Florentine flask

Fig. 5. Diagram of continuous separation of azeotropic mixture of trimethylchlo-rosilane and silicon tetrachloride, which contains acetonitrile. 1 is the tower for separating trimethylchlorosilane 2, 5, 6, 8 are the coolers 3 is the separating (Florentine) flask 4 is the tower for separating silicon tetrachloride 7, 9 are the collectors of the tower section 4. Pure silicon tetrachloride is is collected through cooler 8 in collector 9.

Fig. 46. Production diagram of branched methyloligodiphenylsiloxane 1,5- reactors 2, 6 - batch boxes 3, 8 - coolers 4 - Florentine flask 7,10 - collectors 9- receptacle...

The speed of the distillation of the azeotropic mixture (water + toluene) is regulated by supplying water into the jacket of reactor 1. The distilled water is collected in the lower part of Florentine flask 4, and the separated toluene is sent back into the reactor. To calculate the number of hydroxyl groups, the water poured out of the Florentine flask is measured and sent to biochemical purification. 

Fig. 48. Production diagram of tris ro-butoxyoligo[(propyleneoxy)(ethyleneoxy)-(dimethylsiloxy)] ethylsilane 7, 2, 9,11,12 - batch boxes 3, 10- reactors 4, 21 -coolers 5, 6, 8, 16, 17, 19, 22 - receptacles 7, 18 - pressure filters 13 - packed tower 14 - refluxer 75 - Florentine flask 20 - distillation tank 23 - container...

The target oligomer is synthesised in reactor 10. For this purpose, Laprol is loaded from batch box 11, and toluene is loaded from batch box 12. The agitator is switched on, the temperature in the reactor is increased to 110-130 °C (to 85-110 °C in vapours) by sending vapour into the jacket and at this temperature toluene is subjected to azeotropic drying. The vapour of the azeotropic mixture (toluene + water) rises up packed tower 13 and condenses in refluxer 14. The condensate splits in Florentine flask 15. Toluene from the top part of the apparatus is sent back (through a side choke) to reflux tower 13, and toluene-containing water is collected in receptacle 16. Thus the toluene solution of Laprol is dehydrated until moisture content is not more than 0.01%. 

Fig. 57. Diagram of the hydrolytic condensation of dimethyldichlorosilane by the periodic technique ./, 9, 12 - containers 2, 6 - pumps 3, 5 - coolers 4 - hydrolyser 7 - hydraulic gate 8 - Florentine flask 10 - neutraliser 11 -settling box...

The hydrolysate, which is a mixture of linear and cyclic dimethylsilox-anes and hydrochloric acid, is continuously diverted from hydrolyser 4 into Florentine flask 8 for separation. The process is based on the difference of the densities of the hydrolysate (0.96 g/cm3) and hydrochloric acid (1.12 g/cm3) and insignificant solubility of the hydrolysate in hydrochloric acid. The hydrolysate in apparatus 8 remains in the top layer, whereas hydrochloric acid goes to the bottom. When the mode is established, hydrochloric acid is poured into tanks, and the hydrolysate with up to 0.4% of hydrochloric acid is sent into collectors 8 (the diagram shows one) and pressurised by nitrogen flow into apparatus 10 for neutralisation. Collectors 9 operate at regular intervals while one accepts the hydrolysate, the other issues the hydrolysate for neutralisation. Hydrogen chloride from the... 

The hydrolytic condensation of methyltrichlorosilane is carried out in hydrolyser 6, which is a shell-and-tube heat exchanger cooled with salt solution (-15 °C). Before introducing it into the hydrolyser, the reactive mixture is mixed (in its bottom part) with acetone this mixture then enters the capillaries. At the same time the bottom part of the hydrolyser is filled with water. The reaction takes place in the tubes of the apparatus. The product of hydrolytic condensation is cooled and through the top of the hydrolyser is sent into tower 7, which is a Florentine flask, to split into the aqueous and organic layers. 

The bottom layer, the acidic aqueous-acetone solution, is sent through a hydraulic gate to be neutralised in apparatus 11 the top layer, the toluene solution of the product of hydrolytic condensation, is sent into flusher 12, which is also a Florentine flask. At the same time the flusher is filled with a 10-20% solution of sodium chloride, heated to 50-60 °C. The processed solution of sodium chloride is sent through a hydraulic gate into neutraliser 11, and the toluene solution of the product of hydrolytic condensation is... 

Fig. 65. Production diagram of polymethylsilsesquioxane varnish by the continuous technique 1, 2, 4, 5,8, 10 - batch boxes 3 - agitator 6 - hydrolyser 7, 12 -Florentine flasks 9 - heat exchanger 11 - neutraliser 13 - flusher-receptacle 14, 16, 18 - collectors, 15 - vacuum distillation tank 17 - cooler 19 - balancing tank 20 - druck filter...

