Installation for the purification by distillation of the chlorinated products and methods for purification by distillation at her, carbon tetrachloride, chloroform, trichloroethylene, methylene chloride and perchloroethylene

 

The invention relates to the production of chlorinated organic products, in particular to the field of purification by distillation. Installation for the purification by distillation of chlorinated organic solvents contains connected to a source of solvent cube mounted on a last and communicated with him Packed distillation column of periodic action, the top of which is connected to the reflux condenser, and the latter by leaving it connected to the top of the distillation column and to the tanks for collection of the product distillation, when this installation is further provided with at least two containers for selection of products reactive qualifications and cage selection aqueous intermediate fraction, installed at the outlet of the reflux condenser and connected to a distillation column and capacity to collect Pradhana through the separator, distillation column is composed of three glass-bars of the same height, are tightly interconnected, and the diameter of the Packed distillation column is from 0.06 to 0.07 height of the distillation column at the height of the last from 2800 to 3200 mm, a cube made of enameled cast iron, and a reflux condenser and capacity to collect product distillation - glass. Izobreteniya deep purification by distillation of carbon tetrachloride, chloroform, trichloroethylene, methylene chloride and perchloroethylene. 6 N. p. F.-ly, 1 Il.

The invention relates to the production of chlorinated organic products, in particular to the field of purification by distillation.

Known installation for the distillation of small industrial quantities of solvents containing the evaporation chamber water with an electric heater, a steam pipe, a water cooling system (see RF patent 2068729, CL 01 D 3/32, 10.11.1996.

This installation is quite simple. However, it is not possible to obtain highly pure substances, which limits the scope of use of this setting.

Known treatment plant chlorinated solvents, in particular methylchloride containing distillation column and mounted on the top of the column system refrigerators-capacitor (see application WO 98/37044, class C 07 C 17/38, 27.08.1998).

This system helps to remove impurities from methylchloride. However, it also does not allow to achieve high purity of the obtained product, which is consistent with the limited separation of the product after its release from the top of the distillation column.

Closest to the image is by the installation for the purification by distillation of chlorinated solvents, containing connected to a source of solvent cube mounted on a last and communicated with him Packed distillation column of periodic action, the top of which is connected to the reflux condenser, and the latter by leaving it connected to the top of the distillation column and to the tanks for collection of the product distillation (see Japan patent JP 2001072623, class C 07 C 17/383, 21.03.2001).

This setting allows the cleanup of organochlorine products. However, the performance of this setup is not used in full, due to the fact that it is not possible to obtain several products of the distillation of varying degrees of purity.

Known purification method chlorohydrocarbons methane series, in particular chloroform and methyl chloride, and the selection of methylene chloride in the form of distillate the rectification column. The purification of chloroform carried out with sulfuric acid (see RF patent 2127245, class C 07 C 17/16, 10.03.1999).

However, this method does not allow the production of reactive skills. In particular methylene chloride receive clean all of 99.7%.

A known method of purification of chloroform in the rectifying mode using as oxidant patalastas antimony (see patent R the W production, that also limits the scope of use of this method of purification of chlorinated solvents.

Known purification method organochlorine products from resin and carbon black, in particular methylene chloride, chloroform, carbon tetrachloride and trichloroethylene. The cleaning method is that in organochlorine products before evaporation or distillation of the injected fuel within boiling from 150 to 500°With (see RF patent 2051887, CL 07 With 17/42, 10.01.1996).

This method allows you to achieve cleanup of organochlorine products from tar and soot, but does not allow to achieve purity distillation products reactive qualifications, for example, “pure for analysis”.

Closest to the invention in part of the way, as an object of the invention is a method of purification of chlorinated solvents, namely, that in the cube download source solvent, is heated in the cube to the boiling point and guide couples in a distillation column, from the last pair arrive in the reflux condenser, where they condense and reflux condenser condensate through the separator serves in the upper part of the distillation columns in the form of phlegmy, which, in contact with vapors of the solvent condenses its volatile ingredients of Koghb with the formation of the cube thus residue, and a couple of solvent-enriched volatile nscontainerframe components is sent to the reflux condenser, which is cooled and condensed, and then after stabilization of the operation of the distillation column portion of the condensate is sent in the form of phlegmy in the distillation column, and the other part of the condensate as a product of the distillation is in the tank for collection of the product distillation (see the above-mentioned Japan patent JP 2001072623).

However, this known method of purification of chlorinated organic products does not take into account the peculiarities of the purification by distillation of products such as carbon tetrachloride, chloroform, trichloroethylene, methylene chloride and perchloroethylene, which does not allow full use of the possibilities of a distillation unit and to obtain products of the desired high purity, in particular the products of qualification “chemically pure” or “purity”.

