Method for preparing oligomerized carbonic acid polyol ester
A technology of polyol ester and polycarbonate, applied in the direction of chemical instruments and methods, organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, etc., can solve the ether group content of oligocarbonic acid polyol ester High, reduced network structure density, poor product performance, solvent resistance or acid resistance, etc.
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Examples
Embodiment 2
[0031] The compounds listed in Example 2 and Example 3, different from the theoretical hydroxyl-functionalized target compound, have a terminal methyl ether group, and the content of the compound is determined by 1H NMR detection and the integral calculation of the corresponding signal. The amounts given can be considered as fractions of the listed compounds based on 1 mole of the theoretical target compound having two terminal hydroxyl groups.
Embodiment 1
[0033]Dimethyl carbonate (3.06 g) and 1-hexanol (6.94 g) were mixed with a fixed amount (5.7·10 -6 mol) of the catalyst (see Table 1) was mixed, and then the reaction vessel was sealed with a natural rubber septum having a gas outlet. When the catalyst used is solid at room temperature, it is initially dissolved with one of the reactants. The reaction mixture was heated to 80° C. for 6 hours with stirring. After cooling to room temperature, the product was analyzed using gas chromatography coupled with appropriate mass spectrometry. The content of reaction products (in particular methylhexyl carbonate and dihexyl carbonate) by which the activity of the transesterification catalyst used can be evaluated is determined by integral calculation of a specific gas chromatogram. The results of these activity studies are listed in Table 1.
[0034] Table 1
[0035] Contents of catalysts and reaction products used
[0036] Numbering
catalyst
Methylhexyl carb...
Embodiment 3
[0044] Embodiment 3 (comparative example)
[0045] Preparation of aliphatic oligocarbonate diols using known prior art catalysts
[0046] At the beginning, 1759 grams of 1,6-hexanediol and 0.02 grams of titanium tetraisopropoxide were charged to a 51 pressure reactor equipped with distillation attachment, stirrer and receiver. Nitrogen was introduced at a pressure of 2 bar and the mixture was heated to 160°C. Then 622.75 g of dimethyl carbonate were metered in over the course of 3 hours while the pressure rose to 3.9 bar. The reaction temperature was then raised to 180°C and a further 622.75 g of dimethyl carbonate were added over 1 hour. Finally, 1245.5 g of dimethyl carbonate were metered in again at 185° C. within 2 hours, during which time the pressure rose to 7.5 bar. After the addition was complete, the mixture was stirred at this temperature for a further 1 hour. During the entire transesterification process, the channels leading to the distillation unit and the rec...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More