SU1057062A1 - Method of separating liquid mixtures - Google Patents

Abstract

A METHOD OF SPLITTING LIQUID MIXTURES, in which a liquid mobile phase with a periodic BBOQOM into it razkaza zhitskoy mixture is continuously passed through it with a chain of increase of its mixture through a digging machine filled with a fixed inert liquid. of productivity, a liquid that partially dissolves the components of the mixture is used as the mobile phase, and the introduction of a separable liquid mixture into the column introduces a liquid that has the greatest solubility in liquid compared to the components of this mixture dkoy mobile phase --1 5 J.

Description

The invention relates to physical chemistry, more specifically to the disengagement of liquid mixtures, and can be used in chemistry medicine to obtain pure components. Chromacystippia method is known for disengaging zhitsky mixtures with a limiter, which consists in the fact that before entering the mixture of its mixture into a column filled with an inert relative to the components of the mixture a solid carrier and blown by a gas stream under isothermal conditions , which obpetsatsya pettiness, not less than the other components of the mixture petish. This method also makes it possible to enrich the zo components. pure substances, their physicochemical characteristics can be determined. However, this method can only be used for liquids with sufficient volatility under the conditions of experience. The closest to the proposed method is the separation of liquid mixtures, in which a continuous inert filler is passed through a column filled with a fixed inert filler. liquid mobile phase with periodic injection of split liquid mixture into it. In a known method called liquid column chro. by mathematics, the separation is carried out due to the varying probability yaej of the living substance in the stationary phase of the column fill. The filler can be an inert solid with a large active surface or an inert carrier with a large pore volume saturated with an active separating liquid. The disadvantage of this method is the limited productivity of the digging unit when obtaining pure substances in the preparative variant, which is due to the low permissible load on the column due to the need to work in the field of linearity of sorption isotherms. The purpose of the invention is to increase the productivity of the process in obtaining clean components. The goal is achieved in that according to the method of separation of liquid mixtures, in which through a column filled with an empty Inert, fill it with a continuous mobile liquid phase with periodic introduction of a separated liquid mixture into it as the mobile phase, liquid j is used; the component of the mixture that dissolves limitedly is used, and before introducing the separable liquid mixture into the column, liquid neck compared with the components of the mixture of limited solubility in the liquid mobile phase. When used as a mobile phase, a liquid in which the components of the mixture do not dissolve in any ratios, but are saturated under conditions of & Nor some limiting concentration in this fluid, called dissolves. By the way, the spin-off of the kompshgent-column is recorded in a vice, extended stage, the height of which corresponds to its concentration, f and the length-volume of the mobile phase passing through the column, by dissolving this amount of substance. In order to separate a mixture consisting of several components with different limited solubility in the mobile phase, a liquid is used, called the limiter, which has the greatest limited solubility compared to the components of the mixture. The limiter placed on the column in front of the mixture to be separated causes the components arranged in the order of decreasing solubility in the vice adjacent zones of saturated solutions in the mobile phase. In Fig. 1 is a schematic diagram of the device CP Fig. 2 is a chromatogram of a mixture of two components obtained without introducing a restrictor; Fig. 3 is the same, introducing one of the components of the mixture as a limiter. The device for implementing the proposed method is based on a Fomieic microcontact chromatograph -LOON of Lazso company with UV detector UviiJec1000-W and microsyringe 1, piston syringe moving device 2, feeding piston 3, needle 4 for sampling, tripod 5 for fastening and moving audio the needle 4, column 6, 7 aetektor, recorder 8 uppotn guides connectors 9, podvinshoy phase flow is established by defining a certain speed of movement of the piston microsyringe 1. Sampling occurs when the flow is stopped. On this end, the end of the sampling needle 4 is detached from column 6 and immersed in a bottle with the test liquid (not shown). During the return stroke of the piston, fluid is sucked into the needle 4. Column 6 is made up of a Tefpon thread with an internal diameter of 0.5 mm and a cord of 20 cm, filled with particles of stainless staples with a fraction of 501.5 microns. As a model mixture, the component of which have limited solubility in the mobile phase, nitro-naphthanes are used, and the mobile phase is water. The working wavelength of the ultra violet detector is set to 245 and the sensitivity to the mixture components is approximately equal. The working range of the detector is 0.64 absorption per scale. Primer p. Experiments have been carried out on the development of air mixture components of different compositions using a more soluble component as a limiter. FIG. 2 shows the chromatogram of a mixture of nitromethane and 2-nitropropane in a ratio of 1: 4. Sample volume 0.5 μc | the speed of the coating is 1 µl / min, the speed of the chart tape is 0.25 cm / min. FIG. 3 shows the chromatogram of the same mixture in 62 of the same conditions, but before entering the mixture, a limiting plate (mc of nitromethane) is introduced. The introduction of the limiter leads to the disappearance of the zone of intermediate solubility, corresponding to the scopes of the components of the initial composition, i .e. to separate the mixture. The composition of the mixture is calculated by first determining the solubility of the individual components by introducing a certain amount of them. The concentration of the saturated pact of the thief is calculated by the length of the step. A similar separation is achieved with the introduction of a three component mixture, the stopper is a substance not containing a separable mixture. Thus, it follows from the above examples of nitroalkvine separation that the use of the proposed method makes it possible to drastically improve the efficiency of the release of pure substances in comparison with the prototype, since the loading on the column is very high (several percent of the total column volume).

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Claims (1)

. METHOD FOR SEPARATION OF LIQUID MIXTURES, in which a liquid mobile phase is continuously passed through a column filled with a stationary inert filler with periodic introduction of a mixture of a divided vein into it, characterized in that, with a chain for increasing its productivity, they use as a mobile phase a liquid that partially dissolves the components of the mixture, and pepper, by introducing a shared liquid mixture, a liquid is introduced into the column that has the greatest limited solubility in liquid mobile phase.