Unlock instant, AI-driven research and patent intelligence for your innovation.

New process for refining 2,4-diethyl thiazolone

A diethylthiazolone and process technology, applied in 2 fields, can solve problems such as production inconvenience and cooler residue, and achieve the effects of reducing energy consumption, avoiding high-temperature operations, and mild reaction conditions

Inactive Publication Date: 2013-04-03
邵阳市佳青医药原料有限公司
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] 1, purpose of the invention: because the synthesis of DETX usually adopts high-vacuum distillation, refines, to obtain high-purity product, has the following shortcoming like this: the 1st, require that distillation system has better sealing (distillation reactor inner pressure is at 5mmHg Below), high temperature should be used for the second one, the third material liquid is easy to remain in the cooler, and the fourth material should be crushed after discharge, which will bring inconvenience to production

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • New process for refining 2,4-diethyl thiazolone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1. Add 100kg of crude DETX to a 1000-liter reaction kettle, add 500 liters of methanol, then raise the temperature to 30°C, stir and keep it warm for 1 hour, then cool down to 10°C, separate the solid with a centrifuge, and use it in the next step. This step yield is 88%.

[0024] 2. Add 88kg of crude DETX to the reactor, then add 500kg of toluene, start stirring, raise the temperature to 50°C, stir for 1 hour, add activated carbon, keep warm for 30 minutes, and then filter into another clean reactor. The liquid filtered into the clean reactor was cooled to 30° C., stirred for 1 hour, and filtered to obtain a refined product of DETX with a yield of 85%.

Embodiment 2

[0026] 1. Add 100kg DETX crude product into a 1000-liter reactor, add 500 liters of benzene and 300 liters of n-hexane, then raise the temperature to 50°C, stir and keep it warm for 3 hours, then cool down to 30°C, separate the solid with a filter, and wait for the next step use. The yield of this step is 92%.

[0027] 2. Add 92kg of crude DETX to the reaction kettle, then add 400kg of ethanol, start stirring, raise the temperature to 100°C, stir for 3 hours, add activated carbon, keep warm for 60 minutes, and then filter into another clean reaction kettle. The liquid filtered into the clean reactor was cooled to 1° C., stirred for 5 hours, and filtered to obtain a refined product of DETX with a yield of 90%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to an optical initiator, in particular relates to a method for refining a 2,4-diethyl thiazolone crude product. The method comprises the following steps: (1) adding the 2,4-diethyl thiazolone crude product in a reaction kettle, adding a proper amount of solvent, heating to 30-50 DEG C, insulating temperature for 1-3 hours, then cooling to 10-30 DEG C, and filtering or separating out solids with a centrifugal machine for use in the next step; and (2) adding the 2,4-diethyl thiazolone crude product treated in the step (1) into the reaction kettle, adding the solvent, stirring, heating to 50-100 DEG C, stirring for 1-3 hours, adding activated carbon, insulating for 30-60 minutes, filtering and transferring to another clean reaction kettle, cooling the filtered liquid inthe clean reaction kettle to 1-30 DEG C, stirring for 1-5 hours, and filtering or separating with the centrifugal machine so as to obtain the refined 2,4-diethyl thiazolone product. The process has the advantages of simple crystallization process and less equipment.

Description

technical field [0001] The invention relates to a photoinitiator, in particular to a method for refining the crude product of 2,4-diethylthiazolone (hereinafter referred to as DETX). Background technique [0002] English common name of DETX: [0003] 2,4-diethylthioxanthen-9-one; 2,4-diethyl-9h-thioxanthen-9-one [0004] Chemical name: 2,4-diethylthiazolone, 2,4-diethylthioxanthone. [0005] Structural formula: [0006] [0007] Molecular formula: C 17 h 16 OS [0008] Molecular weight: 268 [0009] Physical and chemical properties: light yellow powder, melting point: 71-75°C. For transparent or colored UV curable inks, adhesives, coatings, etc. [0010] At present, the refining method of photoinitiator DETX generally adopts high vacuum distillation. The brief method is as follows: put the DETX crude product into the high-temperature reaction kettle, raise the temperature to 200-260°C, then start the multi-stage vacuum pump, and slowly start the distillation. The...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07D335/16
Inventor 李自成伍学军苏洪镇杨伟刚范河南张凯淇袁懿
Owner 邵阳市佳青医药原料有限公司