The method of purification of 1,1-differetn extractive distillation
(57) Abstract:The invention relates to the separation of 1,1-differetn from vinyl chloride. The method is realized by means of extractive distillation. A mixture containing 1,1-differetn and vinyl chloride, in contact with at least one extractant selected from the group of hydrocarbons, alcohols and chlorinated hydrocarbons having a normal boiling point of from 10 to 120oWith, and forms a second mixture. From the second mixture is separated 1,1-differetn extractive distillation. The ratio of extractant to 1,1-dottorato is from 1/1 to 10/1. Extractive distillation is carried out at a pressure of from 103,43 to 2413,25 KPa. The technical result - the simplification of the process of purification of 1,1-differetn. 7 C.p. f-crystals, 9 tab., 1 Il. Cross-reference to related applications
This application claims the preferential right of priority according to the first application U.S. 60/030148 registered 1 November 1996 (FL-1019-P1).The scope of the invention
The present invention relates to a method for the separation of vinyl chloride and other compounds from 1,1-differetn by using extractive distillation with the use of aliphatic hydrocarbons, chlorinated hydrocarbons and spirlea from possible destruction fully halogenated harperperennial connections (CFC) were installed new instructions. The compound 1,1-differetn (F2CH3or HFC-152a) is not containing chlorine with fluorocarbon, which is especially valuable as a refrigerant, blowing agent, propellant, and an intermediate chemical compound for the manufacture of winifrida, among other applications.1,1-Differetn can be obtained by reaction of vinyl chloride with hydrogen fluoride in the presence of a catalyst, such as palladium, vanadium, tin or others. The reaction product of such methods in addition to the desired 1,1-dottorato usually contains unreacted vinyl chloride and hydrogen fluoride, hydrogen chloride as a by-product and small amounts of organic by-products such as 1-chloro-1-foraten and viniferin. While the majority of these impurities can be removed by ordinary distillation, vinyl chloride, it is very difficult to separate from 1,1-diflorasone, when the concentration of 1,1-differetn above about 85 mol.%. Depending on the temperature of the vinyl chloride and 1,1-differetn in these concentrations form or azeotropic mixture or azeotropically composition, making it difficult to clean 1,1-differetn by conventional distillation or making it impossible.Pestilentiam this product. You have made numerous attempts to reduce the amount of vinyl chloride remaining in 1,1-diflorasone, but they were inadequate to achieve low levels of vinyl chloride or were too expensive.The present invention solves the problems associated with known methods of cleaning, ensuring the extraction of 1,1-differetn from mixtures containing 1,1-differetn and vinyl chloride, which are simple and effective ways to obtain low levels of vinyl chloride in products 1,1-differetn.The invention
The method has been found for separating 1,1-differetn from the first mixture containing 1,1-differetn and vinyl chloride, comprising the stage of:
contacting the first mixture with at least one extracting a substance selected from the group consisting of: hydrocarbons, alcohols and chlorinated hydrocarbons having a normal boiling point higher than approximately 10oC and lower than approximately 120oWith, for the formation of the second mixture, and
Department of 1,1-differetn from vinyl chloride second mixture by extractive distillation of the second mixture, thereby removing 1,1-differetn mostly free from vinyl is s variants of its embodiment with reference to the accompanying drawing, which depicts a system diagram of extractive distillation that can be used for practical implementation aspect of the invented method.Detailed description
1,1-Differetn (HFC-152a) are usually obtained by fluorination of vinyl chloride monomer (VCM) using hydrogen fluoride in the presence of a catalyst. The product 1,1-differetn may contain a variety of impurities such as by-product hydrogen chloride, by-products, such as 1-chloro-1-foraten, 1,1-dichloroethane and viniferin, as well as, among others, the unreacted vinyl chloride and hydrogen fluoride. While the majority of these impurities can be removed from 1,1-differetn conventional distillation, small amounts of vinyl chloride difficult, if not impossible, to remove using conventional methods of distillation, azeotropic formations or pinch-points between 1,1-defloration and vinyl chloride. The term "conventional distillation" refers to a technique in which separate components are used only relative volatility of the components of the mixture to be split.To determine the relative volatility 1,1-differetn and vinyl