CN109650434B - Preparation process of small-particle-size cerium carbonate - Google Patents
Preparation process of small-particle-size cerium carbonate Download PDFInfo
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- CN109650434B CN109650434B CN201811619976.1A CN201811619976A CN109650434B CN 109650434 B CN109650434 B CN 109650434B CN 201811619976 A CN201811619976 A CN 201811619976A CN 109650434 B CN109650434 B CN 109650434B
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- C—CHEMISTRY; METALLURGY
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- C01F17/247—Carbonates
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- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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Abstract
The invention relates to a preparation process of small-granularity cerium carbonate, which comprises the following steps: (1) adding water into cerium carbonate, stirring and mixing to obtain cerium carbonate slurry; (2) sieving the cerium carbonate slurry obtained in the step (1), and performing sanding treatment to obtain sanded cerium carbonate slurry; (3) adding a dispersing agent into the sand-milled cerium carbonate slurry obtained in the step (2), and continuing grinding; (4) spraying and drying to obtain the product. The cerium carbonate prepared by the method has small granularity, high total amount, high purity, high activity and low bulk density, and is just matched with the condition requirements of the raw material preparation process of cerium sulfide. Low production cost, batch production and high yield.
Description
Technical Field
The invention relates to the technical field of raw material preparation, in particular to a preparation process of small-granularity cerium carbonate.
Technical Field
Cerium carbonate is an important raw material for preparing cerium sulfide pigment, and the particle size, bulk density and activity of the cerium carbonate have great influence on the preparation of cerium sulfide. The granularity of cerium sulfide particles prepared by synthesizing large-particle cerium carbonate is generally larger, and influences the tinting strength and covering power of products, so that the raw material cerium carbonate needs to be subjected to small-granularity treatment before the preparation of the cerium sulfide. The small-particle-size cerium carbonate sold in the market is generally high in price, low in activity and high in bulk density, and cannot meet the use requirement.
In general, cerium carbonate is prepared by charging a cerium precursor in a solution state and a urea reactant into a batch reactor having a certain size and performing a temperature-increasing reaction, thereby obtaining cerium carbonate in a powder form. The heat transfer rate of each part of the reactor of this method is not uniform, and thus the crystal structure, shape and appearance, or size of the finally prepared cerium carbonate powder is not uniform in many cases. Therefore, the increase of the size of the reactor has certain limitation, and is not beneficial to the batch production of cerium carbonate.
Cerium sulfide powder pigment is taken as an inorganic red colorant, and is popular with market users in nylon and plastic industries due to high performance and beautiful color. Cerium carbonate is an important raw material for preparing cerium sulfide pigments, and thus, there is a demand for a method for preparing cerium carbonate having a small particle size with high purity.
Disclosure of Invention
The cerium carbonate prepared by the invention can be used for preparing cerium sulfide, has small granularity, high total amount, high purity, high activity and low bulk density, exactly matches the condition requirements of the raw material preparation process of cerium sulfide, has low production cost, can be produced in batches and has high yield.
The preparation process of the small-granularity cerium carbonate adopts the common cerium carbonate to prepare the small-granularity cerium carbonate by means of sanding, adding a dispersing agent, spray drying and the like, and the prepared cerium carbonate has stable granularity and proper bulk density and activity. The method has simple process and easy operation, and the total cost of the prepared small-granularity cerium carbonate is lower; the activity and bulk density are just matched with the preparation process of cerium sulfide.
The technical scheme of the invention is realized as follows:
the invention provides a preparation process of small-granularity cerium carbonate, which comprises the following steps:
(1) adding water into cerium carbonate, stirring and mixing to obtain cerium carbonate slurry;
(2) sieving the cerium carbonate slurry obtained in the step (1), and performing sanding treatment to obtain sanded cerium carbonate slurry;
(3) adding a dispersing agent into the sand-milled cerium carbonate slurry obtained in the step (2), and continuing grinding;
(4) spraying and drying to obtain the product.
