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Synthetic method of 2,2-diethoxy acetophenone photoinitiator

A technology of diethoxyacetophenone and photoinitiator, which is applied in the field of photoinitiator 2, can solve the problems of high corrosion of hydrogen chloride gas, difficulty of industrial production, inconvenience of industrial production, etc., and achieves no impact on the environment and is suitable for industrial production , Raw and auxiliary materials are cheap and easy to obtain

Inactive Publication Date: 2010-06-16
NANKAI UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, the synthetic method of 2,2-diethoxyacetophenone has not been reported in detail, and hydrogen chloride gas is used as a catalyst in the synthetic method of similar 2,2-dimethoxyacetophenone, and hydrogen chloride gas Corrosion is large, and it is not easy to obtain in industry, which brings great inconvenience to industrial production
At the same time, 2,2-diethoxyacetophenone is unstable and easy to decompose in the process of post-treatment, so it is difficult to industrialize production

Method used

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  • Synthetic method of 2,2-diethoxy acetophenone photoinitiator

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Step a, synthetic ethyl nitrite

[0018] Set a four-necked reaction flask equipped with mechanical stirring and air duct, add 75 grams of sodium nitrite, 46 grams of absolute ethanol and 190 grams of water, add dropwise 270 grams of 20% dilute sulfuric acid at room temperature, and generate ethyl nitrite gas Directly used in step ii reaction.

[0019] Step b, synthetic 2,2-diethoxyacetophenone

[0020] A four-necked reaction flask equipped with mechanical stirring, a thermometer and a gas inlet tube was installed, and 60 grams of acetophenone and a solution mixed with 50 grams of 36% hydrogen chloride ethanol solution and 300 grams of absolute ethanol were added, cooled to 5 ° C, Introduce the ethyl nitrite generated in step i, and continue to incubate at 40° C. for 3 hours after aeration is completed. Ethanol was distilled off under reduced pressure, and the raffinate was neutralized to neutrality with 20% mass concentration of sodium hydroxide solution, then extract...

Embodiment 2

[0022] Step a, synthetic ethyl nitrite

[0023] Set up a reaction kettle equipped with mechanical stirring and air guide port, add 150 kg of sodium nitrite, 92 kg of absolute ethanol and 380 kg of water, and drop 540 kg of 20% dilute sulfuric acid at 25°C to produce ethyl nitrite gas For the reaction of step ii.

[0024] Step b, synthetic 2,2-diethoxyacetophenone

[0025] A reaction kettle equipped with mechanical stirring and gas inlet pipe is set, add 120 kilograms of acetophenone, 100 kilograms of 36% hydrogen chloride ethanol solution and 500 kilograms of dehydrated alcohol, cool to 5 ℃, pass into the ethyl nitrite that step i generates gas, react at 40°C for 3 hours after ventilation is completed, distill ethanol off under reduced pressure, neutralize the residual liquid with 240 kg of 20% mass concentration of sodium hydroxide solution, extract with anhydrous ether, dry over anhydrous sodium sulfate, filter, and remove The crude product was dissolved, and 148 kg of 2,2...

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Abstract

The invention relates to a synthetic method of a 2,2-diethoxy acetophenone photoinitiator, which comprises the following steps: a, synthesizing ethyl nitrite, namely mixing ethanol with 28 percent of aqueous solution of sodium nitrite in a reaction kettle with mechanical stirring and a gas ingress pipe, dripping 20 percent dilute sulphuric acid into the mixture at the temperature of between 20 and 30 DEG C to generate ethyl nitrite gas, and directing introducing the generate ethyl nitrite gas into the step b for reaction, wherein the molar ratio of the ethanol to the sodium nitrite to the dilute sulphuric acid is 1.00:1.09 to 1.68:1.10 to 1.18; and b, synthesizing 2,2-diethoxy acetophenone, namely introducing the ethyl nitrite gas generated by the step a into acetophenone and 36 percent hydrogen chloride ethanol solution, and neutralizing the mixture by using sodium hydroxide solution after a reaction ends to prepare finished products, wherein the molar ratio of the acetophenone to the hydrogen chloride ethanol solution is 1:1. The synthetic method is simple and convenient in process and high in product yield and is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for synthesizing photoinitiator 2,2-diethoxyacetophenone. Background technique [0002] α, α-dialkoxyacetophenone can be regarded as an acetal derivative of phenylglyoxal, and can be used as a photoinitiator in photocurable materials. Among them, 2,2-diethoxyacetophenone (DEAP) has a higher photoinitiation efficiency, and there are weak C-C bonds adjacent to carbonyl and alkoxy groups in its structure, so its photolysis efficiency is relatively high. There is no long-lived substituted benzyl radical structure in the photolysis product of 2,2-diethoxyacetophenone, so the cured coating basically does not appear yellowing after it triggers. The photoinitiation activity of 2,2-diethoxyacetophenone is higher in several types of photoinitiators developed in the early stage. In a homogeneous polymerizable system (such as acrylate), 2,2-diethoxybenzene The photoinitiating activity of ethyl ketone is equivalent to that of DMP...

Claims

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Application Information

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IPC IPC(8): C07C49/84C07C45/64
Inventor 王有名周正洪吴忠华
Owner NANKAI UNIV
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