阅读说明：本技术 一种乙酰丙酮铜的制备方法及应用 (Preparation method and application of copper acetylacetonate ) 是由 郭向荣 王海 于 2020-08-10 设计创作，主要内容包括：本发明公开了一种乙酰丙酮铜的制备方法及应用,所述制备方法包括：(1)向反应釜中加入95％的乙醇,加入氯化亚铜,搅拌充分；(2)调节pH＝10-12,然后滴加乙酰丙酮,混合均匀,补加水分；(3)通入氧气,保持鼓泡状态,搅拌速率200-400转/分钟,温度100℃,进行微波反应,工作电压：380V,微波频率：2.45G Hz,脉冲峰值功率：15000W,连续功率max：1200W,反应2小时,蒸发浓缩冷却过滤洗涤即可。(The invention discloses a preparation method and application of copper acetylacetonate, wherein the preparation method comprises the following steps: (1) adding 95% ethanol and cuprous chloride into the reaction kettle, and stirring fully; (2) adjusting the pH value to 10-12, then dropwise adding acetylacetone, mixing uniformly, and supplementing water; (3) introducing oxygen, keeping a bubbling state, stirring at the speed of 200 and 400 revolutions per minute at the temperature of 100 ℃, carrying out microwave reaction, and ensuring the working voltage: 380V, microwave frequency: 2.45G Hz, pulse peak power: 15000W, continuous power max: 1200W, reacting for 2 hours, evaporating, concentrating, cooling, filtering and washing.)

1. A preparation method of copper acetylacetonate is characterized by comprising the following steps: (1) adding 95% ethanol and cuprous chloride into the reaction kettle, and stirring fully; (2) adjusting the pH value to 10-12, then dropwise adding acetylacetone, mixing uniformly, and supplementing water; (3) introducing oxygen, keeping a bubbling state, stirring at the speed of 200 and 400 revolutions per minute at the temperature of 100 ℃, carrying out microwave reaction, and ensuring the working voltage: 380V, microwave frequency: 2.45GHz, pulse peak power: 15000W, continuous power max: 1200W, reacting for 2 hours, evaporating, concentrating, cooling, filtering and washing.

2. Copper acetylacetonate according to claim 1 wherein said cuprous chloride and acetylacetone are present in a molar ratio of 1: 1.05 to 1.1.

3. Copper acetylacetonate according to claim 1 wherein the pH adjustment is from 10 to 12 by sodium hydroxide.

4. The copper acetylacetonate according to claim 1 wherein the 95% ethanol is added in an amount of 10 to 20 times the mass of the cuprous chloride.

5. The copper acetylacetonate according to claim 1 wherein said additional moisture is added to a 50% ethanol content.

6. Use of copper acetylacetonate according to any one of claims 1-5 wherein said copper acetylacetonate is used as a resin crosslinking agent and a curing accelerator.

Technical Field

The invention relates to the technical field of preparation of copper acetylacetonate, in particular to a preparation method and application of copper acetylacetonate.

Background

The acetylacetone salt is a chemical substance, can be used as a catalyst, a resin cross-linking agent, a resin hardening accelerator, a resin rubber additive, a super conductive film, a heat reflective glass film, a forming agent of a transparent conductive film and the like, and is an environment-friendly auxiliary agent for replacing a lead-containing auxiliary agent.

Copper acetylacetonate is a blue needle crystal or powder, readily soluble in chloroform and soluble in benzene and carbon tetrachloride. As organic synthesis catalysts; as a resin crosslinking agent and curing accelerator; a rubber additive; fuel oil additives, which improve lubricity and flammability, do not prevent carbon deposition.

Disclosure of Invention

The invention aims to provide a preparation method and application of copper acetylacetonate, which are characterized in that 95% ethanol is used as a reaction system, copper acetylacetonate is efficiently synthesized by adopting a microwave mode under a certain pH condition and normal pressure, and the quality and performance of the product are higher than those of the commercial product.

In order to solve the technical problems, the invention adopts the following technical scheme:

a preparation method of copper acetylacetonate comprises the following steps: (1) adding 95% ethanol and cuprous chloride into the reaction kettle, and stirring fully; (2) adjusting the pH value to 10-12, then dropwise adding acetylacetone, mixing uniformly, and supplementing water; (3) introducing oxygen, keeping a bubbling state, stirring at the speed of 200 and 400 revolutions per minute at the temperature of 100 ℃, carrying out microwave reaction, and ensuring the working voltage: 380V, microwave frequency: 2.45GHz, pulse peak power: 15000W, continuous power max: 1200W, reacting for 2 hours, evaporating, concentrating, cooling, filtering and washing.

Further, the molar ratio of the cuprous chloride to the acetylacetone is 1: 1.05-1.1.

Further, the pH adjustment is 10-12 by sodium hydroxide.

Further, the addition amount of the 95% ethanol is 10-20 times of the mass of the cuprous chloride.

Further, the water is supplemented until the ethanol content is 50%.

The application of copper acetylacetonate for resin cross-linking agent and curing accelerator is disclosed.

The invention has the following beneficial effects:

the invention aims to provide a preparation method of copper acetylacetonate, which is characterized in that 95% ethanol is used as a solvent, partial copper salt can be dissolved, cuprous is found to have better matching property with acetylacetone in a laboratory, then oxygen is introduced for oxidation, but the conversion rate is not high enough, the reaction effect is good under the action of high-frequency microwave, the conversion rate is extremely high, and the preparation method has an industrial prospect.

Detailed Description

In order to facilitate a better understanding of the invention, the following examples are given to illustrate, but not to limit the scope of the invention.