CN113135557A - Method for preparing ammonium manganese phosphate crystal - Google Patents
Method for preparing ammonium manganese phosphate crystal Download PDFInfo
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- CN113135557A CN113135557A CN202110495412.7A CN202110495412A CN113135557A CN 113135557 A CN113135557 A CN 113135557A CN 202110495412 A CN202110495412 A CN 202110495412A CN 113135557 A CN113135557 A CN 113135557A
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- manganese
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- 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
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Abstract
The invention relates to a method for preparing an ammonium manganese phosphate crystal, which takes manganese chloride or manganese sulfate as a manganese source reactant, ammonium phosphate as a phosphorus source reactant and starch as a biological regulator to prepare the ammonium manganese phosphate crystal. And (3) sequentially adding a mixture solution of manganese chloride or manganese sulfate, ammonium phosphate, starch and ammonium chloride or ammonium sulfate into a communicated reactor provided with a left ear groove, a right ear groove, a left baffle plate, a middle baffle plate and a right baffle plate, filtering, washing and drying a product after the reaction is finished, thereby obtaining the manganese ammonium phosphate crystal. The purity of the manganese ammonium phosphate crystal prepared by the method reaches 99.0-99.9%, the yield reaches 95-97%, the purity and the crystallinity are high, and the method has the characteristics of simple process, mild reaction conditions, low energy consumption, low cost and the like.
Description
Technical Field
The invention relates to a method for preparing an ammonium manganese phosphate crystal, in particular to a method for preparing the ammonium manganese phosphate crystal by a bionic method, wherein manganese chloride or manganese sulfate is used as a manganese source reactant, ammonium phosphate is used as a phosphorus source reactant, and starch is used as a biological regulator. The invention relates to the preparation of ammonium manganese phosphate crystals in the technical field.
Background
The manganese ammonium phosphate can be used as a catalyst, a flame retardant, a water softener, a leavening agent, a slow-release type phosphorus-manganese-nitrogen compound fertilizer, a precursor for preparing a lithium ion battery and a chemical reagent. The existing preparation method of the manganese ammonium phosphate has the defects of high energy consumption, low purity, complex process and high cost.
In order to overcome the defects of high energy consumption, low purity, complex process and high cost of the preparation method of the manganese ammonium phosphate, manganese chloride or manganese sulfate is used as a manganese source reactant, ammonium phosphate is used as a phosphorus source reactant, and starch is used as a biological regulator, so that the method simulates the method of preparing the manganese ammonium phosphate crystal.
Disclosure of Invention
Aiming at the defects of high energy consumption, low purity, complex process and high cost of the existing preparation method of the ammonium manganese phosphate, the invention provides the preparation method of the ammonium manganese phosphate crystal, which has the advantages of mild reaction conditions, low energy consumption, high purity, simple process and low cost.
The invention relates to a method for preparing an ammonium manganese phosphate crystal, which takes manganese chloride or manganese sulfate as a manganese source reactant, ammonium phosphate as a phosphorus source reactant and starch as a biological regulator to react in a communicating reactor to prepare the ammonium manganese phosphate crystal; the specific technical scheme is as follows:
the communicating reactor is internally provided with a left ear groove, a right ear groove, a left baffle plate, a middle baffle plate, a right baffle plate, a left lower communicating port, a middle upper communicating port and a right lower communicating port; the left ear groove and the right ear groove are respectively arranged on the inner sides of the left side surface and the right side surface of the communicating reactor, and the upper edges of the left ear groove and the right ear groove are 10 cm lower than the upper edge of the communicating reactor and are used for storing reaction materials; the left baffle plate, the middle baffle plate and the right baffle plate separate the communicating reactor into four independent reaction zones, and the four independent reaction zones are communicated through a left lower communicating port, a middle upper communicating port and a right lower communicating port.
