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Preparation method of Schiff base and metal cobalt complex and application thereof in preparing R-propylene glycol

A technology of metal cobalt and complexes, which is applied in the field of preparation of Schiff alkali metal cobalt complexes, can solve the problems of low yield, few times of catalyst application, and low catalyst selectivity, and achieve high application times and high selectivity. high effect

Inactive Publication Date: 2019-03-01
WEIFANG HUITAO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) The prepared Schiff alkali metal cobalt complex has a low yield;
[0005] (2) The selectivity of the Schiff alkali metal cobalt complex catalyst is low; the number of times the catalyst is applied mechanically is small;
[0006] (3) Alkali Schiff cobalt complexes are often used to catalyze the copolymerization of carbon dioxide and epoxides to prepare polycarbonate, but there is no report on the use of cobalt Schiff alkali metal complexes for the preparation of R-propylene glycol

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1 A kind of preparation method of Schiff alkali metal cobalt complex

[0032] (1) Addition reaction

[0033] Put 30kg of trans-cyclohexanediamine tartrate and 34kg of potassium carbonate into the reaction kettle, then add 400kg of fresh methanol, heat and stir to raise the temperature to 60°C, when reflux occurs in the reaction kettle, cool naturally, and cool down to 35°C, Stir for at least 10 more hours;

[0034] The specific rotation of the trans-cyclohexanediamine tartrate is -11°~-13°; the content is ≥98.0%.

[0035] (2) suction filtration

[0036] The reacted liquid was suction-filtered, and after being dried by suction, the filter cake was rinsed twice with 50 kg of methanol, and the filtrate was collected.

[0037] (3) Heating and reflux

[0038] Add 150kg of methanol and 8kg of anhydrous potassium acetate to the filtrate, heat up to 64-66°C, and heat to reflux at this temperature.

[0039] (4) Dissolving 3,5-di-tert-butyl salicylaldehyde

[004...

Embodiment 2

[0054] Example 2 Application of the above-mentioned Schiff alkali metal cobalt complex as a catalyst in the preparation of R-propylene glycol

[0055] It includes the following steps: feeding, bubbling, dripping reaction, and heat preservation reaction.

[0056] For the feeding, after adding propylene oxide, catalyst and p-nitrobenzoic acid, the temperature is lowered to below 4°C.

[0057] The addition quality of described p-nitrobenzoic acid is 0.5% of propylene oxide; The addition quality of described catalyst is 1.0% of propylene oxide.

[0058] For the dripping reaction, the temperature is 3° C., the dripping time is 5 hours, and the total mass of dripping water is 14% of the propylene oxide.

[0059] For the dripping reaction, if the reaction is triggered within half an hour from the dripping of water, the operation of dripping water at a constant speed can be carried out continuously; add water.

[0060] The temperature of the heat preservation reaction is 8°C; the e...

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PUM

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Abstract

The invention provides a preparation method of a Schiff base and metal cobalt complex. The preparation method includes: charging, suction-filtering, heating for reflux, dropwise adding 3, 5-ditert-butyl salicylaldehyde-methanol solution, allowing heat-insulating reaction for the first time, dropwise adding cobalt acetate-methanol solution, and allowing heat-insulating reaction for the second time.The invention further provides application of the complex in preparing R-propylene glycol. A molar ratio of Schiff base to metal cobalt is 2:1, specific rotation is -1200, and yield is 91%. When thecomplex serving as a catalyst is used for preparing R-propylene glycol, content of R-propylene glycol is higher than 99.5%, moisture is lower than 0.5%, and specific rotation is minus 16.8-minus 17.0.

Description

technical field [0001] The invention provides a preparation method of a Schiff alkali metal cobalt complex, which belongs to the technical field of chemical synthesis. Background technique [0002] Schiff base refers to a class of organic compounds containing imino groups (HC—N) or alkylimino groups (RC=N) formed by the shrinkage of two types of substances containing active carbonyl and amino groups. This type of compound was originally developed by Schiff in 1869. Named after the first discovery. Under certain conditions, Schiff bases can also form metal complexes with different stability with most metal elements, and these ligands and complexes can be used in stereochemistry, structure, stereoisomerism, magnetism, spectroscopy, coordination and so on. It plays an important role in the fields of chemistry, catalysis, analytical chemistry, photography, electro-optical display, agriculture and photochromism. [0003] The Schiff alkali metal cobalt complex and its applicatio...

Claims

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Application Information

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IPC IPC(8): C07F15/06B01J31/18C07C31/20C07C29/10
CPCB01J31/1805B01J2531/0252B01J2531/845C07B2200/09C07C29/106C07F15/065C07C31/205
Inventor 刘剑伟张全升韦兰星花现
Owner WEIFANG HUITAO CHEM
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