CN116022837A - Preparation method of praseodymium neodymium carbonate - Google Patents
Preparation method of praseodymium neodymium carbonate Download PDFInfo
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Abstract
The invention discloses a preparation method of praseodymium neodymium carbonate. The preparation method comprises the following steps: (1) Carrying out primary reaction on praseodymium neodymium chloride feed liquid, water and a first ammonium bicarbonate solution in a primary reaction zone of a reaction device to obtain a primary reaction product; (2) Carrying out secondary reaction on the primary reaction product and a second ammonium bicarbonate solution in a secondary reaction zone of a reaction device to obtain a secondary reaction product; (3) Carrying out tertiary reaction on the secondary reaction product and a third ammonium bicarbonate solution in a tertiary reaction zone of a reaction device; (4) Carrying out a fourth-stage reaction on the third-stage reaction product and a fourth ammonium bicarbonate solution in a fourth-stage reaction zone of a reaction device; (5) And carrying out five-stage reaction on the four-stage reaction product and fifth ammonium bicarbonate solution in a five-stage reaction zone of a reaction device. The method can improve the uniformity of the particle size distribution of praseodymium neodymium carbonate.
Description
Technical Field
The invention relates to a preparation method of praseodymium neodymium carbonate, in particular to a method for continuously preparing praseodymium neodymium carbonate.
Background
Rare earth elements are important in the fields of military, agriculture, metallurgical industry, petrochemical industry, glass ceramics and the like. The rare earth carbonate can be used for separating single rare earth products and can be used as a production raw material for preparing rare earth polishing powder or rare earth oxide.
CN115010165a discloses a preparation method of rare earth carbonate. The method mixes the soluble rare earth salt, the precipitator and the water to obtain a mixed solution. Mixing the mixed solution with an organic polymeric flocculant to perform precipitation reaction to obtain rare earth carbonate. This method requires the use of a flocculant, cannot be operated continuously and has poor process stability.
CN104310456a discloses a method for producing fine-grained low-chlorine rare earth carbonate. The method takes rare earth chloride feed liquid as a raw material, bottom water is injected into a precipitation reaction device in advance, and then seed crystal is added to enable the temperature of solution in the precipitation reaction device to reach 20-80 ℃; adding rare earth chloride feed liquid and ammonium bicarbonate solution into a precipitation reaction device in a parallel flow feeding mode, opening a valve at the bottom of the precipitation reaction device after the reaction time reaches 10-30 min, and controlling the outflow speed of the suspension to enable the suspension to continuously flow out; the discharged suspension is directly filtered, washed and dehydrated to obtain the fine-grained rare earth carbonate product. The rare earth carbonate particles obtained by the method have smaller particle size, seed crystal is needed, and the process stability is poor.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for preparing praseodymium neodymium carbonate, which can obtain praseodymium neodymium carbonate with good uniformity of particle size distribution. Further, the method is stable in process, and the particle size difference of praseodymium neodymium carbonate between batches is small. Furthermore, the method can be operated continuously, and the production efficiency is high. The above object is achieved by the following technical scheme.
The invention provides a preparation method of praseodymium neodymium carbonate, which comprises the following steps:
(1) Carrying out primary reaction on praseodymium neodymium chloride feed liquid, water and a first ammonium bicarbonate solution in a primary reaction zone of a reaction device to obtain a primary reaction product;
(2) Carrying out secondary reaction on the primary reaction product and a second ammonium bicarbonate solution in a secondary reaction zone of a reaction device to obtain a secondary reaction product;
(3) Carrying out tertiary reaction on the secondary reaction product and a third ammonium bicarbonate solution in a tertiary reaction zone of a reaction device to obtain a tertiary reaction product;
(4) Carrying out a four-stage reaction on the three-stage reaction product and a fourth ammonium bicarbonate solution in a four-stage reaction zone of a reaction device to obtain a four-stage reaction product;
(5) And carrying out a fifth-stage reaction on the fourth-stage reaction product and fifth ammonium bicarbonate solution in a fifth-stage reaction zone of the reaction device to obtain a fifth-stage reaction product.
