Method for preparing vanadium trioxide from M (V3 (OH) 6 (SO4) 2)

Abstract

The invention discloses a method for preparing vanadium trioxide from M (V3 (OH) 6 (SO4) 2), which comprises the following steps of: adding water into MV3 (SO4) 2 (OH) 6 (M = Na, K) serving as a raw material to prepare slurry, regulating the pH value of the solution to 10-13 by using a sodium hydroxide solution, heating in an inert atmosphere, carrying out alum breaking reaction, carrying out solid-liquid separation, washing and drying to obtain vanadium trioxide solid. According to the method, the low-added-value M (V3 (OH) 6 (SO4) 2) is used as the raw material, the high-added-value vanadium trioxide product is produced through the simple reaction under the alkaline inert atmosphere condition, and the method has the advantages of being simple in process, easy to operate, low in cost, high in efficiency, high in product purity and the like.

Description

Technical Field

[0001] The invention belongs to the technical field of chemical material synthesis, and in particular relates to a method for preparing vanadium trioxide by using M(V3(OH)6(SO4)2). Background Art

[0002] Na(V3(OH)6(SO4)2) is a substance with unique physical properties, but it is rarely used in the prior art, resulting in low added value. There are few studies on the preparation of Na(V3(OH)6(SO4)2). Chinese patent document CN 113336266A discloses a method for preparing Na(V3(OH)6(SO4)2) material using vanadyl sulfate solution. The invention proposes that vanadyl sulfate solution can be prepared into Na(V3(OH)6(SO4)2) material through a simple acidic pressure reaction, thereby simplifying the preparation process of the material. However, how to expand the application scope of M(V3(OH)6(SO4)2) and use it to prepare high value-added vanadium products is of great significance. Summary of the invention

[0003] In order to overcome the problems in the prior art, the present invention provides a method for preparing vanadium trioxide using M(V3(OH)6(SO4)2), which uses M(V3(OH)6(SO4)2) to prepare high value-added vanadium trioxide, and the process is simple and easy to operate, with low cost, high efficiency and high product purity.

[0004] In order to solve the above technical problems, the technical solution proposed by the present invention is:

[0005] The present invention provides a method for preparing vanadium trioxide by using M(V3(OH)6(SO4)2), comprising the following steps:

[0006] S1. Add water to M(V3(OH)6(SO4)2) to prepare a slurry, and adjust the pH value of the solution to 10-13;

[0007] S2, heating under an inert atmosphere to cause the slurry to undergo a vanadium-breaking reaction;

[0008] S3. After the reaction is completed, solid-liquid separation, washing and drying are performed to obtain vanadium trioxide solid.

[0009] In the present invention, M(V3(OH)6(SO4)2) is firstly added with water to prepare a slurry, and the pH is adjusted to 10-13, which is conducive to the occurrence of the vanadium-breaking reaction and to maintaining the stability of the generated vanadium trioxide. At the same time, the vanadium-breaking reaction is carried out by heating. The reaction equation is as follows: 2M(V3(OH)6(SO4)2)+6OH - =3V2O3+M2SO4+3SO4 2-+9H2O (M=Na,K), after the reaction is completed, solid vanadium trioxide is obtained.

[0010] Furthermore, preferably, in step S1, the pH value of the solution is adjusted to 11-12.

[0011] As an optional embodiment, in the method provided by the present invention, the MV3(SO4)2(OH)6 is selected from one or both of NaV3(SO4)2(OH)6 or KV3(SO4)2(OH)6.

[0012] As an optional embodiment, in the method provided by the present invention, in step S1, the mass concentration of the slurry is 5 to 45 wt.%.

[0013] As an optional embodiment, in the method provided by the present invention, in step S2, the inert atmosphere is nitrogen or argon.

[0014] As an optional embodiment, in the method provided by the present invention, in step S2, the temperature of the alum breaking reaction is 80-95° C., and the reaction time is 2-5 hours.

[0015] In the present invention, the temperature of the vanadium-breaking reaction is controlled at 80-95° C., which is conducive to providing an optimal reaction speed. If the temperature is too low, the reaction is difficult to occur and the reaction rate is slow. If the temperature is too high, the solution is easy to evaporate, the energy consumption increases, and no more beneficial effects are produced.

[0016] Furthermore, preferably, the temperature of the alum breaking reaction is 90-95°C.

[0017] As an optional embodiment, in the method provided by the present invention, in step S2, the stirring speed of the alum breaking reaction is 400-600 rpm.

[0018] As an optional embodiment, in the method provided by the present invention, in step S1, a sodium hydroxide solution with a concentration of 0.1 to 10 mol / L is used to adjust the pH.

