Polyhydroxy-containing polymer and preparation method and application thereof
A technology of polymer and hydroxyl, which is applied in application, drug delivery, pharmaceutical formulation, etc., can solve the problems of limited curative effect and few products on the market, and achieve the effect of strong adhesion and good biocompatibility
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[0049] The preparation method of the present invention will be further described in detail in conjunction with specific examples below. It should be understood that the following examples are only for illustrating and explaining the present invention, and should not be construed as limiting the protection scope of the present invention. All technologies realized based on the above contents of the present invention are covered within the scope of protection intended by the present invention.
[0050] The experimental methods used in the following examples are conventional methods unless otherwise specified; the reagents and materials used in the following examples can be obtained from commercial sources unless otherwise specified.
[0051] Material Structure Test 1 HNMR, 13 CNMR was measured by a 600-megapulse Fourier transform nuclear magnetic resonance spectrometer from JOEL; IR was measured by a Fourier transform infrared spectrometer nicolet is50 from Thermofisher; the Tg...
Embodiment 1
[0054] Polybutadiene: commercial polybutadiene block (purchased from Sichuan Petrochemical Co., Ltd., 1,4-cis content ≥ 98%, and 2% 1,4-trans and the structure shown in formula 4 ; Number average molecular weight ) into about 2mm rubber particles.
[0055] Epoxidation: In a 250ml three-necked flask equipped with a stirrer and a thermometer, add 7g of the above-mentioned polybutadiene colloidal particles and 100ml of dichloromethane. Dissolve and stir in a constant temperature water bath. When it is completely dissolved into a viscous shape, nitrogen gas is introduced for several minutes. Add 9.90g of formic acid, and dropwise add 21.40g of 30% hydrogen peroxide aqueous solution while stirring; continue the heat preservation reaction for about 15h, 1 HNMR (CDCl 3 ) analysis, the 1,4-cis double bond characteristic chemical shift peak disappeared (epoxy group characteristic chemical shift δ=2.98, 1,4-cis double bond characteristic chemical shift δ=5.40). The reaction product...
Embodiment 2
[0058] Polybutadiene: Add 180ml of dry petroleum ether (60-90°C) to a 500ml anhydrous and oxygen-free reaction bottle, and dry 1,3-butadiene (Chengdu Keyuan Gas Co., Ltd., purity greater than or equal to 99.5%), absorbed to butadiene 20g. Seal the reaction bottle, put it in a water bath at 40°C, inject 0.4ml of the aging solution of nickel naphthenate and triisobutylaluminum while stirring, and then inject 0.38ml of BF 3 Diethyl ether complex and 0.4ml of n-octanol were stirred for 2h, and 2ml of ethanol was added to terminate the reaction. 200ml of absolute ethanol was added to the reaction solution, and a solid gel was precipitated. After drying, 19 g of polycis-1,4-butadiene was obtained. GPC analysis polybutadiene number average molecular weight 91000. As determined by HNMR, the cis-1,4 double bond ratio is 98.5%, and the gel content is less than 0.1%.
[0059] Epoxidation: step is with embodiment 1.
[0060] Hydrolysis: Step Example 1.
[0061] The prepared solid pr...
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