CN113830748A - Nickel lithium phosphate nano yellow pigment and preparation method thereof - Google Patents
Nickel lithium phosphate nano yellow pigment and preparation method thereof Download PDFInfo
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
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- C01P2006/00—Physical properties of inorganic compounds
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- C01P2006/62—L* (lightness axis)
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- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/63—Optical properties, e.g. expressed in CIELAB-values a* (red-green axis)
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/64—Optical properties, e.g. expressed in CIELAB-values b* (yellow-blue axis)
Abstract
The invention relates to a nickel lithium phosphate nano yellow pigment and a preparation method thereof. The preparation method comprises the following steps: adding a water solution containing polyethylene glycol into a reaction kettle; adding a lithium-containing raw material, a nickel-containing raw material and ammonium phosphate into the aqueous solution containing the polyethylene glycol, stirring to form a mixed solution or a suspension, and keeping mechanical stirring in hydrothermal synthesis to be started all the time; heating the reaction kettle to perform hydrothermal synthesis reaction, and then cooling; discharging the reacted mixed solution, precipitating, and filtering or centrifuging; and washing and drying to obtain the lithium nickel phosphate nano yellow pigment. The preparation method of the invention is convenient for controlling the phase of the formed product, has simple and convenient process, avoids the agglomeration of nano pigment particles due to the addition of the polyethylene glycol, improves the easy dispersibility of the product and is suitable for large-scale low-cost production.
Description
Technical Field
The invention belongs to the field of inorganic nano materials, and particularly relates to a nickel lithium phosphate nano yellow pigment and a preparation method thereof.
Background
In the CMYK color system in the print mode, full color development can be realized by mixing and superimposing four colors using three primary colors (C: cyan; M: magenta; Y: yellow) of coloring materials and black (K) ink. The high quality of these four unit colors becomes the key to achieving this goal.
Organic coloring materials are abundant in types and strong in color-developing ability, and many types of materials can be used as four kinds of unit coloring materials, i.e., CMYK. However, the poor weather and temperature stability of organic colorants is a major disadvantage of such colorants. In the use occasions requiring high weather resistance and high temperature resistance, people tend to find and use inorganic pigments more.
Compared with organic pigments, inorganic pigments have fewer varieties and relatively weaker color development ability. In recent years, as the application of inorganic coloring materials in the fields of cosmetics, plastics and the like has been expanded, particularly, ink jet printing technology has been widely used for ceramic decoration, and the market demand for nano coloring materials has rapidly increased.
The traditional solid-phase sintering method is a main method for preparing micron-sized pigments, and in order to realize application in ink-jet printing, transparent films and the like, the size of the pigments needs to be reduced by means of mechanical grinding and the like. However, the inorganic pigment is reduced in particle size through a grinding process, and when the particle size is reduced to a nanometer level, most pigments are obviously weakened in color development capability due to the fact that surface defects are increased and even partial amorphization occurs. Another problem with the use of inorganic nano-colorants is that as the particle size decreases, the surface area increases dramatically, resulting in difficulty in dispersion and susceptibility to agglomeration during use.
Chemical precipitation, sol-gel, hydrothermal methods, etc. are the main methods for preparing ultrafine powders, and have been widely studied and applied in the field of nano functional materials. These methods have been reported for the preparation of colorants but are not yet widespread on an industrial scale. Among them, hydrothermal synthesis of cobalt blue pigments has been reported in many documents, for example, Zhizhang Chen et al reported that cobalt blue (CoAl) having a particle size of about 70nm was synthesized by a hydrothermal method2O4) Colorant (https: org/10.1016/S0167-577X (02) 00378-6); fangii YU et al compared the preparation of cobalt blue (CoAl) by a sol-gel-calcination process (1000 ℃ C.) and a sol-gel-hydrothermal process (250 ℃ C.)2O4) Colorant (https: // doi.org/10.1016/j.jallcom.2008.01.018), the powder prepared by the hydrothermal process is found to be 50-60 nm in size and uniform in size.
