CN112441617A - Preparation method of lithium molybdate powder - Google Patents
Preparation method of lithium molybdate powder Download PDFInfo
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- CN112441617A CN112441617A CN201910804465.5A CN201910804465A CN112441617A CN 112441617 A CN112441617 A CN 112441617A CN 201910804465 A CN201910804465 A CN 201910804465A CN 112441617 A CN112441617 A CN 112441617A
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- C—CHEMISTRY; METALLURGY
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- C01G39/00—Compounds of molybdenum
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- C—CHEMISTRY; METALLURGY
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- 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
Abstract
The invention relates to a preparation method of lithium molybdate powder, wherein the chemical formula of the lithium molybdate powder is Li2MoO4, and the preparation method comprises the following steps: (1) weighing Li2CO3 powder and MoO3 powder as raw material powder according to the stoichiometric ratio of lithium molybdate, and weighing a proper amount of deionized water; (2) mixing Li2CO3 powder, MoO3 powder and deionized water to obtain a suspension; (3) heating the obtained suspension to 40-99 ℃ until the suspension is clear and no bubbles are generated, thus obtaining a transparent solution; (4) and filtering the obtained transparent solution, and heating and evaporating to dryness to obtain the lithium molybdate powder.
Description
Technical Field
The invention relates to a preparation method of lithium molybdate powder, belonging to the technical field of material preparation.
Background
Lithium molybdate is a white powder, is easily soluble in water and is insoluble in organic solvents; the method is mainly used in the fields of chemical industry, corrosion inhibitors, electrode materials, metal ceramics, resistor materials, refrigeration and the like.
The lithium molybdate is widely applied in the refrigeration industry, particularly in a lithium bromide absorption refrigerator, has a particularly prominent corrosion inhibition effect and causes no pollution to the environment. With global attention to resources and environmental protection, a lithium bromide refrigerator must replace a Freon refrigerator, and the consumption of lithium molybdate is greatly increased. In addition, the dosage of lithium molybdate in electrode materials, cermets and resistor materials is increased year by year, and particularly, high-purity lithium molybdate powder raw materials are also needed for preparing high-purity lithium molybdate crystals for high-energy physical double beta decay detection.
At present, the preparation of lithium molybdate powder generally adopts a solution method or a solid-phase sintering method, but the two methods have respective disadvantages. In the preparation process of the solution method, acid precipitation (nitric acid) and alkali dissolution treatment (lithium hydroxide) are required to be carried out on the raw material (sodium molybdate), impurities are easily introduced, and thus the purity of the lithium molybdate powder is reduced. The solid-phase sintering preparation needs to mix the lithium carbonate and the molybdenum oxide raw materials and then sinter the mixture at a high temperature of more than 450 ℃, so that the energy consumption is high, and impurity components in the raw materials cannot be removed.
Disclosure of Invention
Aiming at the defects of the existing preparation method of lithium molybdate powder, the invention aims to provide a novel preparation method of lithium molybdate powder, which can reduce the reaction temperature, shorten the preparation time and improve the product purity.
In one aspect, the present invention provides a method for preparing a lithium molybdate powder having a chemical formula of Li2MoO4The preparation method comprises the following steps:
(1) according to the formula lithium molybdate (Li)2MoO4) Respectively weighing Li in the stoichiometric ratio2CO3Powder and MoO3Weighing a proper amount of deionized water;
(2) mixing Li2CO3Powder, MoO3Mixing the powder with deionized water to obtain a suspension;
(3) heating the obtained suspension to 40-99 ℃ until the suspension is clear and no bubbles are generated, thus obtaining a transparent solution;
(4) and filtering the obtained transparent solution, and heating and evaporating to dryness to obtain the lithium molybdate powder.
According to the method, the lithium carbonate powder, the molybdenum oxide powder and the deionized water are directly mixed, so that the chemical reaction is rapidly reacted in a solution state, the lithium molybdate solution is formed, the reaction temperature is greatly reduced, no impurity phase is mixed, the preparation time is greatly shortened, and the preparation efficiency and the powder purity of the lithium molybdate powder are effectively improved.
Preferably, in the step (1), the Li is added2CO3Powder, MoO3And sequentially mixing the powder and deionized water to obtain a suspension. The Li2CO3Purity of powder > 99.9%, said MoO3The purity of the powder was > 99.9%. The purity of the lithium molybdate powder obtained by the method is obviously higher than that of the initial raw material powder.
Preferably, in the step (2), the mixing mode is stirring treatment.
In the present disclosure, the above three weights may be randomly mixed. Preferably, in the step (2), the lithium carbonate powder and the molybdenum oxide powder may be mixed first, and then the deionized water may be gradually added.
Preferably, in the step (2), the amount of the deionized water should not be less than the amount of water required for the corresponding saturated solution of lithium molybdate obtained by completely reacting the raw material powder. Preferably, the amount of the deionized water is 1-2 times, and more preferably 1-1.5 times of the amount of water required by a corresponding saturated solution of lithium molybdate obtained by completely reacting raw material powder.
