CN116161692A - Preparation method and application of anhydrous scandium trichloride - Google Patents

Preparation method and application of anhydrous scandium trichloride Download PDF

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CN116161692A
CN116161692A CN202211535425.3A CN202211535425A CN116161692A CN 116161692 A CN116161692 A CN 116161692A CN 202211535425 A CN202211535425 A CN 202211535425A CN 116161692 A CN116161692 A CN 116161692A
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scandium
trichloride
anhydrous
powder
chlorinating agent
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袁庆庆
倪自林
马家豪
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Tongling Xinnoco New Materials Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00—Compounds of rare earth metals
    • C01F17/20—Compounds containing only rare earth metals as the metal element
    • C01F17/253—Halides
    • C01F17/271—Chlorides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00—Compounds of rare earth metals
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    • C—CHEMISTRY; METALLURGY
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Abstract

The invention relates to a preparation method and application of anhydrous scandium trichloride. The preparation method of the anhydrous scandium trichloride comprises the following steps: calcining scandium oxide powder in a hydrogen atmosphere to prepare scandium hydride; under the condition of vacuumizing, heating and decomposing scandium hydride to prepare scandium powder; the scandium powder reacts with a chlorinating agent to prepare anhydrous scandium trichloride, wherein the chlorinating agent is selected from any one or two of chlorine and hydrogen chloride. The preparation method of scandium trichloride adopts a dry process, so that the problem that scandium trichloride is easy to decompose in the wet process during water removal is avoided, and the method is simple in process and can improve the purity of anhydrous scandium trichloride.

Description

Preparation method and application of anhydrous scandium trichloride
Technical Field
The invention relates to the field of chemical synthesis, in particular to a preparation method and application of anhydrous scandium trichloride.
Background
Scandium is a lanthanide rare earth element, and its halide is an important raw material for making metal halide lamps, optical fibers, electronic ceramics, laser materials, and the like. Of these, scandium trichloride (ScCl 3 ) Is one of the most common and important halides. The high-purity anhydrous scandium trichloride is one of important intermediates in the fine chemical industry, and can be used for preparing metal coordination compounds of scandium and other inorganic materials.
Because the rare earth elements have similar properties, the rare earth elements have the problems of difficult separation and purification, and the like, and the anhydrous scandium trichloride has relatively active properties and is easy to combine with oxygen, carbon dioxide or water in the air, and the like, so that scandium oxychloride can be further decomposed into scandium oxide under the heating condition. Therefore, the difficulty of preparing the high-purity anhydrous scandium chloride is high.
The preparation methods of anhydrous scandium chloride reported at present mainly comprise two main types of wet method and dry method. The wet process mainly uses a method of using molten salt or hydrochloric acid and the like to improve the solubility of scandium oxide so as to improve the chlorination reaction rate of scandium oxide, and then the scandium oxide is dissolved into a chlorination solution and then calcined in an inert atmosphere to generate anhydrous scandium chloride. For example, researchers use NaCl-KCl-NH 4 Cl and AlCl 3 Dissolving scandium oxide and calcining to remove NH 4 Cl/AlCl 3 Thus, anhydrous scandium chloride with a purity of 98.92% at the highest was obtained. The wet process has complex water and impurity removing process, and the product is easy to hydrolyze, so that the anhydrous scandium chloride with high purity is not easy to obtain.
The dry process is to mix scandium oxide and a reducing substance and then calcine them in a chlorine-containing atmosphere to produce anhydrous scandium trichloride crystals. The method has harsh pretreatment, airflow and temperature control requirements on raw materials, and is unfavorable for industrial scale-up production. Such as anhydrous Sc which has been previously purified in the conventional art 2 O 3 And mixing with carbon black, and calcining at high temperature under chlorine atmosphere.
Disclosure of Invention
Based on the above, it is necessary to provide a method for preparing anhydrous scandium trichloride, which adopts a dry process to avoid the problem that scandium trichloride is easy to decompose during water removal in a wet process, and has a simple process, so that the purity of the anhydrous scandium trichloride can be improved.
In addition, there is a need to provide an application of anhydrous scandium trichloride.