According to the preparation method of the invention, preferably, the total concentration of praseodymium chloride and neodymium chloride in the praseodymium chloride neodymium feed liquid is 0.1-0.8 mol/L, the concentration of the first ammonium bicarbonate solution is 2.5-3.6 mol/L, and the flow ratio of the praseodymium chloride neodymium feed liquid, the first ammonium bicarbonate solution and water is 1 (0.1-0.4): 0.1-0.4.
According to the preparation method of the invention, preferably, the concentration of the second ammonium bicarbonate solution is 2.5-3.6 mol/L, and the flow ratio of praseodymium neodymium chloride feed liquid to the second ammonium bicarbonate solution is 1 (0.2-0.5).
According to the preparation method of the invention, preferably, the concentration of the third ammonium bicarbonate solution is 2.5-3.6 mol/L, and the flow ratio of praseodymium neodymium chloride feed liquid to the third ammonium bicarbonate solution is 1 (0.2-0.5).
According to the preparation method of the invention, preferably, the concentration of the fourth ammonium bicarbonate solution is 2.5-3.6 mol/L, and the flow ratio of praseodymium neodymium chloride feed liquid to the fourth ammonium bicarbonate solution is 1 (0.3-0.7).
According to the preparation method of the invention, preferably, the concentration of the fifth ammonium bicarbonate solution is 2.5-3.6 mol/L, and the flow ratio of praseodymium neodymium chloride feed liquid to the fifth ammonium bicarbonate solution is 1 (0.1-0.4).
The preparation method according to the present invention preferably further comprises the steps of:
at least a portion of the five-stage reaction product is aged.
According to the preparation method of the invention, preferably, a part of the five-stage reaction product is returned to the first-stage reaction at 1 to 1.8 times of the flow rate of praseodymium chloride neodymium feed liquid to carry out the first-stage reaction; the remaining five-stage reaction product was aged.
According to the production method of the present invention, preferably, the pH of the four-stage reaction system is 4 to 5, and the pH of the five-stage reaction system is 5 to 6.
According to the preparation method of the present invention, preferably, the primary reaction temperature is 38 to 50 ℃, the secondary reaction temperature is 38 to 50 ℃, the tertiary reaction temperature is 38 to 50 ℃, the quaternary reaction temperature is 38 to 50 ℃, and the five-stage reaction temperature is 38 to 50 ℃.
The praseodymium neodymium carbonate obtained by the preparation method has the advantages of uniform particle size distribution, good process stability, small standard deviation of the average particle size of the praseodymium neodymium carbonate obtained by each batch, continuous operation and production efficiency improvement.
Detailed Description
The present invention will be further described with reference to specific examples, but the scope of the present invention is not limited thereto.
According to the invention, the praseodymium neodymium chloride feed liquid is subjected to multistage reaction continuously, so that the uniformity of the particle size distribution of the obtained praseodymium neodymium carbonate is improved, and the standard deviation of the average particle size of each batch of praseodymium neodymium carbonate is small. The flow and the reaction progression of each material have important influence on the uniformity of the particle size distribution of praseodymium and neodymium carbonate and the standard deviation of the average particle size of praseodymium and neodymium carbonate in each batch, and the flow of each material is controlled within the range of the invention, so that the uniformity of the particle size distribution of praseodymium and neodymium carbonate can be further improved, and the standard deviation of the average particle size of praseodymium and neodymium carbonate in each batch can be reduced.
The preparation method of praseodymium neodymium carbonate provided by the invention comprises the following steps: (1) a step of a primary reaction; (2) a step of a secondary reaction; (3) a step of three-stage reaction; (4) a step of a four-stage reaction; (5) a step of five-stage reaction; and (6) aging and post-treatment steps. The reaction device comprises a first-stage reaction zone, a second-stage reaction zone, a third-stage reaction zone, a fourth-stage reaction zone and a fifth-stage reaction zone which are arranged continuously; optionally, a continuously disposed aging zone is also included. The reaction device may be a reaction tank or a reactor. The following is a detailed description.
