A kind of preparation method of pulp, fabric bleaching catalyst ligand
A technology for fabric bleaching and catalyst, which is applied in the field of preparation of bleaching catalyst ligands, can solve problems such as environmental protection restrictions, and achieve the effects of less three wastes, simple preparation method, and easy-to-obtain raw materials
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Embodiment 1
[0017] Ⅰ, Synthesis of 1,4,7-triphenylsulfonyl-diethylenetriamine, add 2000ml of clear water, 100 grams of diethylenetriamine, 390 grams of sodium carbonate, 520 grams of benzenesulfonyl chloride pre-melted liquid in a 5000ml four-necked flask (melting point 14.5°C). Under stirring, react at 60°C for 2 hours, 80°C for 4 hours, cool down to 40°C, filter out the white solid with suction, rinse twice with an appropriate amount of water to obtain the white solid of sulfonylated diethylenetriamine 1,4,7 - 482 grams of triphenylsulfonyl-diethylenetriamine, yield 96.7%, HPLC purity 97.3%.
[0018] Ⅱ. Synthesis of 1,4,7-triphenylsulfonyl-1,4,7-triazacyclononane, in a 3000ml four-neck flask equipped with a stainless steel turbine stirring paddle, adding 1500ml of N,N-diethyl base formamide, 482 grams of 1,4,7-triphenylsulfonyl-diethylenetriamine, 480 grams of potassium carbonate, the temperature is controlled at 75°C to 90°C, 115 grams of ethylene glycol dicarboxylate is added dropwis...
Embodiment 2
[0021] Ⅰ, Synthesis of 1,4,7-triphenylsulfonyl-diethylenetriamine, add 2000ml of clear water, 100 grams of diethylenetriamine, 380 grams of sodium carbonate, 520 grams of benzenesulfonyl chloride pre-melted liquid in a 5000ml four-necked flask (melting point 14.5°C). Under stirring, react at 60°C for 2 hours, 80°C for 5 hours, cool down to 40°C, filter out the white solid with suction, rinse twice with an appropriate amount of water to obtain the white solid of sulfonylated diethylenetriamine 1,4,7 - 482 grams of triphenylsulfonyl-diethylenetriamine, yield 96.7%, HPLC purity 97.3%.
[0022] Ⅱ. Synthesis of 1,4,7-triphenylsulfonyl-1,4,7-triazacyclononane, in a 3000ml four-neck flask equipped with a stainless steel turbine stirring paddle, adding 1500ml of N,N-diethyl base formamide, 482 grams of 1,4,7-triphenylsulfonyl-diethylenetriamine, 480 grams of sodium bicarbonate, the temperature was controlled at 75 ° C ~ 90 ° C, 115 grams of ethylene glycol diacetate was added dropwis...
Embodiment 3
[0025] Ⅰ, Synthesis of 1,4,7-triphenylsulfonyl-diethylenetriamine, add 2000ml of clear water, 150 grams of diethylenetriamine, 600 grams of sodium carbonate, 780 grams of benzenesulfonyl chloride pre-melted liquid in a 5000ml four-necked flask (melting point 14.5°C). Under stirring, react at 60°C for 2 hours, 80°C for 7 hours, cool down to 40°C, filter out the white solid with suction, rinse twice with an appropriate amount of water to obtain the white solid of sulfonylated diethylenetriamine 1,4,7 -724 grams of triphenylsulfonyl-diethylenetriamine, yield 96.8%, HPLC purity 97.3%.
[0026] Ⅱ. Synthesis of 1,4,7-triphenylsulfonyl-1,4,7-triazacyclononane, in a 3000ml four-neck flask equipped with a stainless steel turbine stirring paddle, adding 1500ml of N,N-diethyl base formamide, 724 grams of 1,4,7-triphenylsulfonyl-diethylenetriamine, 750 grams of sodium bicarbonate, the temperature is controlled at 75 ° C ~ 90 ° C, 173 grams of ethylene glycol dicarboxylate is added dropwi...
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