chloride used method, known is both absolute pressure in the chamber of known volume is measured at a constant temperature for various well-known two-component compositions of 1,1-differetn and vinyl chloride. The station reserve fuel facility use method described in the publication "Phase Equilibrium in Process Design", Wiley-Interscience Publisher, 1970, Harold R. Null, pages 124-126; full disclosure of which is incorporated by reference. These measurements of total pressure is converted to compounds with the equilibrium vapor-liquid in the cell through the use of models based on equations with coefficients activity type equations for the two fluids taking into account the interaction (NRTL), which describes not the ideal state of a liquid phase. Using the equation of the activity coefficients, such as the equation for the two liquids taking into account the interaction (NRTL), described in more detail in the publication "The Properties of Gases and Liquids," 4thedition, published by McGraw Hill, the authors Reid, Prausnitz and Poling, page 241-387; and in the publication "Phase Equilibria in Chemical Engineering," published in 1985 by Butterworth Publishers, author Stanley M. Walas, page 165-244. Full disclosure of each of these publications is incorporated by reference. Not wishing to be bound by any theory or explanation, the authors hope that the equation for the two liquids taking into account the interaction (NRTL) can sufficiently predict whether or not mixtures containing 1,1-differetn and vinyl chloride, to behave in an ideal manner, and can sufficiently predict the relative is acetow show relative volatility 1,1-differetn and vinyl chloride equal to approximately 1.0 for the given compositions of 1,1-differetn and vinyl chloride in the range of temperature variations. Relative volatility is approximately equal to 1.0, the mixture shows the formation of azeotropic mixtures. The station reserve fuel facility results of the measurements and the above calculations show that the composition of the azeotropic mixture varies with temperature. Table 1 shows the results of these calculations; especially how the composition of the resulting azeotropic mixture varies according to the temperature range. Due to the formation of azeotropic mixtures is difficult, if not impossible, to completely separate 1,1-differetn and vinyl chloride conventional distillation in those ranges of temperature and pressure, are shown in table 1.Based on the measurements using camera station reserve fuel facility and calculations, azeotropes disappears above a temperature of approximately 39,9-40,0oC. However, above this temperature, the relative volatility 1,1-differetn and vinyl chloride remain close to 1.0, which is indicative of the pinch-point of equilibrium vapor-liquid, which in turn shows that it is still essentially impossible to separate the components by conventional distillation. In predeclared would start with the composition, cleaner than the azeotropic mixture, and the residue 1,1-differetn necessarily at the end would be the same as the azeotropic mixture. Distillation at a temperature below -80oC and pressures below 3,79 KPa (0.55 pounds/square inch) would be a very low-temperature vacuum distillation. Therefore, the use of conventional distillation to obtain high purity 1,1-differetn (HFC-152a) would be expensive and would require a very large columns.The term "azeotropic mixture or azeotrope composition means constantly boiling liquid mixture of two or more substances that behaves as a single substance. One way to characterize the azeotropic composition or mixture is that the vapor produced by partial evaporation or distillation of the liquid has the same composition as the liquid from which it was evaporated or distilleries, for example, the mixture is distilled/delermined without compositional change. Constantly boiling compositions are characterized as azeotropic, because they exhibit either a maximum or minimum boiling point as compared with non-azeotropic mixtures of the same components. The azeotropic composition can also be characterized as the maximum or minimum Under the words "mixture, such azeotrope" is meant a composition that has the characteristic of constant boiling or tend not to fraktsionirovanija boiling or evaporation. The composition of the resulting pair is the same as or substantially the same as the original composition of the liquid. During boiling or evaporation, the composition of the liquid, if it ever changes, the only changes to the minimum or negligible degree.A composition similar to the azeotropic mixture may also be characterized by a plot (graph), which is related to the maximum or minimum vapor pressure. This can be seen when plotting the vapor pressure at a given temperature as a function of molar fraction. In the prior art is that the composition is similar to the azeotropic mixture, if after removal of about 50 wt.