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Separation process of substituted benzaldehyde co-produced products

A production process and technology of deionized water, applied in the separation/purification of carboxylic acid compounds, separation/purification of carbonyl compounds, organic chemistry, etc. The effect of wastewater

Inactive Publication Date: 2013-11-27
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The separation process of this process is complicated, and a considerable amount of high-concentration wastewater containing sodium sulfate is produced

Method used

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  • Separation process of substituted benzaldehyde co-produced products
  • Separation process of substituted benzaldehyde co-produced products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] In a 1000mL flask, add 675mL of p-tert-butyltoluene oxidation feed solution; rectify to remove acetic acid, add water twice to wash off the catalyst in total of 300mL.

[0015] The organic phase after water washing is transferred to a 1000mL three-neck flask with stirring and heating mantle heating, heated to 95°C, and 0.2MPa saturated water vapor is introduced for stripping, and the mixed steam after stripping is sent to the middle end of the fractionation column, and the fractionation column There is a fractionation column bottom bottle at the bottom, and the mixed steam is partially condensed in the fractionation column, and the condensate contacts the steam that continues to rise on the way down, and the two perform heat exchange, and the p-tert-butylbenzaldehyde and p-tert-butyltoluene with high boiling points in the vapor are absorbed Condensation, the water vapor with low boiling point still rises as steam, while the low boiling point components in the condensate ...

Embodiment 2

[0019] In a 1000mL flask, add 675mL of p-tert-butyltoluene oxidation feed solution; rectify to remove acetic acid, add water twice to wash off the catalyst in total of 300mL.

[0020] The organic phase after water washing was transferred to a 1000mL three-necked flask with stirring and heating mantle heating, heated to 95°C, and 0.2MPa nitrogen gas was introduced for stripping, and the mixed steam after stripping was sent to the middle end of the fractionation column. In the bottom bottle of the fractionating column, the mixed vapor is partially condensed in the fractionating column, and the condensate contacts the steam that continues to rise during the descent, and the two perform heat exchange, and p-tert-butylbenzaldehyde and p-tert-butyltoluene with high boiling points in the vapor are condensed, The nitrogen with low boiling point still rises as a vapor, while the low boiling point components in the condensate are heated and vaporized, and the high boiling point component...

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Abstract

The invention discloses a separation process after synthesis of p-tertbutyl benzaldehyde (co-produced p-tertbutyl benzaldehyde). The separation process comprises the steps: rectifying an oxidization feed liquid to remove acetic acid, and washing with water to remove a catalyst; heating a washed organic phase to 95-100 DEG C, introducing saturated vapor or nitrogen, stripping, carrying out fractionation under reduced pressure, for separating vapor or nitrogen, p-tertbutyl benzaldehyde and p-tert-butyltoluene, cooling stripped residual liquid and then extracting by using methylbenzene, distilling the p-tertbutyl benzaldehyde after the methylbenzene is recovered, and then recrystallizing the methylbenzene. According to the separation process, the process step is reduced, and sodium sulfate-containing wastewater is prevented from producing.

Description

technical field [0001] The invention relates to a method for oxidizing substituted toluene and coproducing substituted benzaldehyde and substituted benzoic acid. Background technique [0002] Use p-tert-butyltoluene as raw material to synthesize p-tert-butylbenzaldehyde (co-production of p-tert-butylbenzoic acid), the process includes oxidation reaction, distillation to remove acetic acid, washing with water and alkali, separation of p-tert-butylbenzoic acid , rectification and separation of p-tert-butylbenzaldehyde and other steps. [0003] After a sufficient amount of p-tert-butyltoluene is acidified with acetic acid, a catalyst is added, and oxygen is passed through at a certain temperature for oxidation reaction to generate p-tert-butylbenzaldehyde and p-tert-butylbenzoic acid. The oxidized feed solution is distilled to remove acetic acid, washed to remove the catalyst, and then washed with sodium carbonate alkali to separate the generated p-tert-butylbenzoic acid into ...

Claims

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Application Information

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IPC IPC(8): C07C47/542C07C45/78C07C45/82C07C63/04C07C51/42C07C51/44
Inventor 赵玉明王利超马堂文
Owner NANJING UNIV
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