Step of first-order reaction
And carrying out primary reaction on praseodymium neodymium chloride feed liquid, water and a first ammonium bicarbonate solution in a primary reaction zone of a reaction device to obtain a primary reaction product. The primary reaction is carried out in a primary reaction zone of a reaction device.
The total concentration of praseodymium chloride and neodymium chloride in the praseodymium chloride feed liquid is 0.1-0.8 mol/L; preferably 0.2 to 0.7mol/L; more preferably 0.5 to 0.65mol/L.
The concentration of the first ammonium bicarbonate solution is 2.5-3.6 mol/L; preferably 3 to 3.55mol/L; more preferably 3.2 to 3.55mol/L.
The flow ratio of praseodymium chloride neodymium feed liquid to the first ammonium bicarbonate solution is 1 (0.1-0.4); preferably 1 (0.2-0.3); more preferably 1 (0.23-0.26). In certain embodiments, the flow rate of the praseodymium neodymium chloride feed liquid is 40-55 mL/min; preferably 45 to 50mL/min. The flow rate of the first ammonium bicarbonate solution is 7-15 mL/min; preferably 10 to 13mL/min. Thus, the uniformity of the particle size distribution of the praseodymium neodymium carbonate can be improved, and the standard deviation of the average particle size of the praseodymium neodymium carbonate in each batch can be reduced.
The flow ratio of praseodymium chloride neodymium feed liquid to water is 1 (0.1-0.4); preferably 1 (0.2-0.3); more preferably 1 (0.2-0.25). In certain embodiments, the flow rate of water is 8 to 15mL/min; preferably 10 to 12mL/min. Thus, the uniformity of the particle size distribution of the praseodymium neodymium carbonate can be improved, and the standard deviation of the average particle size of the praseodymium neodymium carbonate in each batch can be reduced.
The primary reaction temperature is 38-50 ℃; preferably 39 to 48 ℃; more preferably 40 to 45 ℃.
In certain embodiments, the praseodymium neodymium chloride feed solution, water, and the first ammonium bicarbonate solution are added to the primary reaction zone of the reaction device in a co-current manner. In other embodiments, the first ammonium bicarbonate solution is fed into the primary reaction zone of the reaction device in countercurrent to the praseodymium neodymium chloride feed solution and water.
Step of the secondary reaction
And carrying out secondary reaction on the primary reaction product and a second ammonium bicarbonate solution in a secondary reaction zone of the reaction device to obtain a secondary reaction product.
The concentration of the second ammonium bicarbonate solution is 2.5-3.6 mol/L; preferably 3 to 3.55mol/L; more preferably 3.2 to 3.55mol/L.
The flow ratio of praseodymium chloride neodymium feed liquid to the second ammonium bicarbonate solution is 1 (0.2-0.5); preferably 1 (0.3 to 0.4); more preferably 1 (0.32-0.35). In certain embodiments, the flow rate of the second ammonium bicarbonate solution is 13 to 20mL/min; preferably 15 to 18mL/min. Thus, the uniformity of the particle size distribution of the praseodymium neodymium carbonate can be improved, and the standard deviation of the average particle size of the praseodymium neodymium carbonate in each batch can be reduced.
The secondary reaction temperature is 38-50 ℃; preferably 39 to 48 ℃; more preferably 40 to 45 ℃.
Step of three-stage reaction
And carrying out tertiary reaction on the secondary reaction product and a third ammonium bicarbonate solution in a tertiary reaction zone of the reaction device.
The concentration of the third ammonium bicarbonate solution is 2.5-3.6 mol/L; preferably 3 to 3.55mol/L; more preferably 3.2 to 3.55mol/L.
The flow ratio of praseodymium chloride neodymium feed liquid to the third ammonium bicarbonate solution is 1 (0.2-0.5); preferably 1 (0.3 to 0.4); more preferably 1 (0.35-0.4). In certain embodiments, the flow rate of the third ammonium bicarbonate solution is 13-22 mL/min; preferably 16 to 19mL/min. Thus, the uniformity of the particle size distribution of the praseodymium neodymium carbonate can be improved, and the standard deviation of the average particle size of the praseodymium neodymium carbonate in each batch can be reduced.
The tertiary reaction temperature is 38-50 ℃; preferably 39 to 48 ℃; more preferably 40 to 45 ℃.
