PROCESS FOR CONTINUOUS PURIFICATION OF HIGH-PURITY TRIMETHYLALUMINUM

Abstract

A process for continuous purification of high-purity trimethylaluminum is provided. The process includes preparing a membrane separator, which is placed vertically for use, and arranging a condenser tube inside of the membrane separator and a heating tube outside of the membrane separator, and a disperser at the top of the membrane separator for dispersing a liquid. The liquid naturally flows down along the inner wall of the heating tube by gravity to form a membrane. The process further includes concentrating liquid components having a low boiling point which are collected by the condenser at different stages and concentrating liquid components having a high boiling point which are collected by the heating wall.

Claims

1. A process for continuous purification of high-purity trimethylaluminum, comprising, S1: preparing a membrane separator, which is placed vertically for use, and arranging a condenser tube inside of the membrane separator and a heating tube outside of the membrane separator, and a disperser at a top of the membrane separator for dispersing a liquid, the liquid naturally flowing down along an inner wall of the heating tube by gravity to form a membrane, and concentrating liquid components having a low boiling point which are collected by the condenser at different stages and concentrating liquid components having a high boiling point which are collected by the inner wall; S2: arranging a number of fraction collection outlets O.sub.1 to O.sub.x at different positions of the membrane separator, wherein liquid collected from the outlets O.sub.1 to O.sub.x contains more components having a low boiling point, and arranging number of fraction collection outlets O.sub.x+1 to O.sub.x+n in a middle of the membrane separator for collecting a mixed liquid, and returning the mixed liquid collected from the outlets O.sub.x+1 to O.sub.x+n to a crude trimethylaluminum tank for subsequent separation; S3: arranging a number of high-purity product collection outlets O.sub.p1 to O.sub.pn in a lower part of the membrane separator and a residual liquid collection outlet O.sub.W at a bottom of the membrane separator, wherein liquid collected from the outlets O.sub.p1 to O.sub.Pn is a qualified product, and the residual liquid is collected from the collection outlet O.sub.w, and arranging a sample collection outlet on each of the collection outlets for sampling and analysis; S4: according to the sampling and analysis results from the sample collection outlet, classifying the collection outlets as the fraction collection outlets, the mixed liquid collection outlets and [[the]] qualified product collection outlets; and S5: charging hot oil and cold oil into the membrane separator, keeping temperatures of the hot oil and the cold oil each be constant at a fixed value so that the temperature accuracy is controlled at ±1° C., wherein the temperature of the hot oil ranges from 40° C. to 80° C., and the temperature of the cold oil ranges from 5° C. to 20° C.

2. The process as claimed in claim 1, wherein the membrane separator is provided with a condensing medium inlet at its bottom, and with a cold medium outlet at its right side of the top.

3. The process as claimed in claim 1, wherein the membrane separator is provided a hot medium inlet at its right side of the bottom, and with a hot medium outlet at its right side of the top.

4. The process as claimed in claim 1, wherein the top of the membrane separator is connected to a micro metering pump through a pipe, and the micro metering pump is connected to the crude trimethylaluminum tank through a pipe.

5. The process as claimed in claim 1, wherein the membrane separator is provided with a liquid disperser at its top, and the trimethylaluminum product in the form of liquid is fed into the membrane separator through a pipe connected with the micro metering pump, and then dispersed into the inner wall of the heating tube to naturally flow down along by gravity to form a membrane.

6. The process as claimed in claim 1, wherein the membrane separator is, at its one side, connected with a fraction storage tank, a high-purity product storage tank and a residual liquid storage tank through a pipe, respectively.

Description

BRIEF DESCRIPTION OF THE DRAWING

[0024] The foregoing summary, as well as the following detailed description of the preferred invention, will be better understood when read in conjunction with the appended drawing. For the purpose of illustrating the preferred invention, there is shown in the drawing an embodiment which is presently preferred. It should be understood, however, that the invention is not limited to the precise arrangements and instrumentalities shown. In the drawing:

[0025] FIG. 1 shows a schematic diagram of the process for continuous purification of high-purity trimethylaluminum according to an embodiment of the present disclosure.

DETAILED DESCRIPTION OF THE INVENTION

[0026] In the following, the technical solutions in the embodiments of the present disclosure will be clearly and completely described in combination with the drawings. Obviously, the examples as described are only a part of the examples of the present disclosure, not all of them.

