CN1482064A

CN1482064A - Method of preparing anhydrous aluminium chloride

Info

Publication number: CN1482064A
Application number: CNA021299978A
Authority: CN
Inventors: 章浩龙
Original assignee: Individual
Current assignee: Individual
Priority date: 2002-09-10
Filing date: 2002-09-10
Publication date: 2004-03-17
Anticipated expiration: 2022-09-10
Also published as: CN1209290C

Abstract

The present invention is one method of preparing anhydride aluminum chloride with simple technological process, no waste gas exhaust and high purity product. The aluminum chloride hexahydrate material is first compounded into water solution, C1-C4 alcohol is then added into the water solution for separating crystal, and the separated crystal as anhydride aluminum chloride product is finally separated from the solid-liquid mixture. The liquid after solid-liquid separation has main component alcohol and may be reused. The said process can eliminate impurity from aluminum chloride hexahydrate to obtain high purity anhydride aluminum chloride.

Description

Preparation method of anhydrous aluminum chloride

Technical Field

The invention relates to a preparation method of inorganic salt, in particular to a preparation method of anhydrous aluminum chloride.

Background

Anhydrous aluminum chloride is widely used in organic synthesis catalysts, petroleum cracking catalysts, and the like, and is also widely used in synthesis of detergents, pesticides, dyes, perfumes, metal refining, and the like. At present, most enterprises generally adopt a metallic aluminum method to produce anhydrous aluminum chloride, and the specific method comprises the following steps: putting the preheated aluminum ingot into a closed chlorination reaction furnace, feeding chlorine into the furnace from the upper part along a guide pipe, and reacting at thetemperature of 800-: and the generated aluminum chloride enters a condenser through a sublimation pipe, and is captured and precipitated to be crystallized, so that a finished product is obtained. The process has the defects that the tail gas is washed by alkaline water in a washing tower during emission, and in addition, the production cost is high.

A process for preparing anhydrous aluminum chloride by using an alundum-fixed bed method is described on page 510 of inorganic salt industry handbook published in 1 month of 1996 by chemical industry publishers. The process takes alumina as a main raw material, coal as a reducing agent, pulp waste liquid as an adhesive and chlorine as an oxidizing agent, and the alumina powder and the pulp waste liquid are reacted under the environment of 850- . The process has the following stepsFoot: firstly, the tail gas contains a small amount of chlorine and is discharged after being treated; secondly, the prepared anhydrous chlorinationThe purity of the aluminum is low, and the high-purity anhydrous aluminum chloride can be obtained only by refining the aluminum by a sublimation method; thirdly, the process is complicated.

Disclosure of Invention

Aiming at the defects, the invention provides the method for preparing the anhydrous aluminum chloride, so that the process for preparing the anhydrous aluminum chloride is simple, no waste gas is discharged, and the prepared anhydrous aluminum chloride has high purity. In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of anhydrous aluminum chloride adopts aluminum chloride hexahydrate as a raw material, and comprises the following specific processes: preparing aluminumchloride hexahydrate into an aqueous solution, adding alcohol into the aqueous solution of aluminum chloride hexahydrate, and carrying out solid-liquid separation after crystals in the solution are completely separated out, wherein the separated crystals are anhydrous aluminum chloride.

According to the above method, water-insoluble impurities can be removed by filtration after aluminum chloride hexahydrate is prepared as an aqueous solution.

By adopting the method, no waste gas is discharged in the whole production process, and the main component of the liquid after solid-liquid separation is alcohol, so that the liquid can be recycled and reused, and the environmental protection is facilitated; in addition, in the preparation process, the purity of the anhydrous aluminum chloride can be further improved through the steps of filtering, crystallizing and the like, and experiments prove that the purity of the anhydrous aluminum chloride prepared by the method can reach 99.5 percent; meanwhile, the invention has simple process and low production cost.

Detailed Description

Example 1

10 g of aluminum chloride hexahydrate is taken and put into a beaker, water is added for dissolving to prepare a solution, 95 percent ethanol is slowly poured into the beaker, after crystals in the beaker are fully separated out, solid-liquid separation is carried out in a centrifugal separator, and white crystals, namely the anhydrous aluminum chloride, are obtained. The concentration of ethanol poured in according to the above method may also be 75%, 99.5%. The solid-liquid separation according to the above method can also be carried out by other methods such as ordinary filtration. It is also possible to remove impurities by filtration after preparation of the aqueous solution.

