Vacuum filter

C. Big secret 2...Quack ...One MUST filter this 600+ ml of ether...but a duck can t do this all at once...so one must fitter in vacuum filter in 200 ml portions...changing the duck paper every time and wash the filter cake with ether...Dr. Quack thinks a vacuum filter (apirator) at this stage is a must..Quack ... 

D. Now the ether will be a deep reddish yellow. Distill off the ether...quack...and take the temp up to 170 C to drive off any other volatiles. Should recover 90%+ of the original weight of oil. Now add 500 ml of saturated bisulfite and stir for 1.5 hours...Quack Vacuum Filter, the duck fat crystals Wash with water and ether, yield dull fine ppt in the filter cake...stable bisulfite addition product...can be stored forever...QuackU Yield -50 to 80% depending on a ducks technique ... 

Of course, there are a couple advantages to using HCI as the hy-drolyzer. Since using hydrochloric acid means that all that fat MDA or amphetamine is in the water solution, the chemist can vacuum filter the solution to get rid of all the tar and crap which will give a remarkably clean water solution. The X is released by basifying and extracting with solvent. 

In a flask the chemist mixes 50g piperonal into 200mL glacial acetic acid, then adds 45mL nitroethane and 17g ammonium acetate. The solution is then refluxed 4 hours and takes on the color of yellow to yellow-orange. After 4 hours and cooling, yellowish crystals of p-nitropropene will spontaneously form. If not, the solution can be diluted with 50ml of dHjO and chilled in an ice bath for an hour to form the crystals with some slushy glacial acetic acid and water intermixed. The mass of crystals is broken up and plopped into a Buchner funnel to be vacuum filtered. The filter cake is washed with a little extra acetic acid or water. All of the filtrate is saved. 

The Ingredients are placed in a reflux set-up and left for three hours. They are then vacuum filtered from the solids and then distilled with vacuum, it s quite simple. 

Vacuum filtering can be a bit tricky, as the filter paper clogs up very quickly and stalls the process. With this stuff it is particularly important to get rid of as much of the solids as possible or your distillation be will very messy. A way round that I have found (that isn t in any book) was to use loads of filter papers, throw them all into a big beaker and then rinse them with solvent, then filter the solvent. Filter tiny amounts at a time, as soon as the paper blocks - stop and change the paper. I normally run the filtrate through at least twice. Any way you can make sure that you have done two... 

What s left in the water now needs to be vacuum filtered and dried. This should be done carefully and under the fume hood. Up to this point the chemistry will have taken around 30 minutes, the drying might take a day or so. Often bromine liquid stays hanging around the crystals which makes them nasty, leave in the buchner funnel of your vacuum filter overnight to get rid of all that bromine. Unless all the bromine has gone, don t go near them without a fume cupboard or a mask. 

The way the chemist knows that she has methylamine and not ammonium chloride is that she compares the look of the two types of crystals. Ammonium chloride crystals that come from this reaction are white, tiny and fuzzy. The methylamine hydrochloride crystals are longer, more crystalline in nature and are a lot more sparkly. The chemist leaves the methylamine crystals in the Buchner funnel of the vacuum filtration apparatus and returns the filtrate to the distillation set up so it can be reduced one last time to afford a second crop. The combined methylamine hydrochloride filter cake is washed with a little chloroform, scraped into a beaker of hot ethanol and chilled. The methylamine hydrochloride that recrystallizes in the cold ethanol is vacuum filtered to afford clean, happy product (yield=50%). 

Pentaerythritol may be nitrated by a batch process at 15.25°C using concentrated nitric acid in a stainless steel vessel equipped with an agitator and cooling coils to keep the reaction temperature at 15—25°C. The PETN is precipitated in a jacketed diluter by adding sufficient water to the solution to reduce the acid concentration to about 30%. The crystals are vacuum filtered and washed with water followed by washes with water containing a small amount of sodium carbonate and then cold water. The water-wet PETN is dissolved in acetone containing a small amount of sodium carbonate at 50°C and reprecipitated with water the yield is about 95%. Impurities include pentaerythritol trinitrate, dipentaerythritol hexanitrate, and tripentaerythritol acetonitrate. Pentaerythritol tetranitrate is shipped wet in water—alcohol in packing similar to that used for primary explosives. 