[0019] Compared with the prior art, the present invention has the following beneficial effects:

[0020] The present invention uses low-value-added M (V3 (OH) 6 (SO4) 2) as raw material, and produces high-value-added vanadium trioxide products through a simple alum-breaking reaction under alkaline inert atmosphere conditions. The present invention has the advantages of simple process, easy operation, low cost, high efficiency, and high product purity. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0022] Figure 1 is a process flow chart of the present invention;

[0023] Figure 2 This is the XRD pattern of vanadium trioxide prepared in the embodiment of the present invention. DETAILED DESCRIPTION

[0024] In order to facilitate the understanding of the present invention, the present invention will be described more comprehensively and meticulously below in conjunction with the accompanying drawings and preferred embodiments of the present invention, but the protection scope of the present invention is not limited to the following specific embodiments.

[0025] Unless otherwise defined, all professional terms used below have the same meanings as those generally understood by those skilled in the art. The professional terms used herein are only for the purpose of describing specific embodiments and are not intended to limit the scope of protection of the present invention.

[0026] Unless otherwise specified, various raw materials, reagents, instruments and equipment used in the present invention can be purchased from the market or prepared by existing methods.

[0027] Example 1

[0028] A method for preparing vanadium trioxide using M(V3(OH)6(SO4)2), the process flow is as follows Figure 1 As shown, the following steps are included:

[0029] Take Na(V3(OH)6(SO4)2) as raw material, add water to prepare slurry with mass concentration of 25wt.%, use 2mol / L sodium hydroxide solution to adjust the solution pH value to 10, under nitrogen atmosphere, control the reaction temperature to 80℃, stirring speed to 500rpm, reaction time to 3h, after the reaction, separate the solid and liquid, wash and dry to obtain vanadium trioxide solid.

[0030] Test results: vanadium recovery rate is 95.35%, and vanadium trioxide purity is 97.03%.

[0031] Example 2

[0032] A method for preparing vanadium trioxide using M(V3(OH)6(SO4)2), the process flow is as follows Figure 1 As shown, the following steps are included:

[0033] Na(V3(OH)6(SO4)2) was used as the raw material, water was added to prepare a slurry with a mass concentration of 25wt.%, and the pH value of the solution was adjusted to 11 with 2mol / L sodium hydroxide solution. Under nitrogen atmosphere, the reaction temperature was controlled to 80°C, the stirring speed was 500rpm, and the reaction time was 3h. After the reaction was completed, the solid-liquid separation, washing and drying were carried out to obtain vanadium trioxide solid.

[0034] Test results: vanadium recovery rate is 97.27%, and vanadium trioxide purity is 98.15%.

[0035] Example 3

[0036] A method for preparing vanadium trioxide using M(V3(OH)6(SO4)2), the process flow is as follows Figure 1 As shown, the following steps are included:

[0037] Na(V3(OH)6(SO4)2) is used as raw material, water is added to prepare a slurry with a mass concentration of 25wt.%, and the pH value of the solution is adjusted to 12 with 2mol / L sodium hydroxide solution. Under nitrogen atmosphere, the reaction temperature is controlled to 80°C, the stirring speed is 500rpm, and the reaction time is 3h. After the reaction is completed, the solid-liquid separation, washing and drying are carried out to obtain vanadium trioxide solid.

[0038] Test results: vanadium recovery rate is 98.24%, and vanadium trioxide purity is 99.28%.

[0039] Example 4

[0040] A method for preparing vanadium trioxide using M(V3(OH)6(SO4)2), the process flow is as follows Figure 1 As shown, the following steps are included:

[0041] Na(V3(OH)6(SO4)2) was used as the raw material, water was added to prepare a slurry with a mass concentration of 25wt.%, and the pH value of the solution was adjusted to 13 with 2mol / L sodium hydroxide solution. Under nitrogen atmosphere, the reaction temperature was controlled to 80°C, the stirring speed was 500rpm, and the reaction time was 3h. After the reaction was completed, the solid-liquid separation, washing and drying were carried out to obtain vanadium trioxide solid.

[0042] Test results: vanadium recovery rate is 97.39%, and vanadium trioxide purity is 97.56%.

[0043] Example 5

[0044] A method for preparing vanadium trioxide using M(V3(OH)6(SO4)2), the process flow is as follows Figure 1 As shown, the following steps are included:

[0045] Na(V3(OH)6(SO4)2) is used as raw material, water is added to prepare a slurry with a mass concentration of 25wt.%, and the pH value of the solution is adjusted to 12 with 2mol / L sodium hydroxide solution. Under nitrogen atmosphere, the reaction temperature is controlled to 90°C, the stirring speed is 500rpm, and the reaction time is 3h. After the reaction is completed, the solid-liquid separation, washing and drying are carried out to obtain vanadium trioxide solid.

