阅读说明：本技术 一种提纯蒸发一体化制备无水氟化铝的方法 (Method for preparing anhydrous aluminum fluoride by purification and evaporation integration ) 是由 曹玉宽 于 2020-06-19 设计创作，主要内容包括：本发明公开了一种提纯蒸发一体化制备无水氟化铝的方法,包括如下步骤：将粗氟化氢气体通入冷凝器冷凝得到氟化氢液体和废气；接着将氟化氢液体转入精馏塔中进行精馏并蒸发至流化床内与氢氧化铝反应制得无水氟化铝,其中,精馏塔塔顶出口的温度为20～22℃。本发明通过对系统的整合,将提纯系统和蒸发系统整合到一个生产系统中,使得氟化氢在不同相态下在该系统中实现共存,保证了生产的连续稳定进行,使得整个生产工艺更加流畅顺利；并且取消了氟化氢储存系统,使得整个生产系统中氟化氢的储存量降低到最小值,提高了安全管理的有效性,并且提纯蒸发系统的合并,减少了设备的投入和管理,减少管理难度。(The invention discloses a method for preparing anhydrous aluminum fluoride by purification and evaporation integration, which comprises the following steps: introducing the crude hydrogen fluoride gas into a condenser for condensation to obtain hydrogen fluoride liquid and waste gas; and then transferring the hydrogen fluoride liquid into a rectifying tower for rectification and evaporating the hydrogen fluoride liquid into a fluidized bed to react with aluminum hydroxide to prepare anhydrous aluminum fluoride, wherein the temperature of an outlet at the top of the rectifying tower is 20-22 ℃. The invention integrates the purification system and the evaporation system into one production system through the integration of the system, so that the hydrogen fluoride can coexist in the system under different phase states, the continuous and stable production is ensured, and the whole production process is smoother; and a hydrogen fluoride storage system is cancelled, so that the storage capacity of hydrogen fluoride in the whole production system is reduced to the minimum value, the effectiveness of safety management is improved, and the combination of purification and evaporation systems reduces the investment and management of equipment and reduces the management difficulty.)

1. A method for preparing anhydrous aluminum fluoride by purification and evaporation integration is characterized by comprising the following steps: introducing the crude hydrogen fluoride gas into a condenser for condensation to obtain hydrogen fluoride liquid and waste gas; and then transferring the hydrogen fluoride liquid into a rectifying tower for rectification and evaporating the hydrogen fluoride liquid into a fluidized bed to react with aluminum hydroxide to prepare anhydrous aluminum fluoride, wherein the temperature of an outlet at the top of the rectifying tower is 20-22 ℃.

2. The method for purifying hydrogen fluoride according to claim 1, wherein the condensation temperature is 14 to 16 ℃.

3. The method for purifying hydrogen fluoride according to claim 1 or 2, wherein an overhead condenser is provided at the top of the rectifying column.

4. The method for purifying hydrogen fluoride according to any one of claims 1 to 3, wherein the temperature of the bottom of the rectifying column is 20 to 22 ℃.

5. The method for purifying hydrogen fluoride according to any one of claims 1 to 4, wherein the exhaust gas is subjected to washing absorption treatment.

Technical Field

The invention relates to the technical field of aluminum fluoride preparation, in particular to a method for preparing anhydrous aluminum fluoride by integrating purification and evaporation.

Background

In the existing production process of anhydrous aluminum fluoride, a purification system and an evaporation system need to be separated due to different phase states of an intermediate product, namely hydrogen fluoride, and in order to ensure continuous and orderly production, transition storage equipment has to be arranged between the purification system and the evaporation system according to the different phase states, so that the normal production can be ensured.

However, this adds virtually to the difficulty of investment and management of the equipment. Moreover, as a highly toxic substance, the safety management points are increased more and more with the increase of equipment and storage capacity, which brings great difficulty and danger to the whole production and management.

Disclosure of Invention

Based on the technical problems in the prior art, the invention provides a method for preparing anhydrous aluminum fluoride by integrating purification and evaporation, and the method integrates a purification system and an evaporation system into one production system by integrating the system, so that hydrogen fluoride can coexist in the system in different phase states, the continuous and stable production is ensured, and the whole production process is smoother; and a hydrogen fluoride storage system is cancelled, so that the storage capacity of hydrogen fluoride in the whole production system is reduced to the minimum value, the effectiveness of safety management is improved, and the combination of purification and evaporation systems reduces the investment and management of equipment and reduces the management difficulty.

The invention provides a method for preparing anhydrous aluminum fluoride by integrating purification and evaporation, which comprises the following steps: introducing the crude hydrogen fluoride gas into a condenser for condensation to obtain hydrogen fluoride liquid and waste gas; and then transferring the hydrogen fluoride liquid into a rectifying tower for rectification and evaporating the hydrogen fluoride liquid into a fluidized bed to react with aluminum hydroxide to prepare anhydrous aluminum fluoride, wherein the temperature of an outlet at the top of the rectifying tower is 20-22 ℃.

Preferably, the condensation temperature is 14-16 ℃.

Preferably, the top of the rectifying tower is provided with an overhead condenser.

Preferably, the temperature of the tower kettle of the rectifying tower is 20-22 ℃.

The rectification process is a continuous process, and the time for rectifying the hydrofluoric acid in the rectification tower is 8-12 min.

Preferably, the exhaust gas is subjected to scrubbing absorption treatment.

The waste gas mainly contains silicon tetrafluoride, sulfur dioxide and the like, the environment pollution is avoided through washing and absorption treatment, and the fluosilicic acid by-product can be prepared through washing and absorption treatment.

The above-mentioned method for producing a crude hydrogen fluoride gas is a conventional method in the art.

The above-mentioned reaction of hydrogen fluoride with aluminum hydroxide to produce anhydrous aluminum fluoride is a conventional method in the art.

Has the advantages that:

the invention firstly carries out condensation treatment on the crude hydrogen fluoride gas, removes most light components to obtain hydrogen fluoride liquid, although the hydrogen fluoride liquid also contains a little light components, the quality of the final product aluminum fluoride is not influenced; the condensation treatment can avoid the problems that the evaporation system equipment is easy to damage due to the direct evaporation of the crude hydrogen fluoride gas, and the quality of the final product aluminum fluoride is influenced by the heavy components (such as sulfuric acid, heavy metal components, phosphorus pentoxide and the like) in the gas along with the evaporation; the top of the rectifying tower is provided with a top condenser, the temperature of an outlet at the top of the rectifying tower is set to be 20-22 ℃, so that the rectifying tower only has the functions of separating heavy components and refluxing and does not have the function of separating residual light components, hydrogen fluoride discharged from the rectifying tower is in a gaseous state and can directly enter a fluidized bed to react with aluminum hydroxide to prepare anhydrous aluminum fluoride, and thus, an independent hydrogen fluoride evaporation system is not required to be arranged, and the purification and evaporation are combined into one; after the two systems are combined, the storage system required between the former two systems is correspondingly removed, the total amount of the hydrogen fluoride in the online operation of the whole production system is also reduced, and the safety management is ensured.

Detailed Description

The technical solution of the present invention will be described in detail below with reference to specific examples.