% composition, for example, evaporation or evaporation, the difference between the original composition and the remaining composition is approximately less than 6% and usually about less than 3% relative to the original composition.1,1-Differetn and vinyl chloride can be partial purified using the above-mentioned azeotropic compositions and such azeotropic mixtures of compounds in the method, which is named pressure in a conventional distillation column. For example, conventional distillation column can be operated at temperature and pressure conditions that induce the formation of an azeotropic and such azeotropic mixtures of compounds. If the amount of 1,1-differetn relatively high compared with vinyl chloride, the concentration of 1,1-differetn more than its concentration in the azeotrope and such azeotropic mixture composition, 1,1-differetn can be recovered in substantially pure form from the bottom of the column, while the azeotropic or similar azeotropic mixture composition is removed from the upper part of the column. On the contrary, if the amount of vinyl chloride is relatively high compared with 1,1-defloration the concentration of vinyl chloride is greater than its concentration in the azeotrope or similar azeotropic mixture composition, the vinyl chloride can be removed in substantially pure form from the bottom of the column, while the azeotropic or similar azeotropic mixture composition is removed from the upper part of the column.The results of measurements using camera station reserve fuel facility and previous calculations for 1,1-differetn and vinyl chloride with various extracting agents are provided below in table 2. Table 2 provides the coefficients activity 1,1-Est and also leads relations activity coefficient of HFC-152a/VCM (relative volatility) at a temperature of 0o(Except where noted in table 2). It is believed that the ratio of the activity coefficient 1,1-differetn at infinite dilution in the proposed extracting the substance to the activity coefficient of chloride at infinite dilution in the proposed extracting the substance is a relative volatility 1,1-differetn relative to vinyl chloride in the presence of the proposed extracting substances. "NBP" normal boiling point compounds at atmospheric pressure.Offer extracting substances for HFC-152a/VCM shown in table. 2.The problems associated with conventional distillation, can be solved through a process of extractive distillation. The extractive distillation can be used when the components of the mixture are such relative volatility, which is insufficient to ensure efficient separation of the components by conventional distillation. In extractive distillation is added extracting a substance that causes the relative volatility of the components of the mixture to change so that the relative volatility becomes sufficient to provide for the separation of components. The difficulty of applying this method sotoudeh effective agent in extractive distillation.Extractive distillation is usually carried out in the process of continuous distillation column, which contains: a multistage distillation column with at least two feed points, such as extracting agent is injected in the first injection point, which is located above the second point of the input used for introduction of the mixture to be split; a boiler; a condenser in the upper part of the column to return phlegmy in the column. Can also be used other similar commercially available device.The authors of the present invention have found that vinyl chloride can be effectively separated from 1,1-diflorasone, method of extractive distillation with extracting a substance selected from the group consisting of: aliphatic hydrocarbons, chlorinated hydrocarbons and alcohols having a normal boiling point greater than approximately 10oAnd less than approximately 120oC. the Preferred extracting agents with a normal boiling point between approximately 60oWith the 100oC. Examples of suitable extracting agents for the method of the present invention are the following: normal pentane, cyclopentane, neuroform), carbon tetrachloride, chlorate, 1,1-dichloroethane, 1,2-dichloroethane, 1,1,2-trichloroethane, methyl alcohol, ethyl alcohol and propyl alcohol. Extracting substances used in the present invention, generally commercially available.Method of extractive distillation of this invention for separating 1,1-differetn from the first mixture containing 1,1-differetn and vinyl chloride, includes the following stages:Contacting the first mixture with extracting a substance selected from the group consisting of: aliphatic hydrocarbons, chlorinated hydrocarbons and alcohols having a normal boiling point higher than approximately 10oC and lower than approximately 120oWith, for the formation of the second mixture, and