Lithium iron phosphate having an olivine crystal structure has been widely studied and applied as a positive electrode material having good safety and low price. The inventors have noted that lithium nickel phosphate with a similar olivine-type crystal structure has a higher working voltage than lithium iron phosphate, whichThe working voltage of lithium is 3.45V (vs. Li/Li)+) And the working voltage of the lithium nickel phosphate is 5.1V (vs. Li/Li)+). The lack of electrolyte matching with lithium nickel phosphate makes it impossible to use the electrolyte as an electrode material. One of the characteristics of such electrode materials is poor conductivity, and when the electrode material is used as an electrode material, the electronic conductivity among particles of the electrode material is generally improved by carbon coating. The lithium nickel phosphate powder prepared by the prior art is grey brown, has different particle sizes and is difficult to be practically applied.
The applicant of the present invention found that when a hydrothermal method is used for preparing lithium nickel phosphate, the obtained material is a bright nano yellow pigment, and then the material is found to present an almost perfect yellow color through colorimetric analysis. Can be used as an inorganic yellow candidate material of one of the three primary colors in a CMYK color matching system.
Disclosure of Invention
In view of the current situation that inorganic pigments are lack of three primary color candidate materials in a CMYK color matching system and the defects of inorganic nano pigments in preparation and post-treatment, the invention aims to provide a yellow inorganic nano pigment with good color development strength and high color purity, and the prepared pigment can achieve good dispersion effect by simple shearing dispersion without high-strength ball milling when in use.
The invention prepares LiNiPO by a hydrothermal method4The nano-scale inorganic pigment can be obtained by one-step method through controlling hydrothermal parameters. By adding polyethylene glycol (PEG) into a hydrothermal system, LiNiPO in the hydrothermal process is inhibited4The growth of crystal grains realizes LiNiPO in the hydrothermal process4The grain size is controlled, and simultaneously the added PEG passes through the synthesized nano-scale LiNiPO4The surface modification keeps the dispersibility of the modified starch in the hydrothermal process and improves the compatibility of the modified starch with an organic solvent, and a dispersing agent and a stabilizing agent are not additionally added, so that a good dispersing effect can be achieved through simple shearing dispersion in use.
The invention provides a method for preparing nano yellow LiNiPO by one-step hydrothermal synthesis4The method specifically comprises the following steps:
A. adding a water solution containing polyethylene glycol (PEG) into a reaction kettle;
B. adding a lithium-containing raw material, a nickel-containing raw material and ammonium phosphate into the aqueous solution containing the polyethylene glycol, stirring to form a mixed solution or a suspension, and keeping mechanical stirring in hydrothermal synthesis to be started all the time;
C. heating the reaction kettle, preserving heat, performing hydrothermal synthesis reaction, and cooling;
D. discharging the reacted mixed solution, precipitating, and filtering or centrifuging;
E. washing and drying to obtain the lithium nickel phosphate (LiNiPO)4) A nanometer yellow pigment.
The filling amount of the PEG-containing aqueous solution is less than 70% of the volume of the reaction kettle, and the mass percentage of PEG in the aqueous solution is 2-10 wt%.
The average weight average molecular weight of the PEG is 200-1000.
Preferably, the average weight average molecular weight of the PEG is 400-600.
The lithium-containing raw material is one or a combination of lithium carbonate, lithium acetate and hydrates thereof, lithium chloride and hydrates thereof, lithium nitrate, lithium sulfate and hydrates thereof, and lithium hydroxide and hydrates thereof; the nickel-containing raw material is one or a combination of nickel nitrate and hydrate thereof, nickel sulfate and hydrate thereof, nickel acetate and hydrate thereof and nickel hydroxide; the ammonium phosphate is one or the combination of diammonium hydrogen phosphate and triammonium phosphate. The ammonium phosphate of the invention is a necessary component, and the ammonium phosphate is a weak alkali source, thereby avoiding impurities from being embedded into LiNiPO4In the grains, thereby reducing the defect density of the product.
