Boiling point vacuum distillation

VACUUM DISTILLATION. Distillation at pressure below atmospheric but not so low that it would be classed as molecular distillation. Since lowering the pressure also lowers the boiling point, vacuum distillation is useful for distilling high-boiling and heat-sensitive materials such as heavy distillates in petroleum, fatty acids, vitamins, etc. 

Distillation is a veiy common method for purifying liquids. Atmospheric distillation (general distillation), vacuum distillation, and steam distillation are the three common methods of distillation. Atmospheric distillation takes place at atmospheric pressure, which means the distillation apparatus is open to the air. Vacuum distillation utilizes reduced pressure to distill a liquid at lower temperature. Vacuum distillation is commonly used to distill liquids, which tend to decompose at their atmospheric boiling points. Vacuum distillation is also used to conveniently distill liquids with relatively high boiling points at a much more efficient temperature. Steam distillation is similar to atmospheric distillation, but steam is used to promote volatility. Steam distillation only works on liquids or solids, which are volatile with steam. 

One of the most important operations in a refinery is the initial distillation of the crude oil into its various boiling point fractions. Distillation involves the heating, vaporization, fractionation, condensation, and cooling of feedstocks. This subsection discusses the atmospheric and vacuum distillation processes which when used in sequence result in lower costs and higher efficiencies. This subsection also discusses the important first step of desalting the crude oil prior to distillation. 

The distillation continues to a boiling point corresponding an atmospheric boiling point of about 535°C. The remaining material is called vacuum residue. 

Removal of maleic and fumaric acids from the cmde malononitrile by fractional distillation is impractical because the boiling points differ only slightly. The impurities are therefore converted into high boiling compounds in a conventional reactor by means of a Diels-Alder reaction with a 1,3-diene. The volatile and nonvolatile by-products are finally removed by two vacuum distillations. The by-products are burned. The yield of malononitrile amounts to 66% based on cyanogen chloride or acetonitrile. 

Vacuum Distillation. Vacuum distUlation evolved as the need arose to separate the less volatile products, such as lubricating oUs, from petroleum without subjecting these higher boiling materials to cracking conditions. The boiling point of the heaviest cut obtainable at atmospheric pressure (101.3 kPa = 760 mm Hg) is limited by the temperature (ca 350°C) at which the residue starts to decompose or crack. It is at this point that distUlation in a vacuum pipe stUl is initiated. 

Heat Sensitivity. The heat sensitivity or polymerization tendencies of the materials being distilled influence the economics of distillation. Many materials caimot be distilled at their atmospheric boiling points because of high thermal degradation, polymerization, or other unfavorable reaction effects that are functions of temperature. These systems are distilled under vacuum in order to lower operating temperatures. For such systems, the pressure drop per theoretical stage is frequently the controlling factor in contactor selection. An exceUent discussion of equipment requirements and characteristics of vacuum distillation may be found in Reference 90. 

Use vacuum distillation to obtain lower boiling point of solvent to allow lower distillation temperature... 

Types of columns and packings. A slow distillation rate is necessary to ensure that equilibrium conditions operate and also that the vapour does not become superheated so that the temperature rises above the boiling point. Efficiency is improved if the column is heat insulated (either by vacuum jacketing or by lagging) and, if necessary, heated to Just below the boiling point of the most volatile component. Efficiency of separation also improves with increase in the heat of vaporisation of the liquids concerned (because fractionation depends on heat equilibration at multiple liquid-gas boundaries). Water and alcohols are more easily purified by distillation for this reason. 

Vacuum distillation. This expression is commonly used to denote a distillation under reduced pressure lower than that of the normal atmosphere. Because the boiling point of a substance depends on the pressure, it is often possible by sufficiently lowering the pressure to distil materials at a temperature low enough to avoid partial or complete decomposition, even if they are unstable when boiled at atmospheric pressure. 

After dilution with 200 ml. of benzene, the solution is transferred to a 2-1. separatory funnel containing 800 ml. of ice water and shaken thoroughly. The aqueous layer is separated, acidified to pH 3-4 with 2-3 ml. of concentrated hydrochloric acid, and extracted with three 100-ml. portions of benzene. All the organic layers are then combined and dried over anhydrous sodium sulfate. Filtration and concentration of the solution with a rotary evaporator, followed by exposure to high vacuum for 2-3 hours, affords 17.3-19.3 g. of the crude product (Note 3). Low-boiling impurities are removed by vacuum distillation (Note 4), the residual oil (14-15 g.) is transferred to a 50-ml. flask equipped with a short-path distillation apparatus, and vacuum distillation is continued. A forerun is taken until no rise in boiling point is observed, and then 7.2-8.6 g. (23-27%) of dimethyl nitrosuccinate is collected as a colorless oil, b.p. 85° (0.07 mm.), 1.4441 (Note 5). 

The dehydrogenation reaction produces crude styrene which consists of approximately 37.0% styrene, 61% ethylbenzene and about 2% of aromatic hydrocarbon such as benzene and toluene with some tarry matter. The purification of the styrene is made rather difficult by the fact that the boiling point of styrene (145.2°C) is only 9°C higher than that of ethylbenzene and because of the strong tendency of styrene to polymerise at elevated temperatures. To achieve a successful distillation it is therefore necessary to provide suitable inhibitors for the styrene, to distil under a partial vacuum and to make use of specially designed distillation columns. 

If two insoluble liquids are heated, each is unaffected by the presence of the other and vaporizes to an extent determined only by its own nature. Such a mixture always boils at a temperature lower than is true for either substance alone. This effect may be applied to substances that would be damaged by overheating if distilled in the usual fashion. Substances can also be distilled at temperatures below their normal boiling points by partially evacuating the still. The greater the vacuum, the lower the distillation temperature. 

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