The preparation method of the anhydrous scandium trichloride comprises the following steps:
calcining scandium oxide powder in a hydrogen atmosphere to prepare scandium hydride;
under the condition of vacuumizing, heating and decomposing the hydride of scandium to prepare scandium powder; a kind of electronic device with high-pressure air-conditioning system
And (3) reacting the scandium powder with a chlorinating agent to prepare anhydrous scandium trichloride, wherein the chlorinating agent is selected from any one or two of chlorine and hydrogen chloride.
In one embodiment, the step of calcining the scandia powder in a hydrogen atmosphere satisfies either or both of the following conditions:
(1) The calcining temperature is 400-900 ℃;
(2) The calcination time is 1-5 h.
In one embodiment, the step of calcining the scandia powder in a hydrogen atmosphere satisfies either or both of the following conditions:
(1) The calcining temperature is 650-800 ℃;
(2) The calcination time is 2-3 h.
In one embodiment, the thermal decomposition temperature is from 100 ℃ to 800 ℃.
In one embodiment, the step of thermally decomposing the hydride of scandium under vacuum comprises:
under the condition of vacuumizing, heating up the hydride of scandium from 10 ℃ to 200 ℃ to 500 ℃ to 700 ℃ for heating up and decomposing, wherein the heating up rate is 5 ℃/min to 10 ℃/min.
In one embodiment, before the step of reacting the scandium powder with a chlorinating agent, further comprising: the scandium powder is repeatedly calcined in the hydrogen atmosphere and then is heated and decomposed at least once under the condition of vacuumizing.
In one embodiment, the chlorinating agent is chlorine gas.
In one embodiment, the step of chlorinating the scandium powder comprises: and igniting the scandium powder and the chlorinating agent, enabling the scandium powder to react with the chlorinating agent, and heating the scandium powder and the chlorinating agent every 30 minutes until the scandium powder and the chlorinating agent react completely after igniting for 2-3 hours.
In one embodiment, D of the scandium oxide powder 50 The grain diameter is 40 mu m to 500μm。
In one embodiment, the anhydrous scandium trichloride, D 50 The grain diameter is 10 μm to 50 μm.
The application of anhydrous scandium trichloride in preparing scandium complex compound is provided, wherein the anhydrous scandium trichloride is prepared by the preparation method of the anhydrous scandium trichloride.
According to the preparation method of the anhydrous scandium trichloride, scandium oxide is reduced through hydrogenation, then vacuum decomposition is carried out, scandium powder is obtained, the purity and the reactivity of the scandium powder are improved through the reaction, and then the scandium powder and at least one of chlorine and hydrogen chloride are subjected to chlorination reaction, so that the phenomenon that the impurity element detection of the product exceeds standard due to the fact that other impurities are introduced in the preparation process of the product is avoided, and the purity of the prepared anhydrous scandium trichloride is greatly improved. The method has relatively simple reaction conditions and equipment, simple operation steps and contribution to further industrial production.
Drawings
Fig. 1 is a process flow diagram of a method for producing anhydrous scandium trichloride according to an embodiment.
Detailed Description
In order that the invention may be readily understood, a more complete description of the invention will be rendered by reference to specific embodiments that are now described. Preferred embodiments of the invention are given in the detailed description. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Unless otherwise indicated or contradicted, terms or phrases used in the present invention have the following meanings:
in the description of the present invention, the meaning of "plurality" means at least two, for example, two, three, etc., unless specifically defined otherwise.
In the present invention, "one or more" means any one, any two or more of the listed items. Wherein "several" means any two or more.
In the invention, the technical characteristics described in an open mode comprise a closed technical scheme composed of the listed characteristics and also comprise an open technical scheme comprising the listed characteristics.
In the present invention, the numerical range is referred to, and both ends of the numerical range are included unless otherwise specified.
In the present invention, the percentage concentrations referred to refer to the final concentrations unless otherwise specified. The final concentration refers to the ratio of the additive component in the system after the component is added.
The words "preferably," "more preferably," and the like in the present invention refer to embodiments of the invention that may provide certain benefits in some instances. However, other embodiments may be preferred under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
When a range of values is disclosed in the present invention, the range is considered to be continuous and includes the minimum and maximum values of the range, as well as each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range description features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to include any and all subranges subsumed therein.
