Cocondensation apparatus

Figure 3.1 Macroscale stationary cocondensation apparatus for investigations of metal atom chemistry. (From Ref. 514, reproduced with permission.)...

Simultaneous with this work, Ozin and co-workers were independently investigating other bimetallic combinations. When Cr and Mo were cocondensed (133) together in Ar, using the apparatus shown in Fig. 11, a controlled pathway to CrMo was found. This molecule had previously been observed in the gas phase (30) from flash photolysis of a mixture of Cr(CO)6 and Mo(CO)g vapors. The molecule was identified (UV-visible spectroscopy) by a series of Cr/Mo/Ar concen-... 

Fig. 2, Apparatus for cocondensing a metal vapor and the vapor of a compound on a gram scale.

Hydrolytic cocondensation is carried out in enameled hydrolyser 7 with a water vapour jacket and an agitator. The hydrolyser is filled with a required amount of water then, under the water layer, the reactive mixture is sent through a siphon from batch box 6. The temperature during hydrolytic cocondensation should not exceed 50-55 °C. Most of the released hydrogen chloride dissolves in the water in the apparatus, and the excess of HC1 passes through backflow condenser 8 and enters tower 9, where is absorbed by water. The vapours of water and reaction products, which are entrained by hydrogen chloride and condensed in the backflow condenser,... 

The settled bottom layer (18-20% hydrochloric acid) is poured through a run-down box into collector 7, and the top layer, the product of hydrolytic cocondensation, is sent into settling box 8. After 2 hours of settling in the apparatus, the top layer is separated from the remaining acid at agitation and 20-25 °C the apparatus is gradually, within 30 minutes, filled through a hatch with a a calculated amount of diy soda ash. The mass is mixed for 1 -2 hours. After that, the medium is sampled for acidity. If the reaction is acid, some soda (as calculated) is added into the apparatus after an addi-... 

The neutralised and dried products of hydrolytic cocondensation are heated to 50 °C in apparatus 10 with vapour (0.3 MPa) sent into the jacket. The apparatus is loaded through a hatch with kil clay (8% of the quantity of the loaded cocondensation product) or cationite KU-23 (1-3%) and agitated at 80 °C for 2-3 hours. Then it is poured into receptacle 11 and by nitrogen flow (0.3 MPa) is sent to pressure filter 12, where clay (or cationite)... 

To flush the product of hydrolytic cocondensation, the hydrolyser is loaded with a calculated amount of water, the contents of the apparatus are agitated for 30 minutes and settled for 1 hour. The lower layer, the flushed solution of the product, is sent into collector 11, and the upper layer (flush waters) is sent into neutraliser 10 and at pH 6-8 is sent to biochemical purification. 

The product from collector 6 is loaded into agitator 8. The apparatus also receives the depolymerisate obtained in the production of SKT. The working mixture is prepared. To obtain SKTV, one takes 0.42 kg of the cocondensation product per 100 kg of the depolymerisate to prepare SKTV-1, 2.1 kg of the cocondensation product per 100 kg of the depolymerisate. The mixture is apparatus 8 is agitated with pump 9 (by circulation) for 3 hours and sampled. If the content of vinylmethylsiloxy elements is appropriate, the working mixture is sent from apparatus 8 with pump 9 into collector 10 and from there to copolymerisation. 

Further polycondensation of the the product of hydrolytic cocondensation (silanol) is carried out as toluene is distilled in apparatuses 15, which are steel enameled apparatuses with anchor agitators and water vapour jackets. As one of apparatuses 15 is filled, silanol is clarified before the distillation of toluene, i.e. separated from traces of moisture, by settling at 70-90 °C. The remaining water is also poured into receptacle 14. 

From container 9 the flushed hydrolysate is sent to partially distil the solvent into tank 77 to produce modified polymethylphenylsiloxane varnishes, it is first mixed with polyester or epoxy polymer in apparatus 7 0, and then sent into the tank. From the tank, the hydrolysate is sent to condensation into three-sectioned apparatus 12. In the first section the solvent is additionally distilled and the product of the hydrolytic cocondensation is partially condensed in the second section it is further condensed at 125-... 

The process of hydrolytic cocondensation is carried out in hydrolyser 10, which is (just as vacuum distillation tank 13) an enameled apparatus with an agitator and a water vapour jacket. 

After the reactive mixture has been introduced, it is kept in the reactor at 150-160 °C for 6-8 hours and sampled to determine the phenylethoxysi-lane content. The content of phenylethoxysilanes (equivalent to phenyl-triethoxysilane) should not be less than 65%. After the synthesis the reactive mixture is cooled to 40-60 °C by sending water into the jacket of the apparatus. The cooled mixture of phenylethoxysilanes, the so-called phenyl paste, is sent into hydrolyser 14 to hydrolytic cocondensation. 

Figure 5. Diagram of Timms ry-freeze " apparatus used for cocondensation of germanium vapor and tiimethylsilane...

Fluorine. An improved synthesis of N3F from a diluted, gaseous mixture of HN3 and F2 in a stainless steel apparatus is described in [33] this method also is suited to generate the N-substituted isotopomers [34]. Earlier investigations of this reaction are given in Fluorine Suppl. Vol. 4, 1986, pp. 405/6, and Fluor Erg.-Bd. 1, 1959, p. 247. Annealing cocondensed HN3 and F2 in Ne or N2 matrices results in formation of HF other bands can be assigned to the HN3 HF moiety [35]. 

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