Task to be solved by the present invention is directed, is to increase the efficiency of the installation for the purification by distillation of the chlorinated products and deep purification by distillation of carbon tetrachloride, chloroform, trichloroethylene, methylene chloride and perchloroethylene.

The specified task in the organic solvents contains connected to a source of solvent cube mounted on the latter and informed him of the Packed distillation column of periodic action, the top of which is connected to the reflux condenser, and the latter by leaving it connected to the top of the distillation column and to the tanks for collection of the product distillation, when this installation is further provided with at least two containers for selection of products reactive qualifications and separator installed at the outlet of the reflux condenser and connected to a distillation column and containers to collect water intermediate fraction and Pradhana through the separator distillation column is composed of three glass-bars of the same height, are tightly interconnected, and the diameter of the Packed distillation column is from 0.06 to 0.07 height of the distillation column at the height of the last from 2800 to 3200 mm, a cube made of enameled cast iron, and a reflux condenser and capacity to collect distillation products from the glass.

In terms of method, as the object of the invention, this problem is solved due to the fact that the method of purification by distillation of carbon tetrachloride is that in the cube load carbon tetrachloride technical (Chu), heat it in the cube to the temperature CI the and condensate through the separator serves in the upper part of the distillation columns in the form of phlegmy, which, contacting with pairs of Chu condenses its volatile ingredients components, Chu in the form of a liquid phase, enriched in volatile ingredients components sent back to the cube with the formation of the cube thus balance, and a pair of Chu enriched volatile nscontainerframe components is sent to the reflux condenser, which is cooled and condensed, and then after stabilization of the operation of the distillation column portion of the condensate is sent in the form of phlegmy in the distillation column, and the other part of the condensate as a product of the distillation vessel to collect the product distillation, supporting reflux number equal to 4, download Cho technical cube produced at room temperature, Chu, while in Cuba support equal to the atmospheric pressure, produce heat, Chu to a temperature 75-77°C and within 30-40 min all condensate from the dephlegmator sent back to the distillation column in the form of phlegmy and support the flow phlegmy from 180 to 200 DM3/h, and the condensate from the dephlegmator is served in the distillation column through a separator, through which are selected from the condensate water of the intermediate fraction and Pradhan, and then taken away after the reflux condenser, the condensate part - prod is Lisa, “chemically pure”, and the selection of the specified condensation is carried out in the following quantities: water, the intermediate fraction from 2.0 to 2.5%, Pradhan from 2 to 6%, “net” - from 28 to 30%, “pure for analysis” - from 25% to 28% and about “chemically pure” - from 28 to 30% on everything from the number loaded into the cube Chu, then the process of distillation ceased, VAT residue disposed of, and the distillation of the products sent to the destination.

Another way, as the object of the invention is a method of purification by distillation of the chloroform, which is that in the cube load chloroform technical, heat it in the cube to the boiling point and guide couples in the distillation column and then in the reflux condenser where they are condensed, from the reflux condensate through the separator serves in the upper part of the distillation columns in the form of phlegmy, which, in contact with vapors of chloroform, condenses its volatile ingredients components chloroform in the liquid phase, enriched in volatile ingredients components sent back to the cube with the formation of the cube thus balance, and a pair of chloroform, enriched volatile nscontainerframe components, is sent to the reflux condenser, which is cooled and condensed, and then injecting the column, and another part of the condensate as a product of distillation in the tank distillation products, supporting reflux a number equal to 4, the loading of chloroform in technical cube is carried out at room temperature chloroform, and in a cube support pressure equal to the atmospheric produce heating of chloroform to a temperature of 60-65°C and within 30-40 min all condensate from the dephlegmator sent back to the distillation column in the form of phlegmy and support the flow phlegmy from 110 to 130 DM3/h, and the condensate from the dephlegmator is served in the distillation column through a separator, through which are selected from the condensate water of the intermediate fraction and Pradhan, and then taken away after a dephlegmator part of the condensation products of reactive qualifications in a separate container in the following order: “clean”, “pure for analysis”, “chemically pure”, and the selection of the specified condensation is carried out in the following quantities: water, the intermediate fraction from 2.0 to 3.0%, Pradhan from 10 to 12%, “clean” from 20 to 25% vol, “pure for analysis” from 28 to 30% and about “chemically pure” from 12 to 15% on everything from the number loaded into the cube of chloroform, then the process of distillation by pregraduation of the invention, is the method of purification by distillation of trichloroethylene, which is that in the cube load trichloroethylene technical, heat it in the cube to the boiling point and guide couples in the distillation column and then in the reflux condenser, where they condense and reflux condenser condensate through the separator serves in the upper part of the distillation columns in the form of phlegmy, which is in contact with the vapors of trichloroethylene, condenses its volatile ingredients components trichloroethylene in the form of a liquid phase, enriched in volatile ingredients components sent back to the cube with the formation of the cube thus residue and vapors of trichloroethylene, enriched with the volatile nscontainerframe components, send in the reflux condenser, which is cooled and condensed, and then after stabilization of the operation of the distillation column portion of the condensate is sent in the form of phlegmy in the distillation column, and the other part of the condensate as a product of the distillation is in the tank for collection of the product distillation, supporting reflux a number equal to 4, the loading of trichloroethylene technical cube is carried out at room temperature trichloroethylene, and in a cube support pressure equal to the atmospheric, production is back to the distillation column in the form of phlegmy, support flow phlegmy from 100 to 120 DM3/h, and the condensate from the dephlegmator is served in the distillation column through a separator, through which are selected from the condensate water of the intermediate fraction and Pradhan, and then taken away after a dephlegmator part of the condensation products of reactive qualifications in a separate container in the following order: “net”, “chemically pure”, “purity”, and the selection of the specified condensation is carried out in the following quantities: water, the intermediate fraction from 1.0 to 2.0%, Pradhan from 15 to 17%, “clean” from 18 to 20%, “chemically pure” - from 28 to 30% and about “purity” - from 10% to 12% on everything from the number loaded into the cube trichloroethylene, then the process of distillation ceased, VAT residue disposed of, and the distillation of the products sent to the destination.