Preferably, in step (1), the mass-to-volume ratio between the cerium carbonate and the water is 1000: 1.2-2.0(w/v, g/L), preferably 1000: 1.5(w/v, g/L);
preferably, in the step (1), the stirring speed is 500-1000 rpm, preferably 500-800 rpm, and more preferably 600 rpm;
preferably, in step (1), the stirring time is 30 to 40 minutes, preferably 30 to 35 minutes, and more preferably 30 minutes;
preferably, in step (2), the screened mesh number is 30-100 meshes, preferably 50-100 meshes, more preferably 60 meshes;
preferably, in the step (2), the sand grinding is carried out in a sand mill, and the rotation speed of the sand mill is 500-1000 r/min, preferably 650-900 r/min, and more preferably 750 r/min;
preferably, in step (2), the sanding is multi-stage sanding;
preferably, in step (2), the sanding time is 36-72 hours, preferably 48 hours;
preferably, in step (2), D is sanded to the slurry501.8-2.5 microns, preferably 2 microns;
preferably, in step (3), the dispersant is selected from organic polymers such as polyethylene glycol (PEG), ammonium Polyacrylate (PAA), etc.; preferably polyethylene glycol;
preferably, in step (3), the mass of the dispersant is 5 to 10 wt%, preferably 5 wt%, of the mass of cerium carbonate in terms of oxide;
preferably, in step (3), the pH value of the dispersant is 8-10, preferably 9;
preferably, in the step (3), the grinding is performed in a grinder, and the rotation speed of the grinder is 600-;
preferably, in step (4), the temperature of the drying is 80-100 ℃, preferably 90 ℃;
preferably, in step (4), the drying time is 3 to 5 hours, preferably 4 hours;
in a specific embodiment, the preparation process of the present invention is as follows:
FIG. 1 is a process flow diagram of the present invention, as shown in FIG. 1, adding 1 ton of cerium carbonate into a size mixing tank, adding 1.2-2.0 cubic meters of water into the size mixing tank, and stirring at a constant speed of 600 rpm for 30-40 minutes to mix.
The adjusted cerium carbonate slurry was passed through a 60 mesh screen and the slurry was pumped into a sand tank using a diaphragm pump. Specifically, the sand mill No. 1 tank was started with agitation, and then the slurry was pumped with a diaphragm pump into the sand mill No. 1 tank. The sand mill was operated at 750 rpm and the inlet pressure of the feed diaphragm pump was 2.0 mpa. (zirconium beads are selected to have a diameter of 0.8-1 mm). Open valve 1 of No. 1 jar of sanding, the diaphragm pump that makes the sand mill feeding communicates with each other with the discharge gate of No. 1 jar of sanding, opens valve 4, makes the discharge gate of sand mill communicate with each other with No. 2 jar feed inlets of sanding, opens the stirring of No. 2 jars of sanding. After waiting that the thick liquid in the sanding 1 number jar is emptied, close valve 1, open valve 2 makes the diaphragm pump of sand mill feeding communicate with each other with the discharge gate of sanding 2 number jar, and open valve 3 closes valve 4, makes the discharge gate of sand mill communicate with each other with sanding 1 number jar feed inlet. Sanding the prepared slurry for 48 hours by a sand mill, uniformly screening sanded slurry samples, performing quality detection, and detecting the granularity D50Is 1.8-2.5 microns.
And adding dispersant polyethylene glycol into the cerium carbonate slurry which is qualified by detection, wherein the mass of the polyethylene glycol is 5-10 wt% of that of the rare earth oxide in 1 ton of cerium carbonate, the pH value of the polyethylene glycol is 8-10, and grinding for 1-3 hours at the rotating speed of 750. Spray drying the cerium carbonate slurry by an LPG high-speed centrifugal spray dryer at the drying temperature of 80-100 ℃ for 3-5 hours. And opening a bottom valve of the feeding tank, gradually increasing the feeding speed of spray drying when the temperature of the outlet air of the spray drying rises, and taking out the dried cerium carbonate product after the drying is finished.
The cerium carbonate with high purity and small granularity is prepared through adding water, grinding, adding dispersant and spray drying.
Compared with the prior art, the technical scheme of this application has following advantage:
1. this application adds water earlier and sieves again, because the cerous carbonate of purchase contains a large amount of water, has viscosity, and easy caking does not mix into thick liquids, and the reciprocating sieve is difficult with its screening, and screening efficiency is low.
