SU50158A1 - Method and device for the distillation of organic substances - Google Patents

Description

The present invention relates to such distillation of materials of organic origin, for example, mineral oils in vacuum, in which the surfaces of evaporation and condensation are located in a common chamber. When such materials are distilled at pressures well below 1 mm of a mercury column, the rate of condensate production may be insignificant, both due to the low vapor density of distillate at this pressure, and due to the low diffusion rate of these vapors from the evaporating surface towards the condensing one. In the proposed method, the distillation of the pre-degassed substance is carried out at a gas pressure remaining in the apparatus of from 0.01 to 0.001 mm Hg, and the distillate vapors are condensed on a surface spaced from the evaporation surface at a distance less than the theoretically calculated average free path of the molecules distillate at the indicated pressure. Due to this mutual arrangement of the evaporating and condensing surfaces, and also due to the high vacuum, most

The molecules of the distillate are transferred to the condensing surface or are not completely colliding along the way with other molecules of the distillate and with the molecules of the residual gas, or the number of such collisions is very small.

If it is required to overtake material of such a kind that its distillation can be accompanied by the formation and rupture of bubbles, spraying or spraying, then the distillation apparatus is supplied with partitions positioned between the condensing surface and the surface of the distillation substance in such a way that the particle leaving the surface of the distilled substance and moving roughly linearly, it is prevented from hitting the condensing surface. Such barriers are preferably heated to about the temperature of the substance to be distilled, so that the condensation of the distillate on them does not occur.

The invention likewise consists in combining with the distillation apparatus of the above type one or more chambers within which successively decreasing pressures are maintained and within which the distilled substance can be subjected to successively increasing temperatures, in order to remove from it before introducing it into the apparatus itself. Present fired gases.

The complete distillation process with its continuous introduction consists in conducting the distillable substance through one or more chambers with decreasing pressure and, if desired, with increased temperature to remove dissolved gases and then heating the distillable substance in the chamber at low pressure, having its surface in close to the cooled condensing surface and remove the distillate or residue, or both, from the apparatus using one or more pump systems.

When used for the distillation of materials belonging to the second of the two types described, the invention provides for the implementation of the very large possible hermetic reservoir with a very rarefied space, as described above, up to the greatest possible degree of advantageous evaporative features, however, without the necessary perfect vacuum, as was supposed.

When the above condition is fulfilled, no noticeable acceleration of distillation will be obtained in the case of better resolution in the apparatus, since if most of the distillate molecules, when mixed from the surface of the substance being distilled to the condensing surface, do not collide with the residual gas molecules, these molecules do not have a noticeable effect. resistance, and single and double collision of molecules of distillate between themselves can be allowed, as the eyes move in one direction, and almost all of them siruyuts collision with the condensing surface. Thus, it is unlikely that collisions between distillate molecules will cause their return to the material being distilled back.

The actual value of the distance between the surface of the distilled substance and the condensing surface can be easily determined with a sufficient degree of accuracy according to modern data from the dynamic theory of gases. For example, the average free path of a mercury molecule in an atmosphere of saturated vapor at room temperature is about 4 cm, and if it is assumed that the actual diameter of a distillate vapor molecule is the same as that of a mercury molecule, then the institute has a free distribution of a distillate molecule in an atmosphere of saturated mercury vapor at room temperature it will be 4 cm. Mercury vapor is the main, if not the only residual Basin inside the apparatus in which the vacuum is created, with the help of the powerful Mercury Hacoda. If the distance between the surface of the distillation substance and the condensing surface is 2 cm, then 60.07% of the distillate molecules reach the condensing surface without colliding with mercury molecules. If, however, the distance between the surface of the distillation substance and the condensing surface is reduced to 1 cm, then 77.5% of the distillation product molecules reach the condensing surface without colliding with mercury molecules. Thus, in the first case, the evaporation rate in the apparatus will constitute more than 60.07% of the evaporation rate, which would have occurred if the apparatus had no other gas than destallate vapor, and in the second case, the evaporation rate would be more 77.5 / of this speed (i.e., speed at a theoretical full vacuum).