Another way, as the object of the invention is a method of purification by distillation of the methylene chloride, which is that in the cube load methylene chloride technical, heat it in the cube to the boiling point and guide couples in the distillation column and then in the reflux condenser, where they condense and reflux condenser condensate through the separator serves in the upper part technollogies components, methylene chloride in the liquid phase, enriched in volatile ingredients components sent back to the cube with the formation of the cube thus balance, and a pair of methylene chloride enriched volatile nscontainerframe components, is sent to the reflux condenser, which is cooled and condensed, and then after stabilization of the operation of the distillation column portion of the condensate is sent in the form of phlegmy in the distillation column, and the other part of the condensate as a product of the distillation is in the tank for collection of the product distillation, supporting reflux number is 4, the loading of methylene chloride technical cube produced at room temperature, methylene chloride, in Cuba support pressure equal to the atmospheric produce heat source solvent to a temperature of 40-44°C and within 30-40 min all condensate from the dephlegmator sent back to the distillation column in the form of phlegmy and support the flow phlegmy from 200 to 240 DM3/h, and the condensate from the dephlegmator is served in the distillation column through a separator, through which are selected from the condensate water of the intermediate fraction and Pradhan, and then taken away after a dephlegmator part condensates clean, moreover, the selection of the specified condensation is carried out in the following quantities: water, the intermediate fraction from 1 to 3%, Pradhan from 13 to 15%, “net” - from 20 to 23.5% and about “chemically pure” - from 45 to 50% on everything from the number loaded into the cube methylene chloride, then the process of distillation ceased, VAT residue disposed of, and the distillation of the products sent to the destination.

Another method of purification by distillation of perchloroethylene lies in the fact that in the cube load perchloroethylene technical, heat it in the cube to the boiling point and guide couples in the distillation column and then in the reflux condenser, where they condense and reflux condenser condensate through the separator serves in the upper part of the distillation columns in the form of phlegmy, which, contacting with pairs of perchloroethylene, condenses its volatile ingredients components, perchlorethylene in the form of a liquid phase, enriched in volatile ingredients components sent back to the cube with the formation of the cube thus balance, and a pair of perchloroethylene, enriched volatile nscontainerframe components, send in the reflux condenser, which is cooled and condensed, and then after stabilization of the operation of the distillation column part contingency - in containers for collection of the product distillation, supporting reflux a number equal to 4, the loading of perchloroethylene technical cube is carried out at room temperature of perchloroethylene in Cuba support pressure equal to the atmospheric produce heating of perchloroethylene to a temperature of 125 to 130°C and within 30-40 min all condensate from the dephlegmator sent back to the distillation column in the form of phlegmy support the flow phlegmy from 120 to 150 DM3/h, and the condensate from the dephlegmator is served in the distillation column through a separator, through which are selected from the condensate water of the intermediate fraction and Pradhan, and then taken away after a dephlegmator part of the condensation products of reactive qualifications in a separate container in the following order: “net”, “chemically pure”, and the selection of the specified condensation is carried out in the following quantities: water, the intermediate fraction from 2.0 to 5.0%, Pradhan from 7 to 9%, “net” - from 40% to 43% about and “chemically pure” - from 38 to 40% on everything from the number loaded into the cube of perchloroethylene, then the process of distillation ceased, VAT residue disposed of, and the distillation of the products sent to the destination.

