Preparation method of N-(4-(2-ethylhexyloxy) phenyl)-1, 1-dioxothiomorpholino

A technology of dioxythiomorpholine and ethylhexyloxy, which is applied in the field of photosensitive materials and heat-sensitive paper stabilizers, can solve the problems of large pollution, high production cost, and many reaction steps, so as to reduce energy consumption, The effect of high yield and low energy consumption index

Inactive Publication Date: 2011-11-23
XIANTAO WYLSON CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The present invention mainly solves the problem that the existing N-(4-(2-ethylhexyloxy)phenyl)-1,1-dioxythiomorpholine (ST124AB stabilizer) production process has many reaction steps and large pollution. Technical issues such as high production costs

Method used

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  • Preparation method of N-(4-(2-ethylhexyloxy) phenyl)-1, 1-dioxothiomorpholino
  • Preparation method of N-(4-(2-ethylhexyloxy) phenyl)-1, 1-dioxothiomorpholino

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Embodiment 1

[0014] Example 1: Add 10 parts by weight of thiodiglycol and 10 parts by weight of water to the reactor, then add 1 part by weight of quaternary ammonium salt tetraethylammonium chloride as a catalyst, start stirring, and at a temperature of 60°C, Add 65 parts by weight of hydrogen peroxide dropwise to the reaction kettle, keep warm after dropping, and let it stand for 1 hour to generate bishydroxyethyl sulfone; then add 9 parts by weight of p-aminophenol, control the temperature at 40°C, perform condensation reaction for 3 hours, and then add 20 parts by weight of isooctane bromide, heated up to 100°C for further condensation reaction for 3 hours to obtain the product stock solution; pour n-heptane as the extraction solvent into the product stock solution, stir and let it stand, take the extract phase and evaporate the solvent to dryness Get the finished product. After calculation, the total yield reaches 86.8%; through gas chromatography analysis, the effective content of N-...

Embodiment 2

[0015] Example 2: Add 10 parts by weight of thiodiglycol and 10 parts by weight of water to the reactor, then add 1.5 parts by weight of quaternary ammonium salt tetraethylammonium chloride as a catalyst, start stirring, and at a temperature of 40°C, Add 70 parts by weight of hydrogen peroxide dropwise to the reaction kettle, keep warm after dropping, and let it stand for 1 hour to generate bishydroxyethyl sulfone; then add 10 parts by weight of p-aminophenol, control the temperature at 50°C, conduct condensation reaction for 3 hours, and then add 21 parts by weight of isooctane bromide, heated up to 80°C for further condensation reaction for 3 hours, to obtain the product stock solution; pour n-heptane as the extraction solvent into the product stock solution, stir and let it stand, take the extract phase and evaporate the solvent to dryness Get the finished product. After calculation, the total yield reaches 86.5%; through gas chromatography analysis, the effective content o...

Embodiment 3

[0016] Example 3: Add 10 parts by weight of thiodiglycol and 10 parts by weight of water to the reactor, then add 2 parts by weight of quaternary ammonium salt tetrabutylammonium bromide as a catalyst, start stirring, and at a temperature of 70°C, Add 75 parts by weight of hydrogen peroxide dropwise to the reaction kettle, keep warm after dropping, and let it stand for 1 hour to generate bishydroxyethyl sulfone; then add 10 parts by weight of p-aminophenol, control the temperature at 45°C, conduct condensation reaction for 3 hours, and then add 25 parts by weight of isooctane bromide, heated up to 95°C for further condensation reaction for 3 hours to obtain the product stock solution; pour n-heptane as the extraction solvent into the product stock solution, stir and let stand, take the extract phase and evaporate the solvent to dryness Get the finished product. After calculation, the total yield reaches 87.8%; through gas chromatography analysis, the effective content of N-(4-...

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Abstract

The invention relates to a preparation method of N-(4-(2-ethylhexyloxy) phenyl)-1, 1-dioxothiomorpholino. The method is characterized by comprising the following steps of: adding 10 parts by weight of thiodiglycol and 10 parts by weight of water to a reaction kettle, then adding 1-2 parts by weight of quaternary ammonium salt as a catalyst, adding 65-75 parts by weight of hydrogen peroxide dropwisely into the reaction kettle, after dropping, preserving the heat of the mixture and allowing it to stand for one hour so as to generate bishydroxyethylsulfone, adding p-aminophenol to conduct a condensation reaction for 3 hours, then adding bromoisooctane for a further condensation reaction for 3 hours, pouring n-heptane into a product stock solution, stirring the solution and allowing it to stand, taking out the extraction phase and evaporating the solvent to dryness, thus obtaining a finished product. Application of the method provided in the invention can prepare products with an overall yield of over 86% and effective content of more than 98%, so the method is completely applicable to large scale industrial production. With substantial economic benefit, social benefit and ecological benefit, the method provided in the invention fully meets the requirements of safety, environmental protection and high efficiency that are advocated by the nation in developing low carbon economy.

Description

technical field [0001] The invention relates to a photosensitive material and a heat-sensitive paper stabilizer, in particular to an N-(4-(2-ethylhexyloxy)phenyl)-1,1-dioxythiomorpholine (ST124AB Stabilizer) preparation method. Background technique [0002] N-(4-(2-ethylhexyloxy)phenyl)-1,1-dioxythiomorpholine, whose product name is ST124AB stabilizer, is an important raw material used in photosensitive materials and thermal paper At present, the main manufacturers are concentrated in Europe, and the technological level of major domestic manufacturers is relatively backward. Generally, mercaptoethanol is used as raw material. The production process has many unfavorable factors such as many reaction steps, heavy pollution, and high production costs. Contents of the invention [0003] The present invention mainly solves the problem that the existing N-(4-(2-ethylhexyloxy)phenyl)-1,1-dioxythiomorpholine (ST124AB stabilizer) production process has many reaction steps and larg...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/096
Inventor 黄平阶
Owner XIANTAO WYLSON CHEM
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