[0027] Referring to the FIG. 1, a process for continuous purification of high-purity trimethylaluminum includes:

[0028] S1: preparing a membrane separator, which is placed vertically for use, and arranging a condenser tube inside and a heating tube outside the membrane separator, and a disperser at the top of the membrane separator for dispersing a liquid, the liquid naturally flowing down along the inner wall of the heating tube by gravity to form a membrane, and concentrating liquid components with low boiling point which collected by the condenser at different stages and concentrating liquid components with high boiling point which collected by the heating wall;

[0029] S2: arranging a number of fraction collection outlets O.sub.1 to O.sub.x at different positions of the membrane separator, wherein the liquid collected from the outlets O.sub.1 to O.sub.x contains more components with low boiling point, and

[0030] arranging a number of fraction collection outlets O.sub.x+1 to O.sub.x+n in the middle of membrane separator for collecting a mixed liquid, and returning the mixed liquid collected from the outlets O.sub.x+1 to O.sub.x+n to a crude trimethylaluminum tank for subsequent separation;

[0031] S3, arranging a number of high-purity product collection outlets O.sub.p1 to O.sub.pn in the lower part of membrane separator and a residual liquid collection outlet O.sub.W at the bottom of the membrane separator, wherein the liquid collected from the outlets O.sub.p1 to O.sub.Pn is a qualified product, the residual liquid is collected from the collection outlet O.sub.w, and

[0032] arranging a sample collection outlet on each of the collection outlets for sampling and analysis;

[0033] S4: according to the sampling and analysis results from the sample collection outlet, classifying the collection outlets as the fraction collection outlets, the mixed liquid collection outlets and the qualified product collection outlets; and

[0034] S5: charging hot oil and cold oil into the membrane separator, keeping temperatures of hot oil and cold oil each be constant at a fixed value so that the temperature accuracy is controlled at ±1° C., wherein the temperature of hot oil ranges from 40° C. to 80° C., and the temperature of cold oil ranges from 5° C. to 20° C.

[0035] In this example, the membrane separator is provided with a condensing medium inlet at its bottom, and with a cold medium outlet at its right side of the top.

[0036] In this example, the membrane separator is provided with a hot medium inlet at its right side of the bottom, and with a hot medium outlet at the right side of the top.

[0037] In this example, the top of the membrane separator is connected to a micro metering pump through a pipe; and the micro metering pump is connected to the crude trimethylaluminum tank through a pipe.

[0038] In this example, the membrane separator is provided with a liquid disperser at its top; the trimethylaluminum product in the form of liquid is fed into the separator through a pipe connected with the micro metering pump, and then dispersed into the inner wall of the heating tube to naturally flow down by gravity to form a membrane.

[0039] In this example, the membrane separator is connected with a fraction storage tank, a high-purity product storage tank and a residual liquid storage tank through a pipe, at its one side, respectively.

[0040] The working principle of the present disclosure is described as follows:

[0041] A membrane separator is placed vertically for use; the membrane separator is provided with a condenser tube inside and a heating tube outside, and with a disperser at its top for dispersing a liquid, wherein the liquid naturally flows down along the inner wall of the heating tube by gravity to form a membrane, and liquid components with low boiling point which collected by the condenser at different stages are concentrated and liquid components with high boiling point which collected by the heating wall are concentrated;

[0042] the membrane separator is provided with high-purity product collection outlets O.sub.p1 and O.sub.pn and a residual liquid collection outlet O.sub.W, wherein the liquid collected from the outlets O.sub.p1 to O.sub.pn is a qualified product, and the residue liquid with high boiling point is collected from the collection outlet O.sub.w; a sample collection outlet is arranged on each of the collection outlets for sampling and analysis;

[0043] the membrane separator is provided with a number of fraction collection outlets O.sub.1 to O.sub.x at its different positions, wherein the liquid collected from the outlets O.sub.1 to O.sub.x contains more components with low boiling point;

[0044] the membrane separator is provided with a number of fraction collection outlets O.sub.x+1 to O.sub.x+n for collecting a mixed liquid, and the mixed liquid collected from the outlets O.sub.x+1 to O.sub.x+n is returned to a crude trimethylaluminum tank for subsequent separation.

[0045] Moreover, in the present disclosure, a continuous purifier is used to purify trimethylaluminum, making it possible to improve the production efficiency of the product and being easy for operation; once the purifier turns on normally, it could be carried out continuously. The trimethylaluminum product is purified in a sub-boiling state, specifically under the conditions of a low process temperature and in a state lowing than a boiling point. The liquid holdup is small during the purification process, which reduces safety risk and safety vulnerabilities.

[0046] The principle of the process of the present disclosure is not only limited to the purification of trimethylaluminum, but also suitable for the purification of various liquid compounds. According to the different physical properties of materials, it is only needed to change the temperature range of the hot medium and the cold medium used in the process.

[0047] It will be appreciated by those skilled in the art that changes could be made to the embodiment described above without departing from the broad inventive concept thereof. It is understood, therefore, that this invention is not limited to the particular embodiments disclosed, but it is intended to cover modifications within the spirit and scope of the present invention as defined by the appended claims.