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Nickel complex and application thereof in preparation of polyether organosilicon copolymer

A technology of polyether organosilicon and nickel complexes, applied to nickel organic compounds and other directions, can solve the problems of expensive platinum catalysts, increase production costs, insufficient contact, etc., and achieve the effects of cheap reagents, low cost and convenient operation.

Pending Publication Date: 2022-05-17
JIANGXI MENHOVER CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This reaction generally uses an inorganic platinum salt catalyst, which has poor fat solubility, and the contact with hydrogen-containing polysiloxane is often insufficient during the reaction, which affects the reaction efficiency; in addition, the platinum catalyst is relatively expensive, which greatly increases the production cost

Method used

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  • Nickel complex and application thereof in preparation of polyether organosilicon copolymer
  • Nickel complex and application thereof in preparation of polyether organosilicon copolymer
  • Nickel complex and application thereof in preparation of polyether organosilicon copolymer

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Experimental program
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preparation example Construction

[0016] Preparation of nickel complexes comprising long alkyl chains (general procedure 1):

[0017] Hydrazide can be prepared by reacting corresponding methyl carboxylate or ethyl ester with excess hydrazine hydrate, and the process steps can be known from open literature.

[0018]

[0019] In the first step, add long-chain hydrazide (10mmol), pyridine formaldehyde (10mmol) and solvent ethanol (20mL) in the reaction flask, and reflux reaction under stirring for 10 hours. After the reaction, extract three times with water and dichloromethane. Remove water layer, the organic layer was dried over anhydrous sodium sulfate, filtered, concentrated, and recrystallized with 20 mL of ethanol to obtain the long alkyl chain ligand L.

[0020] In the second step, add long alkyl chain ligand L (10mmol), nickel salt (11mmol) and water (20mL) into the autoclave, heat up to 150 degrees under stirring and react for 10 hours. After the reaction, cool down and filter. The filter cake was was...

Embodiment 1

[0023] The preparation of embodiment 1 nickel complex M1

[0024]

[0025] According to the general procedure 1, the hydrazide is selected from n-hexyl hydrazide, the pyridine formaldehyde is selected from 5-methoxypyridine-2-carbaldehyde, and the nickel salt is selected from nickel bromide to prepare the nickel complex M1 with a yield of 84%.

Embodiment 2

[0026] The preparation of embodiment 2 nickel complex M2

[0027]

[0028] According to the general procedure 1, the hydrazide is lauryl hydrazide, the pyridine formaldehyde is 3-picoline-2-carbaldehyde, and the nickel salt is nickel acetate to prepare the nickel complex M2 with a yield of 81%.

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Abstract

The invention belongs to the field of chemical engineering, and particularly relates to a nickel complex containing a long alkyl chain and application of the nickel complex in preparation of a polyether organosilicon copolymer. The novel complex is convenient in source and low in cost, and the price of the novel complex is one percent of that of a common platinum / palladium catalyst; besides, the complex contains a relatively long alkyl chain, so that the complex has very good fat solubility and can be fully dissolved with hydrogen-containing polysiloxane and allyl polyether, and the reaction of the hydrogen-containing polysiloxane and the allyl polyether is efficiently catalyzed to prepare the polyether-organosilicon copolymer. In short, the method is cheap in reagent, simpler in formula, more convenient to operate, green, safe, efficient, environmentally friendly and suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of chemical industry, in particular to a class of nickel complexes containing long alkyl chains and their application in the preparation of polyether silicone copolymers. Background technique [0002] Polyether silicone copolymer is a new type of surfactant, its unique molecular structure contains both polysiloxane and polyether. Among them, the polysiloxane part endows the surfactant with the characteristics of low surface tension, antistatic and physiological inertness. By adjusting the degree of polymerization and the ratio of ethylene oxide (EO) and propylene oxide (PO) of polyether, As well as the ratio of polyether and polysiloxane, silicone surfactants with different properties and uses can be obtained, which can be widely used in coating industry, polyurethane, pesticide and daily chemical industry and other industries. [0003] The key reaction in the preparation of polyether silicone copolymer is the additi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/04C08G77/46
CPCC07F15/04C08G77/46
Inventor 张文凯龚国安吴蔚林许杰
Owner JIANGXI MENHOVER CHEM TECH CO LTD