Sulfonated calixarene modified polyurethane tanning agent and preparation method thereof
A technology of sulfonated calixarene and polyurethane tanning agent, which is applied in the field of polymer materials, can solve the problems of weak combination and easy loss of sulfonated calixarene, and achieve the effect of solving the problem of weak combination and easy loss
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[0024] A preparation method of sulfonated calixarene modified polyurethane tanning agent (SCA-WPU), specifically comprising the following steps:
[0025] Step 1, the preparation of p-tert-butylcalixarene:
[0026] Add 8g of p-tert-butylcalixarene, 0.1g of sodium hydroxide particles, and 6mL of formaldehyde solution into a three-necked flask equipped with oil bath heating, mechanical stirring, and reflux condenser device, and react at 110°C for 2h, then cool down to room temperature; add 40mL of diphenyl ether, reheat to 100°C, react for 0.5h; continue to heat up to 180°C, react for 2h, cool down to room temperature; add 40mL of ethyl acetate, stir for 0.5h, static suction filtration, successively use acetic acid Ethyl ester, acetic acid, and water were washed to obtain a white powder, which was p-tert-butylcalix[4]arene, and was designated as substance A.
[0027] Step 2, preparation and purification of sulfonated calixarene (SCA):
[0028] Add 15 mL of concentrated sulfuric...
Embodiment 1
[0035] Step 1: preparation of p-tert-butylcalixarene;
[0036] Add 8g of p-tert-butylcalixarene, 0.1g of sodium hydroxide particles, and 6mL of formaldehyde solution (37wt%) into a three-necked flask equipped with oil bath heating, mechanical stirring, and reflux condenser device, and react at 110°C 2h, then cool down to room temperature; add 40mL diphenyl ether, reheat to 110°C, react for 0.5h; then continue to heat up to 180°C, react for 2h, cool down to room temperature; add 40mL ethyl acetate, stir for 0.5h, static suction filtration , followed by washing with ethyl acetate, acetic acid, and water to obtain a white powder, which is p-tert-butylcalix[4]arene, which is designated as substance A.
[0037] Step 2: preparation and purification of sulfonated calixarene;
[0038] Add 15 mL of concentrated sulfuric acid to 2 g of substance A in a three-necked flask, and stir in a water bath at 80° C. for 4 h to obtain a dark purple viscous liquid. Dilute with water, filter with ...
Embodiment 2
[0042] Step 1: preparation of p-tert-butylcalixarene;
[0043] Add 8g of p-tert-butylcalixarene, 0.1g of sodium hydroxide particles, and 6mL of formaldehyde solution (37wt%) into a three-necked flask equipped with oil bath heating, mechanical stirring, and reflux condenser device, and react at 110°C 2h, then cool down to room temperature; add 40mL diphenyl ether, reheat to 110°C, react for 0.5h; then continue to heat up to 180°C, react for 2h, cool down to room temperature; add 40mL ethyl acetate, stir for 0.5h, static suction filtration , followed by washing with ethyl acetate, acetic acid, and water to obtain a white powder, which is p-tert-butylcalix[4]arene, which is designated as substance A.
[0044] Step 2: preparation and purification of sulfonated calixarene;
[0045] Add 15 mL of concentrated sulfuric acid to 3 g of substance A in a three-necked flask, and stir in a water bath at 80° C. for 4 h to obtain a dark purple viscous liquid. Dilute with water, filter with ...
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