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Treatment method for titanium-containing waste liquid generated in production process of polyolefin catalyst

A polyolefin catalyst and production process technology, applied in chemical instruments and methods, titanium halides, titanium tetrachloride, etc., can solve problems such as high cost, difficult waste liquid treatment, VOC emissions, etc.

Pending Publication Date: 2021-01-19
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The object of the invention is to overcome the organic solvent and TiCl in the processing method of existing titanium-containing waste liquid 4 The recovery rate is low, and the waste liquid treatment is difficult, the cost is high, and there is a problem of VOC emissions. A new treatment method for titanium-containing waste liquid is provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Recycling and treatment of titanium-containing waste liquid A

[0058] Step 1: Add 250 g of titanium-containing waste liquid A into a 500 ml four-necked bottle equipped with mechanical stirring, and keep the stirring rate at 200-300 rpm. Cool to 0°C within 1 hour. Hold at this temperature for 1 hour. Suction. Wash twice with 50 mL of hexane. The solid was transferred to 30 mL of hexane and sucked dry. Obtained 26.0 g of light yellow solid powder with a titanium content of 22.5% and an ethoxy content of 23.0%.

[0059] Step 2: Distill the filtrate under reduced pressure (adjust the degree of vacuum and control the kettle temperature to 90° C.) to recover 120 g of hexane and titanium tetrachloride, wherein titanium tetrachloride accounts for 26% wt. The first recovery of titanium tetrachloride accounts for 29.0% of the total amount of titanium tetrachloride in the titanium-containing waste liquid.

[0060] Analysis of organic impurities in recovered hexane and titan...

Embodiment 2

[0066] Recycling and treatment of titanium-containing waste liquid A

[0067]Step 1: Add 250 g of titanium-containing waste liquid A into a 500 ml four-necked bottle equipped with mechanical stirring, and keep the stirring rate at 200-300 rpm. Cool to -15 to -10°C within 1 hour. Hold at this temperature for 1 hour. Suction. Wash twice with 50 mL of hexane. The solid was transferred to 30 mL of hexane and sucked dry. 38.0 g of light yellow solid powder with a titanium content of 22.5% and an ethoxy content of 23.0% was obtained.

[0068] Step 2: Distill the filtrate under reduced pressure (adjust the degree of vacuum and control the kettle temperature to 90° C.) to recover 160 g of hexane and titanium tetrachloride, wherein titanium tetrachloride accounts for 43 wt%. The first recovery of titanium tetrachloride accounts for 64% of the total amount of titanium tetrachloride in the titanium-containing waste liquid.

[0069] Analysis of organic impurities in recovered hexane...

Embodiment 3

[0075] Recycling and treatment of titanium-containing waste liquid B

[0076] Step 1: Add 250 g of titanium-containing waste solution B into a 500 ml four-necked bottle equipped with mechanical stirring, and keep the stirring rate at 200-300 rpm. Cool to 0°C within 1 hour. Hold at this temperature for 1 hour. Suction. Wash twice with 50 mL of hexane. The solid was transferred to 30 mL of hexane and sucked dry. 11.0 g of light yellow solid powder was obtained, the titanium content was 22.5%, and the ethoxy content was 23.0%.

[0077] Step 2: Distill the filtrate under reduced pressure (adjust the degree of vacuum and control the kettle temperature to 90° C.) to recover 90 g of hexane and titanium tetrachloride, of which titanium tetrachloride accounts for 56 wt%. The first recovery of titanium tetrachloride accounts for 31% of the total amount of titanium tetrachloride in the titanium-containing waste liquid.

[0078] Analysis of organic impurities in recovered hexane and...

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Abstract

The invention relates to a recycling treatment method for titanium-containing waste liquid generated in the production process of a polyolefin catalyst. The method comprises the steps: S1, carrying out primary cooling and primary solid-liquid separation on the titanium-containing waste liquid; S2, carrying out primary reduced pressure distillation on the first liquid obtained in the step S1; S3, carrying out secondary cooling and secondary solid-liquid separation on the residual first liquid obtained in the step S2; and S4, carrying out secondary reduced pressure distillation on the second liquid obtained in the step S3. By using the method disclosed by the invention, titanium tetrachloride and an organic solvent in the titanium-containing waste liquid can be recycled to the maximum extent, the content of generated organic impurities is greatly reduced, and the possibility of coking of a tower kettle is reduced, so that the treatment difficulty of tower kettle residual liquid and the environmental protection problem caused by the treatment difficulty are reduced; and titanium resources and organic matters in the residual liquid can be better recycled.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for recycling and treating titanium-containing waste liquid produced in the production process of polyolefin catalysts. Background technique [0002] There are many methods for preparing Ziegler-Natta catalysts for olefin polymerization. The common method of industrial use is: suspension or solution of magnesium compound and excess titanium tetrachloride (TiCl 4 ) reaction, and reaction treatment such as mixing with an internal electron donor, and separating to obtain the corresponding solid catalyst component. This will produce a large amount of filtrate containing the following components: organic solvents such as (halogenated) alkanes or (halogenated) aromatics organic solvents, unreacted TiCl 4 , related by-products such as alkoxy titanium halides, a small amount of unreacted electron donors such as aromatic and / or aliphatic (di)esters, glycol esters, diethers, etc...

Claims

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Application Information

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IPC IPC(8): C01G23/02C07C7/00C07C7/04C07C9/15C07C15/06
CPCC01G23/024C07C7/005C07C7/04C07C9/15C07C15/06
Inventor 周奇龙谭忠周俊领徐秀东张锐于金华尹珊珊宋维玮李凤奎
Owner CHINA PETROLEUM & CHEM CORP
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