For comparison, we can consider the case (under the above conditions) when the distance between the surface of the distillation substance and the condensing surface is 20 cm. In this case, approximately only one of the 20,000 molecules of distillate vapor avoids collision as it moves towards the condensing surface and the average amount of time spent by any molecule on overcoming this distance will be 100 times longer than the time taken by the pump 154; it flows through the counter / 55 into the tank / 55.

The remainder enters the third distillation apparatus / 57, in which a vacuum is created using a diffusion pump 755, and heating occurs just as described in relation to the distillation apparatus 116 and 142. The condensate from the distillation apparatus / 57 enters through a tube / 5P to receiver 160, from where pump 161 is fed through counter 162 to reservoir / 65, while the remainder enters another distillation apparatus 164, from which condensate is drained to receiver 165. From receiver 165, condensate is supplied by pump 166 through counter 167 to reservoir 168. Residue distillation apparatus 164 is fed to receiver 169, from where it is driven by pump 170 through counter / 7 / to tank / 72.

The degrees of dilution and (or) evaporation temperatures in several successive distillation apparatuses gradually increase, so that the lighter fractions are distilled off, first, in the order of the apparatuses and fed to the respective tanks, while the heavier fractions arrive in the latter in order tanks.

The receivers 136, 153, 160, 165 and 169 are equipped with siphons just as shown in the drawing with respect to the receiver 169, and the vacuum in them is maintained by connecting them to the low vacuum pipeline 111. In addition, all receivers 136, 153, 160, 165, and 169 are jacketed to maintain proper temperatures. Heater 102 is also heated with a water jacket. All of these water jackets are fed with hot water supplied through conduit 109 and discharged via conduit / 07 to a common collection, from which iodine (after subsequent further heating, if this seems desirable) is again pumped into conduit 109. Pumps 173, 137 , 154, 161, 166. and 170 are driven by an electric motor (75).

To indicate the evaporation temperatures in various distillation apparatuses, an electric pyrometer 176 is provided, adapted to be connected, using a multiple switch 777, with any of the thermocouples located in each of the distillation apparatuses, the thermocouples being soldered, welded or otherwise attached to the evaporation trays. For the purpose of measuring the degree of vacuum in different chambers, electrical transformers 178 and / 5 / have a cascade connection to the main network 200 and line 179, and through switches similar to switch 180, with spark gaps 181 located in tubes or channels having the same degree of vacuum as various distillation chambers. By closing the corresponding switch, similar to the / SP switch, and observing the nature of the discharge in the spark gap connected to one of the distillation apparatus, it is possible to determine the degree of vacuum in it.

When using the described method, the distillation of materials can be carried out at an acceptable speed with a significantly greater vacuum and, therefore, at lower temperatures Tpppax than was the case before now. Using the proposed method, products that were not known until now can be obtained. For example, during the distillation of an oil known as Vacuum Arctic C ° at a residual vacuum pressure of about 0.001 mm Hg and at a temperature of from 90 to 120 ° C, the residue after distillation of 50% of the original substance is obtained as a refined oil, slightly more viscous. than the material being distilled, whose vapor pressure at room temperature is lower than that of mercury. This residue is suitable for use in condensation pumps instead of mercury commonly used for this purpose. The rate of distillation under the above conditions is quite high, ranging from 0.1 to 0.5 g of the processed material per hour per square meter. see the surface of the distilled material.

If petroleum jelly is distilled at a residual pressure of about 0.001 mm Hg and at a temperature of from 100 to 320, then 10% of the condensate produced at low temperatures is a colorless oil. The remaining condensate is a paste, the color of which gradually darkens as the feathers continue. From this paste, wax can be obtained by pressing in filter presses, and the remainder is a yellow grease, the vapor pressure of which is less than mm Hg at 70 °. The vapor pressure of this residue is so insignificant that it can be placed inside a continuously evacuated electronic amplifier without compromising its quality („its stability). The distillation rate is sufficient to prepare such a lubricant on an industrial scale.

