CN110745857A - Preparation method and product of high-purity clean cerium nitrate - Google Patents
Preparation method and product of high-purity clean cerium nitrate Download PDFInfo
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- CN110745857A CN110745857A CN201810725449.2A CN201810725449A CN110745857A CN 110745857 A CN110745857 A CN 110745857A CN 201810725449 A CN201810725449 A CN 201810725449A CN 110745857 A CN110745857 A CN 110745857A
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention relates to a preparation method of high-purity clean cerium nitrate and a product, belonging to the technical field of rare earth materials, the method mainly comprises the process flows of cerium nitrate solution preparation, filtration, oil removal, heating concentration, ultrasonic crystallization, aging, centrifugal separation, recrystallization and the like, and the finally prepared cerium nitrate is the high-purity clean cerium nitrate by controlling the pH value, the heating concentration temperature, the crystallization mode, the aging time and the recrystallization mode of the cerium nitrate solution, wherein the mass fraction of non-rare earth impurity elements is less than 0.5 multiplied by 10 < -6 >, and the yield can reach 80-85 percent. The method is simple and easy to implement, has low requirements on equipment and low cost, and is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of rare earth materials, and particularly relates to a preparation method and a product of high-purity clean cerium nitrate.
Background
In the distribution of rare earth elements, cerium accounts for about 50% of light rare earth resources. High purity, clean cerium compounds are one of the host materials for fluorescent, microwave, laser, magneto-optical, precision ceramics and semiconductors, but in most applications, their effectiveness is related to factors such as their purity, physical properties and impurity content. With the increasing application of high-purity cerium, the demand on the non-rare earth content index in the cerium compound is higher and higher.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a method for preparing high-purity cerium nitrate; the second purpose is to provide a high-purity clean cerium nitrate.
In order to achieve the purpose, the invention provides the following technical scheme:
1. a preparation method of high-purity clean cerium nitrate comprises the following steps:
(1) adding cerium nitrate into nitric acid until the cerium nitrate is completely dissolved to prepare a cerium nitrate solution, and adjusting the pH value of the cerium nitrate solution to 0.8-1;
(2) filtering the cerium nitrate solution obtained in the step (1) to obtain a filtrate, and performing oil removal treatment on the filtrate;
(3) concentrating the filtrate treated in the step (2) at the temperature of 120-125 ℃ until a supersaturated cerium nitrate solution is obtained;
(4) crystallizing the supersaturated cerium nitrate solution obtained in the step (3) by using ultrasonic waves under an ice bath condition, and centrifuging after aging to obtain cerium nitrate crystals;
(5) and (4) recrystallizing the cerium nitrate crystal obtained in the step (4) and then centrifuging to obtain the high-purity clean cerium nitrate.
Further, in the step (2), the degreasing treatment is performed by using ultrasonic waves.
Further, in the step (4), when the crystallization is performed by using the ultrasonic wave, the ultrasonic frequency is 20-45kHz, and the ultrasonic power is 350-500W.
Further, in the step (4), the aging time is 0.5-1 h.
Further, in the step (5), the recrystallization specifically includes the steps of:
1) dissolving the cerium nitrate crystal obtained in the step (4) with deionized water, filtering with a microfilter to obtain a filtrate I, concentrating the filtrate I at the temperature of 120-125 ℃ to obtain a supersaturated cerium nitrate solution I, crystallizing the supersaturated cerium nitrate solution I by using ultrasonic waves under the ice bath condition, and centrifuging after aging to obtain the cerium nitrate crystal I;
2) dissolving the cerium nitrate crystal I obtained in the step 1) with deionized water, filtering with an ultrafilter to obtain a filtrate II, concentrating the filtrate II at the temperature of 120-125 ℃ to obtain a supersaturated cerium nitrate solution II, crystallizing the supersaturated cerium nitrate solution II under the ice bath condition by using ultrasonic waves, and centrifuging after aging to obtain high-purity clean cerium nitrate.
Further, in the step 1) and the step 2), when the ultrasonic wave is used for crystallization, the ultrasonic frequency is 20-45kHz, and the ultrasonic power is 350-500W.
Further, in the step 1) and the step 2), the aging time is 0.5-1 h.