In the present invention, the temperature parameter is not particularly limited, and it is allowed to be constant temperature treatment or to be treatment within a predetermined temperature range. The constant temperature process allows the temperature to fluctuate within the accuracy of the instrument control. Unless otherwise indicated, room temperature herein means a temperature of 10℃to 30 ℃.
The terms "comprising" and "having" and any variations thereof in embodiments of the present invention are intended to cover a non-exclusive inclusion. For example, a process, method, system, article, or apparatus that comprises a list of steps or elements is not limited to only those listed steps or elements but may alternatively include other steps or elements not listed or inherent to such process, method, article, or apparatus.
Reference in the specification to "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment may be included in at least one embodiment of the invention. The appearances of such phrases in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. Those of skill in the art will explicitly and implicitly appreciate that the described embodiments of the invention may be combined with other embodiments.
The traditional preparation method of anhydrous scandium trichloride introduces other substances into a reaction system, so that the impurity elements of the finished scandium trichloride are higher, the product purity is low, a reaction device is complex, the reaction conditions are harsh, and the industrial large-scale production is not facilitated. The anhydrous scandium trichloride is prepared by adopting a process of calcining scandium chloride salt at a high temperature by a wet method, the water and impurity removal processes are complex, the product is easy to hydrolyze, and the high-purity anhydrous scandium chloride is not easy to obtain. The inventor finds in experiments that the key point of preparing the high-purity anhydrous scandium trichloride is that not only is that a proper process means is needed to improve the reaction efficiency of the chlorination reaction, but also the atmosphere in the reaction furnace is needed to be controlled, and inert atmosphere or vacuum is used, so that byproducts are avoided from being generated by hydrolysis of the product.
Based on the above, the invention provides a dry preparation process of anhydrous scandium trichloride, which aims to solve the problems that the purity of the anhydrous scandium trichloride in the traditional dry preparation process is insufficient, the conditions are harsh, and scandium trichloride is easy to decompose in the wet process during water removal.
Specifically, referring to fig. 1, a method for preparing anhydrous scandium trichloride according to an embodiment includes the following steps:
step S110: calcining scandium oxide powder in a hydrogen atmosphere to prepare scandium hydride.
Under the condition of saturated hydrogen atmosphere, scandium oxide powder is reduced into scandium metal by hydrogen, and the scandium metal and the hydrogen further generate hydride. By adopting hydrogen reduction conditions, on one hand, other hetero elements are not introduced, high-purity metal scandium is obtained through generating scandium hydride and then through vacuumizing, heating and decomposing, and on the other hand, fine and uniform metal powder, rather than metal particles, can be further obtained through generating the hydride, and finally, powdery anhydrous scandium trichloride is obtained. Other reduction conditions, such as C reduction or CO reduction, are adopted, and although metal scandium can be obtained, other impurities are introduced, so that the purity of the obtained anhydrous scandium trichloride is lower, in addition, the obtained anhydrous scandium trichloride is in a granular form by adopting C reduction or CO reduction, and the obtained anhydrous scandium trichloride is in a powdery form and needs to be further processed in a glove box, so that the process difficulty is increased.
In some embodiments, the temperature of calcination is 400 ℃ to 900 ℃. In a specific example, the calcination temperature may be, but is not limited to, 400 ℃, 450 ℃, 500 ℃, 550 ℃, 600 ℃, 650 ℃, 680 ℃, 700 ℃, 720 ℃, 750 ℃, 780 ℃, 800 ℃, 850 ℃, 900 ℃ or a range consisting of any two of these values. Preferably, the calcination temperature is 650-800 ℃.
In some embodiments, the calcination time is from 1h to 5h. In a specific example, the time of calcination may be, but is not limited to, 1h, 1.5h, 2h, 2.2h, 2.5h, 2.8h, 3h, 3.5h, 4h, 4.5h, 5h, or a range consisting of any two of these values. Preferably, the calcination time is 2 to 3 hours.
In some embodiments, the scandium oxide powder has a purity of 90% to 99%.