When distilled under the same conditions as the material known as Schell Hard flsphalt, 30% of its weight is distilled at a temperature lower than the decomposition temperature, measured at 320 °. Condensate is a thick, odorless, red oil, and the residue is the fragile nature of asphalt.

The proposed method is suitable for separating wax from oils such as lubricating. For example, about 70% of the oil known as Schell Cylinder Oil (Superheat) B / b can be distilled without decomposition and at a rate sufficient for industrial purposes at temperatures below 307 °, at which oil decomposition begins. The condensate is a red-brown paste, from which a light wax can be separated by pressing in filter presses, while the residue is a liquid that is more viscous than the starting material. If you stop the distillation — at a temperature of 250 °, the residue, which is about 60% of the starting material, is noticeably less viscous than the starting material.

The proposed method can also be applied to produce a high freezing point or freezing oil, for example, by distilling the oil known as Schell Cylinder Oil C. 4, at a temperature of –250 the condensate is obtained as a light yellow half viscosity oil compared to the original material. The distillate freezes or solidifies at a temperature slightly below room temperature and is perfectly solid. The npw temperatures at which the starting material is liquid. 80% of this oil can be distilled at a temperature below 340, at which decomposition begins. The process can be carried out with sufficient speed for industrial purposes.

And other grades of oil and oils can be subjected to the described distillation and, generally speaking, the condensates are obtained more transparent than the corresponding fractions obtained by the usual method of distillation in vacuum in the apparatuses usually used for this purpose under industrial conditions of work. In addition, the distillation products obtained, according to the described method, as a rule, almost or in most cases are completely odorless and possess significant color stability. In addition, the oil distilled by the proposed method can be used as high-grade lubricating oil without intermediate purification, which is recognized as necessary in the perfect production of refined lubricating oils.

The subject matter of the invention.

1. A method of distilling organic substances by heating them at a reduced temperature in a chamber under vacuum, characterized in that the organic matter, previously de-carbonated to remove dissolved gases dissolved in it, is introduced into the distillation chamber at a residual gas pressure from 0.01 to 0.001 mm Hg and condense the released pairs of distillate on the surface located above the evaporated liquid so that its distance from the surface of the liquid is less than theoretically the mean free path of the distillate molecules at a given pressure in order to reduce the number of collisions of distillate molecules with residual gas molecules filling the chamber at a given pressure 2. Yappardt for performing the method of claim 1, characterized in that it is in doubt that the molecule consumes to overcome the distance not in 2 cm

In carrying out the present invention, the apparatus is made to operate at a pressure of 1 dyn / cm if possible, which pressure can be easily obtained using mercury condensation pumps, although other types of pumps can be used, and the condensing surface is located about 1 cm from surface of the distilled material. However, in those cases when it is necessary to distill such organic substances, the distillation of which may be accompanied by the formation of sprays or spraying, then, generally speaking, the condensing surface e is arranged so that the distance between this last and the surface of the substance being distilled is less the average free path length of the distillate molecule due to the desirability of including additional partitions between the evaporation and condensation surfaces; in this case, a large part of the distillate molecules will first hit the partitions, and then dissipate in the chamber of the apparatus, finally reaching the condensing surface. It is advantageous that the number of collisions between the molecules of the distillate and other molecules be as small as possible and, therefore, it is desirable that the condensing surface be located as close as possible to the surface of the substance to be distilled. By proper dimensions and vacuum of the chamber, the speed of the apparatus containing partitions can be adjusted to the speed Vio obtained in the apparatus, in which the condensing surface is removed from the surface of the distilled material to a distance less than the average free path of the distillate vapor molecule in the residual gas inside the machine. The degree of distillation in the apparatus with additional partitions can be almost as high as in the apparatus without partitions.

Each distillation apparatus can be designed so that the pressures in different parts of it are different.

