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Preparation method of thermosensitive sensitizer

A kind of sensitizer, dichloroethane technology, applied in ether preparation, ester reaction preparation ether, coating and other directions, can solve the problems of difficult handling, low yield, etc., achieve mild reaction conditions, high yield, raw materials easy-to-get effect

Active Publication Date: 2014-05-07
山东瑞康精化有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] The traditional synthesis methods of heat-sensitive sensitizers mostly adopt Williamson method, active ester alcoholysis method and phase transfer catalyst method, wherein the Williamson reaction time is 15h, the yield is 40%, the active ester alcoholysis method reaction time is 12h, the yield is 50%, The reaction time of the phase transfer catalyst method is 10 hours, and the yield is 76.9%; the reaction temperature is required to exceed 100°C, and the yield is low; and a large amount of strongly alkaline sewage containing organic phenolic substances and phase transfer catalysts is produced, which is difficult to treat by traditional methods

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  • Preparation method of thermosensitive sensitizer
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Examples

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Embodiment 1

[0014] A kind of preparation method of thermosensitive sensitizer, it is characterized in that, 89.1g (0.9 mole) dichloroethane and 200g (1.85 mole) m-cresol and 35ml water are added in the kettle, under the situation of nitrogen protection Stir, add dropwise 49% (weight standard) sodium hydroxide aqueous solution 100g when using 20 minutes, dropwise add 49% sodium hydroxide aqueous solution 72g with 2 hours after dropwise heating reflux 3 hours, then transfer solution to separation Drain the water layer, transfer the oil layer back to the reactor to continue the condensation reaction at 75-80°C for 3 hours, divide the outflow of 95ml of water, then add 175ml of water and heat to 100°C, stir, stand still, and separate layers to obtain 204.7g1,2 - Crude organic layer of bis(3-methylphenoxy)ethane (HPLC detection: 96.5%, yield 93.98%), the crude product was purified by rectification to obtain 195.1g of 1,2-bis(3-methylphenoxy base) ethane (HPLC detection: purity 99.6%, yield 89....

Embodiment 2

[0016] A kind of preparation method of thermosensitive sensitizer, it is characterized in that, 89.1g (0.9 mole) dichloroethane and 200g (1.85 mole) o-cresol and 35ml water are added in the kettle, carry out under the situation that there is nitrogen protection Stir, add dropwise 49% (weight standard) sodium hydroxide aqueous solution 100g when using 20 minutes, dropwise add 49% sodium hydroxide aqueous solution 72g with 2 hours after dropwise heating reflux after 3 hours, then solution is transferred to separator , drain the water layer, turn the oil layer back into the reactor to continue the condensation reaction at 70-75°C for 3 hours, divide the outflow of 95ml of water, then add 175ml of water and heat to 100°C, stir, stand still, and separate layers to obtain 203.9g of 1,2- Bis(3-methylphenoxy)ethane organic layer crude product (HPLC: 96.8%, yield 93.62%), the crude product was purified by rectification to obtain 194.9g of 1,2-bis(2-methylphenoxy) Ethane (HPLC detection...

Embodiment 3

[0018] A kind of preparation method of thermosensitive sensitizer, it is characterized in that, 89.1g (0.9 mole) dichloroethane and 200g (1.85 mole) p-cresol and 35ml water are added in the still, carry out under the situation that there is nitrogen protection Stir, add dropwise 49% (weight standard) sodium hydroxide aqueous solution 100g when using 20 minutes, dropwise add 49% sodium hydroxide aqueous solution 72g with 2 hours after dropwise heating reflux after 3 hours, then solution is transferred to separator , drain the water layer, turn the oil layer back into the reactor to continue the condensation reaction at 75-80°C for 3 hours, divide the outflow of 95ml of water, then add 175ml of water and heat to 100°C, stir, stand still, and separate layers to obtain 205.0g of 1,2- Bis(3-methylphenoxy)ethane organic layer crude product (HPLC: 96.8%, yield 94.12%), the crude product was purified by rectification to obtain 195.6g of 1,2-bis(4-methylphenoxy) Ethane (HPLC detection:...

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Abstract

The invention relates to a preparation method of thermosensitive sensitizer. The preparation method is characterized in that methyl substituted phenol (metacresol, o-cresol or p-cresol) and dichloroethane have condensation reaction at the temperature of 70 to 80 DEG C, then the thermosensitive sensitizer 1,2-dimethyl phenoxyl ethane crude product with the purity of 95 to 98 percent (the main impurity is the single substituted phenoxyl ethane) is obtained in the steps of layering, continuous reaction, extraction and layering, and then the crude product is rectified to obtain the high-purity thermosensitive sensitizer. The method is simple to operate, environmentally friendly, high in yield, moderate in reaction condition and low in production cost; the extracted impurity can be used as the raw material to be continued in the reaction.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of a thermosensitive sensitizer. Background technique [0002] Compound 1,2-bis(alkylphenoxy)ethane is a new thermal sensitizer for thermal recording paper. Compatibility and effect sensitizers to meet different needs, in addition to improving the sensitivity of recording paper to heat and pressure, it also endows the recorded image with high optical density and clarity, which can improve the sensitivity of heat-sensitive recording paper, Thermal stability, sensitivity, color development and other properties. [0003] The traditional synthesis methods of heat-sensitive sensitizers mostly adopt Williamson method, active ester alcoholysis method and phase transfer catalyst method, wherein the Williamson reaction time is 15h, the yield is 40%, the active ester alcoholysis method reaction time is 12h, the yield is 50%, The reaction time of the phase transfer ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/205C07C41/16C09D7/12
CPCC07C41/16C07C43/2055D21H21/14
Inventor 李正元袁晋亭房玉香苏庆云蔺黎明
Owner 山东瑞康精化有限公司
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