed of 180r/min, cooling to 15 ℃ at a cooling speed of 0.12 ℃/min, and performing centrifugal separation to obtain 260g of ammonium sodium phosphate crystals, wherein the indexes are as follows: pH 8.0, P 2 O 5 Content 33.19%, K 2 O content 1.29%, na 2 The content of O is 13.75%, the content of N is 6.29%, 955g of sodium removal mother liquor is obtained, and the indexes are as follows: pH 7.7, P 2 O 5 Content 19.28%, K 2 O content 18.45%, na 2 O content 1.06%, N content 1.81%.
Example 2
The phosphate mother liquor of this example: pH 4.8, P 2 O 5 Content 26.21%, K 2 O content 17.51%, na 2 O content 3.36%, N content 1.31%, and temperature 55 ℃.
The method for separating potassium and sodium in the phosphate mother liquor comprises the following steps:
a. and (3) potassium removal: taking 1500g of the phosphate mother liquor, stirring at a speed of 90r/min, cooling to 20 ℃ at a cooling speed of 0.23 ℃/min, and performing centrifugal separation to obtain 260g of potassium-free mother liquor and potassium salt crystals, wherein the potassium salt crystallization indexes are as follows: pH 4.7, P 2 O 5 Content 50.18%, K 2 The O content is 33.51 percent, na 2 The O content is 0.22 percent, the N content is 0.19 percent, and the obtained potassium salt crystal is returned to a potassium salt production system of a production line;
b. sodium removal process: taking 1200g of potassium-removed mother liquor in the previous step, wherein the indexes are as follows: pH 4.8, P 2 O 5 Content 21.18%, K 2 O content 14.15%, na 2 The O content is 4.02 percent, the N content is 1.54 percent, then the mother liquor is introduced with ammonia gas to adjust the pH value to 8.2, the temperature is 75 ℃, and the slurry is further treated by 16 percentStirring at a rate of 0r/min, cooling to 10 ℃ at a cooling rate of 0.14 ℃/min, and performing centrifugal separation to obtain 304g of sodium ammonium phosphate crystals, wherein the indexes are as follows: pH 8.1, P 2 O 5 Content 32.99%, K 2 O content 1.22%, na 2 O content 13.65%, N content 6.29%, and sodium removal mother liquor 912g is obtained, and the indexes are: pH 7.7, P 2 O 5 Content 16.83%, K 2 O content 18.01%, na 2 O content 0.76% and N content 1.79%.
Example 3
The phosphate mother liquor of this example: pH 4.8, P 2 O 5 Content 26.32%, K 2 O content 17.32%, na 2 The O content is 3.66 percent, the N content is 1.35 percent, the temperature is 55 ℃,
the method for separating potassium and sodium in the phosphate mother liquor comprises the following steps:
a. and (3) potassium removal: taking 1500g of the phosphate mother liquor, stirring at a speed of 60r/min, cooling to 20 ℃ at a cooling speed of 0.16 ℃/min, and performing centrifugal separation to obtain 254g of potassium salt crystals, wherein the indexes are as follows: pH 4.8, P 2 O 5 Content 50.22%, K 2 The O content is 33.52 percent, na 2 O content 0.25%, N content 0.20%, and returning the obtained potassium salt crystal to the potassium salt production system of the company;
b. sodium removal process: taking 1200g of potassium-removed mother liquor in the previous step, wherein the indexes are as follows: pH 4.8, P 2 O 5 Content 21.46%, K 2 O content 14.05%, na 2 O content 4.38%, N content 1.57%; then introducing ammonia gas into the mother liquor to adjust the pH value to 8.0, and further stirring the slurry at a speed of 190r/min, cooling to 20 ℃ at a cooling speed of 0.1 ℃/min, and performing centrifugal separation to obtain 292g of ammonium sodium phosphate crystals, wherein the indexes are as follows: pH 8.0, P 2 O 5 Content 33.25%, K 2 O content 1.17%, na 2 The content of O is 13.75 percent, the content of N is 6.36 percent, 921g of sodium removal mother liquor is obtained, and the indexes are as follows: pH 7.7, P 2 O 5 Content 17.24%, K 2 O content 17.85%, na 2 O content 1.29% and N content 1.71%.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The method for separating potassium and sodium in the phosphate mother liquor is characterized by comprising the following steps of: firstly, separating out potassium in a potassium-sodium-containing phosphate mother solution from the phosphate mother solution in a potassium dihydrogen phosphate mode to obtain a potassium-removed mother solution; then, sodium in the potassium-removed mother solution is crystallized and separated, so that separation of potassium and sodium is realized.
2. The method for separating potassium and sodium in phosphate mother liquor according to claim 1, comprising the steps of:
s1, removing potassium: regulating the pH value of the phosphate mother liquor to 4.0-5.0, cooling and crystallizing, and separating out potassium dihydrogen phosphate crystals by centrifugal separation to obtain a potassium-removed mother liquor;
s2, removing sodium: regulating the pH value of the potassium-removed mother solution to 7.5-8.5, cooling and crystallizing, and separating out sodium ammonium phosphate crystals by centrifugal separation to obtain the sodium-removed mother solution.
3. The method for separating potassium and sodium in phosphate mother liquor according to claim 2, further comprising: s3, returning the obtained sodium removal mother liquor to the step S1.
4. The method for separating potassium and sodium in phosphate mother liquor according to claim 2, wherein in S1, the temperature is reduced to 15-30 ℃ during the cooling crystallization.
5. The method for separating potassium and sodium in phosphate mother liquor according to claim 4, wherein in S1, the cooling rate is 0.1-0.25 ℃/min during cooling and crystallization.
6. The method for separating potassium and sodium in phosphate mother liquor according to claim 2, wherein in the step S1, stirring is further included during cooling crystallization, and the stirring speed is 50-100r/min.
7. The method for separating potassium and sodium in phosphate mother liquor according to claim 2, wherein in S2, the temperature is reduced to 5-20 ℃ during the cooling crystallization.
8. The method for separating potassium and sodium in phosphate mother liquor according to claim 7, wherein in S2, the cooling rate is 0.1-0.15 ℃/min during cooling and crystallization.
9. The method for separating potassium and sodium in phosphate mother liquor according to claim 2, wherein in the step S2, stirring is further included during cooling crystallization, and the stirring speed is 150-200r/min.
10. The method for separating potassium and sodium in a phosphate mother liquor according to claim 2, wherein in S2, ammonia gas is introduced into the potassium-removed phosphate mother liquor when the pH of the potassium-removed phosphate mother liquor is adjusted.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311429566.1A CN117534047A (en) | 2023-10-31 | 2023-10-31 | Method for separating potassium and sodium in phosphate mother liquor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311429566.1A CN117534047A (en) | 2023-10-31 | 2023-10-31 | Method for separating potassium and sodium in phosphate mother liquor |
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| Publication Number | Publication Date |
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| CN117534047A true CN117534047A (en) | 2024-02-09 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311429566.1A Pending CN117534047A (en) | 2023-10-31 | 2023-10-31 | Method for separating potassium and sodium in phosphate mother liquor |
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| Country | Link |
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| CN (1) | CN117534047A (en) |
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- 2023-10-31 CN CN202311429566.1A patent/CN117534047A/en active Pending
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