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

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 technique

Scandium is a lanthanide rare earth element, and its halide is an important raw material for making metal halide lamps, optical fibers, electronic ceramics and laser materials. Among them, scandium trichloride (ScCl ₃ ) is one of the most common and important halides. High-purity anhydrous scandium trichloride is one of the important intermediates in the fine chemical industry, and can be used to prepare scandium metal coordination compounds and other inorganic materials.

Due to the similar properties of rare earth elements, rare earth elements have problems such as separation and purification difficulties, and anhydrous scandium trichloride is relatively active, and it is easy to combine with oxygen, carbon dioxide or water in the air to form scandium oxychloride. It will be further decomposed into scandium oxide under heating conditions. Therefore, it is more difficult to prepare high-purity anhydrous scandium chloride.

The preparation methods of anhydrous scandium chloride reported so far mainly include wet method and dry method. The wet process mainly uses molten salt or hydrochloric acid to increase the solubility of scandium oxide to increase the rate of its chlorination reaction, and then dissolves it into a chlorinated solution and calcines it in an inert atmosphere to generate anhydrous scandium chloride. For example, some researchers used molten salt of NaCl-KCl-NH ₄ Cl and AlCl ₃ to dissolve scandium oxide and then calcined to remove NH ₄ Cl/AlCl ₃ , thus obtaining anhydrous scandium chloride with a purity of up to 98.92%. The process of removing water and impurities in the above-mentioned wet process is relatively complicated and the product is easily hydrolyzed, so it is not easy to obtain high-purity anhydrous scandium chloride.

The dry process is to form anhydrous scandium trichloride crystals by mixing scandium oxide and reducing substances and calcining them in a chlorine-containing atmosphere. This method has strict requirements on raw material pretreatment, air flow and temperature control, which is not conducive to industrial scale-up production. For example, in the traditional technology, pre-purified anhydrous Sc ₂ O ₃ and carbon black are mixed and then calcined at high temperature under a chlorine gas atmosphere.

Contents of the invention

Based on this, it is necessary to provide a preparation method of anhydrous scandium trichloride, which adopts a dry process to avoid the problem that scandium trichloride is easily decomposed when removing water in the wet process, and the method is simple in process and can Improve the purity of anhydrous scandium trichloride.

In addition, it is also necessary to provide an application of anhydrous scandium trichloride.

A preparation method of anhydrous scandium trichloride, comprising the steps of:

Calcining scandium oxide powder in a hydrogen atmosphere to prepare scandium hydride;

Under vacuum conditions, heat and decompose the scandium hydride to prepare scandium powder; and

The scandium powder is reacted with a chlorination reagent to prepare anhydrous scandium trichloride, and the chlorination reagent is selected from any one or both of chlorine gas and hydrogen chloride.

In one of the embodiments, the step of calcining the scandium oxide powder in a hydrogen atmosphere satisfies any one or both of the following conditions:

(1) The calcination temperature is 400°C to 900°C;

(2) Calcination time is 1h～5h.

In one of the embodiments, the step of calcining the scandium oxide powder in a hydrogen atmosphere satisfies any one or both of the following conditions:

(1) The calcination temperature is 650°C to 800°C;

(2) Calcination time is 2h～3h.

In one embodiment, the thermal decomposition temperature is 100°C-800°C.

In one of the embodiments, the step of thermally decomposing the scandium hydride under vacuum condition includes:

Under vacuum conditions, the scandium hydride is heated from 10° C. to 200° C. to 500° C. to 700° C. for thermal decomposition, and the heating rate is 5° C./min to 10° C./min.

In one of the embodiments, before the step of reacting the scandium powder with the chlorinating reagent, it also includes: repeating the steps of calcining the scandium powder in a hydrogen atmosphere, and then heating and decomposing the scandium powder at least once under vacuum conditions .

In one of the embodiments, the chlorination reagent is chlorine gas.

In one of the embodiments, the step of subjecting the scandium powder to the chlorination reaction comprises: igniting the scandium powder and the chlorination reagent, causing the scandium powder to react with the chlorination reagent, After ~3h, heat every 30min until the reaction is complete.