In a communicating reactor, adding manganese chloride or manganese sulfate into a left ear groove and ammonium phosphate into a right ear groove according to the molar ratio of manganese to phosphorus = 1: 1.40-1: 1.60. And then adding a mixture solution containing 0.03-0.05% of starch and 1.5-2.5% of ammonium chloride or ammonium sulfate in percentage by mass into the communicating reactor, so that the liquid level of the mixture solution of the starch and the ammonium chloride or the ammonium sulfate is 1 cm higher than the upper edges of the left ear groove and the right ear groove, and ensuring that reactants in the left ear groove and the right ear groove are communicated through the mixture solution. And finally, covering a cover on the communicating reactor, standing for reaction for 7 days, filtering and washing a product, and drying at 105 ℃ for 1 h to obtain the ammonium manganese phosphate crystal.
The invention has the beneficial effects that: 1) the preparation of the manganese ammonium phosphate crystal is completed at room temperature, and the reaction condition is mild and safe. 2) The reaction is carried out at room temperature, and the energy consumption is low. 3) The communicating reactor is high, and the yield is as high as 97-99%. 4) The purity of the manganese ammonium phosphate crystal is high, and the purity of the manganese ammonium phosphate crystal is 99.0-99.9%. 6) The manganese ammonium phosphate crystal has high crystallinity and complete crystal development. 7) The preparation cost is low. The reaction device is simple, the operation is simple and convenient, and the reaction condition is mild.
Drawings
FIG. 1: the XRD characterization result of the manganese ammonium phosphate crystal prepared by the invention. Comparing the XRD spectrogram of the manganese ammonium phosphate crystal prepared by the invention with a standard spectrogram card JCPDS number 50-0554 of the manganese ammonium phosphate crystal, the XRD characteristic peak position of the manganese ammonium phosphate crystal prepared by the invention is completely consistent with the standard spectrogram, and no impurity peak exists, so that the prepared product is proved to be the manganese ammonium phosphate crystal, and the prepared product has no impurity and high purity. As can be seen from figure 1, the manganese ammonium phosphate crystal prepared by the invention has good crystal growth and high crystallinity.
FIG. 2: schematic of the communicating reactor of the present invention. In fig. 2: a is a left ear groove which is arranged at the inner side of the left side of the communicated reactor, the upper edge of the left ear groove is 10 cm lower than the upper edge of the reactor, and the left ear groove is used for containing reactants; b is a left baffle plate for blocking the upper part; c is a middle baffle plate for blocking the lower part; d is a right baffle plate for blocking the upper part; e is a right lug groove which is arranged at the inner side of the right side of the communicated reactor, the upper edge of the right lug groove is 10 cm lower than the upper edge of the reactor, and the right lug groove is used for containing reactants; f is a left lower communicating port used for communicating the lower part; g is an upper communicating port for communicating the upper part; h is a lower right communication port for communicating the lower part.
Detailed Description
A method for preparing ammonium manganese phosphate crystals according to the present invention will be further described with reference to the following specific examples.
Example 1
In a communicating reactor provided with 2 left ear grooves, 2 right ear grooves, 3 left, middle and right baffle plates, manganese to phosphorus =1 to 1.50 according to molar ratio, manganese chloride is added into the left ear groove, and ammonium phosphate is added into the right ear groove. Then, a mixture solution containing starch and 2.0% of ammonium chloride at a mass ratio of 0.04% is added into the communicating reactor, so that the liquid level of the mixture solution of starch and ammonium chloride is 1 cm higher than the upper edges of the left ear tank and the right ear tank, and the reactants in the left ear tank and the right ear tank are ensured to be communicated through the mixture solution. And finally, covering a cover on the communicating reactor, standing for reaction for 7 days, filtering and washing a product, and drying at 105 ℃ for 1 h to obtain the ammonium manganese phosphate crystal. The yield of the manganese ammonium phosphate crystals was 98% and the purity was 99.5%.
Example 2
In a communicating reactor provided with 2 left ear grooves, 2 right ear grooves, 3 left, middle and right baffle plates, manganese to phosphorus =1 to 1.40 according to molar ratio, manganese chloride is added into the left ear groove, and ammonium phosphate is added into the right ear groove. Then, a mixture solution containing 0.03% of starch and 2.5% of ammonium chloride in mass ratio is added into the communicating reactor, so that the liquid level of the mixture solution of the starch and the ammonium chloride is 1 cm higher than the upper edges of the left ear tank and the right ear tank, and the reactants in the left ear tank and the right ear tank are ensured to be communicated through the mixture solution. And finally, covering a cover on the communicating reactor, standing for reaction for 7 days, filtering and washing a product, and drying at 105 ℃ for 1 h to obtain the ammonium manganese phosphate crystal. The yield of the manganese ammonium phosphate crystals was 97%, and the purity was 99.9%.