Example 2

Taking 10 g of aluminum chloride hexahydrate, putting the aluminum chloride hexahydrate into a beaker, adding water to prepare an aqueous solution, filtering to remove impurities, slowly pouring commercially available methanol, and after crystals in the beaker are fully precipitated, carrying out solid-liquid separation in a centrifugal separator to obtain white crystals, namely the anhydrous aluminum chloride. The solid-liquid separation according to the above method can also be carried out by other methods such as ordinary filtration. Or filtering to remove impurities after preparing the aluminum chloride hexahydrate into an aqueous solution.

Example 3

Taking 10 g of aluminum chloride hexahydrate, putting the aluminum chloride hexahydrate into a beaker, adding water to prepare an aqueous solution, filtering to remove impurities, slowly pouring commercial n-propanol into the beaker, and after crystals in the beaker are fully precipitated, carrying out solid-liquid separation in a centrifugal separator to obtain white crystals, namely the anhydrous aluminum chloride. The solid-liquid separation according to the above method can also be carried out by other methods such as ordinary filtration. Or filtering to remove impurities after preparing the aluminum chloride hexahydrate into an aqueous solution.

Example 4

10 g of aluminum chloride hexahydrate is taken and put into a beaker, water is added to prepare an aqueous solution, after impurities are removed by filtration, commercial ethylene glycol is slowly poured into the beaker, and after crystals in the beaker are fully precipitated, solid-liquid separation is carried out in a centrifugal separator to obtain white crystals, namely the anhydrous aluminum chloride. The solid-liquid separation according to the above method can also be carried out by other methods such as ordinary filtration. Or filtering to remove impurities after preparing the aluminum chloride hexahydrate into an aqueous solution.

Example 5

Taking 10 g of aluminum chloride hexahydrate, putting the aluminum chloride hexahydrate into a beaker, adding water to prepare an aqueous solution, filtering to remove impurities, slowly pouring commercial diethylene glycol, and after crystals in the beaker are fully precipitated, carrying out solid-liquid separation in a centrifugal separator to obtain white crystals, namely the anhydrous aluminum chloride. The solid-liquid separation according to the above method can also be carried out by other methods such as ordinary filtration. Or filtering to remove impurities after preparing the aluminum chloride hexahydrate into an aqueous solution.

Example 6

Taking 10 g of aluminum chloride hexahydrate, putting the aluminum chloride hexahydrate into a beaker, adding water to prepare an aqueous solution, filtering to remove impurities, slowly pouring commercially available propylene glycol, and after crystals in the beaker are fully precipitated, carrying out solid-liquid separation in a centrifugal separator to obtain white crystals, namely the anhydrous aluminum chloride. The solid-liquid separation according to the above method can also be carried out by other methods such as ordinary filtration. Or filtering to remove impurities after preparing the aluminum chloride hexahydrate into an aqueous solution.

Claims

1. A preparation method of anhydrous aluminum chloride is characterized in that aluminum chloride hexahydrate is adopted as a raw material, and the specific process is as follows:

a. preparing aluminum chloride hexahydrate into an aqueous solution;

b. adding alcohol into the aluminum chloride hexahydrate aqueous solution;

c. and carrying out solid-liquid separation after crystals in the solution are fully precipitated.

2. The method for preparing anhydrous aluminum chloride according to claim 1, wherein step a is followed by filtration to remove water-insoluble impurities therefrom.

3. The method for preparing anhydrous aluminum chloride according to claim 1, wherein the alcohol is present in a concentration of 75 to 99.5%.

4. The method for producing anhydrous aluminum chloride according to claim 1, wherein the solid-liquid separation is centrifugal separation.

5. The method of claim 1, wherein the alcohol is a monohydric or polyhydric alcohol selected from the group consisting of c 1-c 4.

6. The method for preparing anhydrous aluminum chloride according to claim 1 or 2, wherein the alcohol is methanol or ethanol or propanol or ethylene glycol or diethylene glycol or propylene glycol.