[0046] Test results: vanadium recovery rate is 98.78%, and vanadium trioxide purity is 99.37%.

[0047] Example 6

[0048] A method for preparing vanadium trioxide using M(V3(OH)6(SO4)2), the process flow is as follows Figure 1 As shown, the following steps are included:

[0049] Take Na(V3(OH)6(SO4)2) as raw material, add water to prepare a slurry with a mass concentration of 25wt.%, use 2mol / L sodium hydroxide solution to adjust the solution pH to 12, under nitrogen atmosphere, control the reaction temperature to 95°C, the stirring speed to 500rpm, and the reaction time to 3h. After the reaction, separate the solid and liquid, wash and dry to obtain vanadium trioxide solid.

[0050] Test results: vanadium recovery rate is 99.04%, and vanadium trioxide purity is 99.24%.

[0051] Example 7

[0052] A method for preparing vanadium trioxide using M(V3(OH)6(SO4)2), the process flow is as follows Figure 1 As shown, the following steps are included:

[0053] Take Na(V3(OH)6(SO4)2) as raw material, add water to prepare slurry with mass concentration of 40wt.%, use 2mol / L sodium hydroxide solution to adjust the solution pH to 12, under nitrogen atmosphere, control the reaction temperature to 95℃, stirring speed to 500rpm, reaction time to 3h, after the reaction, separate the solid and liquid, wash and dry to obtain vanadium trioxide solid.

[0054] Test results: vanadium recovery rate is 99.07%, and vanadium trioxide purity is 99.19%.

[0055] Example 8

[0056] A method for preparing vanadium trioxide using M(V3(OH)6(SO4)2), the process flow is as follows Figure 1 As shown, the following steps are included:

[0057] Take Na(V3(OH)6(SO4)2) as raw material, add water to prepare a slurry with a mass concentration of 25wt.%, use 2mol / L sodium hydroxide solution to adjust the solution pH to 12, under nitrogen atmosphere, control the reaction temperature to 95°C, the stirring speed to 500rpm, and the reaction time to 4h. After the reaction, separate the solid and liquid, wash and dry to obtain vanadium trioxide solid.

[0058] Test results: vanadium recovery rate is 99.12%, and vanadium trioxide purity is 99.22%.

[0059] The product prepared in Example 8 was tested, and the XRD results were as follows: Figure 2 As shown, it indicates that vanadium trioxide was successfully prepared.

[0060] The above contents are further detailed descriptions of the present invention in combination with specific preferred embodiments, and it cannot be determined that the specific implementation of the present invention is limited to these descriptions. For ordinary technicians in the field to which the present invention belongs, several simple deductions or substitutions can be made without departing from the concept of the present invention, which should be regarded as falling within the scope of protection of the present invention.

Claims

1. A method for preparing vanadium trioxide using M(V3(OH)6(SO4)2), characterized in that: The following steps are involved: S1. Add water to M(V3(OH)6(SO4)2) to prepare a slurry, and adjust the pH value of the solution to 10-13; S2, heating under an inert atmosphere to cause the slurry to undergo a vanadium-breaking reaction; S3. After the reaction is completed, solid-liquid separation, washing and drying are performed to obtain vanadium trioxide solid.

2. The method for preparing vanadium trioxide using M(V3(OH)6(SO4)2) according to claim 1, characterized in that: The MV3(SO4)2(OH)6 is selected from one or both of NaV3(SO4)2(OH)6 and KV3(SO4)2(OH)6.

3. The method for preparing vanadium trioxide using M(V3(OH)6(SO4)2) according to claim 1, characterized in that: In step S1, the pH value of the solution is adjusted to 11-12.

4. The method for preparing vanadium trioxide using M(V3(OH)6(SO4)2) according to claim 1, characterized in that: In step S1, the mass concentration of the slurry is 5 to 45 wt.%.

5. The method for preparing vanadium trioxide using M(V3(OH)6(SO4)2) according to claim 1, characterized in that: In step S2, the inert atmosphere is nitrogen or argon.

6. The method for preparing vanadium trioxide using M(V3(OH)6(SO4)2) according to claim 1, characterized in that: In step S2, the temperature of the alum breaking reaction is 80-95° C., and the reaction time is 2-5 hours.

7. The method for preparing vanadium trioxide using M(V3(OH)6(SO4)2) according to claim 1, characterized in that: In step S2, the temperature of the alum breaking reaction is 90-95°C.

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