A kind of unsaturated polyester prepolymer containing ketone group and its preparation method and application
A prepolymer and unsaturated technology, which is applied in the field of organic compound preparation, can solve the problem of difficult separation of protective reagents and achieve good application prospects, mild synthesis conditions, and wide selection of raw materials.
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Embodiment 1
[0032] (1) Synthetic diacetoacetate, as shown in the following formula:
[0033]
[0034]Add butanediol (9.0g, 0.1mol), ethyl acetoacetate (65g, 0.5mol), p-toluenesulfonic acid (0.28 g) and 100 mL of benzene. Azeotrope at a temperature of 90°C for 2 hours to remove water, then distill off the solvent, remove the ethanol generated by the reaction at high temperature, and raise the temperature to 130°C for 6 hours under normal pressure. After the reaction, 200 mL of ethyl acetate was added, washed 3 times with 5% aqueous sodium bicarbonate solution, 100 mL each time, and then washed 3 times with deionized water, and dried overnight by adding anhydrous magnesium sulfate to the organic phase. After anhydrous magnesium sulfate was filtered off, the solvent was distilled off under reduced pressure, and an oil pump was distilled under reduced pressure to obtain 23 g of colorless oily diacetoacetate with a yield of 65%. attached figure 1 Butanediol diacetoacetate 1 (bisacetoace...
Embodiment 2
[0039] (1) Synthetic diacetoacetate, as shown in the following formula:
[0040]
[0041] The number-average relative molecular mass of polyethylene glycol PEG400 is 400, and the average value of x is about 9.
[0042] In a 250mL flask equipped with a stirring rotor, an oil-water separator, a spherical condenser, and a drier, add PEG400 (10g, 0.025mol), ethyl acetoacetate (16g, 0.125mol), 732 type strongly acidic cation exchange resin (3.4 g) and 100 mL of benzene. Azeotrope at a temperature of 90°C for 2 hours to remove water, then distill off the solvent, remove the ethanol generated by the reaction at high temperature, and raise the temperature to 130°C for 6 hours under normal pressure. After the reaction, filter, and wash the ion exchange resin with a small amount of ethyl acetate, and incorporate into the filtrate. The filtrate was distilled under reduced pressure to remove the solvent and excess ethyl acetoacetate to obtain 14.8 g of colorless or light yellow oily ...
Embodiment 3
[0047] (1) Synthetic diacetoacetate, as shown in the following formula:
[0048]
[0049] The number-average relative molecular mass of polyethylene glycol PEG400 is 400, and the average value of x is about 9.
[0050] In a 250mL flask equipped with a stirring rotor, an oil-water separator, a spherical condenser, and a drier, add PEG400 (10g, 0.025mol), ethyl acetoacetate (16g, 0.125mol), 732 type strongly acidic cation exchange resin (3.4 g) and 100 mL of benzene. Azeotrope at a temperature of 90°C for 2 hours to remove water, then distill off the solvent, remove the ethanol generated by the reaction at high temperature, and raise the temperature to 130°C for 6 hours under normal pressure. After the reaction, filter, and wash the ion exchange resin with a small amount of ethyl acetate, and incorporate into the filtrate. The filtrate was distilled under reduced pressure to remove the solvent and excess ethyl acetoacetate to obtain 14.6 g of colorless or light yellow oily ...
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