Synthesis method of trimethylolpropane polyoxypropylene ether

A technology of trimethylolpropane polyoxypropylene ether and methylolpropane polyoxypropylene ether, which is applied in the field of synthesis of trimethylolpropane polyoxypropylene ether, can solve inactivation, long induction period and complex production process and other problems, to achieve the effect of low consumption, stable product quality and simple separation

Active Publication Date: 2022-07-05
ZHEJIANG HUANGMA TECH +3
View PDF6 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But when preparing low unsaturation polyether polyol, there is the shortcoming that induction period is longer, simultaneously Wang Wenhao (Wang Wenhao. DMC catalyst and the research progress of producing low unsaturation polyether [J]. Polyurethane industry, 2006, 21(3): 6-9) et al. proposed that another shortcoming is that it cannot directly use small molecule active hydrogen as an initiator, but needs to use an alkoxylated oligomer with a relative molecular weight greater than 200 as an initiator
However, KOH is still needed as a catalyst in the process of preparing the starter, which requires post-treatment of the starter to remove the residual basic catalyst, because the basic catalyst will reduce or even inactivate the DMC activity.
This complicates the production process and increases the 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
  • Synthesis method of trimethylolpropane polyoxypropylene ether
  • Synthesis method of trimethylolpropane polyoxypropylene ether
  • Synthesis method of trimethylolpropane polyoxypropylene ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The present embodiment provides a method for synthesizing trimethylolpropane polyoxypropylene ether, and the specific steps are as follows:

[0032] Weigh trimethylolpropane 584g, ETS-101.05g (0.05%), put it into the reactor after mixing, and after vacuuming, replace nitrogen in the reactor, replace nitrogen three times, vacuumize after the last replacement, and put it in a vacuum Under the condition of temperature ≥-0.098MPa, heat the reaction kettle to melt the material completely, continuously feed 1513g of propylene oxide, control the reaction temperature at 100±2℃, and the pressure in the reaction kettle ≤0.35Mpa. After adding, keep the temperature and continue the reaction. Until the system pressure in the reaction kettle no longer drops. After the reaction, the reaction mixture was filtered, cooled to 75°C, and the unreacted propylene oxide was removed in vacuo to obtain the finished product. The results of liquid chromatography analysis: the content of propenyl...

Embodiment 2

[0034] The present embodiment provides a method for synthesizing trimethylolpropane polyoxypropylene ether, and the specific steps are as follows:

[0035] Weigh trimethylolpropane 584g, ETS-100.63g (0.03%), put it into the reactor after mixing, and after vacuuming, replace nitrogen in the reactor, replace nitrogen three times, vacuumize after the last replacement, and put it in a vacuum Under the condition of temperature ≥-0.098MPa, heat the reaction kettle to melt the material completely, continuously feed 1513g of propylene oxide, control the reaction temperature at 100±2℃, and the pressure in the reaction kettle ≤0.35Mpa. After adding, keep the temperature and continue the reaction. Until the system pressure in the reaction kettle no longer drops. After the reaction, the reaction mixture was filtered, cooled to 75°C, and the unreacted propylene oxide was removed in vacuo to obtain the finished product. The results of liquid chromatography analysis: the content of propenyl...

Embodiment 3

[0037] The present embodiment provides a method for synthesizing trimethylolpropane polyoxypropylene ether, and the specific steps are as follows:

[0038]Weigh trimethylolpropane 584g, ETS-101.68g (0.08%), put it into the reactor after mixing, and after vacuuming, replace nitrogen in the reactor, replace nitrogen three times, vacuumize after the last replacement, and put it in a vacuum Under the condition of temperature ≥-0.098MPa, heat the reaction kettle to melt the material completely, continuously feed 1513g of propylene oxide, control the reaction temperature at 100±2℃, and the pressure in the reaction kettle ≤0.35Mpa. After adding, keep the temperature and continue the reaction. Until the system pressure in the reaction kettle no longer drops. After the reaction, the reaction mixture was filtered, cooled to 75°C, and the unreacted propylene oxide was removed in vacuo to obtain the finished product. Liquid chromatography analysis results: the content of propenyl alcohol...

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
hydroxyl valueaaaaaaaaaa
hydroxyl valueaaaaaaaaaa
Login to view more

Abstract

The invention provides a synthesis method of trimethylolpropane polyoxypropylene ether, which is characterized in that trimethylolpropane and epoxypropane are used as raw materials and are subjected to polymerization reaction under the catalysis of a titanium silicalite molecular sieve ETS-10 to prepare the trimethylolpropane polyoxypropylene ether. The relative molecular mass distribution of the finally obtained trimethylolpropane polyether is less than or equal to 1.01, the trimethylolpropane residue is less than or equal to 100ppm, the content of allyl alcohol by-products is less than or equal to 10ppm, and the hydroxyl value is 340-360mgKOH / g. In addition, the titanium silicalite molecular sieve ETS-10 catalyst is economical and easy to obtain, can be repeatedly used, and is simple to separate and low in consumption.

Description

technical field [0001] The invention belongs to the technical field of fine chemical product synthesis, in particular to a method for synthesizing trimethylolpropane polyoxypropylene ether. Background technique [0002] Propoxylated trimethylolpropane is an important UV-curable intermediate, mainly used in the synthesis of acrylate reactive diluents, such as the second-generation reactive diluent propoxylated trimethylolpropane triacrylic acid Ester (PO-TMPTA), compared with the first-generation reactive diluent trimethylolpropane triacrylate (TMPTA), it introduces a flexible chain into the molecule to ensure high activity, high solubility, and shrinkage of cured film. , flexibility and adhesion to the substrate are also improved, while the irritation to human skin is greatly reduced. It is used in various fields, such as chemical coatings, 3D printing, machinery production, automobile manufacturing, healthcare and aerospace, etc. [0003] Propoxylated trimethylolpropane i...

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): C08G65/28
CPCC08G65/2609C08G65/266Y02P20/584
Inventor 潘晨波王马济世寇然许林钧
Owner ZHEJIANG HUANGMA TECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap