The reactants, with petrol ether or benzene as solvents, were kept as cold as was possible without a change in phase. Because they react with moist air, the molecular compounds that formed were analysed in the solvent. They were also analysed as dry solids, for these could be recovered by filtering and vishing the precipitates in an atmosphere of nitrogen, followed by complete drying in vacuum. The same analytical method washed for the analyses of the addition compound, whether they were dry solids, or were still immersed in anhydrous solvent.
First, technology took high purity SiCl4 (99.99 wt. %) into photo reactor at the protection of N2 (-150ć) to react with Cl2 for getting primary production. (The purity of Cl2 can be 99.99%, reacting temperature can be at 20- 60ć, reacting pressure can be at 0.3-2Mpa) column (stainless steel) to remove low boiling fractions and high boiling fractions continuously. Then, transfer primary product into flash tower from the top of flash tower, and N2 would come into tower from the bottom of tower, so some Cl2 which do not react with high purity SiCl4 can be removed, and the secondary product can be got. Next, it should transfer secondary product into purification towers, ultra would be got after continuous remove low and high boiling points components. (the reflux ratio can 2-10, the towers can be stainless steel. The pressure can be at 0.2-0.5Mpa), the process flow diagram was showed in Figure 1. The purity of this Product made by technology can be up to 99.9999%, the infrared transmission of most persuades can meet or exceed the indexes of SiCl4 of Mark Company, having meet the requirement of ultra-purity SiCl4.
Using GC tested the chlorosilane impurities content of SiCl4 prepared by this technology; using ICP-MS tested the content of metals impurities; using FT-IR tested the content of impurities with hydrogen. Technology established one online sampling system, which can sample and test online to realize the isolation between detecting system and surrounding, guaranteeing veracity of test results. By those methods, the purification effect was evaluated and improved.
Keep in a tightly sealed container (corrosion resistant) under inert(N2) atmosphere. Store in a cool, dry, well-ventilated area. Containers which are opened must be carefully resealed and kept upright to prevent leakage.
SiCl4 react aggressive with H2O so I can not understand what is your problem with drying. Most (if not all) of water will be destroyed before distillation : SiCl4 + 2H2O -> SiO2 + 4HCl