A kind of nickel complex optical limiting material and preparation method thereof
A technology of nickel complexes and optical limiting, applied in the field of nickel complexes and their preparation, to achieve the effects of wide limiting band, good solubility, and good optical limiting effect
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[0039] 1. Synthesis of Intermediate 1
[0040] In a 500mL round bottom flask, add 12.02g (0.1mol) of diethylene glycol monomethyl ether and dissolve it in 90mL of dichloromethane, add 0.32g catalyst 4-butylammonium bromide and 100mL of a mass concentration of 30% NaOH aqueous solution, Stir and mix evenly, dissolve 32.41g (0.17mol) of 4-methylbenzenesulfonyl chloride in 100mL of dichloromethane and add it dropwise to the reaction system. Once, dry over anhydrous magnesium sulfate for 8-12 hours, take the filtrate after suction filtration, remove the solvent by rotary evaporation, and refrigerate at -2~-6°C for 8-12 hours to obtain the intermediate 1-p-toluenesulfonyl polyethylene glycol 24.4 g of monomethyl ether is a white ice-like solid, and the yield is 89%.
[0041] 1 HNMR (CDCl 3,400MHz,ppm)δ(ppm)=2.46(s,3H),3.28(q,3H),3.42(q,2H),3.53(t,2H),3.67(t,2H),4.28(t,2H ),7.49(d,2H),7.83(d,2H).
[0042] 2. Synthesis of Intermediate 2
[0043] Add NaH4.80g (0.20mol) and 25mL ...
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