In the raw material ratio, the molar ratio of Ni to P is 1: 1, and the molar ratio of Li to Ni is (1.3-3) to 1.
Preferably, the molar ratio of Ni to P in the raw material mixture ratio is 1: 1, and the molar ratio of Li to Ni is (1.5-2) to 1.
The heat preservation temperature of the hydrothermal synthesis is 200-250 ℃, and the heat preservation time is 6-48 hours. When the temperature exceeds 250 ℃, carbonization decomposition of PEG is easy to occur on one hand, and LiNiPO is easy to occur on the other hand4The disordered growth of the crystal grains is easy to agglomerate, thereby leading the obtained pigment to be coloredIs not pure. Preferably, the step C is performed with a programmed gradient temperature rise: heating to 100-110 ℃ at a speed of 10-20 ℃/min, keeping the temperature for 30-40 min, heating to 200-250 ℃ at a speed of 3-5 ℃/min, and carrying out heat preservation reaction.
And (3) precipitating, filtering or centrifuging the mixed solution after the hydrothermal reaction is finished, and separating the synthesized yellow pigment.
In order to recycle PEG in the filtrate and the lithium source which is excessively added for obtaining the target product, the filtrate is supplemented with a proper amount of polyethylene glycol, a lithium-containing raw material, a nickel-containing raw material and ammonium phosphate, and then hydrothermal synthesis is carried out from the step A, so as to prepare the nano lithium nickel phosphate yellow pigment.
At this time, the lithium-containing raw material, nickel-containing raw material and ammonium phosphate which need to be added are carried out according to the stoichiometric ratio of the target product (the molar ratio of Li to Ni to P is 1: 1), and the synthesis of the nickel lithium phosphate yellow pigment can be realized.
The preparation method provided by the invention is convenient for controlling the phase of the formed product, the process is simple and convenient, the agglomeration of nano pigment particles is avoided by adding PEG, the easy dispersibility of the product is improved, and the preparation method is suitable for large-scale low-cost production.
Drawings
FIG. 1 is a total reflection spectrum of the synthesized nano yellow powder in example 1 of the present invention.
FIG. 2 is a powder X-ray diffraction (XRD) pattern of the synthesized nano yellow powder of example 1 of the present invention.
FIG. 3 is a Transmission Electron Microscope (TEM) image of the synthesized nano yellow powder of example 1 of the present invention.
FIG. 4 is a Scanning Electron Microscope (SEM) image of the yellow powder synthesized in comparative example 1.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
Lithium carbonate, lithium acetate and hydrate thereof, lithium chloride and hydrate thereof, lithium nitrate, lithium sulfate and hydrate thereof, and one or combination of lithium hydroxide and hydrate thereof are used as a lithium source; taking one or the combination of nickel nitrate and hydrate thereof, nickel sulfate and hydrate thereof, nickel acetate and hydrate thereof and nickel hydroxide as a nickel source; one or the combination of diammonium phosphate and triammonium phosphate is used as a phosphorus source, and the nano-scale lithium nickel phosphate yellow pigment is prepared by a hydrothermal synthesis method.
In the invention, in order to realize the hydrothermal synthesis of the target product lithium nickel phosphate, excessive lithium-containing raw materials are added into a reaction system, and the atomic ratio of nickel to phosphorus is kept in a stoichiometric ratio. Under the premise of keeping the molar ratio of nickel to phosphorus equal, the synthesis of the target yellow nano coloring material is not influenced by the excessive lithium within the range of 30-200%. The lithium which is added excessively can be reused after the required raw materials are added according to the stoichiometric ratio of the nickel lithium phosphate after the filtrate is recovered.