In one embodiment, the D ₅₀ particle size of the scandium oxide powder is 40 μm˜500 μm.

In one of the embodiments, the D ₅₀ particle size of the anhydrous scandium trichloride is 10 μm˜50 μm.

An application of anhydrous scandium trichloride in the preparation of scandium coordination compounds, wherein the anhydrous scandium trichloride is prepared by the above-mentioned preparation method of anhydrous scandium trichloride.

The preparation method of the above-mentioned anhydrous scandium trichloride first reduces scandium oxide by hydrogenation, and then vacuumizes and decomposes to obtain scandium powder. A chlorination reaction avoids the introduction of other impurities in the product preparation process, which leads to the result that the product heteroelement detection exceeds the standard, and greatly improves the purity of the prepared anhydrous scandium trichloride. Moreover, the reaction conditions and equipment of the above method are relatively simple, and the operation steps are simple, which is beneficial to further industrialized production.

Description of drawings

Fig. 1 is a process flow chart of the preparation method of anhydrous scandium trichloride according to one embodiment.

Detailed ways

In order to facilitate the understanding of the present invention, the following will describe the present invention more fully in combination with specific embodiments. Preferred embodiments of the invention are given in the detailed description. However, the present invention can be embodied in many different forms and is not limited to the embodiments described herein. On the contrary, these embodiments are provided to make the understanding of the disclosure of the present invention more thorough and comprehensive.

Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the technical field of the invention. The terminology used herein in the description of the present invention is only for the purpose of describing specific embodiments, and is not intended to limit the present invention.

Unless otherwise stated or there is a conflict, the terms or phrases used in the present invention have the following meanings:

In the description of the present invention, "plurality" means at least two, such as two, three, etc., unless otherwise specifically defined.

In the present invention, "one or several" refers to any one, any two or any two or more of the listed items. Wherein, "several types" refers to any two or more than two.

In the present invention, the technical features described in open form include closed technical solutions consisting of the enumerated features, as well as open technical solutions including the enumerated features.

In the present invention, when referring to a numerical interval, unless otherwise specified, both endpoints of the numerical interval are included.

In the present invention, the percentage concentration involved refers to the final concentration unless otherwise specified. The final concentration refers to the proportion of the added component in the system after the component is added.

The words "preferably", "more preferably" etc. in the present invention refer to embodiments of the invention which may afford certain advantages, under certain circumstances. However, other embodiments may also 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 numerical range is disclosed herein, the said range is considered continuous and includes the minimum and maximum values of the range and every value between such minimum and maximum values. Further, when a range refers to an integer, every integer between the minimum and maximum of the range is included. Furthermore, when multiple ranges are provided to describe a feature or characteristic, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to encompass any and all subranges subsumed therein.

In the present invention, the temperature parameters involved, unless otherwise specified, are allowed to be treated at a constant temperature, and also allowed to be treated within a certain temperature range. The isothermal treatment allows the temperature to fluctuate within the precision of the instrument control. Unless otherwise specified, in this article, room temperature refers to a temperature of 10°C to 30°C.

The terms "comprising" and "having" and any variations thereof in the embodiments of the present invention are intended to cover non-exclusive inclusion. For example, a process, method, system, product or device comprising a series of steps or units is not limited to the listed steps or units, but optionally also includes unlisted steps or units, or optionally further includes For other steps or components inherent in those processes, methods, products, or devices.

Reference in the present invention to an "embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment can be included in at least one embodiment of the present invention. The occurrences of this phrase 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. It is understood explicitly and implicitly by those skilled in the art that the described embodiments of the invention can be combined with other embodiments.

The traditional preparation method of anhydrous scandium trichloride introduces other substances into the reaction system, which leads to high impurity elements in the finished scandium trichloride, low product purity, complex reaction equipment and harsh reaction conditions, which is not conducive to industrial scale-up Production. Anhydrous scandium trichloride is prepared by wet high-temperature calcination of scandium chloride salt. The process of removing water and impurities is relatively complicated and the product is easily hydrolyzed, so it is not easy to obtain high-purity anhydrous scandium chloride. The inventor found in experiments that the key point of preparing high-purity anhydrous scandium trichloride is not only the need to use appropriate technological means to improve the reaction efficiency of the chlorination reaction, but also the need to control the atmosphere in the reaction furnace, using an inert atmosphere or pumping Vacuum, so as to avoid product hydrolysis to generate by-products.

