阅读说明：本技术 一种钒资源回收利用的方法 (Method for recycling vanadium resources ) 是由 张美杰 和奔流 刘峰 张军丽 杨倩 张建林 张燕平 赵冠杰 杨德 王丽艳 陈建立 于 2021-08-25 设计创作，主要内容包括：本发明公开了一种钒资源回收利用的方法,属于冶金技术领域,解决了传统技术中流程长、能耗高、污染严重的问题,其包括步骤A：在粗四氯化钛精制过程中,不加入除钒剂,得到精四氯化钛；步骤B：在步骤A中的含钒的精四氯化钛中加入还原剂,使四氯化钛中的三氯氧钒还原为三氯化钒；步骤C：将步骤B中得到的含钒溶液进行沉降和固液分离；步骤D：将步骤C中固液分离后的含钒溶液进行蒸馏,并根据生产需求调整溶液中的四氯化钛浓度,最终得到成品,实现了钒的回收利用,简化回收工工序、降低能耗与污染。(The invention discloses a method for recycling vanadium resources, belongs to the technical field of metallurgy, solves the problems of long flow, high energy consumption and serious pollution in the traditional technology, and comprises the following steps: in the refining process of the crude titanium tetrachloride, no vanadium removing agent is added to obtain refined titanium tetrachloride; and B: adding a reducing agent into the vanadium-containing refined titanium tetrachloride in the step A to reduce vanadium oxytrichloride in the titanium tetrachloride into vanadium trichloride; and C: b, settling and carrying out solid-liquid separation on the vanadium-containing solution obtained in the step B; step D: and D, distilling the vanadium-containing solution subjected to solid-liquid separation in the step C, and adjusting the concentration of titanium tetrachloride in the solution according to production requirements to finally obtain a finished product, thereby realizing the recycling of vanadium, simplifying the recycling process and reducing energy consumption and pollution.)

1. A method for recycling vanadium resources is characterized by comprising the following steps:

step A: in the refining process of the crude titanium tetrachloride, no vanadium removing agent is added to obtain refined titanium tetrachloride;

and B: adding a reducing agent into the vanadium-containing refined titanium tetrachloride in the step A to reduce vanadium oxytrichloride in the titanium tetrachloride into vanadium trichloride;

and C: b, settling and carrying out solid-liquid separation on the vanadium-containing solution obtained in the step B;

step D: and D, distilling the vanadium-containing solution subjected to solid-liquid separation in the step C, and adjusting the concentration of titanium tetrachloride in the solution according to production requirements to finally obtain a finished product.

2. The method for recycling vanadium resources according to claim 1, wherein the reducing agent in the step B is activated carbon, and the reaction between titanium tetrachloride and activated carbon is: VOCl₃+C→VCl₃+CO↑。

3. The method for recycling vanadium resources according to claim 1, wherein the reducing agent in the step B is one of aluminum powder, copper wire and organic oil.

4. The method for recycling vanadium resources according to claim 1, wherein the boiling point of titanium tetrachloride in the step D is 136 degrees, the boiling point of vanadium trichloride is 425 degrees, and the concentration of the titanium tetrachloride solution of vanadium is changed by distillation, so that titanium sponge products with different vanadium contents are prepared.

Technical Field

The invention belongs to the technical field of metallurgy, and particularly relates to a method for recycling vanadium resources.

Background

In the refining process of titanium tetrachloride, the more mature vanadium removal process comprises aluminum powder vanadium removal, steel wire vanadium removal, hydrogen sulfide vanadium removal, mineral oil vanadium removal and the like, crude titanium tetrachloride is added into a distillation kettle and then heated to the boiling point, a vanadium removal agent is added into the distillation kettle, vanadium oxychloride is reduced into vanadium oxychloride, and vanadium elements in the titanium tetrachloride are removed through a distillation tower through the difference of the boiling points of the two. Thus, a large amount of vanadium elements are enriched in the bottom substrate of the distillation kettle to become vanadium slag rich in vanadium resources. At present, vanadium pentoxide is prepared from vanadium slag by a calcination method or a leaching method and used as a raw material for vanadium steel smelting, but the methods have the defects of long flow, high energy consumption, heavy pollution and the like.

Therefore, it is necessary to develop a new vanadium extraction process, which realizes short process, low energy consumption and low pollution.

Disclosure of Invention

Aiming at the problems of long flow path, high energy consumption and serious pollution in the prior art, the invention provides a method for recycling vanadium resources, which aims to: the vanadium resource in the titanium tetrachloride is reserved, the recovery of vanadium is realized, the recovery process is simplified, and the energy consumption and pollution are reduced.

