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Method for purifying non-metallic impurities in titanium-containing filtrate

A non-metallic impurity and filtrate technology, which is applied in the field of polyolefin catalysts, can solve the problems of unsatisfactory tetrahalide recovery, removal, and complicated treatment process, and achieve obvious environmental protection and economic benefits and reduce consumption.

Active Publication Date: 2021-11-12
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

One problem with this process is that a large amount of waste acid slag containing various organic substances is produced during the hydrolysis process, which requires further treatment, so it faces increasingly serious environmental and economic pressures
[0007] Although the above-mentioned first method reduces the generation of acid water to a certain extent, the resulting solid waste contains a large amount of organic matter, which obviously requires further subsequent treatment, and the treatment process is complicated.
The second method, although the recovery rate of titanium tetrachloride is improved, but at high temperature, oily lumps are formed in the waste liquid, which affects the subsequent evaporation process
In the third method, although the conditions such as the temperature of the thin-film evaporator are optimized, the problem of high-temperature coking of the material is solved, but the impurities are not effectively removed, and the recovery rate of tetrahalides is still not ideal.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] 1) First use nitrogen to replace the thin film evaporator kit, add 500 ml of titanium titanium-containing filtrate to the measuring bottle; open the vacuum pump to vacuum, adjust the vacuum valve, control the relative vacuum of the thin film evaporator in -50 kPa; to the thin film evaporator Heating oil is passed into a heat oil and gradually warmed to 110 ° C; open the feed valve, add the titanium-containing filtrate to the thin film evaporator, the scraper rotor speed is constant, and the titanium-containing filtrate is dispersed into a film (the liquid film thickness is 1 cm, residence time In 2 minutes), the distillate of the evaporator was collected to obtain a titanium distillate.

[0074] 2) 250 ml of hexanes and 30 ml of ethanol were added to a 500 ml glass reactor with mechanical stirring, reflow condensate and nitrogen protection, and gradually added 50 ml of titanium-containing distillation liquid with stirring, stirred at room temperature for 2 h, and the mixtur...

Embodiment 2

[0076] 1) First use nitrogen to replace the thin film evaporator kit, add 500 ml of titanium titanium-containing filtrate into the metering bottle; open the vacuum pump to vacuum, adjust the vacuum valve, control the relative vacuum of the thin film evaporator in -70KPa; Encaps of hot oil and gradually warmed to 100 ° C; open the feed valve, add titanium-containing filtrate to the thin film evaporator, the scraper rotor speed is constant, and the titanium-containing filtrate is dispersed into a film (the liquid film thickness is 1 cm, residence time For 3 minutes), the distillate of the evaporator was collected to obtain a titanium distillation.

[0077] 2) 200 ml of hexanes and 30 ml of ethanol were added to a 500 ml glass reactor with mechanical stirring, reflow condensate and nitrogen protection, and gradually added 50 ml of titanium-containing distillation liquid with stirring, stir mixed with stirring at room temperature. The mixture can be seen that a black oil mixture appea...

Embodiment 3

[0079] 1) First use nitrogen to replace the thin film evaporator kit, add 500 ml of titanium titanium-containing filtrate into the metering bottle; open the vacuum pump to vacuum, adjust the vacuum valve, control the relative vacuum of the thin film evaporator in -85KPa; to the thin film evaporator Entering hot oil and gradually warmed to 90 ° C; open the feed valve, add the titanium-containing filtrate to the thin film evaporator, the scraper rotor speed is constant, and the titanium-containing filtrate is dispersed into a film (the liquid film thickness is 1 cm, residence time For 4 minutes), the discharged distillate of the evaporator was collected to obtain a titanium distillate.

[0080]2) added to a 500mL glass reactor with mechanical stirring, reflux condenser and nitrogen blanket, a titanium-containing 50ml of distillate was gradually added with stirring 20ml of ethanol and 150ml of hexane, stirring and mixing at room temperature 2h, after the reaction to give dark gray Th...

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Abstract

The invention relates to the field of polyolefin catalysts, and discloses a method for purifying non-metallic impurities in titanium-containing filtrate. The method comprises the following steps: 1) evaporating the titanium-containing filtrate through a film evaporator to obtain titanium-containing distillate; 2) mixing the titanium-containing distillate with an alcohol organic solvent and an inert organic solvent to obtain a mixture of the titanium-containing distillate; 3) standing and layering the mixture, and carrying out liquid-liquid separation on the oily mixture at the lower layer and the supernate; and (4) carrying out distillation separation on the supernate to obtain titanium tetrachloride and an organic solvent, wherein the titanium-containing filtrate is one or a mixture of two or more of mother liquor and titanium treating fluid generated in the ethylene polymerization catalyst preparation process. According to the method, the utilization rate of the raw materials is obviously increased, waste acid residues generated in the treatment process are greatly reduced, non-metal impurities in the filtrate are effectively removed, and the recovery rate of titanium tetrachloride in the titanium-containing distillate is greatly increased.

Description

Technical field [0001] The present invention relates to polyolefin catalysts, and in particular relates to a method for purifying titanium-containing non-metallic impurities in the filtrate. Background technique [0002] In the industrial production of polyolefins, the titanium catalyst due to the high catalytic efficiency and inexpensive to obtain a more widely used. At present a common method for preparing such a catalyst is firstly prepared which is dissolved magnesium, such as magnesium or a magnesium compound by uniformly dispersed in one or more solvents, the further addition of magnesium was prepared under the action of organic builders lysate and phosphorus-containing solution by dissolving magnesium and a halogen-containing compound such as titanium tetrachloride is prepared by reacting magnesium or a magnesium compound as the main structure of the catalyst, during which accelerator may be added for a variety of improved performance, these accelerators , silicon element....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/02
CPCC01G23/024C01G23/001
Inventor 杜宏斌包满祝平李红卫张祥安孙晓薇于连杰甘放遗
Owner CHINA PETROLEUM & CHEM CORP