Example 3
In a communicating reactor provided with 2 left ear grooves, 2 right ear grooves, 3 left, middle and right baffle plates, manganese to phosphorus =1 to 1.60 according to molar ratio, manganese chloride is added into the left ear groove, and ammonium phosphate is added into the right ear groove. Then, a mixture solution containing 0.05% of starch and 1.5% of ammonium chloride in mass ratio is added into the communicating reactor, so that the liquid level of the mixture solution of the starch and the ammonium chloride is 1 cm higher than the upper edges of the left ear tank and the right ear tank, and the reactants in the left ear tank and the right ear tank are ensured to be communicated through the mixture solution. And finally, covering a cover on the communicating reactor, standing for reaction for 7 days, filtering and washing a product, and drying at 105 ℃ for 1 h to obtain the ammonium manganese phosphate crystal. The yield of the manganese ammonium phosphate crystal is 99%, and the purity is 99.0%.
Example 4
Manganese sulfate is added into the left ear groove, and ammonium phosphate is added into the right ear groove in a communicated reactor provided with 2 ear grooves on the left and right, and 3 baffle plates on the left, middle and right according to the molar ratio, wherein the ratio of manganese to phosphorus is = 1: 1.50. Then, a mixture solution containing starch with a concentration of 0.04% and ammonium sulfate with a concentration of 2.0% by mass ratio is added into the communicating reactor, so that the liquid level of the mixture solution of starch and ammonium sulfate is higher than the upper edges of the left ear tank and the right ear tank by 1 cm, and the reactants in the left ear tank and the right ear tank are ensured to be communicated through the mixture solution. And finally, covering a cover on the communicating reactor, standing for reaction for 7 days, filtering and washing a product, and drying at 105 ℃ for 1 h to obtain the ammonium manganese phosphate crystal. The yield of the manganese ammonium phosphate crystals was 98% and the purity was 99.4%.
Example 5
Manganese sulfate is added into the left ear groove, and ammonium phosphate is added into the right ear groove in a communicated reactor provided with 2 ear grooves on the left and right, and 3 baffle plates on the left, middle and right according to the molar ratio, wherein the ratio of manganese to phosphorus is = 1: 1.40. Then, a mixture solution containing 0.03% of starch and 2.5% of ammonium sulfate by mass ratio was fed into the communicating reactor so that the liquid level of the mixture solution of starch and ammonium sulfate was 1 cm higher than the upper edges of the left and right ear tanks to ensure that the reactants in the left and right ear tanks were communicated with each other through the mixture solution. And finally, covering a cover on the communicating reactor, standing for reaction for 7 days, filtering and washing a product, and drying at 105 ℃ for 1 h to obtain the ammonium manganese phosphate crystal. The yield of the manganese ammonium phosphate crystals was 97%, and the purity was 99.8%.
Example 6
Manganese sulfate is added into the left ear groove, and ammonium phosphate is added into the right ear groove in a communicated reactor provided with 2 ear grooves on the left and right, and 3 baffle plates on the left, middle and right according to the molar ratio, wherein the ratio of manganese to phosphorus is = 1: 1.60. Then, a mixture solution containing 0.05% of starch and 1.5% of ammonium sulfate by mass ratio was fed into the communicating reactor so that the liquid level of the mixture solution of starch and ammonium sulfate was 1 cm higher than the upper edges of the left and right ear tanks to ensure that the reactants in the left and right ear tanks were communicated with each other through the mixture solution. And finally, covering a cover on the communicating reactor, standing for reaction for 7 days, filtering and washing a product, and drying at 105 ℃ for 1 h to obtain the ammonium manganese phosphate crystal. The yield of the manganese ammonium phosphate crystal is 99%, and the purity is 99.0%.