In the course once glass, for example of glass Simax collected from three bars of the same height, tightly interconnected with a diameter of from 0.06 to 0.07 from the height of the distillation column at a total height of the distillation column from 2800 to 3200 mm, allows you to get the rectification products qualification “chemically clean” and “pure for analysis” with a total yield of pure product up to 75% of its initial amount, which is economically justified. In addition, if the installation were used materials for use during distillation purification allows to obtain products of reactive qualifications, namely cast iron cube with enamel coating and a fluorine-containing elastomer gaskets in the joints of the structural elements of the installation.

In the course of the study were obtained optimal conditions for purification by distillation of carbon tetrachloride, chloroform, trichloroethylene, methylene chloride and perchloroethylene. For carbon tetrachloride were set the following parameters: reflux a number equal to 4, the downloading of the original solvent in the cube at room temperature and heating the raw product to a temperature 75-77°C. Heating to lower tempera stable operation of the column. The operation of distillation columns “on” for 30-40 min, when all condensate from the dephlegmator sent back to the distillation column as phlegmy and support the flow phlegmy from 180 to 200 l/h allows to reach a stable mode of operation in which it is possible to achieve the required degree of purification of carbon tetrachloride. The flow of condensate from the reflux condenser in the distillation column through the separator allows to make a selection from the condensate water of intermediate fraction and Pradhana. All the above allows to start the selection after a dephlegmator products reactive qualifications in a separate container in the following order: “clean”, “pure for analysis”, “chemically pure”.

Given the stable nature of the work of the distillation column, it is possible to determine the number of selected purified product of the distillation of each of the qualifications of purity, namely the selection in the following quantities: water, the intermediate fraction from 2.0 to 2.5%, Pradhan from 2 to 6%, “net” - from 28 to 30%, “pure for analysis” - from 25% to 28% and about “chemically pure” - from 28 to 30% on everything from the number of loaded source of solvent.

Similarly were experimentation and perchloroethylene. The result had failed to solve in the invention the task is to improve the efficiency of the installation for the purification by distillation of organochlorine products and spend quality purification by distillation of carbon tetrachloride, chloroform, trichloroethylene, methylene chloride and perchloroethylene.

The drawing shows a schematic diagram of an installation for the purification by distillation of the chlorinated solvents.

Installation for the purification by distillation of chlorinated organic solvents contains connected to the source of the original product cube 1, mounted on a last and communicated with him Packed distillation column 2 of the periodic steps, the top of which is connected to the reflux condenser 3, and the latter by leaving it connected to the top of the distillation column 2, and to the tanks 4, 5, 6 for collecting the product of the reactive distillation qualification. Installation is further provided with a separator 8, is installed at the outlet of the reflux condenser 3 and is connected to a distillation column 2 and the tanks 7, 9, respectively, to collect Pradhana and selection of water intermediate fraction. Distillation column 2 is made of three glass-bars of the same height, tightly interconnected with ispwest "H" of the distillation column 2 at the height of the last from 2800 to 3200 mm Cube 1 is made of enameled cast iron, and the receptacles 4, 5, 6 for collecting product distillation - glass.

The method of purification by distillation of carbon tetrachloride is produced as follows. Download cube 1 carbon tetrachloride technical, heat it in a cube 1 to boiling point and guide couples in the distillation column 2 and the next pair is sent to the reflux condenser 3 where vapors by cooling condense. Later in distillation column 2 with its top serves the phlegm, which is in contact with vapors of carbon tetrachloride, condenses the volatile ingredients components carbon tetrachloride with the formation of such remainder, the latter sent back to the cube, and a pair of carbon tetrachloride with volatile nscontainerframe components is sent to the reflux condenser 3, in which the volatile component is cooled and condenses. After this part of the condensate is sent in the form of phlegmy in a distillation column 2, and the other part as a product of the distillation is in the tank 4, 5, 6 for collecting the product of distillation. During distillation reflux support a number equal to 4. Loading of carbon tetrachloride in the cube 1 is carried out at room temperature of carbon tetrachloride, while et is the temperature 75-77°C and within 30-40 min all condensate from the dephlegmator 3 sent back to the distillation column 2 as phlegmy and support the flow phlegmy from 180 to 200 DM3/h, and the condensate from the dephlegmator is served in the distillation column 2 through the separator 8 through which the produce selection from the condensate water of intermediate fraction in a special container 9, and then conduct a selection after separator Pradhana into the container 7 and then dephlegmator make the selection of the condensation product from the reactive qualifications in a separate container in the following order: “net” capacity 4, “pure for analysis” in the tank 5 and “chemically pure” in the tank 6, and the selection of the specified condensation is carried out in the following quantities: water, the intermediate fraction from 2.0 to 2.5% about, Pradhan from 2 to 6%, “net” - from 28 to 30%, “pure for analysis” - from 25% to 28% and about “chemically pure” - from 28 to 30% on everything from the number loaded into the cube 1 carbon tetrachloride. After this, the process of distillation ceased, VAT residue disposed of, and the distillation of the products sent to the destination.