Department of 1,1-differetn from vinyl chloride second mixture by extractive distilling the second mixture in the area of extractive distillation, thus removing 1,1-differetn essentially free of vinyl chloride, as a product taken from the top of the column and from the bottom of zone a third mixture containing the extracting agent and vinyl chloride,
and more Department of extracting substances from the third mixture.By "essentially free" or "CA, usually less than about 0.1 wt.% vinyl chloride and in some cases less than about 10 parts per million by weight (ppm) of vinyl chloride.The first mixture can be obtained from any suitable manufacturing process or source, which produces 1,1-differetn with vinyl chloride as an impurity: typically by the reaction of vinyl chloride with anhydrous hydrogen fluoride in the presence of a metal catalyst. Examples of the metal catalyst, which can be used include, among others: palladium, vanadium and compounds of tin. Although the present invention is able to adapt to a wide range of compositions of 1,1-differetn/vinyl chloride, it is preferable that the content of 1,1-differetn was more than about 85 mol. % and the content of the vinyl chloride was less than about 15 mol. %. If desired, to reduce the initial amount of vinyl chloride or other admixtures can be used by ordinary distillation. That is, conventional distillation can be used to remove relatively large quantities or of clusters of impurities from the first mixture, which is then handled in accordance with the method of this image by the way that increases the volatility 1,1-differetn relative to vinyl chloride, and thus in the presence of more volatile 1,1-differetn becomes possible to extract it from the top of the distillation zone. Usually remote or extracted 1,1-differetn essentially free of vinyl chloride.Optionally, extracting the substance can then be removed from the admixture of vinyl chloride or a mixture of impurities conventional methods of distillation. Extracting the substance can be reused in the column extractive distillation to remove additional quantities of vinyl chloride 1,1-differetn.In one aspect of the invention, the extracting agent is injected in an upper feed point of the column extractive distillation, while the first mixture to be split, is introduced at a relatively lower point in the column. Extracting the substance passes down through the column plate, which is located in the centre of the pillar, and is in contact with the first mixture, thereby forming a second mixture.Since in the presence of extracting substance 1,1-differetn is relatively more volatile than the vinyl chloride, it allows 1,1-dottorato to go to the top of the column. 1,1-Deflorationact irrigation. At least part of this condensed stream can be returned to the top of the column in the form of phlegmy, and the residue can be removed as a useful product, that is essentially in the form of pure 1,1-differetn. If desired, 1,1-differetn may be directed to the second column extractive distillation and/or the second routine of distillation column for further purification.The vinyl chloride, extracting the substance and other possible impurities form the third mixture, which exits the bottom of the column and which may subsequently be sent to desorber or column conventional distillation to separate by conventional distillation or other known methods. Optionally, extracting the substance can then be returned for reuse in the column extractive distillation. In some cases, the vinyl chloride after removal of extracting substances by ordinary distillation is extracted as useful product for sale or other use, for example for the production of 1,1-differetn. The extracted chloride may also be transported to the second or third column of conventional and/or extractive distillation to remove other primase used extracting water-soluble substance, such as ethanol or another alcohol, extracting the substance can optionally be removed from vinyl chloride by other means such as extraction with water. For example, a mixture of vinyl chloride and extracting water-soluble substances pass through the water, whereby the alcohol is mainly extracted.The ratio of the flow of matter emerging from the upper part of the column extractive distillation, which is then condensed and subsequently is returned to the column, to the amount of flow of the material that is recovered as a useful product, commonly referred to as the coefficient of reverse flow (reflux). The coefficient of the return flow will determine the physical characteristics of the column extractive distillation.In General, the growth factor reverse flow will in turn cause