The invention relates to a
continuous production method of high-purity tetraethoxysilane, and belongs to the technical field of tetraethoxysilane preparation. The method comprises a
raw material pretreatment stage and a purification and rectification stage: in the pretreatment stage,
silicon tetrachloride and
ethanol are subjected to an
esterification reaction in a
molar ratio of 1: (3-4) under the protection of
nitrogen, the pH is adjusted to be neutral through
triethylamine, and
triethylamine hydrochloride is removed through reduced pressure
distillation; then, a
cerium oxide-
molecular sieve composite adsorbent with the specific surface area larger than or equal to 800 m / g and the
pore diameter of 2-5 nm is adopted for
dehydration under the pressure of 0.8-1.2 MPa till the
water content is smaller than or equal to 5 ppm, and volatile impurities are removed through high-purity
nitrogen purging; in the purification stage,
metal ions and Cl are synergistically removed through a
titanate modified resin layer and a nano TiOtube layer, and then step-by-step separation is performed through a four-stage
differential pressure rectifying
tower. Through collaborative optimization of structural design of the composite adsorbent, construction of an organic-inorganic
hybrid interface of the resin layer and pressure gradient rectification, 72-hour
continuous production is achieved, the single-pass yield of the product is 92%, and the total amount of
metal impurities is smaller than or equal to 5 ppb.