2. The high-purity clean cerium nitrate prepared by the method.
The invention has the beneficial effects that: the invention provides a preparation method of high-purity clean cerium nitrate and a product, wherein the method comprises the step of controlling the pH value of a cerium nitrate solution, the heating concentration temperature, the crystallization mode, the aging time and the recrystallization mode to ensure that the finally prepared cerium nitrate is the high-purity clean cerium nitrate, wherein the mass fraction of non-rare earth impurity elements is less than 0.5 multiplied by 10 < -6 >, and the yield can reach about 85 percent. Wherein, the pH value of the cerous nitrate solution is controlled to be 0.8-1, and the temperature is controlled to be 120-125 ℃, thereby not only ensuring the supersaturation degree of the cerous nitrate solution and ensuring the yield of the final product as far as possible by separating out cerous nitrate in the later period, but also ensuring that the non-rare earth impurity elements carried by the cerous nitrate crystal are less when the cerous nitrate crystal is separated out in the supersaturation solution. Further, inject and utilize ultrasonic wave crystallization under the ice bath condition, make solution great supersaturation appear through rapid cooling on the one hand, make it surmount metastable zone limit and separate out a large amount of crystal nucleuses, form the crystal grain, and avoid the appearance of cubic crystal, on the other hand, through control ultrasonic frequency and power, with the help of ultrasonic cavitation, can effectively improve nucleation speed, thereby shorten crystallization time, simultaneously can also control the crystal size, improve particle size distribution, more importantly can make the nucleation process realize under low saturation, further promote the yield of end product. The method is simple and easy to implement, has low requirements on equipment and low cost, and is suitable for industrial production.
Drawings
In order to make the object, technical scheme and beneficial effect of the invention more clear, the invention provides the following drawings for explanation:
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The preferred embodiments of the present invention will be described in detail below.
Example 1
The preparation of the high-purity clean cerium nitrate according to the process flow for preparing the high-purity clean cerium nitrate shown in fig. 1 specifically comprises the following steps:
(1) adding cerium nitrate into nitric acid until the cerium nitrate is completely dissolved to prepare a cerium nitrate solution, and adjusting the pH value of the cerium nitrate solution to 0.8;
(2) filtering the cerium nitrate solution obtained in the step (1) by using a plate frame to obtain a filtrate, and performing ultrasonic degreasing treatment on the filtrate;
(3) concentrating the filtrate treated in the step (2) at 125 ℃ to obtain a supersaturated cerium nitrate solution;
(4) crystallizing the supersaturated cerium nitrate solution obtained in the step (3) by using ultrasonic waves under an ice bath condition, wherein the ultrasonic frequency is 32kHz, the ultrasonic power is 350W, aging for 1h, and centrifuging to obtain cerium nitrate crystals;
(5) dissolving the cerium nitrate crystal obtained in the step (4) with deionized water, filtering with a microfilter to obtain a filtrate I, concentrating the filtrate I at 125 ℃ to obtain a supersaturated cerium nitrate solution I, crystallizing the supersaturated cerium nitrate solution I by using ultrasonic waves under ice bath conditions according to the ultrasonic conditions in the step (4), aging for 1h, and centrifuging to obtain the cerium nitrate crystal I;
(6) dissolving the cerium nitrate crystal I obtained in the step (5) with deionized water, filtering with an ultrafilter to obtain a filtrate II, concentrating the filtrate II at 125 ℃ to obtain a supersaturated cerium nitrate solution II, crystallizing the supersaturated cerium nitrate solution II by using ultrasonic waves under ice bath conditions according to the ultrasonic conditions in the step (4), aging for 1h, and centrifuging to obtain high-purity clean cerium nitrate.
Example 2
The preparation of the high-purity clean cerium nitrate according to the process flow for preparing the high-purity clean cerium nitrate shown in fig. 1 specifically comprises the following steps:
(1) adding cerium nitrate into nitric acid until the cerium nitrate is completely dissolved to prepare a cerium nitrate solution, and adjusting the pH value of the cerium nitrate solution to 0.9;
(2) filtering the cerium nitrate solution obtained in the step (1) by using a plate frame to obtain a filtrate, and performing ultrasonic degreasing treatment on the filtrate;
(3) concentrating the filtrate treated in the step (2) at 120 ℃ to obtain a supersaturated cerium nitrate solution;
(4) crystallizing the supersaturated cerium nitrate solution obtained in the step (3) by using ultrasonic waves under an ice bath condition, wherein the ultrasonic frequency is 45kHz, the ultrasonic power is 420W, aging for 0.5h, and centrifuging to obtain cerium nitrate crystals;
(5) dissolving the cerium nitrate crystal obtained in the step (4) with deionized water, filtering with a microfilter to obtain a filtrate I, concentrating the filtrate I at 120 ℃ to obtain a supersaturated cerium nitrate solution I, crystallizing the supersaturated cerium nitrate solution I by using ultrasonic waves under ice bath conditions according to the ultrasonic conditions in the step (4), aging for 0.5h, and centrifuging to obtain a cerium nitrate crystal I;
(6) dissolving the cerium nitrate crystal I obtained in the step (5) with deionized water, filtering with an ultrafilter to obtain a filtrate II, concentrating the filtrate II at 120 ℃ to obtain a supersaturated cerium nitrate solution II, crystallizing the supersaturated cerium nitrate solution II by using ultrasonic waves under ice bath conditions according to the ultrasonic conditions in the step (4), aging for 0.5h, and centrifuging to obtain high-purity clean cerium nitrate.