increased purity 1,1-differetn taken from the upper part of the column, by reducing or eliminating the amount of extractant or other impurities 1.1-diflorasone on the top of the column.Specific conditions that can be used for implementing the method of the present invention is not critical and is dependent on a number of interrelated parameter is in other settings. Working pressure distillation systems can be in the range from approximately 103,43 KPa (15 psi) to 2413,25 KPa (350 psi), usually from about 344,75 KPa (50 psi) to 2068,5 KPa (300 psi). Temperature and heat transfer area of the head of the capacitor is usually sufficient to basically fully condensing distilled product, or, optionally, is sufficient to achieve the desired coefficient of reverse flow through partial condensation.An effective amount extracting substances can vary widely. Basically when you use an increased amount extracting substances will increase the purity 1,1-differetn the top of the column. Usually the ratio of the weight of the extracting agent to the weight of 1,1-differetn is in the range from about 1/1 to about 10/1; however, if necessary, can be used in more high-level relations.The temperature used at this stage in the invented method, is a function of the pressure and characteristics of the design of distillation columns, such as relationships extracting agent to the first mixture.Some aspects of izaberete Lisovets to implement one aspect of the method of extractive distillation of this invention. The first mixture containing 1,1-differetn with vinyl chloride as an impurity, is supplied by pipeline 1 in the extraction column 2. At least one liquid extracting the substance is fed via line 3 to the extraction column 2 and is introduced into the column 2 in position above the point of filing of the first mixture 1 for the formation of the second mixture. The third mixture containing the extracting agent and the vinyl chloride is removed from the bottom of column 2 and is transported to the boiler 4 steam heated. In some cases, the heater 4 is attached to the extractive column 2. The third mixture is delivered through the pipe 5 in the raw material tank 6. Additional liquid extracting a substance also serves to replenish the tank 6 through the pipe 7, thus forming a recirculation of the fourth mixture or extracting substances. The pump 8 transports the fourth mixture in desorbers column 9. Desorbitada column 9 divides the fourth mixture by extracting substances and nextrelease substances. Extracting the substance is removed from the column 9 and fed into the boiler 10 with steam heating. In some cases, the heater 10 is attached to the column 9. The pump 11 transports extracting the substance from Konsta extracting substances can be selected to achieve the refrigerator 12. Usually the refrigerator 13 is used at a temperature of approximately -25oC. After leaving the refrigerator 13 extracting the substance is fed via line 3 to the extraction column 2.The vinyl chloride may extend from the top desorbitada column 9 as exhaust gas and introduced into the condenser 14, which typically operates at a temperature of approximately -25oC. In this case, under conditions of reverse flow pump returns the part of vinyl chloride in desorbers column 9. The remaining part of the vinyl chloride can be removed from the system through the pipeline 16.The exhaust gas may also be removed from the extraction column 2. The exhaust gas may be 1,1-defloration, which is basically free from vinyl chloride and other fluorocarbons. 1,1-Differetn is transported by pipeline 17 to the condenser 18. The capacitor 18 is typically operates at a temperature of approximately -25oC. In this case, under conditions of reverse flow pump 19 returns part 1,1-differetn in the extraction column 2. Product - 1,1-differetn can be removed from the system through the pipeline 20.For extracting the substance was most effective for increasing volatility 1,1-diflorasone, automatic to be greater than approximately 1.0; for practical purposes, it should generally be greater than about 1.1. Normally, this relative volatility was greater than about 1.5, and more preferably, it was more than approximately 2.0.Examples
The following examples are provided to illustrate certain aspects of the present invention and do not limit the scope of the invention defined by the attached claims. The following examples use the parameters of the interaction equations for the two fluids taking into account the interaction (NRTL), identified above. In the following examples, each step is based on 100% efficiency or execution. In order to optimize the performance of each distillation, used different designs of the column and operating modes using different extracting agents. All of the examples of theoretical stages include a condenser and a reboiler, and a condenser is considered to be stage 1.Comparative example 1