The technical scheme adopted by the invention is as follows:

a method for recycling vanadium resources comprises the following steps:

step A: in the refining process of the crude titanium tetrachloride, no vanadium removing agent is added to obtain refined titanium tetrachloride;

and B: adding a reducing agent into the vanadium-containing refined titanium tetrachloride in the step A to reduce vanadium oxytrichloride in the titanium tetrachloride into vanadium trichloride;

and C: b, carrying out sedimentation and solid-liquid separation on the vanadium-containing solution obtained in the step B

Step D: and D, distilling the vanadium-containing solution subjected to solid-liquid separation in the step C, and adjusting the concentration of titanium tetrachloride in the solution according to production requirements to finally obtain a finished product.

By adopting the scheme, under the normal titanium tetrachloride refining process, the vanadium removal process is omitted, the titanium tetrachloride containing vanadium is prepared, vanadium trichloride in the titanium tetrachloride is reduced into vanadium trichloride through activated carbon, and the vanadium trichloride is used as a raw material for producing titanium sponge to prepare a titanium sponge product containing vanadium, so that vanadium resources are recycled, oxygen elements in the vanadium trichloride in the refined titanium tetrachloride are removed, the oxygen elements cannot be introduced in the titanium sponge preparation process, and the titanium sponge finished product is prevented from hardening due to the oxygen elements.

The reducing agent in the step B is activated carbon, and the reaction of titanium tetrachloride and the activated carbon is as follows: VOCl₃+C→VCl₃+CO↑。

By adopting the scheme, the vanadium element in the method is always in the titanium tetrachloride solution and does not enter a slag system, so that the vanadium element is prevented from being extracted from slag again, and the recovery rate of the vanadium element is improved.

And the reducing agent in the step B is one of aluminum powder, copper wire and organic oil.

And D, changing the concentration of the titanium tetrachloride solution of vanadium by distillation to prepare titanium sponge products with different vanadium contents, wherein the boiling point of the titanium tetrachloride in the step D is 136 degrees, the boiling point of the vanadium trichloride is 425 degrees.

By adopting the scheme, the recovery can be realized in the original rectification process, and meanwhile, compared with the traditional vanadium recovery, the method has no roasting process, so that the internal consumption is reduced, no leaching process is carried out, and the water pollution is avoided.

In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:

1. under the normal titanium tetrachloride refining process, the vanadium removal process is omitted, the titanium tetrachloride containing vanadium is prepared, vanadium trichloride in the titanium tetrachloride is reduced to vanadium trichloride through activated carbon, the vanadium trichloride is used as a raw material for producing sponge titanium, and a sponge titanium product containing vanadium is prepared, so that vanadium resources are recycled, oxygen elements in the vanadium trichloride in the refined titanium tetrachloride are removed, the oxygen elements cannot be introduced in the sponge titanium preparation process, and the sponge titanium finished product is prevented from hardening due to the oxygen elements.

2. The method can realize the recovery in the original rectification process, and simultaneously has no roasting process compared with the traditional vanadium recovery, so the internal consumption is reduced, no leaching process is needed, and the water pollution is avoided.

3. The vanadium element in the method is always in the titanium tetrachloride solution and does not enter a slag system, so that the vanadium element is prevented from being extracted from the slag again, and the recovery rate of the vanadium element is improved.

Drawings

The invention will now be described, by way of example, with reference to the accompanying drawings, in which:

FIG. 1 is a schematic flow diagram of one embodiment of the present invention.

Detailed Description

All of the features disclosed in this specification, or all of the steps in any method or process so disclosed, may be combined in any combination, except combinations of features and/or steps that are mutually exclusive.

The present invention will be described in detail with reference to fig. 1.

The first embodiment is as follows:

FIG. 1 is a schematic process flow diagram of an embodiment of the present invention, the embodiment of the present invention is used for recovering vanadium in titanium tetrachloride, and the recovery process mainly comprises: the method comprises the following steps of refining titanium tetrachloride, reducing vanadium oxychloride in the titanium tetrachloride, adjusting the content of vanadium in the titanium tetrachloride, preparing vanadium-containing sponge titanium and the like, and comprises the following operation steps: firstly, no vanadium removing agent is added into a primary kettle, so as to prepare vanadium-containing refined titanium tetrachloride, then excessive activated carbon is added into the vanadium-containing refined titanium tetrachloride, and VOCl is added₃All reduced to VCl₃According to the requirement of vanadium content of vanadium-containing titanium sponge to 10%, the vanadium content of titanium tetrachloride is increased to 0.75% by distillation, the solution is added into a reduction furnace according to a reduction feeding system, vanadium-titanium chloride is synchronously reduced into simple substance sponge metal, magnesium and magnesium chloride in the vanadium-containing titanium sponge are removed by a distillation process, and then the commercial product of the vanadium-containing titanium sponge is obtained by crushing and screening processes.

It should be noted that the distillation is performed by the difference of boiling points of the two solutions, so as to adjust the concentration of the solution to be a mature prior art, and the specific process is not described in detail herein.

The above-mentioned embodiments only express the specific embodiments of the present application, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present application. It should be noted that, for those skilled in the art, without departing from the technical idea of the present application, several changes and modifications can be made, which are all within the protection scope of the present application.