Based on this, the present invention provides a dry preparation process of anhydrous scandium trichloride to solve the problem of insufficient purity of anhydrous scandium trichloride in the traditional dry preparation process, harsh conditions and the presence of scandium trichloride in the wet process. The problem of easy decomposition when removing water.

Specifically, please refer to Fig. 1, the preparation method of anhydrous scandium trichloride of an embodiment, comprises the following steps:

Step S110: calcining scandium oxide powder in a hydrogen atmosphere to prepare scandium hydride.

In the state of saturated hydrogen atmosphere, scandium oxide powder is reduced to metal scandium by hydrogen, and metal scandium and hydrogen further generate hydride. Using hydrogen reduction conditions, on the one hand, without introducing other heteroelements, high-purity metal scandium can be obtained by generating scandium hydrides, followed by vacuum heating and decomposition. On the other hand, the formation of hydrides can further obtain fine and uniform metal powders. Instead of metal particles, you end up with anhydrous scandium trichloride in powder form. Using other reduction conditions, such as C reduction or CO reduction, although metal scandium can be obtained, other impurities are introduced, and the purity of the obtained anhydrous scandium trichloride is low. In addition, the use of C reduction or CO reduction is obtained. Metal particles, the finally obtained scandium trichloride is in the form of granules, which needs to be further processed in the glove box to obtain powdered anhydrous scandium chloride, which increases the difficulty of the process.

In some embodiments, the calcination temperature is 400°C-900°C. In a specific example, the calcination temperature can be but not limited to 400°C, 450°C, 500°C, 550°C, 600°C, 650°C, 680°C, 700°C, 720°C, 750°C, 780°C, 800°C , 850°C, 900°C or any two of these values. Preferably, the calcination temperature is 650°C to 800°C.

In some embodiments, the calcination time is 1 h to 5 h. In a specific example, the calcination time can be but not limited to 1h, 1.5h, 2h, 2.2h, 2.5h, 2.8h, 3h, 3.5h, 4h, 4.5h, 5h or any two of these values composed range. Preferably, the calcination time is 2h-3h.

In some embodiments, the scandium oxide powder has a purity of 90%-99%.

In some embodiments, the D ₅₀ particle size of the scandium oxide powder is 40 μm˜500 μm. In a specific example, the _D50 particle size of the scandium oxide powder is 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. range of composition. Experiments have proved that the method for preparing anhydrous scandium trichloride according to this embodiment does not require complex pretreatment processes for raw materials. Pretreatment has little significance for improving the purity of anhydrous scandium trichloride, and the reaction conditions of the preparation method of anhydrous scandium trichloride in this embodiment are relatively simple, and the operation steps are simple, which is conducive to further industrial production and has the advantages of great practical prospects.

In some embodiments, step S110 includes: calcining scandium oxide powder at 400° C. to 900° C. in a hydrogen atmosphere for 1 h to 5 h to prepare scandium hydride. Further, step S110 includes: calcining the scandium oxide powder at 650°C-800°C in a hydrogen atmosphere for 2h-3h to prepare scandium hydride.

Step S120: Under vacuum conditions, heat and decompose scandium hydride to prepare scandium powder.

In some embodiments, in step S120, the thermal decomposition temperature is 100°C-800°C. In a specific example, the thermal decomposition temperature can be, but not limited to, 100°C, 200°C, 300°C, 400°C, 500°C, 600°C, 700°C, 800°C or a combination of any two of these values scope. Preferably, the thermal decomposition temperature is 200°C to 700°C.

In some of these embodiments, step S120 includes: heating and decomposing scandium hydride from 10°C to 200°C to 500°C to 700°C under vacuum conditions, and the heating rate is 5°C/min to 10°C /min. In a specific example, the heating rate is 5°C/min, 6°C/min, 7°C/min, 8°C/min, 9°C/min, 10°C/min or a combination of any two of these values scope. Preferably, in one of the embodiments, step S120 includes: heating and decomposing the scandium hydride from 200°C to 700°C under a vacuum condition, with a heating rate of 5°C/min.

