Check patentability & draft patents in minutes with Patsnap Eureka AI!

Method for preparing 3-hexine-2,5-glycol under ordinary pressure

A technology of hexyne and normal pressure, which is applied in the field of preparing 3-hexyne-2 under normal pressure, can solve problems such as complex process, and achieve the effects of high equipment requirements, high raw material costs and complicated production operations

Inactive Publication Date: 2012-08-15
JIANGSU TETRA NEW MATERIAL TECH
View PDF4 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis method of 3-hexyne-2,5-diol described in the patent (application number: 201110152117.8, publication number: CN102285867A) of Sichuan Zhijiang Chemical New Material Co., Ltd., the reaction is to adjust the pressure to 0.5- It is carried out under 1.5MPa, the reaction time is 3-10h, the yield is about 70%, and the process is relatively complicated

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 3-hexine-2,5-glycol under ordinary pressure
  • Method for preparing 3-hexine-2,5-glycol under ordinary pressure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1) Add 100mL xylene solution dissolved with 18g potassium tert-butoxide into a reaction kettle under normal pressure, pass through a certain amount of acetylene, add dropwise 25mL xylene solution dissolved with 8.8g acetaldehyde, react at 2°C for 1 hour, add 50mL xylene, continue to react for 2h;

[0025] 2) After washing the organic phase of the reaction solution with water for 3 times to remove the solvent, carry out rectification under reduced pressure, collect the fraction at 119-123°C, and obtain the product 3-hexyne-2,5-diol with a yield of 75.5% and a purity of 99%.

Embodiment 2

[0027] 1) Add 100mL xylene solution dissolved with 20g potassium tert-butoxide in the normal pressure reactor, pass through a certain amount of acetylene, add dropwise 25mL xylene solution dissolved with 8.8g acetaldehyde, react at 2°C for 1 hour, add 50mL xylene, continue to react for 2h;

[0028] 2) After washing the organic phase of the reaction solution with water for 3 times to remove the solvent, carry out rectification under reduced pressure, collect the fraction at 119-123° C., and obtain the product 3-hexyne-2,5-diol with a yield of 76.3% and a purity of 99%.

Embodiment 3

[0030] 1) Add 100mL xylene solution with 18g of potassium tert-butoxide dissolved in an atmospheric pressure reactor, pass through a certain amount of acetylene, add dropwise 25mL of xylene solution with 8.8g of acetaldehyde, react at -2°C for 1 hour, replenish Add 50mL xylene and continue the reaction for 1.75h;

[0031] 2) After washing the organic phase of the reaction solution with water for 3 times to remove the solvent, carry out rectification under reduced pressure, collect the fraction at 119-123°C, and obtain the product 3-hexyne-2,5-diol with a yield of 74.5% and a purity of 99%.

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 a method for preparing 3-hexine-2,5-glycol under ordinary pressure. The method comprises the following steps of: reacting acetylene and acetaldehyde in an ordinary-pressure reaction kettle under the catalysis of an efficient solid catalyst potassium tert-butoxide, wherein acetylene and acetaldehyde serve as raw materials, dimethylbenzene serves as solvent, the molar ratio of acetylene to acetaldehyde equals to 1: 2 to 1: 3, the mass ratio of the efficient solid catalyst to acetaldehyde equals to 0.5: 1 to 1: 1, the mass ratio of dimethylbenzene to acetaldehyde is 15: 1 to 20: 1, the reaction temperature ranges from minus 6 DEG C to 3 DEG C, and the reaction time lasts for 2.5 hours to 3.5 hours; and performing water washing and solvent removal on the organic phase of the reaction liquid, and then performing reduced-pressure rectification to obtain the product 3-hexine-2,5-glycol, wherein the productivity can reach 80%, and the purity reaches 99%. When the method is adopted for synthesizing 3-hexine-2,5-glycol, the reaction can be performed under the ordinary pressure; and the preparation method has the characteristics of simple process, low cost, high efficiency and the like.

Description

technical field [0001] The invention relates to a synthesis method of 3-hexyne-2,5-diol, in particular to a method for preparing 3-hexyne-2,5-diol under normal pressure. Background technique [0002] 3-Hexyne-2,5-diol, molecular formula C 6 h 10 o 2 , see formula 1 for the structural formula. [0003] [0004] Formula 1 [0005] 3-Hexyne-2,5-diol has good wettability, low foaming and defoaming properties, high dispersibility and excellent corrosion inhibition, etc. Various excellent properties make it widely used and can be used in paints and coatings (especially water-based coatings), pharmaceutical intermediates, hypnotics for live fish transportation, special solvents, viscosity reducers, glazing agents for nickel or copper plating, stabilizers for chlorinated hydrocarbons, pesticides, printing and dyeing, ink, Ink, liquid medicine, binder, acid leaching of metal materials, removal of rolled iron and phosphorus, pickling and descaling of metal equipment, acid dip...

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
IPC IPC(8): C07C33/044C07C29/42
Inventor 曹祥来曹祥明乔毅常杨军
Owner JIANGSU TETRA NEW MATERIAL TECH
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

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

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com