In some embodiments, the scandium oxide powder D 50 The grain diameter is 40-500 μm. In a specific example, the scandium oxide powder D 50 The particle diameters are 40 μm, 50 μm, 80 μm, 100 μm, 120 μm, 150 μm, 200 μm,250 μm, 300 μm, 350 μm, 400 μm, 450 μm, 500 μm or any two of these values. Experiments prove that the preparation method of the anhydrous scandium trichloride in the embodiment does not need to carry out a complex pretreatment process on raw materials. The pretreatment has little significance for improving the purity of the anhydrous scandium trichloride, and the reaction condition of the preparation method of the anhydrous scandium trichloride in the embodiment is relatively simple, the operation steps are simple, the further industrial production is facilitated, and the method has great practical prospect.
In some embodiments, step S110 includes: calcining scandium oxide powder at 400-900 ℃ in hydrogen atmosphere for 1-5 h to prepare scandium hydride. Further, step S110 includes: calcining scandium oxide powder at 650-800 ℃ in hydrogen atmosphere for 2-3 h to prepare scandium hydride.
Step S120: under the condition of vacuumizing, heating and decomposing scandium hydride to prepare scandium powder.
In some embodiments, in step S120, the temperature of thermal decomposition is 100 ℃ to 800 ℃. In a specific example, the temperature of the thermal decomposition may be, but is not limited to, 100 ℃, 200 ℃, 300 ℃, 400 ℃, 500 ℃, 600 ℃, 700 ℃, 800 ℃, or a range consisting of any two of these values. Preferably, the temperature of thermal decomposition is 200℃to 700 ℃.
In some of these embodiments, step S120 includes: under the condition of vacuumizing, the hydride of scandium is heated from 10 ℃ to 200 ℃ to 500 ℃ to 700 ℃ for heating decomposition, and the heating rate is 5 ℃/min to 10 ℃/min. In a specific example, the heating rate is 5 ℃/min, 6 ℃/min, 7 ℃/min, 8 ℃/min, 9 ℃/min, 10 ℃/min, or a range comprised of any two of these values. Preferably, in one of the embodiments, step S120 includes: under the condition of vacuumizing, the hydride of scandium is heated from 200 ℃ to 700 ℃ for thermal decomposition, and the heating rate is 5 ℃/min.
The slow heating mode is more conducive to decomposing the hydride into fine powder, and the hydride is directly heated to a higher temperature and then introduced, so that large particles are generated due to incomplete decomposition, and the hidden danger in safety is caused.
It will be appreciated that in some embodiments, after the calcination of step S110 is completed, the temperature is reduced to room temperature or to room temperature to 200 ℃, and then the anti-hydride is decomposed by heating under the condition of vacuum. In this way, the hydride is decomposed into fine and uniform powder, and the operation is safer.
In the present embodiment, the conditions for evacuation are not particularly limited, and the evacuation may be maintained continuously.
Step S130: calcining scandium powder in hydrogen atmosphere repeatedly, and then heating and decomposing at least once under the condition of vacuumizing to prepare purified scandium powder.
In some embodiments, the step of calcining scandium powder in the hydrogen atmosphere is the same as the step of calcining in step S110, and will not be described again. The step of thermal decomposition under the vacuuming condition is the same as the step of thermal decomposition in step S120, and will not be described again. It will be appreciated that in step S130, the temperature and time of calcination may be the same as or different from the temperature and time in step S110, and only need be within the temperature and time ranges. Similarly, in step S130, the temperature for thermal decomposition under the vacuum condition may be the same as or different from the temperature in step S120, and may be within the above range.
The purity of the scandium powder can be further improved through the steps. It will be appreciated that in some embodiments, step S130 may not be performed if the purity requirements for the scandium powder are not high.
It is understood that the step of repeating calcination in a hydrogen atmosphere and then thermal decomposition under vacuum conditions at least once means to calcine in a hydrogen atmosphere and then thermal decomposition under vacuum conditions into one cycle, which is performed once, twice, three times, etc. in step S130. Further, the scandium powder is repeatedly calcined in the hydrogen atmosphere, and then is heated and decomposed twice to three times under the condition of vacuumizing. Step S140: and (3) reacting the purified scandium powder with a chlorinating agent to prepare anhydrous scandium trichloride.
In some embodiments, the chlorine reagent is selected from any one or a combination of several of chlorine and hydrogen chloride. Other chlorinating agents such as carbon tetrachloride are adopted, carbon elements are introduced, and the prepared scandium trichloride has obviously lower purity and larger particles. Preferably, the chlorinating agent is chlorine gas. Experiments prove that the purity of the prepared scandium trichloride can be further improved by adopting chlorine to carry out chlorination reaction.