Preferably, in the step (3), the stirring is performed while the heating treatment is performed.
Preferably, in the step (4), the water solution is heated to evaporate the water gradually until the water is completely evaporated.
In another aspect, the present invention provides a lithium molybdate powder prepared according to the above preparation method, wherein the purity of the lithium molybdate powder is greater than or equal to the purity of the raw material, preferably greater than or equal to 99.99%.
In the present disclosure, the high-purity lithium molybdate powder prepared by the above method can be used for various purposes including the preparation of high-purity lithium molybdate crystals. Compared with other methods, the method can effectively improve the product purity: on one hand, no external impurities are introduced, and on the other hand, water-insoluble impurities in the raw materials can be effectively removed through filtering.
Compared with the prior art, the invention has the following advantages:
(1) the raw materials are mixed at room temperature, so that the raw materials can quickly and fully react in a solution state, and the reaction temperature is greatly reduced;
(2) the reaction time of the raw materials is greatly shortened by means of stirring, heating and the like, and the production efficiency is improved; meanwhile, the whole preparation process is easy to operate and control, and has low requirements on equipment and environment;
(3) through filtering the reaction solution, water-insoluble materials can be removed, and the purity of the lithium molybdate powder is improved.
Drawings
FIG. 1 is a schematic diagram illustrating a process for preparing a lithium molybdate powder according to the present invention;
fig. 2 is an X-ray diffraction pattern of the lithium molybdate powder prepared in example 1, and it can be seen from the pattern that the X-ray diffraction peak of the prepared sample completely corresponds to the diffraction peak of the lithium molybdate standard card, and there is no diffraction peak of other impurity phases.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
In the present disclosure, raw materials of lithium carbonate powder and molybdenum trioxide powder are directly mixed and added with deionized water, and a lithium molybdate solution is formed after direct reaction in an aqueous solution state, thereby avoiding the introduction of impurities, and simultaneously shortening the preparation time and lowering the reaction temperature. And then filtering, heating and evaporating to dryness, thereby improving the purity and preparation efficiency of the lithium molybdate powder and reducing the preparation cost. Wherein, the whole preparation process is in an atmospheric environment.
The method for preparing the lithium molybdate powder material is simple, short in required time, low in energy consumption, high in purity of the obtained powder, and suitable for batch production. As shown in fig. 1, the following exemplary method for preparing the lithium molybdate powder according to the present invention is described.
And (4) weighing the materials. Weighing lithium carbonate powder and molybdenum trioxide powder according to the stoichiometric ratio (1:1) of the lithium molybdate powder. The purity of the adopted raw materials of lithium carbonate powder and molybdenum trioxide powder is more than 99.9 percent.
And (3) mixing materials. Putting the weighed raw materials into a container, and uniformly stirring to obtain mixed powder. In the step, the raw materials are directly mixed and uniformly stirred. Then deionized water is gradually added into the suspension while stirring continuously to obtain a suspension. The total amount of deionized water added should be not less than the amount of water required to form a saturated solution corresponding to lithium molybdate.
And (4) reacting. And heating the obtained suspension, controlling the temperature of the suspension to be between 40 and 99 ℃, and stirring the solution until the solution is clear and no bubbles are generated, so as to obtain a transparent solution. It should be noted that the heating treatment of the suspension includes, but is not limited to, microwave, water bath, electric furnace, oven, alcohol lamp, and the like. The suspension may be stirred while being heated, or may be stirred after being heated.
And (5) filtering. And filtering the transparent solution by using filter paper to remove water-insoluble substances to obtain filtrate.
And (5) drying. And heating and evaporating the filtrate to dryness to obtain white lithium molybdate powder. The drying process includes, but is not limited to, microwave, water bath, electric furnace, oven, alcohol burner, etc.
In the invention, the purity of the lithium molybdate powder prepared by the process is high (more than 99.99 percent), and the purity is measured by a glow discharge mass spectrometer. And the high-purity lithium molybdate powder can be further used for preparing lithium molybdate crystals.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below. Unless otherwise specified, the following examples relate to the use of raw material lithium carbonate powder and molybdenum trioxide powder each having a purity of more than 99.9%.
Example 1
Weighing 26.42g of lithium carbonate powder and 51.48g of molybdenum trioxide powder in sequence, placing the powder in a clean beaker, mixing and stirring uniformly, gradually adding about 120mL of deionized water into the beaker, and continuously stirring for about 30 minutes to obtain a blue-cyan suspension; heating the suspension to 40-99 ℃ after the suspension is neutralized for about 1 minute by a microwave oven, taking out the suspension and continuously stirring until the solution is clear and does not bubble any more; filtering the solution, and placing the filtrate on an alcohol lamp to be heated and dried to obtain white lithium molybdate powder. The purity of the obtained white lithium molybdate powder is more than 99.99 percent.