Step of four-stage reaction
And carrying out four-stage reaction on the three-stage reaction product and the fourth ammonium bicarbonate solution in a four-stage reaction zone of a reaction device.
The concentration of the fourth ammonium bicarbonate solution is 2.5-3.6 mol/L; preferably 3 to 3.55mol/L; more preferably 3.2 to 3.55mol/L.
The flow ratio of praseodymium chloride neodymium feed liquid to fourth ammonium bicarbonate solution is 1 (0.3-0.7); preferably 1 (0.4-0.6). In certain embodiments, the flow ratio of praseodymium neodymium chloride feed solution to fourth ammonium bicarbonate solution is 1 (0.45-0.5). In other embodiments, the flow ratio of praseodymium neodymium chloride feed solution to fourth ammonium bicarbonate solution is 1 (0.42-0.44). The flow rate of the fourth ammonium bicarbonate solution can be 18-27 mL/min; preferably 21 to 25mL/min. Thus, the uniformity of the particle size distribution of the praseodymium neodymium carbonate can be improved, and the standard deviation of the average particle size of the praseodymium neodymium carbonate in each batch can be reduced.
The four-stage reaction temperature is 38-50 ℃; preferably 39 to 48 ℃; more preferably 40 to 45 ℃.
The pH of the four-stage reaction system is 4-5.
Step of five-stage reaction
And carrying out five-stage reaction on the four-stage reaction product and fifth ammonium bicarbonate solution in a five-stage reaction zone of a reaction device.
The concentration of the fifth ammonium bicarbonate solution is 2.5-3.6 mol/L; preferably 3 to 3.55mol/L; more preferably 3.2 to 3.55mol/L.
The flow ratio of praseodymium chloride neodymium feed liquid to fifth ammonium bicarbonate solution is 1 (0.1-0.4); preferably 1 (0.2-0.3); more preferably 1 (0.25) to 0.3). In certain embodiments, the flow rate of the fifth ammonium bicarbonate solution is 7 to 15mL/min; preferably 9 to 13mL/min. Thus, the uniformity of the particle size distribution of the praseodymium neodymium carbonate can be improved, and the standard deviation of the average particle size of the praseodymium neodymium carbonate in each batch can be reduced.
The five-stage reaction temperature is 38-50 ℃; preferably 39 to 48 ℃; more preferably 40 to 45 ℃.
The pH of the five-stage reaction system is 5-6.
The five-stage reaction product may be split into two portions, five-stage reaction product a and five-stage reaction product B, respectively. The five-stage reaction product A returns to the first-stage reaction zone to carry out the first-stage reaction. The five-stage reaction product B flows into an aging zone of the reaction device. The flow of the fifth-stage reaction product A is 1 to 1.8 times of the flow of praseodymium chloride neodymium feed liquid; preferably 1.2 to 1.7 times; more preferably 1.4 to 1.6 times.
Aging and post-treatment step
At least a portion of the five-stage reaction product is aged. Preferably, the fifth stage reaction product B is aged. The ageing is carried out in an ageing zone of the reaction device.
The aging time can be 1-15 h; preferably 2 to 13 hours; more preferably 3 to 10 hours.
After aging, a solid and a supernatant were obtained. And (3) washing and drying the solid substance to obtain praseodymium neodymium carbonate. The content of praseodymium neodymium carbonate in the supernatant is less than or equal to 0.08g/L.
The test method is described as follows:
the particle size (D10, D50, D90) of praseodymium neodymium carbonate is that the praseodymium neodymium carbonate, water and dispersing agent are placed in a beaker, and then ultrasonic is carried out for 10min by an ultrasonic instrument, thus obtaining the sample to be detected. And (3) placing the sample to be measured into a circulating dispersion sample injection system of a laser particle analyzer, and measuring, analyzing and calculating to obtain a result.
The uniformity of the particle size distribution is indicated by (D90-D10)/D50. Large values indicate poor distribution uniformity and small values indicate good distribution uniformity.
