Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for preparing 1,3-propane sultone

A technology of propane sultone and propane sulfonic acid, which is applied in the field of preparing 1,3-propane sultone, can solve the problems of easy oxidation of acrolein, high cost, and high requirements for reaction equipment, and achieve low output of three wastes, Low toxicity, reduction of raw materials and operating costs

Inactive Publication Date: 2018-06-29
抚顺东科新能源科技有限公司
View PDF2 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The raw material acrolein used in this method is easily oxidized and requires hydrogenation reduction, which requires high reaction equipment and relatively high cost

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
  • Method for preparing 1,3-propane sultone
  • Method for preparing 1,3-propane sultone
  • Method for preparing 1,3-propane sultone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1. Add 40g sodium sulfite (1.0eq), 50g (1.0eq) of 1-bromo-3-chloropropane, 250 milliliters of ethanol to the reaction flask, heat up to 80°C and react for 8 hours after adding, cool to 10°C, filter to obtain Crude sodium 1-chloro-3-propanesulfonate.

[0033] ②Put the crude sodium 1-chloro-3-propanesulfonate obtained in the previous step into the reaction bottle, add 100 ml of water, add hydrochloric acid below 20 degrees to adjust the pH=1-3, concentrate under reduced pressure to remove most of the water, and add 80 ml of ethanol , cooled to 10 degrees, filtered, and the filtrate was concentrated to dryness to obtain 48 g of 1-chloro-3-propanesulfonic acid.

[0034] ③ The 1-chloro-3-propanesulfonic acid obtained in the previous step was subjected to a lactonization reaction at 140-200° C. under high vacuum (-0.1 MPa), and the distillate was received at the same time to obtain 32 g of 1.3-propane sultone. The total yield of the product is 83%, and its purity is more tha...

Embodiment 2

[0036] ①Add 10.4g of sodium sulfite (1.0eq), 50g of 1,3-dibromopropane (3.0eq), and 200ml of ethanol into the reaction flask, heat up to 80°C and react for 10 hours after adding, cool down to 10°C, and filter to obtain Crude sodium 1-bromo-3-propanesulfonate, (unreacted 1,3-dibromopropane is in the filtrate and can be recovered).

[0037] ②Put the sodium 1-bromo-3-propanesulfonate obtained in the previous step into the reaction flask, add 60 ml of water, add hydrochloric acid below 20 degrees to adjust the pH=1-3, concentrate under reduced pressure to remove most of the water, add 35 ml of ethanol, Cool down to 10°C, filter, and concentrate the filtrate to dryness to obtain 15 g of 1-bromo-3-propanesulfonic acid.

[0038] ③The 1-bromo-3-propanesulfonic acid obtained in the previous step was subjected to a lactonization reaction at 140-200°C under high vacuum (-0.1MPa), and the distillate was received at the same time to obtain 8.1 g of 1.3-propane sultone. The total yield of ...

Embodiment 3

[0040] ①At room temperature, add 18.6g of sodium sulfite (1.0eq), 50g of 1,3-dichloropropane (3.0eq), and 200ml of ethanol into the reactor. After the addition, raise the temperature to 80°C for 16 hours, then cool down to 10°C , and filtered to obtain crude sodium 1-chloro-3-propanesulfonate (unreacted 1,3-dichloropropane is in the filtrate and can be recovered).

[0041] ②Put the sodium 1-chloro-3-propanesulfonate obtained in the previous step into the reaction flask, add 60 ml of water, add hydrochloric acid below 20 degrees to adjust the pH=1-3, concentrate under reduced pressure to remove most of the water, add 35 ml of ethanol, Cool down to 10°C, filter, and concentrate the filtrate to dryness to obtain 19 g of 1-chloro-3-propanesulfonic acid.

[0042] ③ The 1-chloro-3-propanesulfonic acid obtained in the previous step was subjected to a lactonization reaction at 140-200° C. under high vacuum (-0.1 MPa), and the distillate was received at the same time to obtain 12.4 g o...

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 discloses a method for preparing 1,3-propane sultone. The method comprises the following steps: 1) mixing 1,3-dihalopropane and a sulfonating agent and a solvent, and performing a sulfonation reaction under certain temperature to obtain 1-halogenated-3-sodium 1-propanesulfonate; 2) adding the 1-halogenated-3-sodium 1-propanesulfonate in water, adding strong acid for adjusting a pH value to 1-3, performing acidifying treatment, performing concentration, filtering the material to remove inorganic salt, and performing concentration to a dry state to obtain 1-halogenated-3-moropholino ethanesulfonic acid; and 3) heating the 1-halogenated-3-moropholino ethanesulfonic acid under vacuum condition, and performing a lactonization reaction to obtain the 1,3-propane sultone. The methodhas the advantages that 1) the toxicity of an used raw material 1,3-dihalopropane is smaller, the 1,3-dihalopropane is safer, is easily available, and is recoverable and repeatedly used, and is convenient for storage, so that raw material and operation cost of the raw material can be greatly reduced; and 2) three-waste output in the method is less, environment pollution is reduced, environment pollution is reduced, the purity of the produced product is high and can reach more than 99%, and the water content of the product is lower than 0.1%.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for preparing 1,3-propane sultone. Background technique [0002] 1,3-Propane sultone is an important intermediate in organic synthesis. It is a colorless or light yellow transparent liquid or a colorless transparent crystal. It has important industrial applications in different aspects, such as surfactants Synthesis of sulfonating agents, tanning, ink and sensitizing dyes; synthesis of electroplating intermediates, pharmaceuticals, lithium secondary batteries, inks, etc. With the continuous expansion of its use, the market demand is also increasing. Currently, the common method for synthesizing 1,3-propane sultone is as follows: [0003] Method 1: Using allyl alcohol and sodium bisulfite as raw materials, the target product is obtained through sulfonation, acidification, dehydration, refining and other steps in the presence of an initiator. The s...

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 Applications(China)
IPC IPC(8): C07D327/04
CPCC07D327/04
Inventor 于森
Owner 抚顺东科新能源科技有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com