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

Synthetic method for bis-trimethylolpropane n-octoate used for carbon fiber oil agent

A technology of ditrimethylolpropane and n-octanoate, which is applied in the field of synthesis of ditrimethylolpropane n-octanoate for carbon fiber oil, can solve problems such as unsatisfactory yield, and achieve simple separation and reaction The effect of mild conditions and simplified procedures

Inactive Publication Date: 2016-07-06
PETROCHINA CO LTD
View PDF1 Cites 8 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 2007, Wuhan University disclosed the patent "an ionic liquid catalyst for esterification reaction and its preparation method and application" (application number: 200710052175.7) using N-alkylpyrrolidone and methanesulfonic acid to react to produce Bronsted acidic ionic liquid of pyrrolidone group , can be used for alkyd esterification reaction, but the yield of the ionic liquid in the alkyd esterification reaction containing polyol is not ideal, the highest is 93%

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
  • Synthetic method for bis-trimethylolpropane n-octoate used for carbon fiber oil agent
  • Synthetic method for bis-trimethylolpropane n-octoate used for carbon fiber oil agent
  • Synthetic method for bis-trimethylolpropane n-octoate used for carbon fiber oil agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] In a reaction kettle equipped with an electric stirrer, thermometer and condenser, add 55 grams of acidic ionic liquid [Hmim]HSO in sequence 4 , 53 grams of 95wt% ditrimethylolpropane and 124 grams of 98wt% n-octanoic acid. When the temperature is 100°C, the heating rate should be controlled and the temperature should be increased slowly. When the temperature reaches 135°C, keep for 3.5 hours, and the reaction is over.

[0034] The above reaction liquid is cooled to room temperature and separated into layers at rest, the upper layer is the product of ditrimethylolpropane n-octanoate, and the lower layer is an ionic liquid rich in water and containing a trace amount of unreacted octanoic acid raw material. The ditrimethylolpropane n-octanoate in the upper layer is washed with water and dried to obtain a light yellow oily product, and the yield of the esterification reaction product is 97.15%. After the lower layer of ionic liquid is vacuum dehydrated, it is cyclically appli...

Embodiment 2

[0037] Add 56 grams of acidic ionic liquid [Hmim]HSO to the reactor equipped with electric stirrer, thermometer and condenser 4 , 53 grams of 95wt% ditrimethylolpropane and 131 grams of 98wt% n-octanoic acid. Heat up the temperature. When the temperature is 100°C, control the heating rate and slowly increase the temperature. When the temperature reaches 138°C, keep it for 2.5 hours and the reaction ends.

[0038] The above reaction liquid was cooled to room temperature and separated into layers at rest, the upper layer was the product of ditrimethylolpropane n-octanoate, and the lower layer was the ionic liquid rich in water and containing a trace amount of unreacted octanoic acid raw materials. The bistrimethylolpropane n-octanoate in the upper layer was washed with water and dried to obtain a light yellow oily product, and the yield of the esterification reaction product was 97.63%. After the lower layer of ionic liquid is vacuum dehydrated, it is cyclically applied.

[0039] Th...

Embodiment 3

[0041] In a reactor equipped with an electric stirrer, thermometer, and condenser, add 90 grams of acidic ionic liquid [Hmim]HSO in sequence 4 (Recycled application), 53 grams of 95wt% ditrimethylolpropane and 98wt% of n-octanoic acid 128g. Heat up the temperature. When the temperature is 100°C, the temperature rise rate should be controlled and the temperature rise slowly. When the temperature reaches 140°C, keep it for 2 hours, and the reaction ends.

[0042] The above reaction liquid was cooled to room temperature and separated into layers at rest, the upper layer was the product of ditrimethylolpropane n-octanoate, and the lower layer was the ionic liquid rich in water and containing a trace amount of unreacted octanoic acid raw materials. The ditrimethylolpropane n-octanoate in the upper layer was washed with water and dried to obtain a light yellow oily product, and the yield of the esterification reaction product was 97.87%. After the lower layer of ionic liquid is vacuum ...

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

PropertyMeasurementUnit
tensile strengthaaaaaaaaaa
tensile strengthaaaaaaaaaa
tensile strengthaaaaaaaaaa
Login to View More

Abstract

A synthetic method for bis-trimethylolpropane n-octoate used for a carbon fiber oil agent includes the steps of successively adding an acidic ionic liquid [Hmim]HSO4, bis-trimethylolpropane, and n-octanoic acid into a reaction kettle provided with an electronic stirrer, a temperature meter and a condensing tube, slowly increasing the temperature, and performing reflux for certain time with the reaction temperature controlled, decreasing the temperature of the reaction liquid when the reaction is finished, allowing the reaction liquid to stand for layering, and water-washing and drying the supernatant bis-trimethylolpropane n-octoate to obtain a light-yellow oily product.

Description

Technical field [0001] The invention relates to a method for synthesizing bistrimethylolpropane n-octanoate for carbon fiber oiling agent. Background technique [0002] Polyol fatty acid ester is the main component of carbon fiber oil agent. It has high temperature resistance, hydrolysis resistance, acid and alkali resistance, and more importantly, no toxicity. Researchers from Matsumoto Oil and Fat Company proposed in the patent (JP2006-070706, CN1013263313A) ), the use of ester compounds containing more than 3 ester groups in the molecule and polydimethylsiloxane as the main components of carbon fiber oil agent is the main development direction of carbon fiber low silicone oil agent, and it has also attracted more and more attention; Trimethylolpropane n-octanoate is a fatty acid ester with tetrahydric alcohol, which has obvious advantages compared with existing polyhydric alcohol esters. There is a flexible ether bond in the bistrimethylolpropane ester molecule, which can ens...

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): C07C69/33C07C67/08
Inventor 刘宇韩小平王淑娟张宏宇
Owner PETROCHINA CO LTD
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