Examples 1 to 2
(1) Praseodymium neodymium chloride feed liquid, water and a first ammonium bicarbonate solution are added into a primary reaction zone of a reaction device in a parallel flow mode, and primary reaction is carried out at 42 ℃ to obtain a primary reaction product.
(2) The first-stage reaction product flows to a second-stage reaction zone of the reaction device, and the second ammonium bicarbonate solution is added into the second-stage reaction zone of the reaction device to carry out the second-stage reaction at 43 ℃ to obtain the second-stage reaction product.
(3) And the second-stage reaction product flows to a third-stage reaction zone of the reaction device, and the third ammonium bicarbonate solution is added into the third-stage reaction zone of the reaction device to perform a third-stage reaction at 43 ℃ to obtain a third-stage reaction product.
(4) And the third-stage reaction product flows to a fourth-stage reaction zone of the reaction device, and the fourth ammonium bicarbonate solution is added into the fourth-stage reaction zone of the reaction device to carry out the fourth-stage reaction at the temperature of 43 ℃ to obtain the fourth-stage reaction product.
(5) The four-stage reaction product flows to a five-stage reaction zone of the reaction device, the fifth ammonium bicarbonate solution is added into the five-stage reaction zone of the reaction device, and the five-stage reaction is carried out at 43 ℃ to obtain the five-stage reaction product.
The five-stage reaction product is split into two parts, namely a five-stage reaction product A and a five-stage reaction product B. The five-stage reaction product A is returned to the first-stage reaction zone of the reaction device for first-stage reaction. The five-stage reaction product B flows into the aging zone of the reaction device.
(6) And (3) aging the five-stage reaction product B in an aging zone of the reaction device for 3.5 hours to obtain a solid substance and a supernatant. And collecting a batch of solid matters every 3.5 hours, and washing and drying the solid matters to obtain praseodymium neodymium carbonate.
Example 1A total of 3 batches of solid material were collected to give three batches of praseodymium neodymium carbonate, designated 1A, 1B and 1C, respectively. Example 2A total of 1 batch of solid material was collected to give a batch of praseodymium neodymium carbonate, designated 2A.
The specific parameters are shown in table 1. The properties of the obtained praseodymium neodymium carbonate are shown in Table 2.
TABLE 1
| Example 1 | Example 2 | |
| Concentration (mol/L) of praseodymium chloride neodymium feed liquid | 0.64 | 0.6 |
| Concentration of ammonium bicarbonate solution (mol/L) | 3.55 | 3.40 |
| Flow rate of praseodymium neodymium chloride feed liquid (mL/min) | 49.5 | 45.5 |
| Flow of first ammonium bicarbonate solution (mL/min) | 12.18 | 11.66 |
| Flow of Water (mL/min) | 11.4 | 10.56 |
| Flow of second ammonium bicarbonate solution (mL/min) | 16.98 | 15.15 |
| Flow of third ammonium bicarbonate solution (mL/min) | 18.89 | 16.8 |
| Flow of fourth ammonium bicarbonate solution (mL/min) | 23.74 | 22.49 |
| Flow of fifth ammonium bicarbonate solution (mL/min) | 12.58 | 9.96 |
| Flow of five-stage reaction product A (mL/min) | 79.20 | 72.8 |
| Content (g/L) of praseodymium neodymium carbonate in the supernatant | ≤0.08 | ≤0.08 |
Note that: the concentrations of the first ammonium bicarbonate solution, the second ammonium bicarbonate solution, the third ammonium bicarbonate solution, the fourth ammonium bicarbonate solution, and the fifth ammonium bicarbonate solution are all the same, and are all expressed in table 1 as the concentrations of the ammonium bicarbonate solutions.
Example 3
Example 1 was repeated except that the flow rate of the fourth ammonium bicarbonate solution was 21.53 mL/min.
Example 3 three batches of solid material were collected to give three batches of praseodymium neodymium carbonate, designated 3A, 3B and 3C, respectively.
Comparative example 1
Dividing the secondary reaction product into two parts, namely a secondary reaction product A and a secondary reaction product B, without performing the steps (3) - (5); the second-stage reaction product A returns to a first-stage reaction zone of the reaction device to carry out first-stage reaction; the procedure of example 1 was followed except that the second reaction product B was aged in the third reaction zone of the reaction apparatus. The properties of the obtained praseodymium neodymium carbonate are shown in Table 2.
