阅读说明：本技术 一种从水溶液中回收钒的方法 (Method for recovering vanadium from aqueous solution ) 是由 彭浩 郭静 邱虹智 王彩琼 郝智会 张晨渝 李兵 吕利平 黄辉胜 于 2021-08-12 设计创作，主要内容包括：本发明申请属于溶液中钒离子的回收技术领域,具体公开了一种从水溶液中回收钒的方法,包括以下步骤：(1)将含钒溶液pH调节至1-5之间；(2)根据溶液中钒的浓度加入适量氨基化合物沉钒剂；(3)水浴加热反应,反应温度为30-90℃皆可；反应时间与氨基化合物的用量有关,氨基化合物用量多,反应时间为最少10min；(4)反应一段时间后压滤得到含钒沉淀和滤液；(5)滤液经处理后排放,将含钒沉淀在一定温度下进行加热煅烧可以得到五氧化二钒沉淀和氨基化合物。本方案主要用于钒离子回收,解决了现有技术中回收钒离子容易将铵盐残留在水中对环境造成伤害的问题。(The invention belongs to the technical field of recovery of vanadium ions in a solution, and particularly discloses a method for recovering vanadium from an aqueous solution, which comprises the following steps: (1) adjusting the pH value of the vanadium-containing solution to 1-5; (2) adding a proper amount of amino compound vanadium precipitation agent according to the concentration of vanadium in the solution; (3) heating in water bath at 30-90 deg.C for reaction; the reaction time is related to the dosage of the amino compound, the dosage of the amino compound is more, and the reaction time is at least 10 min; (4) after reacting for a period of time, performing pressure filtration to obtain vanadium-containing precipitate and filtrate; (5) and (3) treating the filtrate, discharging, and heating and calcining the vanadium-containing precipitate at a certain temperature to obtain vanadium pentoxide precipitate and an amino compound. The scheme is mainly used for recovering vanadium ions, and solves the problem that the ammonium salt is easy to remain in water to cause damage to the environment when the vanadium ions are recovered in the prior art.)

1. A method for recovering vanadium from an aqueous solution, comprising the steps of:

(1) adjusting the pH value of the vanadium-containing solution to 1-5;

(2) adding a proper amount of an amino compound vanadium precipitation agent according to the concentration of vanadium in the solution, wherein the mass ratio of the amino compound to vanadium ions is n (amino compound)/n (V) is 0.2-3.0;

(3) heating in water bath at 30-90 deg.C for reaction; the reaction time is related to the dosage of the amino compound, the dosage of the amino compound is more, and the reaction time is at least 10 min;

(4) reacting for 10-180min, and press-filtering to obtain vanadium-containing precipitate and filtrate;

(5) the filtrate is discharged after being treated, and vanadium-containing precipitate is heated and calcined at the temperature of 200-600 ℃ to obtain vanadium oxide compounds and amino compounds.

2. The method of claim 1, wherein the pH is adjusted to 1.8 in step (1).

3. The method for recovering vanadium from aqueous solution according to claim 1, wherein the vanadium precipitating agent in the step (2) is mainly amino compound, and the amino compound comprises urea, melamine, natural amino acid, glycine, glutamic acid and lysine.

4. The method for recovering vanadium from an aqueous solution according to claim 1, wherein the mass ratio of the amino compound to the vanadium ion solution in the step (3) is n (amino compound)/n (v) 1.0.

5. The method for recovering vanadium from an aqueous solution according to claim 1, wherein the water bath heating reaction temperature in the step (4) is 90 ℃.

6. The method of claim 1, wherein the amino compound in step (5) can be separated from the vanadium by heating.

Technical Field

The invention belongs to the technical field of recovery of vanadium ions in a solution, and particularly discloses a method for recovering vanadium from an aqueous solution.

Background

The recovery method of vanadium ion in solution is many, mainly including chemical precipitation method (ammonium salt precipitation method), solvent extraction, ion exchange, etc. The ammonium salt precipitation method has higher temperature and higher requirement on initial vanadium concentration (generally more than 10 g/L), and the excessive ammonium salt causes great harm to the environment. Solvent extraction or ion exchange methods are expensive and difficult to industrialize, and most of them are concentrated on laboratory research.

In the prior art, vanadium ions are generally precipitated by using ammonium salt to remove vanadium in water solution, and after the ammonium salt is used, the ammonium salt remains in water, which causes harm to the environment.

Disclosure of Invention

The invention aims to provide a method for recovering vanadium from an aqueous solution, which aims to solve the problem that ammonium salt is easy to remain in water to cause harm to the environment when vanadium ions are recovered in the prior art.