Example 2
Weighing 42.51g of lithium carbonate powder and 82.81g of molybdenum trioxide powder in sequence, placing the powder in a clean beaker, mixing and stirring uniformly, and gradually adding about 200mL of deionized water into the beaker; the solution was heated in a beaker in a water bath at about 80 ℃ while continuing to stir until the solution was clear and no more bubbling (time required was about half an hour); filtering the solution, placing the filtrate in an air-blast drying oven, setting the temperature at 120 ℃ for evaporation treatment, and drying to obtain white lithium molybdate powder.
Example 3
127.53g of lithium carbonate powder and 248.43g of molybdenum trioxide powder are sequentially weighed, placed in a clean beaker, mixed and stirred uniformly, and then added with about 600mL of deionized water gradually; placing the solution on an electric furnace by using a beaker, heating to about 50 ℃, and simultaneously continuing stirring until the solution is clear and does not generate bubbles; filtering the solution, placing the filtrate on an electric furnace, setting the temperature at 150 ℃ for evaporation treatment, and drying to obtain white lithium molybdate powder. The purity of the obtained white lithium molybdate powder is more than 99.99 percent.
Example 4
127.53g of lithium carbonate powder and 248.43g of molybdenum trioxide powder are sequentially weighed, placed in a clean beaker, mixed and stirred uniformly, and then gradually added with about 600mL of deionized water, and stirred continuously for about 30 minutes to obtain white suspension; heating the suspension to about 90 ℃ by using an oven, and continuously stirring until the solution is clear and does not bubble any more; filtering the solution, placing the filtrate on an electric furnace, heating at 180 ℃, and drying to obtain white lithium molybdate powder. The purity of the obtained white lithium molybdate powder is more than 99.99 percent.
Example 5
170.04g of lithium carbonate powder and 331.24g of molybdenum trioxide powder are sequentially weighed, placed in a clean beaker, mixed and stirred uniformly, and then gradually added with about 800mL of deionized water; heating the solution to about 50 ℃ by using an alcohol lamp, and simultaneously continuing stirring until the solution is clear and does not generate bubbles; filtering the solution, placing the filtrate on an electric furnace, heating at 180 ℃, and drying to obtain white lithium molybdate powder. The purity of the obtained white lithium molybdate powder is more than 99.99 percent.
Claims (8)
1. A preparation method of lithium molybdate powder is characterized in that the chemical formula of the lithium molybdate powder is Li2MoO4The preparation method comprises the following steps:
(1) weighing Li according to the stoichiometric ratio of lithium molybdate2CO3Powder and MoO3Taking the powder as raw material powder, and measuring a proper amount of deionized water;
(2) mixing Li2CO3Powder, MoO3Mixing the powder with deionized water to obtain a suspension;
(3) heating the obtained suspension to 40-99 ℃ until the suspension is clear and no bubbles are generated, thus obtaining a transparent solution;
(4) and filtering the obtained transparent solution, and heating and evaporating to dryness to obtain the lithium molybdate powder.
2. The production method according to claim 1,in the step (1), the Li is added2CO3Powder, MoO3And sequentially mixing the powder and deionized water to obtain a suspension.
3. The production method according to claim 1 or 2, wherein in the step (1), the mixing is performed by stirring.
4. The preparation method according to any one of claims 1 to 3, wherein in the step (2), the mass of the deionized water added is not less than the water amount required by the saturated solution of lithium molybdate generated by the complete reaction of the raw material powder.
5. The method according to claim 4, wherein in the step (2), the amount of the deionized water is 1 to 2 times of the amount of water required for a corresponding saturated solution of lithium molybdate obtained by completely reacting the raw material powder.
6. The production method according to any one of claims 1 to 5, wherein in the step (3), stirring is performed while the heat treatment is performed.
7. A lithium molybdate powder prepared according to the preparation method of any one of claims 1 to 6, wherein the purity of the lithium molybdate powder is significantly higher than that of the raw material powder.
8. Use of the lithium molybdate powder of claim 7 for the preparation of lithium molybdate crystals.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104229894A (en) * | 2013-06-17 | 2014-12-24 | 华南理工大学 | Sol-gel method for preparation of lithium ion battery lithium molybdate cathode material |
| CN105293579A (en) * | 2015-09-19 | 2016-02-03 | 江西赣锋锂业股份有限公司 | Preparation method of lithium molybdate |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104229894A (en) * | 2013-06-17 | 2014-12-24 | 华南理工大学 | Sol-gel method for preparation of lithium ion battery lithium molybdate cathode material |
| CN105293579A (en) * | 2015-09-19 | 2016-02-03 | 江西赣锋锂业股份有限公司 | Preparation method of lithium molybdate |
Non-Patent Citations (2)
| Title |
|---|
| HAO ZHANG等: "Preparation of Li2MoO4 using aqueous solution method and microwave dielectric properties after sintering", 《J MATER SCI: MATER ELECTRON》 * |
| O. P. BARINOVA等: "GROWTH OF Li2MoO4 CRYSTALS FROM ACTIVATED WATER SOLUTIONS", 《GLASS AND CERAMICS》 * |
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Application publication date: 20210305 |