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Preparation method of 1,5-cyclooctadiene

A technology of cyclooctadiene and butadiene, which is applied in the field of preparation of 1,5-cyclooctadiene, can solve the problem of low activity, achieve enhanced activity and stability, reduce the incidence of side reactions, and mild reaction conditions Effect

Inactive Publication Date: 2018-05-08
濮阳盛华德化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Yamamoto published an iron-based complex catalytic system, and in US.pat.No.3565875, bozik, et, al proposed a three-way catalytic system with iron salts to catalyze diene polymerization. The above-mentioned catalytic system has the disadvantage of low activity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A preparation method of 1,5-cyclooctadiene, in an anhydrous inert environment in a pressure reactor, under the conditions of a temperature of 80-120°C and a gauge pressure of 0.10-0.60MPa, 1,3-butadiene is divided into Add the nickel-aluminum-phosphorus system catalyst into the inert hydrocarbon solvent several times to carry out the reaction of 1,3-butadiene cyclodimerization into 1,5-cyclooctadiene. After the reaction is completed, the synthesis liquid is transferred to Negative pressure refining in the rectification tower to obtain the finished product of 1,5-cyclooctadiene.

[0023] The preparation method comprises the following steps: a. Manufacturing an anhydrous inert environment: repeatedly replacing the dried pressure reactor with nitrogen, adding an inert hydrocarbon solvent dehydrated by molecular sieves, and measuring that the moisture content in the pressure reactor is less than 30ppm, Keep the gauge pressure at 0.1~0.25MPa, add nickel-aluminum-phosphorus s...

Embodiment 2

[0035] A preparation method of 1,5-cyclooctadiene, in an anhydrous inert environment in a pressure reactor, under the conditions of a temperature of 80-120°C and a gauge pressure of 0.10-0.60MPa, 1,3-butadiene is divided into Add the nickel-aluminum-phosphorus system catalyst into the inert hydrocarbon solvent several times to carry out the reaction of 1,3-butadiene cyclodimerization into 1,5-cyclooctadiene. After the reaction is completed, the synthesis liquid is transferred to Negative pressure refining in the rectification tower to obtain the finished product of 1,5-cyclooctadiene.

[0036] The preparation method comprises the following steps: a. Manufacturing an anhydrous inert environment: repeatedly replacing the dried pressure reactor with nitrogen, adding an inert hydrocarbon solvent dehydrated by molecular sieves, and measuring that the moisture content in the pressure reactor is less than 30ppm, Keep the gauge pressure at 0.1~0.25MPa, add nickel-aluminum-phosphorus s...

Embodiment 3

[0048] A preparation method of 1,5-cyclooctadiene, in an anhydrous inert environment in a pressure reactor, under the conditions of a temperature of 80-120°C and a gauge pressure of 0.10-0.60MPa, 1,3-butadiene is divided into Add the nickel-aluminum-phosphorus system catalyst into the inert hydrocarbon solvent several times to carry out the reaction of 1,3-butadiene cyclodimerization into 1,5-cyclooctadiene. After the reaction is completed, the synthesis liquid is transferred to Negative pressure refining in the rectification tower to obtain the finished product of 1,5-cyclooctadiene.

[0049] The preparation method comprises the following steps: a. Manufacturing an anhydrous inert environment: repeatedly replacing the dried pressure reactor with nitrogen, adding an inert hydrocarbon solvent dehydrated by molecular sieves, and measuring that the moisture content in the pressure reactor is less than 30ppm, Keep the gauge pressure at 0.1~0.25MPa, add nickel-aluminum-phosphorus s...

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Abstract

The invention discloses a preparation method of 1,5-cyclooctadiene. In water-free inert environment in a pressure reaction kettle, under the conditions of the temperature being 80 to 120 DEG C and thesurface pressure being 0.10 to 0.60MPa, 1,3-butadiene is added into an inert hydrocarbon solvent dissolved with Ni-Al-P system catalysts for many times; a reaction of performing 1,3-butadiene cyclizing dimerization to synthesize 1,5-cyclooctadiene is performed; after the reaction is completed, synthesis liquid is transferred into a rectifying tower to be subjected to negative pressure refining toobtain a finished product of 1,5-cyclooctadiene. Generally, the preparation method has the advantages that the reaction conditions are mild; the operation is simple and convenient; the raw material conversion rate is high; the reaction selectivity is high; the operation links can be effectively reduced; the synthesis efficiency is improved; the yield is high; the pollution is small; the product quality is high; the use value is very high.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis and relates to a preparation method of 1,5-cyclooctadiene. Background technique [0002] 1,5-Cyclooctadiene is an important intermediate in organic synthesis, mainly used to prepare suberic acid, suberic acid, tetrachlorocyclooctane, and also the monomer of polyamide fiber, the activity of epoxy resin thinner. The preparation of 1,5-cyclooctadiene usually adopts the cyclodimerization of 1,3-butadiene, and the catalyst used is usually a multi-component composite catalyst with a transition metal complex as the active center. Yamamoto published an iron-based complex catalyst system. In US.pat.No.3565875, bozik, et, al proposed a three-way catalyst system using iron salts to catalyze diene polymerization. The above catalyst system has the disadvantage of low activity. The purpose of the present invention is to provide a preparation method with mild reaction conditions, high reactivity, st...

Claims

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Application Information

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IPC IPC(8): C07C2/46C07C13/263B01J31/14
CPCB01J31/143C07C2/465C07C13/263
Inventor 王书生孙维华陈全胜李德彪
Owner 濮阳盛华德化工有限公司
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