In order to achieve the purpose, the technical scheme of the invention is as follows: a method for recovering vanadium from an aqueous solution comprising the steps of:

(1) adjusting the pH value of the vanadium-containing solution to 1-5;

(2) adding a proper amount of an amino compound vanadium precipitation agent according to the concentration of vanadium in the solution, wherein the mass ratio of the amino compound to vanadium ions is n (amino compound)/n (V) is 0.2-3.0;

(3) heating in water bath at 30-90 deg.C for reaction; the reaction time is related to the dosage of the amino compound, the dosage of the amino compound is more, and the reaction time is at least 10 min;

(4) reacting for 10-180min, and press-filtering to obtain vanadium-containing precipitate and filtrate;

(5) the filtrate is discharged after being treated, and vanadium-containing precipitate is heated and calcined at the temperature of 200-600 ℃ to obtain vanadium oxide compounds and amino compounds.

Further, the pH was adjusted to 1.8 in step (1).

Further, the vanadium precipitation agent in the step (2) is mainly an amino compound, and the amino compound comprises urea, melamine, natural amino acid, glycine, glutamic acid and lysine.

Further, in step (3), the mass ratio of the amino compound to the vanadium ion solution is n (amino compound)/n (v) 1.0.

Further, the water bath heating reaction temperature in the step (4) is 90 ℃.

Further, the amino compound in the step (5) can be separated from the vanadium by heating.

The working principle and the beneficial effects of the technical scheme are as follows: (1) the method effectively combines amino and vanadium oxide compounds together by utilizing the strong action force of molecular hydrogen bonds, and realizes the high-efficiency precipitation (adsorption) of vanadium. The scheme mainly comprises the step of reacting an amino compound with vanadyl ions. When the amino compound is not reacted, the reaction principle is different; for example, ammonium salt, urea and the like are used, ammonium salt and urea are hydrolyzed at high temperature under acidic conditions to obtain ammonium ions, and the ammonium ions and vanadyl ions react to obtain vanadium-containing precipitates, so that the effect of precipitating vanadium is achieved. The use of amino acids, melamine, and the like causes the efficient adsorption of vanadium by hydrogen bonds between amino groups and vanadium oxide compounds.

(2) In the scheme, the vanadium-containing precipitate is calcined at the temperature of 200-600 ℃, so that a vanadium oxide compound and an amino compound can be obtained, the obtained amino compound can be reused for vanadium precipitation, and the cyclic utilization of the vanadium precipitation agent can be realized.

Detailed Description

The following is further detailed by way of specific embodiments:

examples substantially as follows, a method for recovering vanadium from an aqueous solution comprising the steps of:

(1) the pH of the vanadium-containing solution can be adjusted to 1-5, and in this embodiment, the pH is preferably 1.8, i.e., 1.6-2.0 is preferable; in this example, using melamine as an experimental case, when the pH is 1.6, 1.7, 1.8, 1.9, and 2.0, the vanadium deposition rates are 99.56%, 99.63%, 99.97%, 99.74%, and 99.68%, respectively.

(2) Adding a proper amount of vanadium precipitation agent according to the concentration of vanadium in the solution; in the embodiment, the vanadium precipitation agent is mainly an amino compound, such as urea, melamine, amino acid and the like; the inventors also can use unmodified natural amino acids, such as glycine, glutamic acid, lysine, etc., and through a large number of experiments, the compounds containing amino groups can be obtained. The dosage range of the amino compound in the embodiment is n (amino compound)/n (v) 0.2-3.0, wherein 1.0 has the best effect; in this example, in the case of using melamine as an experimental case, when the ratios of the amount of melamine to the amount of vanadium ion are 0.2, 0.4, 0.6, 0.8, and 1.0, the precipitation rates are 96.21%, 97.89%, 99.94%, 99.91%, and 99.97%, respectively.

(3) Heating in water bath to react at 30-90 deg.c for optimal 90 deg.c effect; the reaction time is related to the dosage of the amino compound, the dosage of the amino compound is more, the reaction time is only 10min, the dosage of the amino compound is less, and the reaction time needs to be correspondingly longer;

in this example, in the case of using melamine as an experimental example, when the amount of melamine used was such that n (melamine)/n (vanadium) was 1.0, the reaction temperatures were 20 ℃, 35 ℃, 50 ℃, 75 ℃ and 90 ℃, respectively, and the vanadium deposition rates were 99.97%, and 99.98%, respectively.

(4) After reacting for a period of time, performing pressure filtration to obtain vanadium-containing precipitate and filtrate;

(5) and (3) discharging the filtrate after treatment, and heating and calcining the vanadium-containing precipitate at a certain temperature to obtain a vanadium oxide compound and an amino compound, wherein the amino compound is ammonia gas and/or melamine and can be other types of amino compounds. In this example, the amino compound may be separated from the vanadium by heating.

In the scheme, through multiple experiments, the inventor obtains that the amino and the vanadium oxide compound are effectively combined together by using the vanadium precipitation agent and utilizing the strong acting force of molecular hydrogen bonds under the acidic condition, so that the efficient precipitation of vanadium is realized.

The foregoing is merely an example of the present invention and common general knowledge of known specific structures and features of the embodiments is not described herein in any greater detail. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent.