Hydrophobically associating polymer and preparation method thereof
A hydrophobic association, polymer technology, applied in drilling compositions, chemical instruments and methods, luminescent materials, etc., can solve the problems of researching hydrophobic association polymers, single nature, disadvantage and so on
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[0023] The present invention also provides a method for preparing a hydrophobically associated polymer, the method comprising the following steps:
[0024] (1) In the presence of an inert gas and a first organic solvent, under weakly alkaline conditions, utilize p-toluenesulfonyl chloride (TsCl) to activate the terminal hydroxyl groups of polyethylene glycol (PEG) to obtain an activated polyethylene glycol solution; Wherein, the effect of the above-mentioned p-toluenesulfonyl chloride is to activate the terminal hydroxyl group of polyethylene glycol, and its addition amount is suitable for satisfying the effect on the activation of the terminal hydroxyl group. Preferably, the molar ratio of PEG to TsCl is 1:1-2; the first The amount of organic solvent can be the amount of conventional reaction solvent, for example, the weight ratio of PEG to the first organic solvent is 1:10-50;
[0025] (2) In the presence of an inert gas and a second organic solvent, mix pyrene methanol (PyM...
Embodiment approach
[0034] According to a preferred embodiment of the present invention, the method also includes purifying the product obtained in step (3), the method of purifying includes: removing part of the reaction solution by rotary evaporation, precipitating the remaining solution dropwise in diethyl ether, and removing the precipitate After filtration, it was dissolved in methanol and placed in dry ice. The hydrophobic association polymer product precipitated and was collected by filtration. This step is preferably repeated 2-3 times to remove impurities and unreacted chemical reagents in the product. The obtained pyrene hydrophobically modified polyethylene glycol product can be dried under vacuum.
[0035] According to a preferred embodiment of the present invention, step (1) also includes purifying the activated polyethylene glycol product, the method of said purification comprising: removing part of the reaction solution by rotary evaporation, and precipitating the remaining solutio...
specific Embodiment approach
[0037] According to a specific embodiment of the present invention, the preparation method of the hydrophobic association polymer is as follows figure 2 As shown in the reaction flow diagram, it specifically comprises the following steps:
[0038] (1) Dissolve quantitative PEG in dichloromethane (DCM) at 0°C and inert gas. The weight ratio of PEG to DCM is 1:20. After adding an appropriate amount of triethylamine (TEA), add the excess For p-toluenesulfonyl chloride (TsCl), the weight ratio of PEG to TEA is 1:10, and the weight ratio of TEA to TsCl is 10:1, and magnetic stirring is carried out. After 12-20 hours, the reaction solution was removed by rotary evaporation and precipitated dropwise in ether at 0°C. The precipitate was collected by filtration and the precipitation process was repeated 2-3 times to remove impurities and unreacted chemical reagents in the product. . The final product was vacuum dried at 40-50°C.
[0039](2) Dissolve excessive pyrenemethanol (PyMe) ...
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