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A kind of method that sodium dichromate oxidation prepares hexanal

A technology of sodium dichromate and oxidizing solution, which is applied in the direction of oxidative preparation of carbonyl compounds, carboxylate esters, carbon-based compounds, etc., can solve the problems of limited application, achieve simple methods, low equipment requirements, and save costs Effect

Active Publication Date: 2019-03-19
ZITONG HUIQUAN PERFUME CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above processes have high requirements on the type, quality and loading mode of the catalyst, which limits its industrial application

Method used

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  • A kind of method that sodium dichromate oxidation prepares hexanal

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Experimental program
Comparison scheme
Effect test

Embodiment 1. preparation approach preparation example 1

[0022] 1. Preparation of reaction solution and oxidation solution:

[0023] In a 2000mL distillation apparatus with stirring, put 170g of n-hexanol, 0.5g of manganese sulfate, 30g of water, and heat in a negative pressure (P=-0.09MPa) oil bath;

[0024] Preparation of oxidizing solution: 150g of sodium dichromate, 200g of sulfuric acid, and 860g of water for later use.

[0025] 2. Oxidation reaction and fractionation products:

[0026] Taking Beijing time sequence operation as an example, other time and sequence can refer to the following time and sequence:

[0027] 8:30 The material liquid is boiling, the column temperature is 58 degrees, the oil bath is 80 degrees, and the oxidation solution is started to be added dropwise

[0028] 8:46 The column temperature is 67 degrees, the oil bath is 83 degrees, and the material liquid is evaporated, (oil-water azeotrope)

[0029] 8:52 The column temperature is 68 degrees, the oil bath is 84 degrees, the material is discharged norma...

Embodiment 2. preparation approach preparation example 2

[0039] 1. Preparation and preparation of reaction solution and oxidation solution: see Example 1

[0040] 2. Oxidation reaction and fractionation products:

[0041] 1) When the internal temperature of the fractionation device reaches 60 degrees, the water pump depressurizes, the reaction solution boils, and the oxidizing solution is added dropwise, and the resulting product is continuously distilled; keep a stable distillation within one hour, and continuously increase the temperature of the oil bath;

[0042] 2), when the column temperature is 74 degrees, add 1 / 2 of the oxidation solution;

[0043] 3), bubbles appear in the reaction solution after adding, and the column temperature is 78 degrees, continue to distill the remaining oxides under reduced pressure until there is no more oily matter;

[0044] 4), no change after this, when the foam disappears, the column temperature is 80 degrees, and the oil bath is 99 degrees, the reaction stops.

[0045] In the distillate, 50%...

Embodiment 3. preparation approach preparation example 3

[0047] 1. Preparation and preparation of reaction solution and oxidation solution: see Example 1

[0048] 2. Oxidation reaction and fractionation product steps:

[0049] 1), when the column temperature is 58 degrees, the oil bath is 80 degrees, the reaction solution is boiling, add chromic acid dropwise, and continue to heat up;

[0050] 2) When the column temperature is 79 degrees and the oil bath is 98 degrees, after adding the oxidizing solution, reduce the pressure and distill;

[0051] 3), distillation, wherein the organic layer is analyzed by chromatography: hexanal 51.1%, hexanol 42.5%;

[0052] 4), continue to distill under reduced pressure, the organic layer that distillates is analyzed by chromatography: hexanal: 22.4%, hexanol 22%

[0053]5), continue vacuum distillation, the organic layer product after distilling is few, is the high-boiling point impurity; The water layer is merged and heated up azeotropic distillation, and goes out fraction No. 1 and No. 2.

[...

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Abstract

The invention provides a preparation method of n-hexyl aldehyde by sodium dichromate oxidation of n-hexyl alcohol. The method comprises the following steps: 1) adding n-hexyl alcohol in a reaction device; 2) controlling the reaction temperature, and adding a sodium dichromate oxidation liquid; and 3) distilling and collecting a product n-hexyl aldehyde, and collecting unreacted n-hexyl alcohol, a by-product of hexyl hexanoate and chromium-containing sulfate from the reaction bed material by an extraction layering method. The product obtained by the preparation method of n-hexyl aldehyde by sodium dichromate oxidation of n-hexyl alcohol does not contain chlorine, and is more advanced compared to the prior art.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for preparing n-hexanal by oxidizing n-hexanol with sodium dichromate. Background technique [0002] N-hexanal is an intermediate in the synthesis of perfumes. The process of preparing n-hexanal from n-hexanol can produce high economic added value, so the research on this process is of great significance. The process of preparing n-hexanal from n-hexanol is divided into two processes: catalytic oxidation method and catalytic dehydrogenation method. For example, "Preparation of n-hexanal by Catalytic Oxidation of n-Hexanol" (Lin Shuqin et al., 2011) describes the process of synthesis of n-hexanal by gas-solid phase catalytic oxidation of n-hexanol using air as oxidant and supported copper oxide as catalyst. For the main catalyst , co-catalyst, and catalyst carrier were screened, and the influence of process conditions such as reaction temperature, liquid-air...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/29C07C45/78C07C45/82C07C47/02C07C29/86C07C31/125C07C67/08C07C67/58C07C69/24C01G37/08
CPCC01G37/08C07C29/86C07C45/292C07C45/78C07C45/82C07C67/08C07C67/58C07C47/02C07C31/125C07C69/24
Inventor 钟利明
Owner ZITONG HUIQUAN PERFUME CHEM