Fig. 68. Production diagram of polyphenylsilsesquioxane from triacetoxyphenylsi-lane 1 - 4 - batch boxes 5 - reactor 6, 12 - coolers 7 - Florentine flask 8 - nutsch filter 9, 10, 13 - collectors 11 - distillation tank...

The azeotropic drying of potassium acetate is carried out with toluene, fed into reactor 5 from batch box 4. The excess of toluene is sent through Florentine flask 7 into collector 9 and from there to regeneration. 

Fig. 71. Production diagram of polydimethylphenylsiloxane and polymethylphen-ylsiloxane varnishes by the continuous technique 1 - weight batch box 2 - tower 3, 5,1 - hydro ejectors 4, 6, 8 - Florentine flasks 9 - container 10 - agitator 11 -distillation tank 12 - condensation apparatus...

A toluene solution of organochlorosilane mixture is sent from weight batch box 7 into jet mixer (hydroejector) 3 with a certain amount of water. The consumption of the components is monitored by rotameters. The reaction of hydrolytic cocondensation takes place in the mixing chamber of hydroejector 3. To complete the hydrolytic cocondensation, the reactive mixture is sent into tower 2, from where the mixture is poured into Florentine flask 4. There the products of hydrolytic cocondensation and hydrochloric acid split. 

The acid is sent to biochemical purification, and the hydrolysate is subjected to two-stage flushing with water in hydroejectors 5 and 7. The hydrolysate is flushed until pH is 5- 6 and separated from flush waters in Florentine flasks 6 and 8 and in container 9. 

Fig. 106. Diagram of continuous production of O-ethyldichlorothiophosphate (ethyl dichloride) 1 - synthesis reactor 2, 3, 8 - batch boxes 4 - flusher 5 - Florentine flask 6 -neutraliser 7- agitator 9- dichloride collector 10- collector...

After flushing the reactive mixture is continuously sent to separate in Florentine flask 5. The top acid aqueous alcohol layer from Florentine flask (the alcohol content —23%) is sent through a siphon into neutraliser 6 at agitation. The acid aqueous alcohol layer is neutralised with 10% alkali... 

The lower layer, flushed ethyl dichloride, continuously moves out of Florentine flask 5 through a siphon into dichloride collector 9. 

Fig. 110. Production diagram of O-methyldichlorothiophosphate (methyl dichloride) and 0,0-dimethylchlorothiophosphate (methyl monochloride) 1, 10 - synthesis reactors 2, 3, 9, 11, 12 - batch boxes 4 - ager 5 - flusher 6 - cooler 7-Florentine flask 8, 14-16 - collectors 13 - flushing settling box...

In continuous steam distillation, an insulated conveying system with superheated steam as carrier is used for providing a countercurrent flow of steam and pulverised plant material. During transport, the oil is transferred into the vapour phase and exits the system with the steam. A cyclonic vessel separates the gas phase from the solid phase. In the last step the gas phase (steam and oil) is condensed, the oil is separated using a Florentine flask and the water recycled to the boiler [27]. 

I chose a Florentine flask, on account of its lightness, capacity, and shape, which is peculiarly adapted to the experiment for the vapours raised by the ebullition circulated for a short time, thro the wide cavity of the vial, but were soon collected upon its sides, like dew, and none of them seemed to reach the neck, which continued perfecdy dry to the end of the experiment. ... 

FIGURE 4.18 (See color insert following page 468.) Oil and muddy water in the Florentine flask. 

FIGURE 4.19 Orris distillation, Florentine flask at nearly 98°C. 

FIGURE 4.24 Scheme of the BIOLANDES continuous production unit. A biomass B distillation vat C condenser D Florentine flask E extraction unit F solvent recovery G exhausted biomass. 

The following is a controversial method for essential oil extraction by comparison with classical hydrodistillation methods. In this method, the steam enters the distillation chamber from the top passes through the biomass in the still pot (e.g., the distillation chamber) and percolates into the condenser located below it. Separation of the oil from the aqueous phase occurs in a battery of Florentine flasks. It is claimed that this method is very gentle and thus suitable for the treatment of sensitive plants. The biomass is held in the still chamber (e.g., still pot) on a grid that allows easy disposal of the spent plant matter at the completion of the distillation. The whole apparatus is relatively small, distillation times are reduced, and there is less chance of the oil being overheated. It appears that this method is fairly costly and thus likely to be used only for very high-priced biomass. 

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