Example 3
The preparation of the high-purity clean cerium nitrate according to the process flow for preparing the high-purity clean cerium nitrate shown in fig. 1 specifically comprises the following steps:
(1) adding cerium nitrate into nitric acid until the cerium nitrate is completely dissolved to prepare a cerium nitrate solution, and adjusting the pH value of the cerium nitrate solution to 1;
(2) filtering the cerium nitrate solution obtained in the step (1) by using a plate frame to obtain a filtrate, and performing ultrasonic degreasing treatment on the filtrate;
(3) concentrating the filtrate treated in the step (2) at 123 ℃ to obtain a supersaturated cerium nitrate solution;
(4) crystallizing the supersaturated cerium nitrate solution obtained in the step (3) by using ultrasonic waves under an ice bath condition, wherein the ultrasonic frequency is 20kHz, the ultrasonic power is 500W, and then aging for 0.8h and centrifuging to obtain cerium nitrate crystals;
(5) dissolving the cerium nitrate crystal obtained in the step (4) with deionized water, filtering with a microfilter to obtain a filtrate I, concentrating the filtrate I at 123 ℃ to obtain a supersaturated cerium nitrate solution I, crystallizing the supersaturated cerium nitrate solution I by using ultrasonic waves under ice bath conditions according to the ultrasonic conditions in the step (4), aging for 0.8h, and centrifuging to obtain a cerium nitrate crystal 1;
(6) dissolving the cerium nitrate crystal I obtained in the step (5) with deionized water, filtering with an ultrafilter to obtain a filtrate II, concentrating the filtrate II at 123 ℃ to obtain a supersaturated cerium nitrate solution II, crystallizing the supersaturated cerium nitrate solution II by using ultrasonic waves under ice bath conditions according to the ultrasonic conditions in the step (4), aging for 0.8h, and centrifuging to obtain high-purity clean cerium nitrate.
The yield and the content of non-rare earth impurity elements of the high-purity clean cerium nitrate prepared in examples 1 to 3 were measured, and the test results are shown in table 1.
TABLE 1 test results of yield and content of non-rare earth impurity elements of high purity clean cerium nitrate prepared in examples 1 to 3
As can be seen from Table 1, the yield of the cerium nitrate prepared by the method of the present invention is about 85%, and the mass fraction of non-rare earth impurity elements in the finally prepared cerium nitrate is less than 0.5X 10-6.
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (8)
1. A preparation method of high-purity clean cerium nitrate is characterized by comprising the following steps:
(1) adding cerium nitrate into nitric acid until the cerium nitrate is completely dissolved to prepare a cerium nitrate solution, and adjusting the pH value of the cerium nitrate solution to 0.8-1;
(2) filtering the cerium nitrate solution obtained in the step (1) to obtain a filtrate, and performing oil removal treatment on the filtrate;
(3) concentrating the filtrate treated in the step (2) at the temperature of 120-125 ℃ until a supersaturated cerium nitrate solution is obtained;
(4) crystallizing the supersaturated cerium nitrate solution obtained in the step (3) by using ultrasonic waves under an ice bath condition, and centrifuging after aging to obtain cerium nitrate crystals;
(5) and (4) recrystallizing the cerium nitrate crystal obtained in the step (4) and then centrifuging to obtain the high-purity clean cerium nitrate.
2. The method according to claim 1, wherein in the step (2), the degreasing treatment is performed by using ultrasonic waves.
3. The method as claimed in claim 1, wherein in the step (4), when the crystallization is performed by using ultrasonic waves, the ultrasonic frequency is 20-45kHz, and the ultrasonic power is 350-500W.
4. The method according to claim 1, wherein in step (4), the aging time is 0.5 to 1 hour.
5. The method according to claim 1, wherein in step (5), the recrystallization specifically comprises the steps of:
1) dissolving the cerium nitrate crystal obtained in the step (4) with deionized water, filtering with a microfilter to obtain a filtrate I, concentrating the filtrate I at the temperature of 120-125 ℃ to obtain a supersaturated cerium nitrate solution I, crystallizing the supersaturated cerium nitrate solution I by using ultrasonic waves under the ice bath condition, and centrifuging after aging to obtain the cerium nitrate crystal I;
2) dissolving the cerium nitrate crystal I obtained in the step 1) with deionized water, filtering with an ultrafilter to obtain a filtrate II, concentrating the filtrate II at the temperature of 120-125 ℃ to obtain a supersaturated cerium nitrate solution II, crystallizing the supersaturated cerium nitrate solution II under the ice bath condition by using ultrasonic waves, and centrifuging after aging to obtain high-purity clean cerium nitrate.
6. The method as claimed in claim 5, wherein in step 1) and step 2), the ultrasonic frequency is 20-45kHz and the ultrasonic power is 350-500W when the ultrasonic wave is used for crystallization.
7. The method of claim 5, wherein in step 1) and step 2), the aging time is from 0.5 to 1 hour.
8. A high purity clean cerium nitrate prepared by the method of any one of claims 1-7.
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Application publication date: 20200204 |