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Method for preparing decane dialdehyde intermediate

A technology of deca-carbon dialdehyde and intermediates, which is applied in the field of intermediates for the preparation of deca-carbon dialdehydes, and can solve problems such as low yield, environmental pollution, and equipment corrosion

Active Publication Date: 2020-11-17
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with other routes, the total yield of synthesis is improved, but the use of Lewis acid catalysts has certain pollution to the environment, and the requirements for equipment are also very high
[0009] In summary, in the method for synthesizing dedecenal intermediates, there are problems such as low yield, difficult recovery of catalysts, serious corrosion of equipment, etc.

Method used

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  • Method for preparing decane dialdehyde intermediate
  • Method for preparing decane dialdehyde intermediate
  • Method for preparing decane dialdehyde intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Preparation method of the present embodiment provides a decadialdehyde intermediate, such as process diagram figure 1 As shown, specifically includes the following steps:

[0055] (1) 130.1g 2,5- dimethoxy-2,5-dihydrofuran with 106.1g trimethyl orthoformate to give the mixed solution A, 1.3g of the catalyst I (activated carbon catalyst is ferric chloride) and 160.2 g of methanol were mixed to give solution B. The propenyl ether 133.9g, 267.7g toluene solution was mixed with solution D; 0.26g catalyst II (SO 4 2- -Tio 2 -Fe 3 O 4 Solid superacid catalyst) adsorbed and fixed in a microchannel.

[0056] (2) Step (1) Solution A and Solution B were obtained via a metering pump and a metering pump 2 to feed flow ratio of 1.2: entering a continuous flow microreactor (channel hydraulic diameter 0.3mm) 1, wherein the metering the flow rate of the pump 1 is 2.4ml / min, the flow rate of the metering pump 2 was 2ml / min, acetalization reaction is carried out at 50 ℃, the residence t...

Embodiment 2

[0067] (1) 104.1g 2,5- dimethoxy-2,5-dihydrofuran and 93.4g trimethyl orthoformate to give a mixed solution of A, and 3.1g of the catalyst I (ferric bromide activated carbon catalyst) and 76.9 g of methanol were mixed to give solution B. The propenyl ether 135.1g, 731.2g toluene solution was mixed with solution D; 0.41g catalyst II (SO 4 2- -Tio 2 -Al 2 O 3 Solid superacid catalyst) adsorbed and fixed in a microchannel.

[0068] (2) Step (1) Solution A and Solution B were obtained via a metering pump 2 and the metering pump 1 at a feed flow rate ratio of 2: 1 to enter a continuous flow microreactor (channel hydraulic diameter 0.5mm), wherein the metering the flow rate of the pump 1 is 2.4ml / min, the flow rate of the metering pump 2 is 1.2ml / min, acetalization reaction is carried out at 40 ℃, the residence time of the material in a continuous-flow micro-reactor is 85s, the resulting reaction solution stored in the storage tank 10 (e.g. figure 2 ) As shown, referred to as solut...

Embodiment 3

[0072] (1) 130.1g 2,5- dimethoxy-2,5-dihydrofuran and 95.5g trimethyl orthoformate to give a mixed solution of A, and 1.95g of the catalyst I (activated carbon catalyst is ferric chloride) and 160.2 g of methanol were mixed to give solution B. The propenyl ether 180.3g, 360.6g toluene solution was mixed with solution D; 0.18g catalyst II (SO 4 2- -Tio 2 -Fe 3 O 4 Solid superacid catalyst) adsorbed and fixed in a microchannel.

[0073] (2) Step (1) Solution A and Solution B were obtained via a metering pump and a metering pump 2 to feed flow ratio of 1.1: 1 to enter a continuous flow microreactor (channel hydraulic diameter 1mm), wherein the metering pump 1 is a flow rate 2.2ml / min, the flow rate of the metering pump 2 was 2ml / min, acetalization reaction is carried out at 10 ℃, the residence time of the material in a continuous-flow micro-reactor is 72s, the resulting reaction solution was stored at storage tank 10 (e.g. figure 2 ) As shown, referred to as solution C; sample f...

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Abstract

The invention relates to a method for preparing a decane dialdehyde intermediate in a continuous flow microsystem. The continuous flow microsystem comprises a first-stage continuous flow microreactorand a second-stage continuous flow microreactor, wherein a storage tank is arranged between the first-stage continuous flow microreactor and the second-stage continuous flow microreactor, and a filtersieve and a water absorption molecular sieve are arranged in the storage tank. According to the method for preparing the decane dialdehyde intermediate, by-products can be reduced, and the conversionrate and the yield are increased; and the continuous flow microsystem disclosed by the invention can be used for continuously carrying out two-step reaction in the preparation process of the decadialdehyde intermediate, so that the manual operation steps in the intermediate process are reduced.

Description

Technical field [0001] The present invention relates to the field of fine chemicals, particularly relates to a process for preparing a continuous flow microreactor decadialdehyde through an intermediate, wherein said intermediate decadialdehyde refers to the preparation of the aldehyde intermediate for two ten carbons. Background technique [0002] High market value of carotenoids, feed additives, food coloring agents, nutritional supplements and other wide applications. As my country's demand for increasing carotenoid synthesis pathway to develop a much-needed efficient and environmentally friendly. [0003] 2,7-dimethyl-2,4,6-octatriene-1,8-dialdehyde, decadialdehyde also known, it is a key intermediate in the synthesis of carotenoids in β- carotene, yellow angle synthetic pigment astaxanthin and other factors play a key role. 1,8-methoxy-1,3,6,8-tetramethoxy-2,7-dimethyl-4-octene is a key intermediate in the synthesis decadialdehyde process, to find effective prepared ten ways...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/54C07C43/315B01J27/128B01J27/053B01J19/00
CPCC07C41/54C07C41/50B01J27/128B01J27/053B01J19/0093C07C43/303C07C43/315
Inventor 王嘉辉张涛吕英东刘英瑞沈宏强杨宗龙潘亚男郭劲资李莉张弈宇宋军伟
Owner WANHUA CHEM GRP CO LTD