The method of slowly raising the temperature is more conducive to the decomposition of the hydride into fine powder. Direct heating to a higher temperature and then feeding the hydride may lead to incomplete decomposition and the formation of large particles. In addition, there are hidden dangers in terms of safety.

It can be understood that, in some embodiments, after the calcination in step S110 is completed, when the temperature is lowered to room temperature or to room temperature to 200° C., the resistant hydride is heated and decomposed under vacuum conditions. This method is beneficial to decompose the hydride into fine and uniform powder, and the operation is safer.

In this embodiment, there is no particular limitation on the conditions of vacuuming, as long as the state of vacuuming is maintained continuously.

Step S130: repeating the step of calcining the scandium powder in a hydrogen atmosphere, and then heating and decomposing it under vacuum conditions at least once to prepare purified scandium powder.

In some embodiments, the step of calcining the scandium powder in a hydrogen atmosphere is the same as the step of calcining in step S110 , and will not be repeated here. The step of thermally decomposing under vacuum conditions is the same as the step of thermally decomposing in step S120, and will not be repeated here. It can be understood that in step S130, the temperature and time of calcination may be the same as or different from those in step S110, as long as they are within the range of temperature and time. Similarly, in step S130, the temperature of heating and decomposing under vacuum conditions may be the same as or different from the temperature in step S120, as long as it is within the above range.

Through the above steps, the purity of the prepared scandium powder can be further improved. It can be understood that, in some embodiments, if the requirement for the purity of the scandium powder is not high, step S130 may not be performed.

It can be understood that repeating the steps of calcining the scandium powder in a hydrogen atmosphere and then heating and decomposing it under a vacuum condition at least once means that it is calcined in a hydrogen atmosphere and then heating and decomposing it under a vacuum condition as a cycle. Step S130 performs this loop once, twice, three times, etc. Further, the steps of calcining the scandium powder in a hydrogen atmosphere and then heating and decomposing under vacuum conditions are repeated for two to three times. Step S140: reacting the purified scandium powder with a chlorination reagent to prepare anhydrous scandium trichloride.

In some embodiments, the chlorine reagent is selected from any one or a combination of chlorine gas and hydrogen chloride. Using other chlorination reagents such as carbon tetrachloride and introducing carbon elements, the purity of the prepared scandium trichloride is obviously lower and the particles are larger. Preferably, the chlorinating agent is chlorine gas. Experiments have proved that the purity of the prepared scandium trichloride can be further improved by using chlorine gas for chlorination reaction.

In some embodiments, step S140 includes: igniting the purified scandium powder and the chlorination reagent, and heating every 30 minutes after igniting for 2 hours to 3 hours until the reaction is complete. In the actual process, the color of scandium trichloride is white, and scandium powder is gray, so the end point of the reaction can be judged according to the color change. At the beginning of the reaction, it is necessary to start the ignition device to ignite, and the reaction can proceed spontaneously without heating after the start of the reaction. After reacting for 2 hours to 3 hours, the reactor was heated every 30 minutes to maintain the reaction rate until the scandium powder reacted completely.

In some embodiments, excess chlorine gas from the reaction can be absorbed with an ice-water bath of calcium chloride.

The preparation method of the above-mentioned anhydrous scandium trichloride has at least the following advantages:

(1) The preparation method of the above-mentioned anhydrous scandium trichloride is to reduce scandium oxide by hydrogenation, then decompose in a vacuum to obtain high-purity scandium powder, and then directly chlorinate it, avoiding the introduction of other impurities in the product preparation process and resulting in product The detection of foreign elements exceeding the standard greatly improves the purity of the prepared anhydrous scandium trichloride.

(2) The preparation method of the above-mentioned anhydrous scandium chloride improves the purity and reactivity of the scandium powder by increasing the cycle operation of hydrogenation reduction and then vacuum calcination and decomposition in the production process, thereby improving the efficiency of the follow-up chlorination reaction process and saving The energy consumption required for the reaction is reduced, and the production cost is reduced.