Comparative example 1 three batches of solid material were collected to give three batches of praseodymium neodymium carbonate, designated 4A, 4B and 4C, respectively.
TABLE 2
The present invention is not limited to the above-described embodiments, and any modifications, improvements, substitutions, and the like, which may occur to those skilled in the art, fall within the scope of the present invention without departing from the spirit of the invention.
Claims (10)
1. The preparation method of praseodymium neodymium carbonate is characterized by comprising the following steps:
(1) Carrying out primary reaction on praseodymium neodymium chloride feed liquid, water and a first ammonium bicarbonate solution in a primary reaction zone of a reaction device to obtain a primary reaction product;
(2) Carrying out secondary reaction on the primary reaction product and a second ammonium bicarbonate solution in a secondary reaction zone of a reaction device to obtain a secondary reaction product;
(3) Carrying out tertiary reaction on the secondary reaction product and a third ammonium bicarbonate solution in a tertiary reaction zone of a reaction device to obtain a tertiary reaction product;
(4) Carrying out a four-stage reaction on the three-stage reaction product and a fourth ammonium bicarbonate solution in a four-stage reaction zone of a reaction device to obtain a four-stage reaction product;
(5) Carrying out a fifth-stage reaction on the fourth-stage reaction product and fifth ammonium bicarbonate solution in a fifth-stage reaction zone of a reaction device to obtain a fifth-stage reaction product;
wherein, the first-stage reaction zone, the second-stage reaction zone, the third-stage reaction zone, the fourth-stage reaction zone and the fifth-stage reaction zone are continuously arranged in the reaction device.
2. The preparation method according to claim 1, wherein the total concentration of praseodymium chloride and neodymium chloride in the praseodymium chloride neodymium feed liquid is 0.1-0.8 mol/L, the concentration of the first ammonium bicarbonate solution is 2.5-3.6 mol/L, and the flow ratio of the praseodymium chloride neodymium feed liquid, the first ammonium bicarbonate solution and water is 1 (0.1-0.4): 0.1-0.4.
3. The preparation method according to claim 1, wherein the concentration of the second ammonium bicarbonate solution is 2.5-3.6 mol/L, and the flow ratio of praseodymium neodymium chloride feed liquid to the second ammonium bicarbonate solution is 1 (0.2-0.5).
4. The preparation method according to claim 1, wherein the concentration of the third ammonium bicarbonate solution is 2.5-3.6 mol/L, and the flow ratio of praseodymium neodymium chloride feed liquid to the third ammonium bicarbonate solution is 1 (0.2-0.5).
5. The preparation method according to claim 1, wherein the concentration of the fourth ammonium bicarbonate solution is 2.5-3.6 mol/L, and the flow ratio of praseodymium neodymium chloride feed liquid to the fourth ammonium bicarbonate solution is 1 (0.3-0.7).
6. The preparation method according to claim 1, wherein the concentration of the fifth ammonium bicarbonate solution is 2.5-3.6 mol/L, and the flow ratio of praseodymium neodymium chloride feed liquid to the fifth ammonium bicarbonate solution is 1 (0.1-0.4).
7. The method of manufacturing according to claim 1, further comprising the step of:
at least a portion of the five-stage reaction product is aged.
8. The method according to claim 7, wherein a part of the five-stage reaction product is returned to the first-stage reaction at a flow rate of praseodymium neodymium chloride feed liquid 1 to 1.8 times, and the first-stage reaction is carried out; the remaining five-stage reaction product was aged.
9. The process according to claim 1, wherein the pH of the four-stage reaction system is 4 to 5 and the pH of the five-stage reaction system is 5 to 6.
10. The production method according to any one of claims 1 to 9, characterized in that:
the primary reaction temperature is 38-50 ℃, the secondary reaction temperature is 38-50 ℃, the tertiary reaction temperature is 38-50 ℃, the quaternary reaction temperature is 38-50 ℃, and the five-stage reaction temperature is 38-50 ℃.
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