Similarly, but with the above operating parameters and parameters selection of the products of rectification spend cleaning chloroform, trichloroethylene, methylene chloride and perchloroethylene.

Example 1

Feedstock carbon tetrachloride GOST 4-84 “High” and what is 400 DM3.

Cube 1 is heated by steam (P=0.7-1.2 at).

Pair of carbon tetrachloride climb the Packed part of the distillation column 2, and then pass through the steam line temperature vapor, which is measured by a thermometer (t=75-77°C). After the steam, vapors are condensed in the reflux condenser 3, the cooling with cold water.

The condensed vapors enter the separator 8 and is returned back into the distillation column 2. Return phlegmy 180-200 DM3/hour. Distillation column 2 is “on” 30-40 minutes

In the process of the distillation column 2 “on” selection is made of the water of intermediate fraction accumulating in the upper layer of the separator 8, which open the valve and drain the water fraction in the collector 9. As water abstraction product in the separator 8 is gradually lightened. Distillation column 2 is “on” before full clarification of carbon tetrachloride.

The number of filters depends on the quality of raw materials, namely from the presence of water and varies in volume from 8 to 10 DM3.

After working distillation column 2 “on” starts the selection of Pradhana in volume 8-24 DM3. Open the valve and Pradhan enters the collector (capacity) 7. atory in the next two selections Pradhana within 1-0.5°C and a positive laboratory analysis can proceed to the selection of the finished product.

First select the product qualification “clean” in the amount of 112-120 DM3in a container (collection) 4, which open the valves at its input, then select the product qualification “pure for analysis” in the amount of 100-112 DM3for this , close the valve on the tank 4 and open the valve on the container 5. Filling capacity 5, close the valve on the tank and open the valve on the tank 6 to select the product qualification “chemically pure” in the amount of 112-120 DM3. After the selection of the finished product, close the valves at the outlet of the reflux condenser.

For shutdown of the column stop the supply of steam to the jacket of the cube 1. Cool the top of the distillation column 2 to room temperature, then shut off the water in the reflux condenser 3. The cube is cooled to 30°C. Pradhan, product and VAT residue is subjected to physico-chemical methods of analysis quality. VAT residue poured into drums for disposal. Distillation column 2 begin to prepare for the next launch, as described above.

Example 2

Raw materials (chloroform GOST 20015-88, the highest and first grade or technical) is loaded from drums collection under vacuum (P=0.5 at). From the latest source raw material is poured into a cube in the amount of 400 DM3

A pair of chloroform climb the Packed part of the distillation column 2, are the steam, the temperature of the vapor which is measured by a thermometer (t=60 to 65°C). After the steam, vapors are condensed in the reflux condenser 3, the cooling with cold water.

The condensed vapors enter the separator 8 and is returned back into the distillation column 2. Column 2 is “on” 30-40 minutes

In the process columns “on” selection is made of the water of intermediate fraction accumulating in the upper layer of the separator 8, which open the gate input capacitance (collector) 9. The number of filters depends on the quality of raw materials, namely from the presence of water. The total number of selection is 8-12 DM3.

After work columns “on” starts the selection of Pradhana in volume 40-48 DM3. Pradhan enters the tank 7. After selection of Pradhana (average temperature in Cuba 62°C, and in the upper part of the rectifying column - 61.2°C) proceed to the selection of a commercial product.

First select the product qualification “clean” in the amount of 80-100 DM3in tank 4, which open the valves at its input, then select the product qualification “pure for analysis” in the amount of 112-120 d is eating the valve on the tank 5 and open valve capacity 6 for selection of product qualification “chemically pure” in the amount of 48-60 DM3. After the selection of the finished product, close the gates.

For shutdown of the distillation column 2 stop the supply of steam to the jacket of the cube 1. Cube 1 is cooled by water through the jacket. Cool the top of the distillation column 2 to room temperature, then shut off the cooling water in the reflux condenser 3. The cube is cooled to 30°C. Pre Pradhan, product and VAT residue is subjected to physico-chemical methods of analysis on the quality of the wash is 21 DM3the chloroform. VAT residue poured into drums for disposal. Pradhan poured into drums for disposal. The product from the tanks 4, 5, 6 are sent for packing, pre-stabilized ethyl alcohol (1% by weight of the finished product), column start to prepare for the next launch, as described above.

Example 3

Raw materials (trichloroethylene technical) is loaded from drums collection under vacuum (P=0.5 at). From the latest source raw material is poured into a cube in the amount of 400 DM3.

Before you begin column open air line. Cube 1 is heated by steam (P=0.5 at). Why open the corresponding valve in the line supplying steam from the steam generator and the valves for selection of a condensate of steam.

A pair of trichloroethylene rise by thermometer (t=89-95°C). After the steam, vapors are condensed in the reflux condenser 3, the cooling with cold water.