(3) the preparation method of the above-mentioned anhydrous scandium chloride can obtain uniform and fine scandium powder through the cycle steps of reduction-decomposition, thereby ensuring that the anhydrous scandium trichloride generated is also powdery rather than granular, and more conducive to practical application.

(4) The reaction conditions and equipment of the above-mentioned anhydrous scandium chloride preparation method are relatively simple, and the operation steps are simple, which is conducive to further industrial production and has great practical prospects.

The anhydrous scandium trichloride prepared by the method for preparing anhydrous scandium trichloride in the above embodiment has high purity.

In some embodiments, the purity of the anhydrous scandium trichloride is > 96%. Further, the purity of the anhydrous scandium trichloride is ≥98%. The heteroelement contents of the anhydrous scandium trichloride are all less than 20ppm. Further, the purity of the anhydrous scandium trichloride is ≥99%. Furthermore, the purity of the anhydrous scandium trichloride is ≥99.5%.

In some embodiments, the anhydrous scandium trichloride is in powder form. Further, the D ₅₀ particle size of the anhydrous scandium trichloride is 10 μm to 50 μm. In a specific example, the D ₅₀ particle size of anhydrous scandium trichloride is 10 μm, 15 μm, 20 μm, 25 μm, 30 μm, 35 μm, 40 μm, 45 μm, 50 μm or a range consisting of any two of these values. The above-mentioned anhydrous scandium trichloride has high purity and low content of impurity elements. Moreover, the anhydrous scandium trichloride is powdery, which is more conducive to practical application.

The present invention also provides an application of anhydrous scandium trichloride in the preparation of scandium coordination compounds according to one embodiment.

The above-mentioned anhydrous scandium trichloride has high purity and less heteroelement content, and can be used to prepare scandium coordination compounds.

In order to make the purpose and advantages of the present invention clearer, the preparation method and the effect thereof of the anhydrous scandium trichloride of the present invention will be further described in detail below in conjunction with specific examples. It should be understood that the specific examples described here are only used for The present invention is explained, but should not be used to limit the present invention. The following examples do not include other components except unavoidable impurities unless otherwise specified. The drugs and instruments used in the examples are all routine choices in the art unless otherwise specified. The experimental methods for which specific conditions are not indicated in the examples are implemented according to conventional conditions, such as the conditions described in literature, books or the method recommended by the manufacturer.

Example 1

The present embodiment provides a kind of preparation method of anhydrous scandium trichloride, specifically comprises the following steps:

(1) 10 g of scandium oxide powder with a purity of 99% (D ₅₀ particle size of 41.1 microns) was calcined and reduced at 800° C. for 3 hours under hydrogen to generate scandium hydride.

(2) After the reduction is completed and the temperature is lowered to room temperature, the scandium hydride is decomposed at a rate of 5°C/min to 700°C under vacuum conditions to obtain scandium powder.

(3) After the reaction in step (2) is lowered to room temperature, continue to calcinate the scandium powder obtained in the previous step (2) for 3 hours under a hydrogen atmosphere at 800 ° C. Under the conditions, the temperature was raised to 700°C at a rate of 5°C/min and decomposed to obtain purified scandium powder.

(4) After passing dry chlorine gas into the reactor for 10 minutes, ignite to start the chlorination reaction, and anhydrous scandium trichloride begins to form. After reacting for 2 hours, heat the reactor every 30 minutes to maintain the system temperature at 500°C . Continue to react for 10 hours, so that scandium powder is completely chlorinated to generate anhydrous scandium trichloride.

Example 2

This embodiment provides a method for preparing anhydrous scandium trichloride, the specific preparation process is similar to that of Example 1, the difference is that between step (3) and step (4), step (3) is added once , That is, in this embodiment, three cycles of hydrogenation reduction and vacuum calcination have been carried out accumulatively, and other steps are the same as in Embodiment 1.

Example 3

This example provides a method for preparing anhydrous scandium trichloride. The specific preparation process is similar to that of Example 2, the difference is that in step (1), the scandium oxide powder is further ground and pulverized to make the oxidized Scandium powder D ₅₀ particle size is 19.6 microns, other steps are the same as in Example 2.