In some embodiments, step S140 includes: igniting the purified scandium powder and a chlorinating agent, and heating the scandium powder for 2 to 3 hours at intervals of 30 minutes until the reaction is complete. In the actual process, scandium trichloride is white in color and scandium powder is gray, so that the end point of the reaction can be judged according to the color change. The ignition device needs to be started to ignite at the beginning of the reaction, and the reaction can be spontaneously performed without heating after the beginning of the reaction. After 2 to 3 hours of reaction, the reactor was heated every 30 minutes to maintain the reaction rate until the scandium powder was completely reacted.
In some embodiments, the excess chlorine gas from the reaction may be absorbed with an ice water bath of calcium chloride.
The preparation method of the anhydrous scandium trichloride has at least the following advantages:
(1) According to the preparation method of the anhydrous scandium trichloride, the scandium oxide is reduced through hydrogenation, then the high-purity scandium powder is obtained through vacuumizing and decomposing, and then the impurity element detection exceeding result of the product due to the fact that other impurities are introduced in the preparation process of the product is avoided through the direct chlorination mode, so that the purity of the prepared anhydrous scandium trichloride is greatly improved.
(2) According to the preparation method of anhydrous scandium chloride, the purity and the reactivity of scandium powder are improved through the cyclic operation of adding hydrogenation reduction and then vacuum calcination decomposition in the preparation process, so that the efficiency of a subsequent chlorination reaction process is improved, the energy consumption required by the reaction is saved, and the production cost is reduced.
(3) According to the preparation method of anhydrous scandium chloride, uniform and fine scandium powder can be obtained through the reduction-decomposition circulating steps, so that the generated anhydrous scandium chloride is also in a powdery state rather than in a granular state, and the actual application is facilitated.
(4) The reaction condition and equipment of the preparation method of anhydrous scandium chloride are relatively simple, the operation steps are simple, the further industrial production is facilitated, and the preparation method has great practical prospect.
The purity of the anhydrous scandium trichloride prepared by the method for preparing anhydrous scandium trichloride according to the above embodiment is high.
In some embodiments, the purity of the anhydrous scandium trichloride is greater than or equal to 96%. Further, the purity of the anhydrous scandium trichloride is more than or equal to 98 percent. The impurity element content of the anhydrous scandium trichloride is less than 20ppm. Further, the purity of the anhydrous scandium trichloride is more than or equal to 99 percent. Furthermore, the purity of the anhydrous scandium trichloride is more than or equal to 99.5 percent.
In some embodiments, the anhydrous scandium trichloride is in powder form. Further, anhydrous scandium trichloride D 50 The grain diameter is 10 μm to 50 μm. In a specific example, anhydrous scandium trichloride D 50 Particle diameters of 10 μm, 15 μm, 20 μm, 25 μm, 30 μm, 35 μm, 40 μm, 45 μm, 50 μm or any two of these values. The anhydrous scandium trichloride has high purity and low content of impurity elements. And the anhydrous scandium trichloride is in powder form, which is more beneficial to practical application.
The invention also provides an application of the anhydrous scandium trichloride in preparing the scandium coordination compound.
The anhydrous scandium trichloride has high purity and low content of hetero elements, and can be used for preparing the coordination compound of scandium.
In order to make the objects and advantages of the present invention more apparent, the following more detailed description of the method for preparing anhydrous scandium trichloride and the effects thereof will be given in connection with the specific examples, which are to be construed as merely illustrative and not limitative of the present invention. The following examples, unless otherwise specified, do not include other components than the unavoidable impurities. The drugs and apparatus used in the examples are all routine choices in the art, unless specifically indicated. The experimental methods without specific conditions noted in the examples were carried out according to conventional conditions, such as those described in the literature, books, or recommended by the manufacturer.
Example 1
The embodiment provides a preparation method of anhydrous scandium trichloride, which specifically comprises the following steps:
(1) 10g of scandium oxide powder (D) 50 Particle size of 41.1 μm) was calcined and reduced at 800 c under hydrogen for 3 hours to produce scandium hydride.