2. The invention adopts water adding and grinding, the grinding speed, the grinding time and the particle size of the finally ground slurry are controlled within a proper range, the grinding speed is too low, the sand mill generates heat seriously, the viscosity of the slurry is increased, and the sand mill and a pipeline are easy to block. The grinding speed is too high, and the sanding efficiency is low. When the grinding time is too low, the particle size of the slurry is high, and when the grinding time is too high, the particle size of the slurry is not reduced any more, and the particle size sometimes increases due to serious agglomeration. The particle size of the slurry directly determines the particle size of the cerium carbonate after drying, and the smaller the particle size, the better, but the particle size of the slurry is set to 2 μm in consideration of cost and process problems.
3. The invention adds the dispersant in order to reduce the agglomeration phenomenon of carbonic acid. The dispersant inhibits agglomeration mainly by 3 actions in solution: 1) the surface tension of the interface is reduced by adsorption; 2) a layer of liquid film is formed on the surfaces of the particles through the action of the micelle to prevent the particles from approaching each other; 3) is to use steric hindrance. The dispersant is not added, the agglomeration phenomenon of the cerium carbonate is obvious, the granularity is large, and the bulk density is large.
4. The temperature of the drying process needs to be controlled to be 80-100 ℃, the temperature is too low, the cerium carbonate has high water content, and the TREO is low. When the temperature is too high, TREO is high, but cerium carbonate contains too much cerium oxide, which affects the activity of cerium carbonate.
Drawings
In order to more clearly illustrate the technical solution of the present invention, the drawings required to be used in the embodiments will be briefly described below.
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Adding 1 ton of cerium carbonate into a batching tank, adding 1.2 cubic meters of water into the batching tank, and uniformly stirring at the rotating speed of 600 revolutions per minute for 40 minutes to prepare slurry. The prepared cerium carbonate slurry is subjected to sanding for 60 hours by a sand mill through a 60-mesh sieve, the sand mill uniformly screens sanded slurry samples at 750 revolutions per minute, and the quality detection is carried out, wherein the granularity D is502.0 μm, 5 wt% polyethylene glycol was added, pH 8, and stirred at 750 rpm for 1 hour. Spray drying the cerium carbonate slurry by an LPG high-speed centrifugal spray dryer at the drying temperature of 100 ℃ for 3 hours to obtain the granularity D of the small-granularity cerium carbonate502.5 micron, total TREO 62 wt%, purity 99.9%, bulk density 0.6g/cm3。
Example 2
Adding 1 ton of cerium carbonate into a blending tank, adding 1.5 cubic meters of water into the blending tank, and uniformly stirring at the rotating speed of 600 revolutions per minute for 30 minutes to prepare slurry. The prepared cerium carbonate slurry is subjected to sanding for 48 hours by a sand mill through a 60-mesh sieve, the sand mill uniformly screens sanded slurry samples at 750 revolutions per minute, and the quality detection is carried out, wherein the granularity D is50At 1.8 μm, 8 wt% polyethylene glycol was added, pH 8, and stirred at 750 rpm for 2 hours. Spray drying the cerium carbonate slurry by an LPG high-speed centrifugal spray dryer at the drying temperature of 80 ℃ for 5 hours to obtain the small-granularity cerium carbonate D502 microns, total TREO 63 wt%, purity 99.9%, bulk density 0.56g/cm3。
Example 3
1 ton of cerium carbonateAdding into a mixing tank, adding 2 cubic meters of water into the mixing tank, and uniformly stirring at a rotating speed of 600 revolutions per minute for 30 minutes to mix slurry. The prepared cerium carbonate slurry is subjected to sanding for 48 hours by a sand mill through a 60-mesh sieve, the sand mill uniformly screens sanded slurry samples at 750 revolutions per minute, and the quality detection is carried out, wherein the granularity D is50At 2.0 microns, 10% polyethylene glycol was added at pH 10 and stirred at 750 rpm for 2 hours. Spray drying the cerium carbonate slurry by an LPG high-speed centrifugal spray dryer at the drying temperature of 80 ℃ for 5 hours to obtain the small-granularity cerium carbonate D502.1 micron, total TREO 65 wt%, purity 99.9%, bulk density 0.5g/cm3。
Example 4
