Polyester macromers containing 1,1-dicarbonyl-substituted 1-alkenes
A technology of macromonomers and dihydrocarbyl dicarboxylates, which is applied in the field of preparing the novel compounds and compositions, and can solve problems such as difficult crosslinking of polyesters
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[0126] The following examples are provided to illustrate the invention and are not intended to limit its scope. All parts and percentages are by weight unless otherwise indicated.
[0127] A typical reaction procedure is described as follows: A 100 mL three-necked round bottom flask with distillation head, thermometer, vacuum adapter and collection flask was assembled using high vacuum grade grease along with a heating mantle, thermocouple and magnetic stir bar. The reaction mixture is stirred, typically in the range of 400-600 rpm. Vacuum was used to remove subsequent by-products from the reaction mixture, the different pressures are indicated below along with the mixing time in each case. In some cases, nitrogen was used instead of vacuum to flush the mixture, and where applicable, as indicated below. In each case, molar equivalents are relative to the diethylmethylenemalonate ("DEMM") monomer used.
[0128] The reaction mixture was analyzed by NMR spectroscopy using 300 ...
Embodiment 1
[0135] Example 1 - Preparation of Difunctional Monomers from Pentylene Glycol and DEMM
[0136] A round bottom flask was charged with DEMM (172 g, 1 mol), pentanediol (26 g, 0.25 mol) and 5 wt % CALB lipase enzyme (8.6 g) (purchased from CLEA) based on DEMM. The round bottom flask was placed on a rotary evaporator preheated to 45 °C and a pressure of 150 mm Hg was applied. After 1 hour, the reaction was checked for completion by GCMS and HNMR. Once the pentanediol is consumed, the reaction is complete. The product mixture was about a 65 / 35 mixture of difunctional monomer and DEMM. Filter the reaction mixture to remove enzymes. A 3-neck round bottom flask equipped with a mechanical stirrer, thermometer and condenser was charged with the resulting reaction mixture. The reaction mixture was distilled at 65 °C and a pressure of <0.800 mmHg for 2 hours or until the amount of difunctional monomer was less than 65% by weight of the solution. A typical product composition is: 67%...
Embodiment 2
[0138] Example 2 - Termination of Diethyl Malonate with Pentylene Glycol
[0139] A round bottom flask was charged with pentanediol (260 g, 2.5 mol), DEM (159 g, 1 mol) and 7 wt% CALB lipase enzyme (18 g) (purchased from CLEA) based on pentanediol. The round bottom flask was placed on a rotary evaporator and preheated to 45 °C, and a pressure of 150 mm Hg was applied. After 1 hour, the reaction was checked for completion by GCMS and HNMR. Once the DEM is consumed, the reaction is complete. Filter the reaction mixture to remove enzymes. A 3-neck round bottom flask equipped with a mechanical stirrer, thermometer and condenser was charged with the reaction mixture which was distilled at 100 °C and below 0.800 mmHg for 2 hours or until the amount of pentanediol was about 10% by weight (as determined by GCMS). A typical product composition is about 90% by weight pentylene glycol-terminated diethyl malonate and about 10% by weight pentylene glycol.
[0140]
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Abstract
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