Evaporation, vacuum

V acuum drying Vacuum dynamics Vacuum evaporation Vacuum furnaces Vacuum gas oil Vacuum gas oils (VGO)... 

In the commonly used Welland process, calcium cyanamide, made from calcium carbonate, is converted to cyanamide by reaction with carbon dioxide and water. Dicyandiamide is fused with ammonium nitrate to form guanidine nitrate. Dehydration with 96% sulfuric acid gives nitroguanidine which is precipitated by dilution. In the aqueous fusion process, calcium cyanamide is fused with ammonium nitrate ia the presence of some water. The calcium nitrate produced is removed by precipitation with ammonium carbonate or carbon dioxide. The filtrate contains the guanidine nitrate that is recovered by vacuum evaporation and converted to nitroguanidine. Both operations can be mn on a continuous basis (see Cyanamides). In the Marquerol and Loriette process, nitroguanidine is obtained directly ia about 90% yield from dicyandiamide by reaction with sulfuric acid to form guanidine sulfate followed by direct nitration with nitric acid (169—172). 

Fig. 2. Simple schematic lepiesentation of (a) vacuum evaporation and (b) cathodic sputtering.

The Stamicarbon (22) and Kaltenbach high concentration processes are designed to use the evaporated water vapor produced by pressure neutralization to heat the evaporator used for concentration. The Kaltenbach neutralizer operates at 350 kPa (3.5 bar) and 175°C, and produces steam used to concentrate the solution to 95% in a vacuum evaporator. A recent variation uses a final atmospheric evaporator to produce a 99.7% melt (22). 

Since about 1965, efficient vacuum evaporators have been used in most plants. Second stage evaporators, where the ammonium nitrate is concentrated to more than 99%, are designed to retain only a small volume of melt, have short residence times, and are protected from overheating and contamination by sensitizers. Falling film units are especially suited for this appHcation. 

Fig. 1. Vacuum evaporation process with use of electron beam heating where A represents the material to be deposited. The flux profile ( ) is at a...

Processes involving oxygen and nitrogen oxides as catalysts have been operated commercially using either vapor- or Hquid-phase reactors. The vapor-phase reactors require particularly close control because of the wide explosive limit of dimethyl sulfide in oxygen (1—83.5 vol %) plants in operation use Hquid-phase reactions. Figure 2 is a schematic diagram for the Hquid-phase process. The product stream from the reactor is neutralized with aqueous caustic and is vacuum-evaporated, and the DMSO is dried in a distillation column to obtain the product. 

Vacuum Deposition. Vacuum deposition, sometimes called vacuum evaporation, is a PVD process in which the material is thermally vaporized from a source and reaches the substrate without coUision with gas molecules in the space between the source and substrate (1 3). The trajectory of the vaporized material is therefore line-of-sight. Typically, vacuum deposition takes place in the pressure range of 10 10 Pa (10 10 torr), depending on the level of contamination that can be tolerated in the resulting deposited film. Figure 3 depicts a simple vacuum deposition chamber using a resistively heated filament vaporization source. 

Thiosulfates are generally prepared by treating aqueous solutions of either calcium or barium thiosulfate with the corresponding carbonate or sulfate of the desired metal. The insoluble calcium or barium sulfates or carbonates are filtered and the thiosulfate recovered from the filtrate by vacuum evaporation. 

Both anatase and mtile are broad band gap semiconductors iu which a fiUed valence band, derived from the O 2p orbitals, is separated from an empty conduction band, derived from the Ti >d orbitals, by a band gap of ca 3 eV. Consequendy the electrical conductivity depends critically on the presence of impurities and defects such as oxygen vacancies (7). For very pure thin films, prepared by vacuum evaporation of titanium metal and then oxidation, conductivities of 10 S/cm have been reported. For both siugle-crystal and ceramic samples, the electrical conductivity depends on both the state of reduction of the and on dopant levels. At 300 K, a maximum conductivity of 1 S/cm has been reported at an oxygen deficiency of... 

Photochromic silver—copper haUde films were produced by vacuum evaporation and deposition of a mixture of the components onto a sUicate glass substrate (13). The molar ratio of the components was approximately 9 1 (Ag Cu) and film thicknesses were in the range of 0.45—2.05 p.m. Coloration rate upon uv exposure was high but thermal fade rates were very slow when compared with standard silver haUde glass photochromic systems. 

Simultaneous deposition of cadmium chloride and copper chloride by vacuum evaporation onto fused siUca or optical glass resulted in photochromic thin films (14). The thickness ranged from 0.25 to 1.3 pm. 

Extract is stored in insulated tanks prior to drying. Because high soluble soHds concentration is deskable to reduce aroma loss and evaporative load in the driers, most processors concentrate the 15—30% extract to 35—55% prior to drying (33). This may be accompHshed by vacuum evaporation or freeze concentration. Clarification of the extract, normally by centrifiigation, may be used to assure the absence of insoluble fine particles. 

Fig. 1. Lacquer-coated optical readout laser disk master. Plating by (a) electroless silver spray coating and by (b) vacuum evaporation. Scale bar, cm.

