4 results about "Propargyl alcohol" patented technology

This invention relates to the field of lithium battery electrolyte technology, specifically a method for synthesizing tripropynyl phosphate, comprising the following steps: 1) In a dry reaction vessel, an organic solvent is added, and phosphorus oxychloride is dissolved in the organic solvent, and stored under an inert atmosphere at low temperature; 2) A mixture of propynyl alcohol and triethylamine is slowly added dropwise, and the reaction is continuously stirred while maintaining a low temperature; 3) The mixture is slowly added dropwise, and the reaction is stirred after the temperature is raised to room temperature; 4) The mixture is slowly added to the reaction vessel, and the reaction is stirred after the temperature is raised to room temperature; 5) The triethylamine hydrochloride is removed by filtration, and the filtrate is distilled under reduced pressure to obtain a crude product, which is then purified by reduced pressure distillation or column chromatography. This invention effectively solves the problems of violent exothermic reactions, numerous side reactions, harsh reaction conditions, and difficulties in post-processing and purification of the product in existing synthesis methods by rationally designing reaction steps and precisely controlling reaction conditions and molar ratios.

This application provides a method for preparing methylcarboxylic acid-2-propynyl ester, comprising the following steps: (1) mixing dimethyl carbonate and propargyl alcohol, adding a first alkaline catalyst, stirring and heating to a temperature of 90-105°C, and distilling out methanol by reactive distillation to obtain a first component; (2) performing solid-liquid separation on the first component to obtain a first liquid, and performing vacuum distillation on the first liquid to remove propargyl alcohol and dimethyl carbonate to obtain methylcarboxylic acid-2-propynyl ester and residue; (3) performing vacuum distillation on the residue, replenishing dimethyl carbonate and the second alkaline catalyst with the distillate for reaction, and reusing the reaction liquid in step (2). This application uses the transesterification reaction of propargyl alcohol and dimethyl carbonate to synthesize methylcarboxylic acid-2-propynyl ester, which has high safety, low overall reaction temperature, fewer by-products and waste, and high yield.

The present application relates to the technical field of analytical detection, and particularly relates to a method for determining water content in a propynol system sample by adding an organic solvent, comprising the following steps: (1) taking a to-be-detected layered sample containing water, n-propyl acetate and propynol in a propynol production process; (2) adding an alcohol organic solvent to the to-be-detected layered sample, stirring uniformly, and changing the sample from a water-oil layered state to a uniform clear solution; (3) determining water content in the uniform clear solution obtained in step (2) by using a Karl Fischer method. The present application has the advantages that the method eliminates the interference of water-oil layering on water content determination, improves the accuracy and repeatability of determination, and is suitable for propynol production process control.