Claims (1)
1. A method for preparing ammonium manganese phosphate crystals is characterized by comprising the following steps: the method comprises the steps of taking manganese chloride or manganese sulfate as a manganese source reactant, ammonium phosphate as a phosphorus source reactant and starch as a biological regulator, and reacting in a communicated reactor to prepare an ammonium manganese phosphate crystal; the specific technical scheme is as follows:
the communicating reactor is internally provided with a left ear groove, a right ear groove, a left baffle plate, a middle baffle plate, a right baffle plate, a left lower communicating port, a middle upper communicating port and a right lower communicating port; the left ear groove and the right ear groove are respectively arranged on the inner sides of the left side surface and the right side surface of the communicating reactor, and the upper edges of the left ear groove and the right ear groove are 10 cm lower than the upper edge of the communicating reactor and are used for storing reaction materials; the left baffle plate, the middle baffle plate and the right baffle plate divide the communicating reactor into four independent reaction zones, and the four independent reaction zones are communicated through a left lower communicating port, a middle upper communicating port and a right lower communicating port;
adding manganese chloride or manganese sulfate into a left ear groove and adding ammonium phosphate into a right ear groove in a communicating reactor according to the molar ratio of manganese to phosphorus = 1: 1.40-1: 1.60; then adding a mixture solution containing 0.03-0.05% of starch and 1.5-2.5% of ammonium chloride or ammonium sulfate in percentage by mass into a communicating reactor, so that the liquid level of the mixture solution of the starch and the ammonium chloride or the ammonium sulfate is higher than the upper edges of the left ear groove and the right ear groove by 1 cm, and ensuring that reactants in the left ear groove and the right ear groove are communicated through the mixture solution; and finally, covering a cover on the communicating reactor, standing for reaction for 7 days, filtering and washing a product, and drying at 105 ℃ for 1 h to obtain the ammonium manganese phosphate crystal.
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| CN202110495412.7A CN113135557A (en) | 2021-05-07 | 2021-05-07 | Method for preparing ammonium manganese phosphate crystal |
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| CN202110495412.7A CN113135557A (en) | 2021-05-07 | 2021-05-07 | Method for preparing ammonium manganese phosphate crystal |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115231544A (en) * | 2022-08-09 | 2022-10-25 | 湖北万润新能源科技股份有限公司 | Preparation method of manganese ammonium phosphate and lithium ion battery anode material |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3141732A (en) * | 1961-12-12 | 1964-07-21 | Grace W R & Co | Process for preparing metal ammonium phosphates |
| WO2007003969A2 (en) * | 2005-07-06 | 2007-01-11 | Cambridge University Technical Services Limited | Divalent metal ion phosphates and uses thereof |
| CN104085870A (en) * | 2014-06-17 | 2014-10-08 | 湖北富邦科技股份有限公司 | Synthetic method of slow release manganese fertilizer |
| CN109133136A (en) * | 2018-11-12 | 2019-01-04 | 南昌航空大学 | A kind of room temperature self-diffusion prepares the method and device of carbonic acid strontium crystal |
-
2021
- 2021-05-07 CN CN202110495412.7A patent/CN113135557A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3141732A (en) * | 1961-12-12 | 1964-07-21 | Grace W R & Co | Process for preparing metal ammonium phosphates |
| WO2007003969A2 (en) * | 2005-07-06 | 2007-01-11 | Cambridge University Technical Services Limited | Divalent metal ion phosphates and uses thereof |
| CN104085870A (en) * | 2014-06-17 | 2014-10-08 | 湖北富邦科技股份有限公司 | Synthetic method of slow release manganese fertilizer |
| CN109133136A (en) * | 2018-11-12 | 2019-01-04 | 南昌航空大学 | A kind of room temperature self-diffusion prepares the method and device of carbonic acid strontium crystal |
Non-Patent Citations (1)
| Title |
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| 徐玉娜: "水热法制备磷酸镧晶体的研究", 《万方学术论文》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115231544A (en) * | 2022-08-09 | 2022-10-25 | 湖北万润新能源科技股份有限公司 | Preparation method of manganese ammonium phosphate and lithium ion battery anode material |
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