In order to control the crystal growth of the nickel lithium phosphate in the hydrothermal process and keep the crystal growth in a nano scale, a proper amount of polyethylene glycol (PEG) is added into a reaction system. The addition of PEG can not only inhibit the overgrowth of the nickel lithium phosphate, but also keep the good dispersion performance of the synthesized yellow pigment in an organic system, and show excellent multifunctional composite performance.
In the invention, the lithium source, the nickel source and the phosphorus source can be any combination of one or more of the raw materials, and the synthesis of the target yellow nano pigment is not influenced.
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 merely one example of suitable ranges, i.e., those skilled in the art can select within suitable ranges through the description herein, and are not intended to be limited to the specific values exemplified below. The raw materials in the examples were purchased from chemical reagents of the national pharmaceutical group of China.
Example 1
6kg of aqueous solution containing polyethylene glycol with the weight-average molecular weight of 600 and the mass percentage concentration of 3 percent is added into a 10L 316L stainless steel reaction kettle, 110.839g of lithium carbonate, 581.62g of nickel nitrate hexahydrate and 260.12g of diammonium hydrogen phosphate are added, mechanical stirring is started after sealing, the rotating speed of a stirrer is 300rpm, the temperature is increased to 230 ℃ from room temperature after pre-stirring for 30 minutes, and the temperature is kept for 24 hours. Cooling to below 100 deg.c, eliminating pressure, further cooling, discharging, filtering, washing and drying to obtain yellow pigment powder. The lithium added to the system was 150% of the stoichiometric ratio and the concentration of the product formed was about 5%.
The prepared powder was bright yellow, and its L ═ 80.02, a ═ 6.44, and b ═ 73.75 were measured by a colorimeter, indicating that it was nearly pure yellow and high in lightness. FIG. 1 shows the total reflection spectrum of the prepared powder, which has strong reflection ability in the wavelength region of yellow light, and the reflection peak at the wavelength of 590nm, showing that the powder has strong reflection ability for light in the yellow band, and is consistent with the test result of a colorimeter. FIG. 2 is the powder X-ray diffraction (XRD) pattern of the prepared powder, wherein the diffraction peaks can be totally attributed to LiNiPO4Diffraction peaks show that the obtained phase is olivine type nickel lithium phosphate, and the purity and the crystallization degree are high. FIG. 3 is a Transmission Electron Microscope (TEM) image of the prepared powder, which has a particle size of 100nm or less, and is well dispersed and weakly agglomerated.
Example 2
6kg of aqueous solution containing polyethylene glycol with the weight-average molecular weight of 300 and the mass percentage concentration of 5 percent is added into a 10L 316L stainless steel reaction kettle, 87.178g of lithium hydroxide, 696.752g of nickel acetate tetrahydrate and 375.312g of triammonium phosphate are added, mechanical stirring is started after sealing, the rotating speed of a stirrer is 300rpm, the temperature is increased to 200 ℃ from room temperature after pre-stirring for 30 minutes, and the temperature is kept for 48 hours. Cooling to below 100 deg.c, eliminating pressure, further cooling, discharging, filtering, washing and drying to obtain yellow pigment powder. The lithium added to the system was 130% of the stoichiometric ratio and the concentration of the product formed was about 7%. The prepared powder was bright yellow and tested by colorimeter with L ═ 80.12, a ═ 6.40, and b ═ 74.05.
Example 3
6kg of aqueous solution containing polyethylene glycol with the weight-average molecular weight of 600 and the mass percentage concentration of 5 percent is added into a 10L 316L stainless steel reaction kettle, 71.85g of lithium hydroxide, 197.97g of lithium acetate, 185.42g of nickel hydroxide, 262.85g of nickel sulfate hexahydrate, 268.357g of triammonium phosphate and 156.072g of diammonium hydrogen phosphate are added, mechanical stirring is started after sealing, the rotating speed of a stirrer is 300rpm, the temperature is increased to 200 ℃ from room temperature after 30 minutes of pre-stirring, and the temperature is kept for 48 hours. Cooling to below 100 deg.c, eliminating pressure, further cooling, discharging, filtering, washing and drying to obtain yellow pigment powder. The lithium added to the system was 200% of the stoichiometric ratio and the concentration of the product formed was about 7.5%. The prepared powder is bright yellow, and the color meter tests that the powder has L of 80.02, a of 6.41 and b of 73.95.