Filtration is the separation of two phases, particulate form, ie, soHd particles or Hquid droplets, and continuous, ie, Hquid or gas, from a mixture by passing the mixture through a porous medium. This article discusses the more predominant separation of soHds from Hquids. Filtration of soHd particles or Hquid droplets from gases is dealt with elsewhere (see Airpollution controlmethods). The oldest recorded appHcations of filtration are the purifications of wine and water practiced by the ancient Greeks and Romans. Cake filters, such as the rotary vacuum filter and the filter press, were developed much later from the necessity to filter sewage. 

In the precoat mode, filter aids allow filtration of very fine or compressible soHds from suspensions of 5% or lower soHds concentration on a rotary dmm precoat filter. This modification of the rotary dmm vacuum filter uses an advancing knife continuously to skim off the separated soHds and the... 

Dewatering of high value products and particle systems sensitive to high pressure drops are the most likely candidates for electrofiltration. The Dorr-OHver Electrofilter is a commercial example of a vacuum filter adapted for electrofiltration. 

The most important feature of the pressure filters which use hydrauHc pressure to drive the process is that they can generate a pressure drop across the medium of more than 1 x 10 Pa which is the theoretical limit of vacuum filters. While the use of a high pressure drop is often advantageous, lea ding to higher outputs, drier cakes, or greater clarity of the overflow, this is not necessarily the case. Eor compressible cakes, an increase in pressure drop leads to a decrease in permeabiUty of the cake and hence to a lower filtration rate relative to a given pressure drop. 

This reduction in permeabiUty due to cake consoHdation or coUapse may be so large that it may nullify or even overtake the advantage of using high pressures in the first place and there is then no reason for using the generally more expensive pressure filtration hardware. While a simple Hquid pump may be cheaper than the vacuum pump needed with vacuum filters, if air displacement dewatering is to foUow filtration in pressure filters, an air compressor has to be used and is expensive. 

In vacuum filters, the driving force for filtration results from the appHcation of a suction on the filtrate side of the medium. Although the theoretical pressure drop available for vacuum filtration is 100 kPa, in practice it is often limited to 70 or 80 kPa. 

In apphcations where the fraction of fine particles in the soHds of the feed slurry is low, a simple and relatively cheap vacuum filter can yield cakes with moisture contents comparable to those discharged by pressure filters. Vacuum filters include the only truly continuous filters built in large sizes that can provide for washing, drying, and other process requirements. 

Vacuum filters are available in a variety of types, and are usually classified as either batch operated or continuous. An important distinguishing feature is the position of the filtration area with respect to gravity, ie, horizontal or non-horizontal filtering surface. 

Horizontal filter surfaces also allow a high degree of control over cake formation. Allowances can be made for changed feeds and/or different cake quality requirements. This is particularly tme of the horizontal belt vacuum filters. With these units the relative proportions of the belt allocated to filtration, washing, drying, etc, as well as the belt speed and vacuum quality, can be easily altered to suit process changes. 

Fig. 11. Schematic diagram of a horizontal belt vacuum filter.

Horizontal belt filters are well suited to either fast or slowly draining soHds, especially where washing requirements are critical. Multistage countercurrent washing can be effectively carried out due to the sharp separation of filtrates available. Horizontal belt vacuum filters are classified according to the method employed to support the filter medium. 

Another type of horizontal belt vacuum filter uses reciprocating vacuum trays mounted under a continuously traveling filter cloth. The trays move forward with the cloth as long as the vacuum is appHed and return quickly to their original position after the vacuum is released. This overcomes the problem of friction between the belt and the trays because there is no relative movement between them while the vacuum is being appHed. The mechanics of this filter are rather complex, and the equipment is expensive and requires intensive maintenance. A range of solvents can be used. Widths up to 2 m and areas up to 75 m are available. The cloth can be washed on both sides. 

Some horizontal belt vacuum filter designs incorporate a final compression stage for maximum mechanical dewatering. This is achieved by another compression belt which presses down on the cake formed in the preceding conventional filtration stage. 

The pressure versions of the nutsche filter, which falls into this category, are either simple pressurized filter boxes or more sophisticated agitated nutsches, much the same in design as the enclosed agitated vacuum filters described eadier. These are extremely versatile, batch-operated filters, used in many industries, eg, agrochemistry, pharmaceuticals, or dyestuff production. 

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