Example 4

This example provides a method for preparing anhydrous scandium trichloride. The specific preparation process is similar to Example 2, the difference is that in step (1), the hydrogen reduction temperature is 500°C, and other steps are the same as Example 2. .

Example 5

This embodiment provides a preparation method of anhydrous scandium trichloride, the specific preparation process is similar to that of embodiment 2, the difference is that in step (4), the chlorination process uses hydrogen chloride instead of chlorine, and other steps are the same as in embodiment 2 same.

Example 6

This example provides a method for preparing anhydrous scandium trichloride. The specific preparation process is similar to that of Example 2, the difference is that in the vacuum calcination process of step (2), the temperature is raised to 500 ° C, and other steps are the same as those of Example 2. 2 is the same.

Example 7

This embodiment provides a kind of preparation method of anhydrous scandium trichloride, and its specific preparation process is similar to embodiment 2, and difference is: between step (3) and step (4), added step (3) ), that is, four cycles of hydrogenation reduction and vacuum calcination have been carried out in total in this embodiment, and other steps are the same as in embodiment 2.

Example 8

This example provides a method for preparing anhydrous scandium trichloride, and its specific preparation process is similar to that of Example 1, except that step (3) is not performed.

Comparative example 1

Comparative example 1 provides a kind of preparation method of anhydrous scandium trichloride, and specific process is as follows:

Using the method described in the literature Acta Chem Scand, 1994, 48, 294, 10g of scandium oxide and 5g of carbon black were mixed and calcined at 900°C for 5 hours under a chlorine atmosphere to finally obtain large-grained anhydrous scandium trichloride crystals.

Comparative example 2

Comparative example 2 provides a kind of preparation method of anhydrous scandium trichloride, and its specific preparation process is similar to embodiment 1, difference is: the hydrogen reduction condition of step (1) is replaced by CO reduction, and other steps are the same as embodiment 1 .

Comparative example 3

Comparative example 3 provides a kind of preparation method of anhydrous scandium trichloride, and its specific preparation process is similar to embodiment 2, and difference is: in step (4), chlorination process adopts carbon tetrachloride instead of chlorine, and other steps are the same as Example 2 is the same.

The element types, purity, particle size, etc. of the anhydrous scandium trichloride prepared in the above examples and comparative examples were tested, and the experimental data shown in Table 1 below were obtained.

The experimental characterization data of the anhydrous scandium trichloride prepared by each embodiment and comparative example of table 1

It can be seen from the above data that the preparation method of anhydrous scandium trichloride in the above embodiment can obtain anhydrous scandium trichloride with the highest purity>99.5%, and increasing the number of times of hydrogenation reduction and vacuum calcination decomposition can significantly improve the obtained The purity of Scandium Trichloride. Carrying out further grinding pretreatment to scandium oxide powder in embodiment 3 is not very helpful for improving the purity of the prepared scandium trichloride, and the side proves that the anhydrous scandium trichloride with sufficiently high purity can be obtained based on the above-mentioned preparation method, There is no need for further complex pretreatment of the raw material, or the pretreatment has little significance in improving the purity of the product.

In Comparative Example 1, the traditional dry process was adopted, and the prepared scandium trichloride had a relatively low purity and a relatively large particle size. In the subsequent process, pulverization in a glove box was required to obtain powdered 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 the prepared scandium trichloride was significantly lower than that of the examples.

The technical features of the above-mentioned embodiments can be combined arbitrarily. To make the description concise, all possible combinations of the technical features in the above-mentioned embodiments are not described. However, as long as there is no contradiction in the combination of these technical features, should be considered as within the scope of this specification.

The above-mentioned embodiments only express several implementation modes of the present invention, which are convenient for a specific and detailed understanding of the technical solution of the present invention, but should not be construed as limiting the protection scope of the invention patent. It should be noted that those skilled in the art can make several modifications and improvements without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. It should be understood that the technical solutions obtained by those skilled in the art through logical analysis, reasoning or limited experiments on the basis of the technical solutions provided by the present invention are all within the protection scope of the appended claims of the present invention. Therefore, the protection scope of the patent for the present invention shall be determined by the content of the appended claims, and the description and drawings may be used to interpret the content 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; and

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 ℃; and

(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 ℃; and

(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.

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