Example 4
In this example, the filtrate obtained by hydrothermal synthesis in example 1 was used, and PEG contained therein and an excessive amount of lithium source were used. The collected filtrate was supplemented with 73.89g of lithium carbonate, 581.62g of nickel nitrate hexahydrate, and 260.12g of diammonium phosphate, and then treated in the same manner as in example 1. The supplemental raw materials in this example were added in stoichiometric proportions to produce lithium nickel phosphate, with results consistent with example 1.
Example 5
This example is essentially the same as example 2, except that the amount of lithium hydroxide added to the formulation was 201.18 g. The lithium added to the system was 300% of the stoichiometric ratio and the concentration of the product formed was about 7%. The prepared powder is bright yellow, and the color meter tests that the powder has L of 80.11, a of 6.41 and b of 74.05, which is similar to the result obtained in example 2.
Comparative example 1
This comparative example is different from example 1 in that polyethylene glycol was not added to the system, and other preparation conditions were the same as example 1.
The obtained powder is bright yellow, the L, a, b and b of the powder are respectively 80.12, 6.43 and 73.72 according to a colorimeter test, and the XRD test result is similar to the graph I, so that the olivine type nickel lithium phosphate with good crystallinity is generated after hydrothermal treatment. The scanning electron microscope picture of the powder is shown in figure 4, and the test result shows that the granularity of the obtained product is not uniform and is mostly in a micron scale.
Example 6
This example is substantially the same as the embodiment 1 except that: carrying out a programmed gradient temperature rise on the hydrothermal reaction: heating to 110 deg.C at a rate of 15 deg.C/min, maintaining for 30min, heating to 230 deg.C at a rate of 5 deg.C/min, and maintaining for 24 h. The particle size of the bright yellow nano nickel lithium phosphate powder obtained in the embodiment is within the range of 80-100 nm, and compared with that of the bright yellow nano nickel lithium phosphate powder obtained in the embodiment 1, the particle size of the bright yellow nano nickel lithium phosphate powder is more uniform, the dispersibility of the bright yellow nano nickel lithium phosphate powder is better, and the product quality of the bright yellow nano nickel lithium phosphate powder is higher.
Claims (10)
1. A preparation method of a lithium nickel phosphate nano yellow pigment is characterized by comprising the following steps:
A. adding a water solution containing polyethylene glycol into a reaction kettle;
B. adding a lithium-containing raw material, a nickel-containing raw material and ammonium phosphate into the aqueous solution containing the polyethylene glycol, stirring to form a mixed solution or a suspension, and keeping mechanical stirring in hydrothermal until the mechanical stirring is started;
C. heating the reaction kettle, preserving heat, performing hydrothermal synthesis reaction, and cooling;
D. discharging the reacted mixed solution, precipitating, and filtering or centrifuging;
E. and washing and drying to obtain the lithium nickel phosphate nano yellow pigment.
2. The method of claim 1, wherein: the average weight average molecular weight of the polyethylene glycol is 200-1000.
3. The method of claim 1, wherein: the average weight average molecular weight of the polyethylene glycol is 400-600.
4. The method of claim 1, wherein: the mass concentration percentage of the polyethylene glycol in the aqueous solution in the step A is (2-10) wt%.
5. The method of claim 1, wherein: the lithium-containing raw material is one or the combination of lithium carbonate, lithium acetate, lithium chloride, lithium nitrate, lithium sulfate and lithium hydroxide; the nickel-containing raw material is one or a combination of nickel nitrate and hydrate thereof, nickel sulfate and hydrate thereof, nickel acetate and hydrate thereof and nickel hydroxide; the ammonium phosphate is one or the combination of diammonium hydrogen phosphate and triammonium phosphate.