The condensed vapors enter the separator 8 and is returned back into the distillation column 2. Column 2 is “on” 30-40 min. Consumption phlegmy 100-120 DM3/PM

In the process columns “on” selection is made of the water of intermediate fraction accumulating in the upper layer of the separator 8, which open the gate input capacitance (collector) 9. The number of filters depends on the quality of raw materials, namely from the presence of water. The total number of selection is 4-8 DM3.

After work columns “on” starts the selection of Pradhana in volume 60-68 DM3.Pradhan enters the tank 7. After selection of Pradhana proceed to the selection of a commercial product.

First select the product qualification “clean” in the amount of 72-80 DM3in tank 4, which open the valves at its input, then select the product qualification “chemically pure” in the amount of 112-120 DM3for this , close the valve on the tank 4 and open the valve on the container 5. Filling capacity 5, close the valve on the tank 5 and open valve capacity 6 for selection of product qualification “special clean ifications column 2 stop the supply of steam to the jacket of the cube 1. Cube 1 is cooled by water through the jacket. Cool the top of the distillation column 2 to room temperature, then shut off the cooling water in the reflux condenser 3. The cube is cooled to 30°C. Pre Pradhan, product and VAT residue is subjected to physico-chemical methods of analysis quality. VAT residue poured into drums for disposal. Pradhan poured into drums for disposal. The product from the tanks 4, 5, 6 refer to the packing, the column begin to prepare for the next launch, as described above.

Example 4

Raw materials (methylene chloride technical) is loaded from drums collection under vacuum (P=0.5 at). From the latest source raw material is poured into a cube in the amount of 400 DM3.

Before you begin column open air line. Cube 1 is heated by steam (P=0.5 at). Why open the corresponding valve in the line supplying steam from the steam generator and the valves for selection of a condensate of steam.

A pair of methylene chloride climb the Packed part of the distillation column 2, are the steam, the temperature of the vapor which is measured by a thermometer (t=40-44°C). After the steam, vapors are condensed in the reflux condenser 3, the cooling with cold water.

The condensed vapors into Zaphod phlegmy 200-240 DM3/PM

In the process columns “on” selection is made of the water of intermediate fraction accumulating in the upper layer of the separator 8, which open the gate input capacitance (collector) 9. The number of filters depends on the quality of raw materials, namely from the presence of water. The total number of selection is 4-12 DM3.

After work columns “on” starts the selection of Pradhana in volume 52-60 DM3. Pradhan enters the tank 7. After selection of Pradhana proceed to the selection of a commercial product.

First select the product qualification “clean” in the amount of 80-94 DM3in tank 4, which open the valves at its input, then select the product qualification “chemically pure” in the amount of 180-200 DM3for this , close the valve on the tank 4 and open the valve on the container 5. After the selection of the finished product, close the gates.

For shutdown of the distillation column 2 stop the supply of steam to the jacket of the cube 1. Cube 1 is cooled by water through the jacket. Cool the top of the distillation column 2 to room temperature, then shut off the cooling water in the reflux condenser 3. The cube is cooled to 30°C. Pre Pradhan, product and VAT residue is subjected physics to waste. The product from the tanks 4, 5 is sent to the packing, the column begin to prepare for the next launch, as described above.

Example 5

Raw materials (perchloroethylene technical) is loaded from drums collection under vacuum (P=0.5 at). From the latest source raw material is poured into a cube in the amount of 400 DM3.

Before you begin column open air line. Cube 1 is heated by steam (P=0.5 at). Why open the corresponding valve in the line supplying steam from the steam generator and the valves for selection of a condensate of steam.

Pair of perchloroethylene climb the Packed part of the distillation column 2, are the steam, the temperature of the vapor which is measured by a thermometer (t=125 to 130°C). After the steam, vapors are condensed in the reflux condenser 3, the cooling with cold water.

The condensed vapors enter the separator 8 and is returned back into the distillation column 2. Column 2 is “on” 30-40 min. Consumption phlegmy is 120-150 DM3/PM

In the process columns “on” selection is made of the water of intermediate fraction accumulating in the upper layer of the separator 8, which open the gate input capacitance (collector) 9. The number of filters depends on the quality ishodovani “on” starts the selection of Pradhana in volume 28-36 DM3.Pradhan enters the tank 7. After selection of Pradhana proceed to the selection of a commercial product.

First select the product qualification “clean” in the amount of 160-172 DM3in tank 4, which open the valves at its input, then select the product qualification “chemically pure” in the amount of 152-160 DM3for this , close the valve on the tank 4 and open the valve on the container 5. After the selection of the finished product, close the gates.

For shutdown of the distillation column 2 stop the supply of steam to the jacket of the cube 1. Cube 1 is cooled by water through the jacket. Cool the top of the distillation column 2 to room temperature, then shut off the cooling water in the reflux condenser 3. The cube is cooled to 30°C. Pre Pradhan, product and VAT residue is subjected to physico-chemical methods of analysis quality. VAT residue poured into drums for disposal. Pradhan poured into drums for disposal. The product from the tanks 4, 5 is sent to the packing, the column begin to prepare for the next launch, as described above.