For this, the outflow of the distillation product from the edge of one tray over the edge of another tray or partition or condensing surface is directed so as to entrain the residual gas inside the chamber and thus contribute to an increase in vacuum in other parts of it. Condensing surfaces in the distillation apparatus can be subdivided into a large number of parts, each of which can be equipped with a special removal device, so that the condensates of different parts can be collected separately. Thus, by maintaining different jacTH of the distilled material at different temperatures and (or) at different pressures within different zones of the distillation apparatus, it is possible to obtain a large number of fractions in one distillation apparatus from opjnoro source material.

In the attached drawing of FIG. 1 shows a longitudinal section of a distillation apparatus according to the inventive method. FIG. 2 is a plan view of a portion of the distillation tray and a portion of the condensing surface of the apparatus of FIG. 1. In FIG. 3 shows a longitudinal section of the apparatus of FIG. 1 by a plane perpendicular to the plane of this fig. 1. FIG. 4 shows a longitudinal section of an apparatus equipped with a device for discharging individual distillate fractions. FIG. Figure 5 shows a partial longitudinal section of the apparatus, in which the distillate from the tray is retracted in such a way as to increase the degree of dilution in the lower parts of the apparatus. FIG. A vertical section through the apparatus for the distillation of materials sucked or sprayed during the distillation process is shown. FIG. 7 shows in plan one of the trays of the apparatus in FIG. b. FIG. 8 is a modification of the apparatus of FIG. b, and in fig. 9 shows diagrams of a complete continuous installation for the treatment (distillation) of organic substances.

From FIG. 1-3, it is clear that the trays H for the material to be distilled are clamped between the nuts 3, screwed onto the bolts / 2. Latest fastener to cover / 4

airtight chamber 75. The material to be distilled is pretreated to remove all gases dissolved therein; thereafter, it enters the chamber / 5 at one end of the uppermost tray through the siphon tube 16, flows through the tortuous channel formed by the slots / 7 at the bottom of the tray, and then is drained to the underlying tray.

Above each of the trays 10, an inclined condensing surface 21 is installed with the aid of tides 22 fixed between the nuts 23 on the bolts 24 that are hung from the f4 cover. Condensing surfaces 2 / are maintained at an appropriate temperature using some medium circulating through the tube 25, soldered or otherwise attached to the 2L surface. In addition, the cooling medium can circulate through the jacket 27 around the chamber walls using tubes 28 and 29 to ensure condensation of all distillate vapors not condensed on surfaces 2 /, and in order to maintain the entire apparatus under appropriate temperature conditions. The trays W are heated by the medium circulating through the tube 26, conjugated to the tray JO by soldering or otherwise, providing thermal contact with the bottom surfaces of the trays.

All connections in the chamber are air-tight, for example, by welding, and the chamber itself is manufactured with sufficient strength to withstand external atmospheric pressure.

A tube 30 is provided in the lid 7 of the chamber, connected to a pump that provides and maintains the highest degree of vacuum. Such a pump may, for example, be a mercury condensation pump. The condensate flows down the inclined condensing surfaces 2 / through their edges and collects in the lower part of the vessel, from where it is removed using a siphon tube 57, while the remainder from the last tray comes through the tube J8 into the well 7P and leaves the apparatus through a siphon tube 20 ,

FIG. Figure 4 shows a modified apparatus in which condensate is collected from individual condensing surfaces, for which the latter are provided with condensate troughs 32. Of these troughs, 32 condensate is fed through pipes 33 to chutes 34, mounted to the chamber walls, and communicating with siphon tubes 35, by which condensate is drained from the apparatus. Individual chutes 34 can be arranged for each individual condensing surface of the apparatus or, as shown in the drawing, two or more condensing surfaces of the Mory 01 can be serviced by a single chute. With the design of the apparatus shown in FIG. 4, a large number of fractions can be obtained from one initial distilled liquid.