6. The method of claim 1, wherein: in the raw material ratio, the molar ratio of Ni to P is 1: 1, and the molar ratio of Li to Ni is (1.3-3) to 1.
7. The method of claim 1, wherein: the heat preservation temperature of the hydro-thermal synthesis is 200-250 ℃, and the heat preservation time is 6-48 hours; the temperature is increased according to the following program gradient: heating to 100-110 ℃ at a speed of 10-20 ℃/min, keeping the temperature for 30-40 min, heating to 200-250 ℃ at a speed of 3-5 ℃/min, and then carrying out heat preservation.
8. The method of claim 1, wherein: the following operation step F is carried out after the step E: and (3) after the filtrate after filtration or centrifugation is supplemented with polyethylene glycol, a lithium-containing raw material, a nickel-containing raw material and ammonium phosphate, preparing the target yellow pigment according to the step flow from A to E.
9. The method of claim 8, wherein: and F, calculating the mixture ratio of the lithium-containing raw material, the nickel-containing raw material and the ammonium phosphate supplemented into the filtrate according to the stoichiometric ratio of the nickel and the lithium phosphate.
10. The lithium nickel phosphate nano yellow pigment prepared by the preparation method according to any one of claims 1 to 9.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003119408A (en) * | 2001-10-17 | 2003-04-23 | Kinya Adachi | Color-controllable rare earth phosphate-based pigment and method for producing the same |
| EP1479731A1 (en) * | 2003-05-20 | 2004-11-24 | MERCK PATENT GmbH | Coloured pigments comprising complex phosphate systems |
| CN101047242A (en) * | 2007-03-12 | 2007-10-03 | 胜利油田华鑫石油材料有限公司 | Method for preparing equal dispersion ferric phosphate lithium nano crystal by hydrothermal synthetis method |
| CN103569990A (en) * | 2013-11-20 | 2014-02-12 | 苏州大学 | Inorganic substrate phosphate pigment and preparation method and application of inorganic substrate phosphate pigment |
| CN107069029A (en) * | 2017-04-12 | 2017-08-18 | 四川国创成电池材料有限公司 | A kind of lithium battery high-voltage anode material and preparation method thereof |
| CN112938918A (en) * | 2019-12-10 | 2021-06-11 | 湖南杉杉能源科技股份有限公司 | Preparation method of cobalt phosphate powder material |
| WO2021116030A1 (en) * | 2019-12-12 | 2021-06-17 | Chemische Fabrik Budenheim Kg | Phosphate-containing anti-corrosive pigment |
-
2021
- 2021-09-10 CN CN202111096000.2A patent/CN113830748A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003119408A (en) * | 2001-10-17 | 2003-04-23 | Kinya Adachi | Color-controllable rare earth phosphate-based pigment and method for producing the same |
| EP1479731A1 (en) * | 2003-05-20 | 2004-11-24 | MERCK PATENT GmbH | Coloured pigments comprising complex phosphate systems |
| CN101047242A (en) * | 2007-03-12 | 2007-10-03 | 胜利油田华鑫石油材料有限公司 | Method for preparing equal dispersion ferric phosphate lithium nano crystal by hydrothermal synthetis method |
| CN103569990A (en) * | 2013-11-20 | 2014-02-12 | 苏州大学 | Inorganic substrate phosphate pigment and preparation method and application of inorganic substrate phosphate pigment |
| CN107069029A (en) * | 2017-04-12 | 2017-08-18 | 四川国创成电池材料有限公司 | A kind of lithium battery high-voltage anode material and preparation method thereof |
| CN112938918A (en) * | 2019-12-10 | 2021-06-11 | 湖南杉杉能源科技股份有限公司 | Preparation method of cobalt phosphate powder material |
| WO2021116030A1 (en) * | 2019-12-12 | 2021-06-17 | Chemische Fabrik Budenheim Kg | Phosphate-containing anti-corrosive pigment |
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