(2) And after the reduction is finished and the temperature is reduced to room temperature, heating up scandium hydride to 700 ℃ at a speed of 5 ℃/min under the condition of vacuumizing, and decomposing to obtain scandium powder.
(3) And (3) continuously calcining scandium powder obtained in the previous step (2) for 3 hours in a hydrogen atmosphere at 800 ℃ after the reaction in the step (2) is cooled to room temperature, and after the reduction is finished and cooled to room temperature, heating up scandium hydride to 700 ℃ at a speed of 5 ℃/min under the condition of maintaining vacuum pumping to decompose scandium powder after purification.
(4) After the reactor was charged with dry chlorine gas for 10 minutes, the chlorination reaction was started by ignition, anhydrous scandium trichloride was started to be produced, and after 2 hours of reaction, the reactor was heated at intervals of 30 minutes to maintain the system temperature at 500 ℃. The reaction was continued for 10 hours, and the scandium powder was totally chlorinated to produce anhydrous scandium trichloride.
Example 2
The present example provides a method for preparing anhydrous scandium trichloride, which is similar to example 1 in specific preparation process, except that: between the step (3) and the step (4), a step (3) was added, that is, the cycle of hydrogenation reduction and vacuum calcination was performed three times in this example, and the other steps were the same as in example 1.
Example 3
The present example provides a method for preparing anhydrous scandium trichloride, which has a specific preparation process similar to that of example 2, except that: in the step (1), scandium oxide powder D is obtained by subjecting scandium oxide powder to further grinding and pulverizing treatment 50 The particle size was 19.6 microns, and the other steps were the same as in example 2.
Example 4
The present example provides a method for preparing anhydrous scandium trichloride, which has a specific preparation process similar to that of example 2, except that: in the step (1), the hydrogen reduction temperature was 500℃and the other steps were the same as in example 2.
Example 5
The present example provides a method for preparing anhydrous scandium trichloride, which has a specific preparation process similar to that of example 2, except that: in the step (4), the chlorination process uses hydrogen chloride instead of chlorine, and the other steps are the same as in example 2.
Example 6
The present example provides a method for preparing anhydrous scandium trichloride, which has a specific preparation process similar to that of example 2, except that: in the vacuum calcination process of step (2), the temperature was raised to 500℃and the other steps were the same as in example 2.
Example 7
The present example provides a method for preparing anhydrous scandium trichloride, which has a specific preparation process similar to that of example 2, except that: in this example, the cycle of hydrogenation reduction and vacuum calcination was performed four times in a lump, and the other steps were the same as in example 2, except that step (3) was added between step (3) and step (4).
Example 8
The present example provides a method for preparing anhydrous scandium trichloride, which is similar to example 1 in specific preparation process, except that: step (3) is not performed.
Comparative example 1
Comparative example 1 provides a method for preparing anhydrous scandium trichloride, which comprises the following specific procedures:
10g of scandium oxide and 5g of carbon black were mixed and calcined for 5 hours at 900℃under a chlorine atmosphere using the method described in the literature Acta Chem Scand,1994,48,294, to finally obtain large-particle anhydrous scandium trichloride crystals.
Comparative example 2
Comparative example 2 provides a process for the preparation of anhydrous scandium trichloride, the specific preparation being similar to example 1, with the difference that: the hydrogen reduction conditions of step (1) were replaced with CO reduction, and the other steps were the same as in example 1.
Comparative example 3
Comparative example 3 provides a process for the preparation of anhydrous scandium trichloride, the specific preparation being similar to example 2, except that: in the step (4), the chlorination process uses carbon tetrachloride instead of chlorine, and the other steps are the same as in example 2.
The anhydrous scandium trichloride prepared in the above examples and comparative examples was tested for the kind of element, purity, particle diameter and the like, and experimental data shown in table 1 below were obtained.
Table 1 experimental characterization data for anhydrous scandium trichloride prepared in each of the examples and comparative examples
Figure BDA0003977433360000111
From the above data, it can be seen that the anhydrous scandium trichloride preparation method in the above embodiment can obtain anhydrous scandium trichloride with the highest purity of >99.5%, and the increase of the times of hydrogenation reduction and vacuum calcination decomposition can significantly improve the purity of the prepared scandium trichloride. Further grinding pretreatment of scandium oxide powder in example 3 did not help much to improve the purity of scandium trichloride produced, and it was demonstrated on the side that anhydrous scandium trichloride of sufficiently high purity could be produced according to the production method described above, without further complicated pretreatment of the raw materials, or that pretreatment did not make great significance in improving the purity of the product.