The present invention can be used in chemical and perfume industry.

Claims

1. Installation for the body cube mounted on the latter and informed him of the Packed distillation column of periodic action, the top of which is connected to the reflux condenser, and the latter by leaving it connected to the top of the distillation column and to the tanks for collection of the product distillation, characterized in that the installation is further provided with at least two containers for selection of products reactive qualifications and separator installed at the outlet of the reflux condenser and connected to a distillation column and containers to collect water intermediate fraction and Pradhana through the separator distillation column is composed of three glass-bars of the same height, are tightly interconnected, and the diameter of the Packed distillation column is from 0.06 to 0.07 height of the distillation column at the height of the last from 2800 to 3200 mm, a cube made of enameled cast iron, and a reflux condenser and capacity to collect distillation products from the glass.

2. The method of purification by distillation of carbon tetrachloride, namely, that in the cube load carbon tetrachloride technical (Chu), heat it in the cube to the boiling point and guide couples in the distillation column and then in defle the th column in the form of phlegmy, which, contacting with pairs of Chu condenses its volatile ingredients components, Chu in the form of a liquid phase, enriched in volatile ingredients components sent back to the cube with the formation of the cube thus balance, and a pair of Chu enriched volatile nscontainerframe components, is sent to the reflux condenser, which is cooled and condensed, and then after stabilization of the operation of the distillation column portion of the condensate is sent in the form of phlegmy in the distillation column, and the other part of the condensate as a product of the distillation is in the tank for collection of the product distillation, characterized in that the support reflux number equal to 4, download Cho technical cube produced at room temperature, Chu, while in Cuba support equal to the atmospheric pressure, produce heat, Chu to a temperature 75-77°C and within 30-40 min all condensate from the dephlegmator sent back to the distillation column in the form of phlegmy and support the flow phlegmy from 180 to 200 DM3/h, and the condensate from the dephlegmator is served in the distillation column through a separator, through which are selected from the condensate water of the intermediate fraction and Pradhan, and then taken away after a dephlegmator part to what is pure for analysis”, “chemically pure”, and the selection of the specified condensation is carried out in the following quantities: water, the intermediate fraction from 2.0 to 2.5 vol.%, Pradhan from 2 to 6 vol.%, “pure” - from 28 to 30 vol.%, “pure for analysis” - from 25 to 28 vol.% and “chemically pure” - from 28 to 30 vol.%, everything from the number loaded into the cube Chu, then the process of distillation ceased, VAT residue disposed of, and the distillation of the products sent to the destination.

3. The method of purification by distillation of the chloroform, namely, that in the cube load chloroform technical, heat it in the cube to the boiling point and guide couples in the distillation column and then in the reflux condenser where they are condensed, from the reflux condensate through the separator serves in the upper part of the distillation columns in the form of phlegmy, which, in contact with vapors of chloroform, condenses its volatile ingredients components chloroform in the liquid phase, enriched in volatile ingredients components sent back to the cube with the formation of the cube thus balance, and a pair of chloroform, enriched volatile nscontainerframe components, is sent to the reflux condenser, in which they are cooled and condensed, and then after stabilization of the operation of the distillation column of coduct distillation - in containers for collection of the product distillation, characterized in that the reflux support number is 4, the loading of chloroform in technical cube is carried out at room temperature chloroform, and in a cube support equal to the atmospheric pressure, produce heating of chloroform to a temperature of 60-65°C and within 30-40 min all condensate from the dephlegmator sent back to the distillation column in the form of phlegmy and support the flow phlegmy from 110 to 130 DM3/h, and the condensate from the dephlegmator is served in the distillation column through a separator, through which are selected from the condensate water of the intermediate fraction and Pradhan, and then taken away after a dephlegmator part of the condensation products of reactive qualifications in a separate container in the following order: “clean”, “pure for analysis”, “chemically pure”, and the selection of the specified condensation is carried out in the following quantities: water, the intermediate fraction from 2.0 to 3.0 vol.%, Pradhan from 10 to 12 vol.%, “pure” is from 20 to 25 vol.%, “pure for analysis” from 28 to 30 vol.% and “chemically pure” from 12 to 15 vol.%, everything from the number loaded into the cube of chloroform, then the process of distillation ceased, VAT residue disposed of, and products perezagrujat trichloroethylene technical, heat it in the cube to the boiling point and guide couples in the distillation column and then in the reflux condenser, where they condense and reflux condenser condensate through the separator serves in the upper part of the distillation columns in the form of phlegmy, which is in contact with the vapors of trichloroethylene, condenses its volatile ingredients components trichloroethylene in the form of a liquid phase, enriched in volatile ingredients components sent back to the cube with the formation of the cube thus residue and vapors of trichloroethylene, enriched volatile nscontainerframe components is sent to the reflux condenser, which is cooled and condensed, and then after stabilization of the operation of the distillation column portion of the condensate is sent in the form of phlegmy in the distillation column, and the other part of the condensate as a product of the distillation is in the tank for collection of the product distillation, characterized in that the reflux support number is 4, the loading of trichloroethylene technical cube is carried out at room temperature trichloroethylene, and in a cube support equal to the atmospheric pressure, produce heating of trichloroethylene to a temperature 89-95°C and within 30-40 min all condensate from the dephlegmator send back the antibodies of the dephlegmator served in the distillation column through the separator, through which is taken from the condensate water of the intermediate fraction and Pradhan, and then taken away after a dephlegmator part of the condensation products of reactive qualifications in a separate container in the following order: “net”, “chemically pure”, “purity”, and the selection of the specified condensation is carried out in the following quantities: water, the intermediate fraction from 1.0 to 2.0 vol.%, Pradhan from 15 to 17 vol.%, “pure” - from 18 to 20 vol.%, “chemically pure” - from 28 to 30 vol.% and “purity” - from 10 to 12 vol.%, everything from the number loaded into the cube trichloroethylene, then the process of distillation ceased, VAT residue disposed of, and the distillation of the products sent to the destination.