In this example, the distillation column with 100 theoretical stages is used to clear the flow of incoming material consisting of 453,59 kg/h (1000 lb/h) of the crude differetn HFC-152a, from incoming material no. The incoming material is entered at step 50 with the pressure of the condenser of the column, equal 259,94 KPa (37,7 pounds/square inch). The temperature of the distillate is approximately equal to 0oC, and the temperature in the lower part of the column is approximately equal to 1.8oC. Under these operating conditions the product HFC-152a will be released from the column in the flow of the lower part of the column. Speed phlegmy in the column is set to satisfy the following composition: 10 parts per million of vinyl chloride VCM in the product HFC-152a bottom of the column. The diameter of the column is chosen such as to have a maximum F-factor (a standard measure of allowable volumetric flow rates per unit cross-sectional area of the column) equal to 1.3 or below. In this example, the diameter of the column is equal to 101.6 cm (40 inches) and F-factor equal to 1.12. This distillation process is shown below in table 3.Comparative example 2
This test is performed under the same conditions as in comparative example 1, except that the pressure in the column is 101,36 KPa (14.7 psi), the temperature of the distillate is approximately equal to -24oC, and the temperature in the lower part of the column is approximately equal -19,7oC. In this example, the diameter of the column is equal 71.12 cm (28 Dunny example 3
This test is performed under the same conditions as in comparative example 1, except that the pressure in the column is 27,92 KPa (4,05 pounds/square inch), the temperature of the distillate is approximately equal -49,7oC, and the temperature in the lower part of the column is approximately equal -39,5oC. In this example, the diameter of the column is equal to 60,96 cm (24 inches) and F-factor equal to 1.19. The results of this distillation process is shown below in table 5.The above-mentioned comparative examples 1, 2 and 3 show that conventional distillation is relatively ineffective for separating vinyl chloride VCM from HFC-152a and has a very low yield of HFC-152a. However, these examples show how the concentration of vinyl chloride VCM can be reduced in mixtures containing VCM vinyl chloride and HFC-152a by azeotropic distillation.Example 1
In this example, the column extractive distillation with 37 theoretical stages is used to clear the flow of incoming material consisting of 453,59 kg/h (1000 lb/h) of the crude differetn HFC-152a, containing 0,045 kg/h (0.1 lb/h) of the vinyl chloride VCM, VCM concentration of 100 parts per million. No other impurities in the incoming material no. The incoming material is introduced at stage 25 and extragere the temperature of the distillate equal -2,7oC, and the temperature in the lower part of the column equal to 100.0oC. Under these operating conditions the product HFC-152a will be released from the column in the flow of the upper part of the column. The VCM vinyl chloride and n-hexane will be released in the stream bottom of the column. The flow rate of extracting substances is set such as to satisfy the composition is 1 part per million of vinyl chloride VCM in the product HFC-152a upper part of the column. The flow rate of phlegmy in the column is set to meet the part - 10 part per million extracting substances in the product HFC-152a upper part of the column. The speed of the distillate is adjusted to remove 452,68 kg/h (998,0 lb/h) product HFC-152a in the flow of the upper part of the column. The diameter of the column is chosen such as to have an F-factor of 1.3 or below. In this example, the diameter of the column is equal to 101.6 cm (40 inches) and F-factor equal to 1.12. The results of using this method of extractive distillation is shown below in table 6.Example 2
In this series of test conditions are the same as in example 1, except where noted. The following table 7 summarizes the processes of extractive distillation using n-hexane and other hydrocarbons extracting substances, the applicable entrace VCM vinyl chloride and extracting the substance in the product HFC-152a are 1 and 10 parts per million by weight, respectively. The geometry of the column, a stream extracting substances and flow phlegmy vary in order to achieve these results (see tab. 7).Example 3
Conditions, flow rate and purity of HFC-152a in this example are the same as in example 1, except that modified some alcohols as extracting agents. String design was modified, as shown in the final table 8.Example 4
