The invention relates to a preparation method of tough SiO2 
aerogel fibers post-processed through 
isocyanate. The preparation method comprises steps as follows: a 
spinning solution is prepared from 
silicate or 
silanol sol; an acid solution is used for a coagulating bath; the 
spinning solution is added to the coagulating bath, the mixture has a reaction, wet 
spinning is performed, orthosiliconic acid / 
silicate fibers are obtained, wound, aged, washed, soaked in a 
tetrahydrofuran solution of 
isocyanate for 48 h, then taken out and washed with 
acetone, 
solvent replacement is performed through water or 
ethanol, and the tough SiO2 
aerogel fibers are obtained after 
drying. The method has the characteristics that the raw materials are cheap and easy to obtain, the reaction process is simple, and the spinnability is good; the SiO2 
aerogel fibers are toughened through high polymers, the prepared tough SiO2 aerogel fibers have rich pores, a high specific surface area and certain 
toughness and is high-temperature-resistant and chemical-
corrosion resistant, and the specific surface area of the fibers is adjustable.