5. The method of purification by distillation of the methylene chloride, which consists in the fact that in the cube load methylene chloride technical, heat it in the cube to the boiling point and guide couples in the distillation column and then in the reflux condenser, where they condense and reflux condenser condensate through the separator serves in the upper part of the distillation columns in the form of phlegmy, which, contacting with pairs of methylene chloride, condense its volatile ingredients components methylene chloride in the liquid phase, enriched Trudel what about methylene, enriched volatile nscontainerframe components, is sent to the reflux condenser, which is cooled and condensed, and then after stabilization of the operation of the distillation column portion of the condensate is sent in the form of phlegmy in the distillation column, and the other part of the condensate as a product of the distillation is in the tank for collection of the product distillation, characterized in that the reflux support number is 4, the loading of methylene chloride technical cube produced at room temperature, methylene chloride, and in a cube support equal to the atmospheric pressure, produce heat source solvent to a temperature of 40-44°C and within 30-40 min all condensate from the dephlegmator sent back to the distillation column in the form of phlegmy and support the flow phlegmy from 200 to 240 DM3/h, and the condensate from the dephlegmator is served in the distillation column through a separator, through which are selected from the condensate water of the intermediate fraction and Pradhan, and then taken away after a dephlegmator part of the condensation products of reactive qualifications in a separate container in the following order: “net” and “chemically pure”, and the selection of the specified condensate wire is 23,5% vol. and “chemically pure” - from 45 to 50 vol.%, everything from the number loaded into the cube methylene chloride, then the process of distillation ceased, VAT residue disposed of, and the distillation of the products sent to the destination.

6. The method of purification by distillation of perchloroethylene, namely, that in the cube load perchloroethylene technical, heat it in the cube to the boiling point and guide couples in the distillation column and then in the reflux condenser, where they condense and reflux condenser condensate through the separator serves in the upper part of the distillation columns in the form of phlegmy, which, contacting with pairs of perchloroethylene, condenses its volatile ingredients components, perchlorethylene in the form of a liquid phase, enriched in volatile ingredients components sent back to the cube with the formation of the cube thus balance, and a pair of perchloroethylene, enriched volatile nscontainerframe components, send in the reflux condenser, which is cooled and condensed, and then after stabilization of the operation of the distillation column portion of the condensate is sent in the form of phlegmy in the distillation column, and the other part of the condensate as a product of the distillation is in the tank for collection of the product distillation, characterized in that supports the e perchloroethylene, in Cuba support equal to the atmospheric pressure, produce heating of perchloroethylene to a temperature of 125 to 130°C and within 30-40 min all condensate from the dephlegmator sent back to the distillation column in the form of phlegmy and support the flow phlegmy from 120 to 150 DM3/h, and the condensate from the dephlegmator is served in the distillation column through a separator, through which are selected from the condensate water of the intermediate fraction and Pradhan, and then taken away after a dephlegmator part of the condensation products of reactive qualifications in a separate container in the following order: “net”, “chemically pure”, and the selection of the specified condensation is carried out in the following quantities: water, the intermediate fraction from 2.0 to 5.0 vol.%, Pradhan from 7 to 9 vol.%, “pure” is from 40 to 43% vol. and “chemically pure” - from 38 to 40 vol.%, everything from the number loaded into the cube of perchloroethylene, then the process of distillation ceased, VAT residue disposed of, and the distillation of the products sent to the destination.



 

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