Method for recovering titanium (halo) alkoxide from a waste liquid

A technology of alkoxide and alkoxide compound, which is applied in the field of recovering titanium (halogenated) alkoxide from waste liquid

Inactive Publication Date: 2019-03-01
CLARIANT INT LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Nevertheless, separation methods that rely on heat treatment have their inherent disadvantages from the standpoint of energy conservation and high equipment requirements

Method used

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  • Method for recovering titanium (halo) alkoxide from a waste liquid
  • Method for recovering titanium (halo) alkoxide from a waste liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 900 g of spent liquor 1 from the preparation of Ziegler-Natta catalysts for polypropylene production was subjected to figure 1 The method of the present invention is carried out in the process apparatus illustrated in . The effluent 1 contains about 89% by weight of TiCl 4 , 10% by weight of Ti chloroalkoxide compound and 0.5-1% by weight of diisobutyl phthalate (DiBP) as main components.

[0028] The hot waste liquid 1 leaving the reaction vessel is first cooled with a coolant in the outer cooling jacket of the longitudinally extending crystallizer (A). The temperature inside the crystallizer was maintained at about 10° C. and the spent liquor was continuously stirred at a rate of 400 rpm for 3 hours by a rotor rotating inside the cooling crystallizer. The resulting slurry 2 was then filtered through filter (B), and the isolated crystalline solid 3 was further washed by hexane and dried by gaseous nitrogen to obtain 62 g of white to light yellow crystals containing ...

Embodiment 2

[0031] For another 900 g of effluent from the same Ziegler-Natta catalyst production process, Example 1 was essentially repeated, except that the liquid residue (totalling about 30 g) is delivered back to the crystallizer (A), as figure 2 As shown in , for repeated cooling crystallization treatments under the same operating conditions: the internal temperature was maintained at 10 °C for 3 hours with continuous stirring at a constant rate of 400 rpm. After filtration through filter (B), washing with hexane and subsequent nitrogen drying, 8.2 g of white to pale yellow crystalline solid were obtained, composed of >90% by weight of ethoxylated titanium trichloride (TiCl 3 OC 2 h 5 ) and 4 Composition, as measured by gas chromatography.

Embodiment 3

[0033] 140 kg of spent liquor 1 from the preparation of Ziegler-Natta catalysts for polypropylene production was subjected to figure 1 The method of the present invention is carried out in the process apparatus illustrated in . The effluent 1 contains about 89% by weight of TiCl 4 , 10% by weight of Ti chloroalkoxide compound and 0.5-1% by weight of diisobutyl phthalate (DiBP) as main components.

[0034] The hot waste liquid 1 leaving the reaction vessel is first cooled with a coolant in the outer cooling jacket of the longitudinally extending crystallizer (A). The temperature inside the crystallizer was maintained at about -5°C and the waste liquor was continuously stirred at a rate of 100 rpm for 3 hours by a rotor rotating inside the cooling crystallizer. The resulting slurry 2 was then filtered through filter (B) and the isolated crystalline solid 3 was further washed by hexane and dried by gaseous nitrogen to obtain 4.5 kg of white to light yellow crystals containing ...

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Abstract

A method for separating one or more titanium (halo) alkoxides from a liquid mixture comprising titanium tetrachloride TiCl4 and at least one titanium (halo) alkoxide, said method comprising: agitatingand cooling the liquid mixture until crystallization of at least one titanium (halo) alkoxide occurs in the liquid mixture; separating the crystallized titanium (halo) alkoxide from the mixture; andoptionally, washing the separated, crystallized titanium (halo) alkoxide with a solvent.

Description

technical field [0001] The present invention relates to from containing titanium tetrachloride (TiCl 4 ) and at least one titanium (halo) alkoxide liquid mixture recovery of titanium (halo) alkoxide method. In particular said liquid mixture may result from the manufacture of titanium-based catalysts for the polymerization of olefins. More particularly, the spent liquor may contain additional components such as conventional electron donors, hydrocarbon solvents and additional chemical complexes formed by the titanium-based catalyst manufacturing process. Background technique [0002] In modern polyolefin production processes and especially for polypropylene production, titanium based Ziegler-Natta catalysts are commonly used. Methods for preparing such Ziegler-Natta catalysts have long been known in the art and are described in numerous patents, such as U.S. Patent Nos. 3,759,884, 3,993,588, and 4,728,705, each of which is incorporated herein by reference . Typically, the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/02C02F9/10B01D9/02
CPCB01D9/0013B01D9/0045B01D9/0059C01G23/024C07F7/28B01D3/10Y02W10/40B01D9/02C07B2200/13
Inventor 苏静郑仲平W·K·舒曼
Owner CLARIANT INT LTD
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