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Method for separating reaction mixtures and recycling of quaternary salts and bases

A technology of reaction mixtures and mixtures, applied in chemical instruments and methods, preparation of organic compounds, catalytic reactions, etc.

Inactive Publication Date: 2005-05-25
BAYER MATERIALSCIENCE AG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the method here also does not directly address the reusable products A, B and D

Method used

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  • Method for separating reaction mixtures and recycling of quaternary salts and bases
  • Method for separating reaction mixtures and recycling of quaternary salts and bases
  • Method for separating reaction mixtures and recycling of quaternary salts and bases

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0139] 5432 g of the reaction solution from the oxidative direct carbonylation process were extracted at 80°C with 33 ml of a 48% HBr solution in 543 g of water. 556.2 g of aqueous extract are obtained. Table 1 gives the composition of the solution after the single-step extraction.

[0140] mn

Embodiment 2

[0142] 200 g of 4% by weight tetrabutylammonium bromide, 4% by weight tetrabutylammonium phenate, 6% by weight phenol, 20 A solution of wt % DPC and 66 wt % chlorobenzene was used for extraction. The aqueous phases were then combined. Table 2 gives the composition of the solution.

Embodiment 3

[0147] A mixture of 50 g tetraphenylphosphonium bromide, 60 g chlorobenzene, 40 g phenol and 100 g diphenyl carbonate was distilled on a 5 cm high column packed with Rasching rings. Initially, the system was operated at a vacuum of 200 mbar until the temperature of the bottom of the column rose to about 180°C, then the vacuum was reduced to about 20 mbar and distillation was continued until the maximum temperature of the bottom of the column was about 200°C. The total amount of compound found in the distillate was calculated by adding the compositions of the fractions. 69.1 g of material from the reaction remained at the bottom of the column. The results are shown in Table 3.

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Abstract

The present invention relates to a process for the separation and recycling of catalyst components of a chemical reaction mixture involving oxidative direct carbonylation.

Description

technical field [0001] The present invention provides a method for the separation and recycling of catalyst components present in a chemical reaction mixture from oxidative direct carbonylation. Background technique [0002] During the oxidative direct carbonylation of aromatic hydroxy compounds in the presence of CO, O 2 An inert metal catalyst, preferably palladium, and typically an inorganic co-catalyst (such as manganate, or cobalt salt), base, quaternary salt, various organic co-catalysts (such as quinone or hydroquinone), and a drying agent (See eg DE-OS 27 38 437, US-A 4 349 485, US-A 5 231 210, EP-A 667 336, EP-A 858 991, US-A 5 760 272). This process can be performed in a solvent. [0003] After carrying out the reactions, product mixtures are obtained from these reactions, which in particular comprise one or more quaternary salts A, hydroxyaromatic compounds B, reaction products C such as for example water and diaryl carbonates, bases D (including deprotonation ...

Claims

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Application Information

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IPC IPC(8): B01J31/32B01J31/40B01J38/00B01J38/48C07C37/72C07C37/74C07C68/08C07C69/96C07C277/06C07C279/04
CPCB01J31/0214B01J31/0215B01J31/0235B01J31/0239B01J31/0268B01J31/26B01J31/28B01J31/4015B01J31/4053B01J38/48B01J2231/34C07C37/72C07C37/74C07C68/08Y02P20/10Y02P20/52Y02P20/584C07C69/96C07C39/04C07C277/06C07F9/02
Inventor P·菲舍尔S·M·汉森C·-P·赖辛格尔
Owner BAYER MATERIALSCIENCE AG
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