Conditions, flow rate and purity of HFC-152a in this example are the same as in example 1, except those modified for the use of certain chlorinated hydrocarbons as extracting agents. String design was modified, as shown in the final table of 9.Provided that the presence of azeotropic mixtures in molar fractions of 1,1-differetn is greater than about 81% in a mixture with vinyl chloride (table 1), a surprising and unexpected result was that the vinyl chloride may be separated from 1,1-differetn to obtain essentially pure 1,1-differetn by extractive distillation using some easily available and cheap connections, free from Fernie vinyl chloride, include: aliphatic hydrocarbons, chlorinated hydrocarbons and/or alcohols having a normal boiling point higher than approximately 10oC and lower than approximately 120oC.For each of the three classes extracting substances (hydrocarbons, alcohols, chlorinated hydrocarbons) required parameters: stream extracting substances and the number of steps decreases as you increase the ratio of the activity coefficients (i.e. the higher the ratio, the better). Although the best extracting substances at the proposed conditions of this table is usually n-hexane and carbon tetrachloride, the most effective extracting agent in an industrial environment may depend on the precise level of concentration and composition of impurities and the ability of extracting substances to provide simultaneous removal of other impurities, which may also be present.Although there have been described in detail some specific aspects of the invention, a specialist should understand what is covered and other variants of embodiments and variations. 1. The method of purification of 1,1-differetn extractive distillation from the first mixture containing 1,1-differetn and vinyl chloride, comprising contacting PV, alcohols and chlorinated hydrocarbons having a normal boiling point higher than approximately 10oWith, and lower than about 120oWith, for the formation of the second mixture, and separating 1,1-differetn from the second mixture by extractive distillation of the second mixture, thereby removing 1,1-differetn, mostly free from chloride.2. The method according to p. 1, characterized in that the first mixture consists essentially of 1,1-diflorasone, 1-chloro-1-floridana, 1,1-dichloroethane, vinyl chloride, winifrida, hydrogen fluoride and hydrogen chloride.3. The method according to p. 1, wherein the 1,1-differetn, resulting in this stage of separation, contains less than approximately 50 hours per million of vinyl chloride.4. The method according to p. 1, wherein extracting the substance includes at least one compound selected from the group consisting of normal pentane, cyclopentane, normal hexane, cyclohexane, normal heptane, chloromethane, dichloromethane (methylene chloride), trichloromethane (chloroform), carbon tetrachloride, chlorethane, 1,1-dichloroethane, 1,2-dichloroethane, 1,1,2-trichloroethane, methyl alcohol, ethyl alcohol and propyl alcohol.6. The method according to p. 1, wherein the extractive distillation is carried out at a pressure of from about 103,43 KPa (15 psi) to 2413,25 KPa (350 psi).7. The method according to p. 1, characterized in that the ratio of the weight of the extracting agent to the weight of 1,1-differetn is from about 1/1 to 10/1.8. The method according to p. 1, characterized in that the specified 1,1-differetn and vinyl chloride first mixture is azeotropic mixture.
FIELD: ecology; hydrochemistry; analytical chemistry; methods of extraction of the volatile organic substances from the water medium.
SUBSTANCE: the invention is pertaining to the field of ecology, hydrochemistry, analytical chemistry and may be used for extraction of the organic compounds from the water mediums, in particular, from the mineral waters including sulfide mineral waters. For realization of the method of extraction of the volatile organic substances from the water medium into the organic dissolvent conduct the joint condensation of the extracted substance produced as a result of distillery and the vapor of the dissolvent. For production of the joint condensate they gate the vapor-shaped dissolvent through the water sample or preliminary add it into the water sample with the subsequent distillation. The organic dissolvent is chosen from the following row: ethanol, acetonitrile, acetone, hexane. The method ensures the single-stage extraction of the dissolved organic substances into the dissolvents, the unlimited their mixing with the water, reduction of the thermal action on the researched sample, the increase of the extraction ratio.
EFFECT: the invention ensures the single-stage extraction of the dissolved organic substances into the dissolvents, their unlimited mixing with the water, the reduced the thermal action on the researched sample, the increased extraction ratio.
2 cl, 1 tbl, 5 ex