FIG. Figure 5 shows a modification of the apparatus in which the removal of part of the distillate from the surface of the substance to be distilled promotes an increase in the degree of vacuum in the chamber. In this form of the apparatus, the edges of the trays JO come out somewhat beyond the edges of the condensing surfaces 27, provided with troughs 32 for collecting condensate, which then flows into the tapers 34; between the cholob 32 and the edges of the JO trays such a passage is provided that part of the distillate can go in the direction indicated by arrows and condenses on the cooled walls of the chamber, also entering cholob 34, this distillate carries with it a part of the residual gas bottom of the camera. Therefore, it is sufficient to produce some vacuum, for example, 50 dyn / cm at the top of the chamber, so that a higher degree of vacuum is needed to distill less volatile components, for example, 1 din / cm, to turn out at the bottom of the chamber.

The apparatus shown in FIG. b-7, has the shape of a cylinder and its walls form a condensing surface. The distilled substance enters, preferably after removing the dissolved gases from it through pipe 40 to the siphon 4 / and from there to the uppermost tray 42. After that, the distilled

the substance travels along the winding path formed by the projections 43 to the outlet nozzle 44 of the tray, with which nozzle it is fed to the next lower tray and in this way sequentially moves to the very bottom of its apparatus tray.

Trays having a cylindrical shape and a cross section shown in FIG. b, preferably made of yellow copper and fitted to the central tube 45,. through which the heating medium can circulate, for example, betting The heat of the heating medium through the tube 45 is communicated to the body of the tray 42 and from it to the distilled substance. The trays can also be heated by means of electrical elements located inside the central tube 45 or mounted on trays. Above the uppermost tray is a partition 46, heated to the same temperature and in the same way as trays 42. This partition has a hanging rib 47 preventing any particle leaving the surface of the distilled substance and moving approximately straight from the impact into the chamber wall. Trays 42 are also provided with hanging ribs 48 acting as partitions for protecting particles that are thrown from the surface of the distillate contained in the next lower tray from impact into the condensing surface. In addition, the trays are provided with annular channels 49 into which drops of the distilled material can fall from protruding ribs 47 to 48. The annular channels 49 are connected to the bottom surface of the trays by means of channels 50, by means of which the distilled material collected in the channels 49 is fed to the next lower tray. From the lower trough, the remainder of the distillation material flows through nozzle 44 into well 51, from where it is removed through tube 52.

The walls of the chamber are equipped with a jacket 53, as well as a tube 54 leading to a vacuum pump, which is made with a slope so that the condensate formed in it drains back.

into the camera. The condensate formed on the walls of the chamber flows into an annular well 55, from where it is removed through tube 56.

In the modified apparatus shown in FIG. 8, the outer edges of the chutes 42 are made in the form of protruding upward ribs, so that the distillate is directed upwards, thus facilitating the creation of a vacuum in the chamber in the same way as is the case in the design of FIG. 5. In addition, chutes 57 are provided in the atinarate, in which condensate is collected from the part of the column located directly above the chute, and tubes 5 are also provided to remove condensate from the chutes 57, so that several fractions of liquid to be distilled can be collected in one apparatus .

In the general distillation apparatus shown in FIG. 9, a distillable substance, for example, crude oil, preferably freed from the most volatile substances, fills the tank 100, from where it is pumped through the meter 173, the meter 101, the heater 102 and the pipeline 103 is fed into the chamber 104 to preliminarily remove the gases dissolved in it . Chamber 104 is a simple cylindrical vessel, from the lower end of which oil is removed through a siphon tube 105 and enters the second chamber 106 to remove gases. Chambers 104 and 106 are heated with hot water (or other medium) flowing into the jacket 108. the pipeline 107 and flowing into the pipeline 109.