Adding 1 ton of cerium carbonate into a batching tank, adding 1.8 cubic meters of water into the batching tank, and uniformly stirring at the rotating speed of 600 revolutions per minute for 35 minutes to prepare slurry. The prepared cerium carbonate slurry is subjected to sanding for 60 hours by a sand mill through a 60-mesh sieve, the sand mill uniformly screens sanded slurry samples at 750 revolutions per minute, and the quality detection is carried out, wherein the granularity D is50At 1.8 μm, 5% polyethylene glycol was added, pH 8, and the mixture was stirred at 750 rpm for 3 hours. Spray drying the cerium carbonate slurry by an LPG high-speed centrifugal spray dryer at the drying temperature of 100 ℃ for 3 hours to obtain the granularity D of the small-granularity cerium carbonate501.8 micron, total TREO 67 wt%, purity 99.95%, bulk density 0.4g/cm3。
Example 5
Adding 1 ton of cerium carbonate into a blending tank, adding 1.5 cubic meters of water into the blending tank, and uniformly stirring at the rotating speed of 600 revolutions per minute for 30 minutes to prepare slurry. The prepared cerium carbonate slurry is subjected to sanding for 48 hours by a sand mill through a 60-mesh sieve, the sand mill uniformly screens sanded slurry samples at 750 revolutions per minute, and the quality detection is carried out, wherein the granularity D is50At 2 microns, 5 wt% polyethylene glycol was added, pH 9, and stirred at 750 rpm for 3.5 hours. Feeding cerium carbonate slurry into an LPG high-speed centrifugal spray dryerSpray drying at 90 deg.C for 4 hr to obtain small-particle cerium carbonate particle size D502.0 micron, total TREO 68 wt%, purity 99.95%, bulk density 0.5g/cm3。
Example 6Influence of polishing speed
The same protocol as in example 5 was used except that the milling rates were 500 rpm, 600 rpm, 750 rpm, 900 rpm, 1000 rpm and the time to reach a slurry particle size of 2 microns was as shown in table 1 below:
TABLE 1 influence of different grinding speeds on sanding time
From the above results, it can be seen that the grinding speed is less than 500 rpm, the heat generation of the sand mill is serious, the slurry viscosity is increased, the sand mill and the pipeline are easily blocked, and the grinding time is increased. The grinding speed is higher than 1000 r/min, and the sanding efficiency is low.
Example 7Influence of grinding time
The same protocol as in example 5 was used except that the milling time was 24 hours, 36 hours, 48 hours, 60 hours, 70 hours and the results of the slurry particle size test are shown in table 2:
TABLE 2 Effect of different grinding times on slurry particle size
According to the results, the particle size of the slurry can only reach about 4 microns at 24 hours of grinding, about 2 microns at 48 hours, and 1.8-2 microns at 48-60 hours, so that the sanding efficiency is low, the particle size change is small, the time and resources are wasted, and the particle size of the slurry can not be reduced any more at more than 60 hours, and the particle size sometimes increases due to serious agglomeration. The particle size of the slurry directly determines the particle size of the cerium carbonate after drying, and the smaller the particle size, but the particle size of the slurry is set to 2 μm in consideration of cost and process problems.
Example 8
The same protocol as in example 5 was used except that the dispersant polyethylene glycol was added in an amount of 0 wt%, 3 wt%, 5 wt%, 8 wt%, 10 wt% based on the mass of cerium carbonate in terms of oxide, and the particle size and bulk density results of cerium carbonate are shown in Table 3 below:
TABLE 3 Effect of dispersant amount on cerium carbonate particle size and bulk Density
From the above results, it can be seen that the more the dispersant, the smaller the particle size and the smaller the bulk density, but the smaller the particle size of cerium carbonate required for the synthesis of cerium sulfide is, the better, but the bulk density cannot be made too small. When the bulk density is too small, the amount of the material to be charged at the time of synthesis is small, and the color of cerium sulfide is low.
Example 9
The same protocol as in example 5 was used except that the drying temperatures were 80, 85, 90, 95, 100 ℃ 110 ℃ and the results of the total amount of all-phase rare earth oxide (TREO) of cerium carbonate and the content of cerium oxide were as shown in Table 4 below:
TABLE 4 TREO and Ceria content of dried cerium carbonate at different temperatures
Comparative example 1
1 ton of cerium carbonate passes through a 60-mesh sieve, because the cerium carbonate contains certain moisture and has high viscosity, the cerium carbonate can agglomerate during sieving, the blanking speed is low, the sieving efficiency is extremely low at the moment and needs more than 5 hours, and the water is added firstly, and the slurry is prepared and then sieved for only 30 minutes.
