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Treatment method of titanium-containing waste solution

A treatment method and technology for titanium waste liquid, applied in chemical instruments and methods, water/sewage multi-stage treatment, water/sludge/sewage treatment, etc., can solve the problems of low waste liquid treatment efficiency and low recovery rate, etc. Facilitate separation and treatment, improve recovery rate, and increase the effect of precipitation

Active Publication Date: 2014-11-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to overcome either organic solvent and TiCl in the processing method of existing titanium-containing waste liquid 4 The recovery rate is low, or the shortcomings of waste liquid treatment efficiency are low, and 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

[0031] The titanium-containing waste liquid used in Example 1 and Comparative Examples 1-3 is the waste liquid produced in the process of preparing the solid component of the olefin polymerization catalyst according to the following steps: under nitrogen protection conditions, 450kg MgCl 2 2.6EtOH carrier and 1700L hexane were first mixed and pre-cooled to -20°C, and then added to 3300L of titanium tetrachloride that was also pre-cooled and cooled. After mixing for 3 hours, the temperature was raised to 110°C. During the heating process, at 20 Add 96kg internal electron donor (ester compound) at ℃, control the reaction pressure to 0.2MPa, and the reaction temperature to 110℃, carry out constant temperature reaction for 0.5h, and finally carry out standing, decanting, suction and pressure filtration to obtain titanium-containing waste liquid.

Embodiment 2

[0032] The titanium-containing waste liquid used in embodiment 2 is the waste liquid produced in the process of preparing the solid component of the olefin polymerization catalyst according to the following steps: under nitrogen protection conditions, 450kg MgCl 2 2.6EtOH carrier and 2400L hexane were first mixed and pre-cooled to -20°C, and then added to 2650L of titanium tetrachloride which was also pre-cooled and cooled. After mixing for 3 hours, the temperature was raised to 110°C. During the heating process, at 20 Add 96kg internal electron donor (ester compound) at ℃, control the reaction pressure to 0.2MPa, and the reaction temperature to 110℃, carry out constant temperature reaction for 0.5h, and finally carry out standing, decanting, suction and pressure filtration to obtain titanium-containing waste liquid.

Embodiment 3

[0033] The titanium-containing waste liquid used in embodiment 3 is the waste liquid produced in the process of preparing the solid component of the olefin polymerization catalyst according to the following steps: under nitrogen protection conditions, 450kg MgCl 2 2.6EtOH carrier and 1300L hexane were first mixed and pre-cooled to -20°C, and then added to 3700L of titanium tetrachloride that was also pre-cooled and cooled. After mixing for 3 hours, the temperature was raised to 110°C. During the heating process, at 20 Add 96kg internal electron donor (ester compound) at ℃, control the reaction pressure to 0.2MPa, and the reaction temperature to 110℃, carry out constant temperature reaction for 0.5h, and finally carry out standing, decanting, suction and pressure filtration to obtain titanium-containing waste liquid.

[0034] Example 1

[0035] Under nitrogen protection conditions, the titanium-containing waste liquid (titanium tetrachloride, chloroethoxytitanium in titanium te...

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Abstract

The invention provides a treatment method of a titanium-containing waste solution which contains titanium tetrachloride, an organic solvent and halogenated alkoxy titanium and / or ester-titanium complexes. The method includes following steps: performing a separation process to the titanium-containing waste solution for separating the organic solvent and the titanium tetrachloride to enable the organic solvent in a residual solution to account for 0-20% by weight of the residual solution; and successively performing a temperature-decreasing process and a solid-liquid separation process to the residual solution. By means of the method, recovery rates of the titanium tetrachloride and the organic solvent can be significantly increased. In addition, solid can be precipitated at a high temperature, thereby increasing a precipitation efficiency of solid impurities and effectively increasing waste solution treatment efficiency.

Description

technical field [0001] The invention relates to a treatment method for titanium-containing waste liquid. Background technique [0002] There are a number of methods for preparing Ziegler-Natta catalysts for olefin polymerization which generate large amounts of waste streams containing: unreacted TiCl 4 , also contains a certain amount of related by-products such as titanium alkoxide (halogen-containing), optional conventional electron donors such as aromatic and / or aliphatic (di)esters, glycol esters, diethers, etc. and optionally Solvents such as paraffins, and / or aromatics. For economic cost considerations, the TiCl 4 And some organic solvents need to be recovered and recycled. In addition, for environmental protection reasons, the waste liquid containing titanium tetrachloride is dangerous, because titanium tetrachloride will produce very corrosive HCl gas when it contacts with water, so the tetrachloride in the waste liquid should be recovered as much as possible. It...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/02C02F9/10
Inventor 刘萃莲高富堂秦金来郭正阳冯超王宇任春红王迎洪挺付梅艳雷世龙
Owner CHINA PETROLEUM & CHEM CORP
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