In comparative example 1, the prepared scandium trichloride has lower purity and larger granularity by adopting a traditional dry process, and the scandium trichloride is required to be crushed in a glove box in the subsequent process to obtain powdery scandium trichloride. In comparative example 2, carbon monoxide reduction was used instead of hydrogen reduction, and the other steps were the same, and the purity of scandium trichloride prepared was significantly lower than in the examples.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples merely represent a few embodiments of the present invention, which facilitate a specific and detailed understanding of the technical solutions of the present invention, but are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. It should be understood that, based on the technical solutions provided by the present invention, those skilled in the art can obtain technical solutions through logical analysis, reasoning or limited experiments, which are all within the protection scope of the appended claims. The scope of the patent is therefore intended to be covered by the appended claims, and the description and drawings may be interpreted as illustrative of the contents of the claims.

Claims (10)

1. The preparation method of the anhydrous scandium trichloride is characterized by comprising the following steps:
calcining scandium oxide powder in a hydrogen atmosphere to prepare scandium hydride;
under the condition of vacuumizing, heating and decomposing the hydride of scandium to prepare scandium powder; a kind of electronic device with high-pressure air-conditioning system
And (3) reacting the scandium powder with a chlorinating agent to prepare anhydrous scandium trichloride, wherein the chlorinating agent is selected from any one or two of chlorine and hydrogen chloride.
2. The method for producing anhydrous scandium trichloride according to claim 1, wherein the step of calcining the scandium oxide powder in a hydrogen atmosphere satisfies either or both of the following conditions:
(1) The calcining temperature is 400-900 ℃; a kind of electronic device with high-pressure air-conditioning system
(2) The calcination time is 1-5 h.
3. The method for producing anhydrous scandium trichloride according to claim 2, wherein the step of calcining the scandium oxide powder in a hydrogen atmosphere satisfies either or both of the following conditions:
(1) The calcining temperature is 650-800 ℃; a kind of electronic device with high-pressure air-conditioning system
(2) The calcination time is 2-3 h.
4. The method for producing anhydrous scandium trichloride according to claim 1, wherein the thermal decomposition temperature is 100 ℃ to 800 ℃.
5. The method for producing anhydrous scandium trichloride according to claim 4, wherein the step of decomposing the hydride of scandium by heating under vacuum conditions comprises:
under the condition of vacuumizing, heating up the hydride of scandium from 10 ℃ to 200 ℃ to 500 ℃ to 700 ℃ for heating up and decomposing, wherein the heating up rate is 5 ℃/min to 10 ℃/min.
6. The method for producing anhydrous scandium trichloride according to any one of claims 1 to 5, further comprising, before the step of reacting the scandium powder with a chlorinating agent: the scandium powder is repeatedly calcined in the hydrogen atmosphere and then is heated and decomposed at least once under the condition of vacuumizing.
7. The method for producing anhydrous scandium trichloride according to any one of claims 1 to 5, wherein the step of subjecting the scandium powder to a chlorination reaction comprises: and igniting the scandium powder and the chlorinating agent, enabling the scandium powder to react with the chlorinating agent, and heating the scandium powder and the chlorinating agent every 30 minutes until the scandium powder and the chlorinating agent react completely after igniting for 2-3 hours.
8. The method for producing anhydrous scandium trichloride according to any one of claims 1 to 5, wherein D of the scandium oxide powder 50 The grain diameter is 40-500 μm.
9. The method for producing anhydrous scandium trichloride according to claim 8, wherein the anhydrous scandium trichloride has D 50 The grain diameter is 10 μm to 50 μm.
10. Use of anhydrous scandium trichloride in the preparation of a complex compound of scandium, characterized in that the anhydrous scandium trichloride is produced by the method for producing anhydrous scandium trichloride according to any of claims 1 to 9.
CN202211535425.3A 2022-12-02 2022-12-02 Preparation method and application of anhydrous scandium trichloride Pending CN116161692A (en)

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