Claims (24)
1. A preparation process of small-particle-size cerium carbonate comprises the following steps:
(1) adding water into cerium carbonate, stirring and mixing to obtain cerium carbonate slurry;
(2) sieving the cerium carbonate slurry obtained in the step (1), and performing sanding treatment to obtain sanded cerium carbonate slurry;
(3) adding a dispersing agent into the sand-milled cerium carbonate slurry obtained in the step (2), and continuing grinding;
(4) spraying and drying to obtain the product;
in the step (2), the sand grinding is carried out in a sand mill, and the rotating speed of the sand mill is 500-; the sanding is multi-stage sanding; the sanding time is 36-72 hours; sanding to slurry D501.8-2.5 microns;
in the step (3), the dispersant is polyethylene glycol; the mass of the dispersing agent is 3-10 wt% of the mass of cerium carbonate calculated by oxide; the grinding is carried out in a grinding machine, and the rotating speed of the grinding machine is 600-1000 revolutions per minute;
in the step (4), the temperature of the drying is 80-100 ℃.
2. The production process according to claim 1, wherein in step (1), the mass-to-volume ratio between the cerium carbonate and the water is 1000: 1.2-2.0(w/v, g/L).
3. The production process according to claim 1, wherein in step (1), the mass-to-volume ratio between the cerium carbonate and the water is 1000: 1.5(w/v, g/L).
4. The process according to claim 1, wherein in step (1), the stirring speed is 500-1000 rpm.
5. The process according to claim 1, wherein in step (1), the stirring speed is 500-800 rpm.
6. The process according to claim 1, wherein in the step (1), the stirring speed is 600 rpm.
7. The process according to claim 1, wherein in the step (1), the stirring time is 30 to 40 minutes.
8. The process according to claim 1, wherein in the step (1), the stirring time is 30 to 35 minutes.
9. The production process according to claim 1, wherein in the step (1), the stirring time is 30 minutes.
10. The process according to claim 1, wherein in the step (2), the mesh number of the screen is 30 to 100 mesh.
11. The process according to claim 1, wherein in the step (2), the mesh number of the screen is 50 to 100 mesh.
12. The process according to claim 1, wherein in the step (2), the mesh number of the screen is 60 meshes.
13. The preparation process according to claim 1, wherein in step (2), the rotation speed of the sand mill is 650-.
14. The process according to claim 1, wherein in the step (2), the rotation speed of the sand mill is 750 rpm.
15. The process of claim 1, wherein in step (2), the sanding time is 48 hours.
16. The process of claim 1, wherein in step (2), the sand is sanded to D of the slurry50Is 2 microns.
17. The production process according to claim 1, wherein in step (3), the mass of the dispersant is 5 wt% of the mass of cerium carbonate in terms of oxide.
18. The production process according to claim 1, wherein in the step (3), the pH of the dispersant is 8 to 10.
19. The production process according to claim 1, wherein in the step (3), the dispersant has a pH of 9.
20. The process according to claim 1, wherein in step (3), the rotation speed of the grinder is 650-900 rpm.
21. The process according to claim 1, wherein in the step (3), the rotation speed of the mill is 750 rpm.
22. The production process according to claim 1, wherein in the step (4), the temperature of the drying is 90 ℃.
23. The production process according to claim 1, wherein in the step (4), the drying time is 3 to 5 hours.
24. The production process according to claim 1, wherein in the step (4), the drying time is 4 hours.
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Effective date of registration: 20210903 Address after: 014000 Jiuyuan District Industrial Park, Baotou City, Inner Mongolia Autonomous Region Patentee after: Inner Mongolia Kalesi rare earth environmental protection Pigment Co.,Ltd. Address before: 014030 C-610, software park, entrepreneurship center, Baotou rare earth high tech Zone, Inner Mongolia Autonomous Region Patentee before: BAOTOU HONGBO TE TECHNOLOGY Co.,Ltd. |
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