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A method for synthesizing 9-hydroxyl-4-oxa-7-thianonene

A technology of thionone and oxa, applied in the field of synthesis of 9-hydroxy-4-oxa-7-thionone, can solve the problem of lack of 9-hydroxy-4-oxa-7-thionone problems such as the industrialized preparation method of alkene, to achieve the effect of increasing the contact area of ​​gas and liquid phase, fully reacting, and optimizing process parameters

Active Publication Date: 2018-07-27
锦西化工研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to solve the problem of the lack of suitable industrial preparation methods for 9-hydroxyl-4-oxa-7-thianonene, and can improve the reaction rate and control the production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In a 200L stainless steel reactor equipped with a stirrer and a reflux condenser (the reactor is equipped with a coil and small feeding ports are evenly distributed on the coil), add 27.2kg of solid alkali (industrial product, purity 99.0%), 124.5kg of sulfur Diethylene glycol (industrial product, purity 99.0%), slowly increase the temperature to 40°C, and react at 40±2°C for 1.5 hours to generate sodium thiodiglycol; add 52.0kg of chloropropene into a 100L stainless steel metering tank, Propylene chloride enters the reactor through the small feeding ports evenly distributed on the coil inside the kettle. Add chloropropene dropwise for 1 to 2 hours at 40~50℃. After the addition, heat up to 100℃ at 100±2℃ , React for 1.5 hours. After the reaction liquid is cooled, it is treated with concentrated hydrochloric acid to neutrality, filtered and desalted to obtain the filtrate, which is the crude 9-hydroxy-4-oxa-7-thianonene, which is then subjected to vacuum distillation to c...

Embodiment 2

[0022] In a 200L stainless steel reactor equipped with a stirrer and a reflux condenser (the reactor is equipped with a coil and small feeding ports are evenly distributed on the coil), add 27.2kg of solid alkali (industrial product, purity 99.0%), 166.0kg of sulfur Diethylene glycol (industrial product, purity 99.0%), slowly increase to 34°C, react at 34±2°C for 3 hours to generate sodium thiodiglycol; add 51.0kg of chloropropene into a 100L stainless steel metering tank, Propylene chloride enters the reactor through the small feeding ports evenly distributed on the coil inside the kettle. Add chloropropene dropwise for 1 to 2 hours at 40~50℃. After the addition, heat up to 100℃ at 100±2℃ , React for 1.5 hours. After the reaction liquid is cooled, it is treated with concentrated hydrochloric acid to neutrality, filtered and desalted to obtain the filtrate, which is the crude 9-hydroxy-4-oxa-7-thianonene, which is subjected to vacuum distillation to collect at 135~142℃( 1.33kP...

Embodiment 3

[0024] In a 200L stainless steel reactor equipped with a stirrer and a reflux condenser (the reactor is equipped with a coil and small feeding ports are evenly distributed on the coil), add 27.2kg of solid alkali (industrial product, purity 99.0%), 206.7kg of sulfur Diethylene glycol (industrial product, purity 99.0%), slowly increase the temperature to 46°C, react at 46±2°C for 1.5 hours to generate sodium thiodiglycol; add 52.0kg of chloropropene into a 100L stainless steel metering tank, Propylene chloride enters the reactor through the small feeding ports evenly distributed on the coil inside the kettle. Add chloropropene dropwise for 2 to 3 hours at 40~50℃. After the addition, increase the temperature to 120℃, at 120±2℃ , React for 2.5 hours. After the reaction liquid is cooled, it is treated with concentrated hydrochloric acid to neutrality, filtered and desalted to obtain the filtrate, which is the crude 9-hydroxy-4-oxa-7-thianonene, which is subjected to vacuum distilla...

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Abstract

The invention relates to a method for synthesizing 9-hydroxy-4-oxa-7-thianonene. The method is characterized by comprising the following steps: A, adding solid caustic soda and thiodiglyco into a reaction kettle, slowly raising the temperature to 30 to 50DEG C, and reacting for 1 to 3 hours to generate thiodiglycolic sodium; B, adding chloropropene into a metering tank, then charging materials into the reaction kettle, and dropwise adding the chloropropene at the temperature of 30 to 50DEG C for 1 to 4 hours; after adding, raising the temperature to 80 to 130DEG C, reacting for 1 to 3 hours, and cooling a reaction solution; C, carrying out acidizing, filtering and desalting treatment on the cooled reaction solution to obtain a crude product of 9-hydroxy-4-oxa-7-thianonene; then rectifying, and collecting fractions to obtain colorless or pale yellow transparent 9-hydroxy-4-oxa-7-thianonene. The method disclosed by the invention has the advantages that the raw materials are low in price and easily obtained, and the yield of a product is high; the method is suitable for industrially producing the 9-hydroxy-4-oxa-7-thianonene.

Description

Technical field [0001] The invention belongs to the technical field of organic chemical production, and specifically relates to a synthetic method of 9-hydroxy-4-oxa-7-thianonene. Background technique [0002] 9-Hydroxy-4-oxa-7-thianonene is a colorless or light yellow transparent liquid. It is a grafting agent for the surface of polymer hollow microspheres. It can also be used as a double bond capping agent for high molecular polymers. Molecular weight regulator. At present, it is widely used as the molecular weight regulator of liquid polythioether rubber and the synthetic raw material of grafted polymer hollow microspheres. By adjusting the addition amount of 9-hydroxy-4-oxa-7-thianonene, the molecular weight of the polymer can be effectively adjusted to meet the performance requirements of different sealants. Hollow polymer microspheres synthesized with 9-hydroxy-4-oxa-7-thianonene as grafting agent have good affinity with a variety of polymers, making the polymer hollow mi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C319/20C07C323/12
CPCC07C319/20C07C323/12
Inventor 赫平马天野李放张卓
Owner 锦西化工研究院有限公司
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