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Method for reclaiming and purifying titanium tetrachloride for preparing olefin polymerization catalysts

A technology of titanium tetrachloride and olefin polymerization, applied in the direction of titanium halide, etc., can solve the problems of low recovery rate of titanium tetrachloride, complicated process, inconvenient operation, etc., and achieve simplified impurity removal and purification process, high purity, The effect of reducing production costs

Inactive Publication Date: 2010-06-02
LIAONING DINGJIDE PETROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages are: one, this method needs rough steaming and rectification, the process is cumbersome and inconvenient to operate
Second, due to the process of rectification, heat exchange is required and energy consumption is high
The 3rd, the recovery rate of titanium tetrachloride is low, and loss is bigger

Method used

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  • Method for reclaiming and purifying titanium tetrachloride for preparing olefin polymerization catalysts
  • Method for reclaiming and purifying titanium tetrachloride for preparing olefin polymerization catalysts

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Such as figure 1 Shown, a kind of recovery purification device of titanium tetrachloride that prepares olefin polymerization catalyst: comprise intermediate storage tank I (1), pre-cooling still (2), cryogenic still (7) and intermediate storage tank II (8), Intermediate storage tank I (1), pre-cooling kettle (2), deep-cooling kettle (7) and intermediate storage tank II (8) are connected by pipelines; pre-cooling kettle (2) is provided with stirring blade I (3 ), the pre-cooling kettle (2) is provided with a water jacket (4); the cryogenic kettle (7) is provided with a stirring paddle II (5), and the cryogenic kettle (7) is provided with a refrigerant jacket (6).

[0020] The recovery and purification method of titanium tetrachloride for preparing olefin polymerization catalyst is as follows:

[0021] 1) Pretreatment: Add the titanium tetrachloride mother liquor produced during the preparation of the olefin polymerization catalyst into the intermediate storage tank I (1...

Embodiment 2

[0026] The recovery and purification device is the same as in Example 1.

[0027] The recovery and purification method of titanium tetrachloride for preparing olefin polymerization catalyst is as follows:

[0028] 1) Pretreatment: Add the titanium tetrachloride mother liquor produced during the preparation of the olefin polymerization catalyst into the intermediate storage tank I (1), and then enter the pre-cooling tank (2) through the pipeline, and the pre-cooling water at about 30°C passes through the water inlet (11) enter in the water jacket (4), circulate through the water outlet (12), stir, and the stirring speed is 100~300 rpm;

[0029] 2) Cold analysis and sedimentation: Transfer the pretreated titanium tetrachloride mother liquor into the cryogenic kettle (7), Freon at -35°C enters the refrigerant jacket (6) through the refrigerant medium inlet (9), and passes through the refrigerant medium (10) Carry out circulation, make the temperature of titanium tetrachloride mo...

Embodiment 3

[0033] The recovery and purification device is the same as in Example 1.

[0034] The recovery and purification method of titanium tetrachloride for preparing olefin polymerization catalyst is as follows:

[0035] 1) Pretreatment: Add the titanium tetrachloride mother liquor produced during the preparation of the olefin polymerization catalyst into the intermediate storage tank (1), water at about 10°C enters the water jacket (4) through the water inlet (11), and passes through the water Outlet (12) is circulated, stirred, and the stirring speed is 100~300 revs / min;

[0036] 2) Cold analysis and sedimentation: Transfer the pretreated titanium tetrachloride mother liquor into the cryogenic kettle (7), and the frozen brine at about -5°C enters the refrigerant jacket (6) through the refrigerant medium inlet (9), and passes through The refrigerant medium outlet (10) is circulated to gradually reduce the temperature of the titanium tetrachloride mother liquor to between 0°C and -5...

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Abstract

The invention relates to a method for reclaiming and purifying titanium tetrachloride for preparing olefin polymerization catalysts. The adopted technical scheme comprises the following steps of: adding a titanium tetrachloride mother solution produced in the preparation process of the olefin polymerization catalysts to an intermediate storage tank I; introducing circulating water with the temperature of 10 DEG C to 30 DEG C to a water jacket for stirring, wherein the stirring rotation speed is 100 to 300 rpm; transferring pretreated titanium tetrachloride mother solution to a cryogenic kettle; introducing refrigerant medium with the temperature of 5 DEG C below zero to 35 DEG C below zero to a refrigerant jacket; gradually reducing the temperature of the titanium tetrachloride mother solution to be between 0 DEG C and 25 DEG C below zero; controlling the stirring rotation speed to be 10 to 150 rpm; carrying out cold separation and settlement for 2 to 12 hours under stirring; and separating a supernatant and crystallinesubstance in the titanium tetrachloride mother solution, and transferring the supernatant to an intermediate storage tank II through a pipeline. The invention has simple process, low energy consumption and high recovery ratio, and is environment friendly.

Description

technical field [0001] The invention relates to a method for recovering and purifying titanium tetrachloride, in particular to a method for recovering and purifying excess titanium tetrachloride used in the production of olefin polymerization catalysts by adopting a low-temperature cold crystallization method. Background technique [0002] The ZIELER-NATLA catalyst system is used to prepare the olefin polymerization catalyst, which is composed of magnesium chloride as the carrier, titanium tetrachloride as the active substance, and internal and external electron donors. In the process of preparing the above catalyst, in the steps of dealcoholization activation and titanium loading, it is necessary to process solid alkoxymagnesium and chloroalkoxymagnesium with excessive titanium tetrachloride, and the by-product (alkoxytitanium) also needs An excess of titanium tetrachloride is used as solvent, so that excess titanium tetrachloride is removed during the treatment and subsequ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/02
Inventor 张再明
Owner LIAONING DINGJIDE PETROCHEM
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