The invention discloses a preparation process of microcrystal vacuum glass. The microcrystal vacuum glass is prepared from, by weight, 30-80% of vanadium-titanium-containing iron tailings, 15-60% of fluorite tailings, 1-50% of dolomite and 10-20% of sodium carbonate and by mass, 5-7 parts of magnesium oxide, 20-24 parts of zinc oxide, 9-10 parts of aluminum oxide, 145-160 parts of arsenic oxide and 2-3 parts of boron oxide. By means of the preparation process, the service life of a glass product is effectively prolonged, and the safety performance and transparency of the glass product are effectively improved.