Ultrafiltration (qv) (uf) is increasingly used to remove water, salts, and other low molecular-weight impurities (21) water may be added to wash out impurities, ie, diafiltration. Ultrafiltration is rarely used to fractionate the proteins because the capacity and yield are too low when significant protein separation is achieved. Various vacuum evaporators are used to remove water to 20—40% dry matter. Spray drying is used if a powdery intermediate product is desired. Tyophilization (freeze-drying) is only used for heat-sensitive and highly priced enzymes. 

The reconcentration of dilute (50—60%) sulfuric acid is one of the more costly operations in the manufacture of ethanol by this process. An acid reboiler, followed by a two-stage vacuum evaporation system, raises acid concentration to about 90%. The 90% acid is then brought to 96—98% strength by fortification with 103% oleum (fuming sulfuric acid). 

Thin films of metal can be prepared by vacuum evaporation and condensation on a suitable support. For exatrrple, tlrin films of silver can be formed on a... 

There are numerous applications in solvent recovery processes where evaporation equipment are employed. Figure 14 provides an example of a process scheme for toluene-di-isocyanate recovery. This is an example of continuous vacuum evaporation of distillation residues. 

The crude ketal from the Birch reduction is dissolved in a mixture of 700 ml ethyl acetate, 1260 ml absolute ethanol and 31.5 ml water. To this solution is added 198 ml of 0.01 Mp-toluenesulfonic acid in absolute ethanol. (Methanol cannot be substituted for the ethanol nor can denatured ethanol containing methanol be used. In the presence of methanol, the diethyl ketal forms the mixed methyl ethyl ketal at C-17 and this mixed ketal hydrolyzes at a much slower rate than does the diethyl ketal.) The mixture is stirred at room temperature under nitrogen for 10 min and 56 ml of 10% potassium bicarbonate solution is added to neutralize the toluenesulfonic acid. The organic solvents are removed in a rotary vacuum evaporator and water is added as the organic solvents distill. When all of the organic solvents have been distilled, the granular precipitate of 1,4-dihydroestrone 3- methyl ether is collected on a filter and washed well with cold water. The solid is sucked dry and is dissolved in 800 ml of methyl ethyl ketone. To this solution is added 1600 ml of 1 1 methanol-water mixture and the resulting mixture is cooled in an ice bath for 1 hr. The solid is collected, rinsed with cold methanol-water (1 1), air-dried, and finally dried in a vacuum oven at 60° yield, 71.5 g (81 % based on estrone methyl ether actually carried into the Birch reduction as the ketal) mp 139-141°, reported mp 141-141.5°. The material has an enol ether assay of 99%, a residual aromatics content of 0.6% and a 19-norandrost-5(10)-ene-3,17-dione content of 0.5% (from hydrolysis of the 3-enol ether). It contains less than 0.1 % of 17-ol and only a trace of ketal formed by addition of ethanol to the 3-enol ether. 

The reaction mixture is diluted with 250 ml of water, the mixture is transferred to a 2 liter flask using methanol as a wash liquid, and the organic solvents are distilled at 20-25 mm using a rotary vacuum evaporator. The product separates as a solid and distillation is continued until most of the residual toluene has been removed. The solid is collected on a 90 cm, medium porosity, fritted glass Buchner funnel and washed well with cold water. After the material has been sucked dry, it is covered with a little cold methanol, the mixture is stirred to break up lumps, and the slurry is kept for 5 min. The vacuum is reapplied, the solid is rinsed with a little methanol followed by ether, and the material is air-dried to give 9.1 g (85%), mp 207-213° after sintering at ca. 198°. Reported mp 212-213°. The crude material contains 1.0-1.5% of unreduced starting material as shown by the UV spectrum. Further purification may be effected by crystallization from methanol. 

In a 250 ml Erlenmeyer flask covered with aluminum foil, 14.3 g (0.0381 mole) of 17a-acetoxy-3j5-hydroxypregn-5-en-20-one is mixed with 50 ml of tetra-hydrofuran, 7 ml ca. 0.076 mole) of dihydropyran, and 0.15 g of p-toluene-sulfonic acid monohydrate. The mixture is warmed to 40 + 5° where upon the steroid dissolves rapidly. The mixture is kept for 45 min and 1 ml of tetra-methylguanidine is added to neutralize the catalyst. Water (100 ml) is added and the organic solvent is removed using a rotary vacuum evaporator. The solid is taken up in ether, the solution is washed with water and saturated salt solution, dried over sodium sulfate, and then treated with Darco and filtered. Removal of the solvent followed by drying at 0.2 mm for 1 hr affords 18.4 g (theory is 17.5 g) of solid having an odor of dihydropyran. The infrared spectrum contains no hydroxyl bands and the crude material is not further purified. This compound has not been described in the literature. 

Fig. 2. TEM image of a CNT obtained by CVD of 2-methyl-1,2 -naphlhylketone on a vacuum-evaporated nickel film (5 nm in thickness) at 700°C.

Filter Cool and vacuum evaporate 1 Heat in oxygen above 1000 ... 

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