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Catalyst and preparation method of 2, 7-octadiene-1-ol

A catalyst and octadiene technology, which is applied in the preparation of organic compounds, chemical instruments and methods, and the preparation of hydroxyl compounds, can solve the problems of low activity, long reaction time, and large loss of active metals, and achieve high catalytic activity and high Reactivity, activity-enhancing effect

Pending Publication Date: 2022-07-08
HAIKE GRP RES INST OF INNOVATION & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be seen that in the existing 2,7-octadienol-1 synthetic route, there are homogeneous catalyzed preparation and recovery methods that are complicated, active metal loss is large, and the cost is high, while the technical scheme of heterogeneous catalysts, then There are problems of low activity, long reaction time and low production efficiency

Method used

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  • Catalyst and preparation method of 2, 7-octadiene-1-ol
  • Catalyst and preparation method of 2, 7-octadiene-1-ol
  • Catalyst and preparation method of 2, 7-octadiene-1-ol

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preparation example Construction

[0053] In the present invention, the preparation method of the catalyst preferably includes: in a protective atmosphere, the catalyst is obtained after the organic phosphorus ligand, the palladium salt and the solvent are mixed and reacted.

[0054]In the present invention, the catalyst is preferably a catalyst for temperature-controlled solid-liquid separation.

[0055] In the present invention, the catalyst preferably dissolves in a solvent system at a temperature above 70°C, and precipitates into a solid in the solvent system at 20°C to achieve solid-liquid separation.

[0056] The organophosphine ligands prepared by the present invention are characterized.

[0057] see figure 1 , figure 1 The nuclear magnetic H spectrum of the organophosphine ligand with the structure represented by formula (I) prepared in the present invention.

[0058] see figure 2 , figure 2 The nuclear magnetic H spectrum of the organophosphine ligand with the structure represented by formula (I...

Embodiment 1

[0097] Weigh 0.1 g of palladium acetate, 1.0 g of ligand A, and 50 g of sulfolane into a 250-ml reaction kettle, pass nitrogen gas, and react at 20° C. for 1 h. Subsequently, 30 g of sulfolane, 80 g of water, 30 g of butadiene, and 24 g of triethylamine were added, and carbon dioxide was introduced into the reactor to reach a pressure of 0.5 Mpa, and the reaction was carried out at 70° C. for 1 h. Wherein, ligand A is first prepared by radical reaction of 2.2-dimethylbiphenyl and N-bromosuccinimide to obtain 2.2-dibromomethylbiphenyl, and then reacted with diphenylphosphine under the catalysis of n-butyllithium Prepared by reaction at -70°C. Ligand B was prepared in the same manner as Ligand A by 3.3.5.5-Tetramethylbiphenyl.

[0098] After the reaction was completed, the temperature was lowered to room temperature, the catalyst was filtered, and the sample was analyzed by gas chromatography. The conversion rate of butadiene was 92.9%, and the selectivity of 2.7-octadien-1-ol ...

Embodiment 2

[0100] The preparation and evaluation of the catalyst were carried out according to the method of Example 1. The difference was that Ligand A was replaced with Ligand B. After the reaction was completed, the temperature was lowered to room temperature, the catalyst was filtered, and the sample was analyzed by gas chromatography. The conversion rate of butadiene was 98.9%. 2.7-Octadien-1-ol selectivity 98.1%.

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Abstract

The invention provides a catalyst. The catalyst comprises an organic phosphine ligand and palladium, the organic phosphine ligand has a structure as shown in a formula (I) and / or a formula (II). According to the catalyst prepared by taking the organic phosphine ligand as the carrier, the characteristic that the organic phosphine ligand is dissolved in a solvent at a high temperature is utilized, homogeneous catalysis is realized, relatively high catalytic activity is obtained, and solid-liquid separation of the catalyst after reaction is realized in a manner that the organic phosphine ligand is separated into a solid at a low temperature in the solvent, so that the loss of the catalyst is reduced. The homogeneous catalyst provided by the invention can be separated in a split-phase manner, the problem of cost increase caused by catalyst separation can be avoided, a specific ligand structure is taken as a carrier, the activity of active metal is improved by utilizing a unique electronic structure in the carrier, higher reaction activity is achieved, and higher yield is obtained.

Description

Technical field [0001] The invention belongs to the technical field of preparation of 2,7-octadien-1-ol, and relates to a catalyst and a preparation method of 2,7-octadien-1-ol. Background technique [0002] The synthesis process of n-octanol includes natural fatty alcohol process, Ziegler alcohol process, 1-heptene OXO process, butadiene telomerization process, bio-based route, 1-octene epoxy hydrogenation process, etc., among which The telomerization of butadiene to prepare 2,7-octadienol-1, and the subsequent hydrogenation of 2,7-octadienol-1 to prepare 1-octanol are traditional synthesis routes, and this process is also used in existing industrial production. Technical solution, but using a homogeneous catalyst in this process has the problems of difficulty in catalyst reuse and low recovery rate, resulting in high catalyst cost. For example, in the existing technology, there are also technical solutions for using palladium catalysts with water-soluble ligands, and Afte...

Claims

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Application Information

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IPC IPC(8): B01J31/24C07C29/36C07C33/02
CPCB01J31/2409C07C29/36B01J2531/824B01J2531/0241B01J2231/20C07C33/02Y02P20/584
Inventor 赵兴涛修阳宋现成赵立伟姜鹏马俊青
Owner HAIKE GRP RES INST OF INNOVATION & TECH
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