Chamber 104 is maintained at a moderate vacuum through tube 110 connected to conduit 111, which in turn is connected to pump 7/2 to create moderate vacuum and to gauge 113. The second chamber 106 is provided with a spiral plate or tray 114, which is in good condition. thermal contact with the walls of the chamber heated by water flowing in the jacket 108. Oil coming out of the siphon 105 flows a thin layer along the tray 114. The vacuum in the chamber 106 is maintained through tubes 22, 25,

connected to a vacuum pump 120, in aid of which the previously mentioned pump / 72 is operating.

The gas-free oil is removed from the bottom of the chamber 106 through the Siphon tube 115 and enters the first distillation unit 7/6, as used from those described above (the apparatus in Fig. 6 is shown in the drawing). The vacuum in the distillation apparatus 775 is supported through tubes 777, 118 connected to a vacuum pump 779, in which pumps 120 and 772 operate, driven by an electric motor 727. The distillation apparatus's sheets are heated by an electrical current, conducted through the conductors 727, 128 by a transformer 72 through the switch 725.

If the distillation apparatus 116 corresponds to that shown in FIG. b and 7 or 8, the electric heating elements may be located inside the central tube 45 or they may be attached to the trays or placed in their body. If the distillation apparatus corresponds to that shown in FIG. 1, 2, 3, 4 or 5, the electrical heating elements can be attached to the bottom of the trays or placed in their body.

The walls of the distillation apparatus 775 are maintained at the proper temperature by using a medium circulating through the vessel 729. It is usually desirable to keep the jacket as cold as possible unless the condensate has a high pour point, or when the condensate vapor pressure is low at temperatures up to 100 in which case, the temperature in the jacket may rise to 100 ° without harm to the operation of the apparatus.

Accordingly, the jacket 129 can be connected at its lower end with the aid of a tube 752 a or with a conduit 755 for cold water or with a conduit 09 for hot water, and at its upper (output) end with a conduit 757.

Condensate collected in the ring well 75- at the bottom of the distillation apparatus 776 is removed along

tube 755, which can be bent by siphon and fed to receiver 756, from where it is pumped through pump 757 through stetchik 755 to tank 75P. The residue collected in distillation unit 776 in well J40, leaves the apparatus through siphon tube J4J and enters the second a distillation apparatus 142, which is heated by an electric current supplied through conductors and 725 transformer 72 via switch M4.

The walls of the distillation apparatus J42 are jacketed into which the corresponding medium is fed through conduit J09 or / 55 and through the discharge tube of the jacket of the first apparatus is diverted by conduit 757. The distillation apparatus, instead of directly connecting to the high-voltage pipeline P8, connects with a diffusion channel 146. a pump using mercury or oil as the working medium. For channel J46, such a slope is provided that the condensate formed in it flows back into the distillation unit 142. The channel duct can be connected to pipelines 55 and 757. When condensation that solidifies in the channel is formed, the latter’s jacket can be periodically connected to pipeline 109, thanks to whereby the solidified condensate becomes liquid and flows back to apparatus 142; the channel of the channel can be permanently connected to the pipeline J09. It seems, however, desirable to keep the channel of the duct cold so that the smallest possible amount of distillate is supplied to the condensation pump in the form of steam. The jacket of the condensation pump is connected to the cold water pipe 755 and the discharge pipe 757. Heat is supplied to the diffusion pump using an electric heater 7f7, to which current is supplied through wires 148 and 49 and using a two-pole switch 150 from the main network 200.

The condensate formed in the distillation apparatus is collected in an annular well at the bottom of it and is led through tube 752 to receiver 755, from where

It consists of a series of installed one above the other, in the form of a column, evaporating trays 10 and condensing surfaces 27, fixed on the required mutual distance with screws 72 and nuts 13 and equipped with tools 32, 33, 34 to collect individual distillate fractions from each condensing surface and to increase the degree of vacuum in this case (Fig. 1, 2, 3, 4 and 5).

3. Modification of the apparatus according to claim 2, characterized by a cylindrical shape of the walls, equipped with a solid jacket 53 and serving as a condensing surface, and the use of disc-shaped trays heated by the central tube 45.

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the patent of the company of the United Society of the electric industry № 50158