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Preparation method of diether type electron donor

A technology of electron donor and diether, which is applied in the field of preparation of diether electron donor, can solve the problems of high preparation cost and low total yield, and achieve the effects of reducing preparation cost, increasing total yield and improving efficiency

Inactive Publication Date: 2012-05-02
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
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  • Claims
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AI Technical Summary

Problems solved by technology

[0009] The invention provides a method for preparing a diether-type electron donor, which is used to solve the problems of high preparation cost and low synthesis yield in the prior art

Method used

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Examples

Experimental program
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Embodiment 1

[0035] 1. Preparation of 2-isopropyl-5-methyl-2-hexenal

[0036] In a 1000ml stainless steel pressure reactor with stirring, add 750g the mixture that is made up of 3-methylbutyraldehyde and water, the addition ratio 3-methylbutanal:H 2 O is 4:3 (mass ratio, the same below). Stirring with N 2 After the replacement, the temperature was raised to 130°C. use N 2 50 g of 7.5% NaOH aqueous solution was pressed in to start the reaction. During the process, the reaction temperature is 130°C, the reaction pressure is 0.5MPa, and the reaction time is 35 minutes. After the reaction, the water layer is separated, and part of the unreacted raw materials and by-products are removed by distillation, and the resulting product 2-isopropyl-5-methanol Base-2-hexenal, the content of GC analysis is >96%, and the product yield is 94.2%.

[0037] 2. Preparation of 2-isopropyl-5-methylhexanal

[0038] Add 2-isopropyl-5-methyl-2-hexenal 220g and ethanol 440g obtained by step 1 in a 1000ml stain...

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Abstract

The invention discloses a preparation method of a diether type electron donor. The method comprises the following steps: 1, carrying out a condensation reaction on 3-methylbutyraldehyde under a preset reaction pressure with an aqueous solution of NaOH as a catalyst to obtain 2-isopropyl-5-methyl-2-hexenal; 2, carrying out a reduction reaction on 2-isopropyl-5-methyl-2-hexenal obtained in step 1 and H2 under the action of a Pd / C catalyst to obtain 2-isopropyl-5-methylhexanal; 3, reacting 2-isopropyl-5-methylhexanal obtained in step 2 with an aqueous solution of formaldehyde under the action of an inorganic alkali to obtain 2-isopropyl-2-isopentyl-1,3-propanediol; and 4, dissolving 2-isopropyl-2-isopentyl-1,3-propanediol in an organic solvent, and carrying out an etherification reaction on 2-isopropyl-2-isopentyl-1,3-propanediol and CH3Cl in the presence of the alkali to obtain 2-isopropyl-2-isopentyl-1,3-dimethoxypropane. By utilizing NaOH / H2O as the catalyst in the invention, technological conditions are optimized, the preparation cost is reduced, the total product yield is improved, and the efficiency is substantially improved.

Description

technical field [0001] The invention relates to the technical field of diether organic compounds, in particular to a preparation method of a diether electron donor. Background technique [0002] 2-Isopropyl-2-isopentyl-1,3-dimethoxypropane is a diether type compound. Many literatures have introduced that the use of this compound as an electron donor for olefin polymerization catalysts can obtain excellent catalytic performance. But there are few reports about the synthesis method of this compound, especially the method of mass production. [0003] In the prior art, it relates to a kind of synthetic method of 2-isopropyl-2-isoamyl-1,3-dimethoxypropane, which takes isovaleraldehyde as the initial raw material through four-step chemical reactions and multiple The target product is obtained in the step of intermediate treatment, the total yield of this method is very low, and some more expensive raw materials are used in the middle. [0004] In response to the shortcomings of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/10C07C41/01
Inventor 冯静郭浩然王红红朱丽琴
Owner CHINA PETROLEUM & CHEM CORP
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