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Method of producing multicomponent solution of krypton-xenon mixture and special purity solvent and apparatus for realising said method. RU patent 2520216.

Method of producing multicomponent solution of krypton-xenon mixture and special purity solvent and apparatus for realising said method. RU patent 2520216.
IPC classes for russian patent Method of producing multicomponent solution of krypton-xenon mixture and special purity solvent and apparatus for realising said method. RU patent 2520216. (RU 2520216):

F25J3/02 - by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream (F25J0003080000 takes precedence);;
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The invention is pertaining to the field of the cryogenic engineering, in particular, to the control of the rectifying plants operation on rectification and separation of the krypton-xenon concentrate produced by the air-fractionating apparatus. The method of control of the rectification plant operation for reprocessing the compressed mixtures includes the control over consumptions of the source mixture in the plant and feeding of the rectifying columns, the pressures and amounts of the top and bottom products gated out of the columns. The rectifying columns are equipped with the sampling devices arranged in their concentration section and the condensers-evaporators with the intermediate coolant in the closed cavity. The mixture at the inlet of the plant is stabilized by the temperature and pressure. Consumption of the mixture by the plant is controlled by the throttle valve, ensuring the pressure drop on the throttle valve for the critical efflux of the mixture. In addition conduct the analysis from the still bottom evaporation area. At that for each column they determine the key components and their share in the preliminary analysis and the analysis from the still bottom evaporation area. The concentrations of the key components are regulated by variation in the contact device of the vapor and the condensate streams. The separation of the top product is conducted in the gaseous form with the constant consumption, the still bottom product is taken out permanently or periodically in the vapor and (or) fluidic form depending on the results of the share of the key component in the mixture from the still evaporation area with the subsequent gasification before the control valve. The useful volume of the still is magnified concerning the hourly productivity of the appropriate column for the bottom product no less than two times, and the pressure in the contact device of the columns is set by variation of the pressure and (or) amount of the intermediate coolant and the heat power of the still boiler of a beck. Usage of the invention ensures the power saving control over the rectifying plant at production of the especially pure target components.

FIELD: chemistry.

SUBSTANCE: method of producing a multicomponent solution of a krypton-xenon mixture and a special purity solvent involves feeding a multicomponent solution into a precursor solution line, preliminary physical-chemical purification from explosive and hardening impurities, cooling and fractional separation in columns. Said columns are equipped with samplers in the concentration part or blow line and the vapour zone of the bottom. A krypton-xenon mixture containing volatile impurities and a stream of a solvent containing volatile impurities are obtained in the column for obtaining a krypton-xenon mixture. The method also includes purifying the stream of the solvent fraction in a column for obtaining special purity solvent from volatile impurities to obtain a special purity solvent. All impurities that are volatile relative to krypton are removed with the stream of the solvent fraction, wherein the part of said impurities which is semi-volatile relative to the solvent is removed in a column for purification from intermediate impurities. An apparatus for carrying out said method is described.

EFFECT: invention reduces content of impurities in a krypton-xenon mixture, simplifies and reduces the cost of processing said mixture.

3 cl, 1 dwg

 

The claimed invention relates to cryogenic engineering, in particular to the technology of low-temperature rectification mixtures, and can be used in chemical, petrochemical and metallurgical industries.

A method of obtaining from the solution of kryptonxenon concentrate and cleaning solvent (see RF patent №2430015 C1, IPC SB 23/00). The method provides for gasification of the liquid solution containing krypton and xenon, purification and distillation split with the formation of the flow of production of kryptonxenon concentrate and flow of solvent.

The disadvantage of this method is the low quality of kryptonxenon concentrate because of the content of volatile against the krypton impurities, which complicates and increases the cost of further processing.

A method of obtaining kryptonxenon mixture and purity oxygen (see RF patent №2406047 C1, IPC F25J 3/02, SW 23/00, SW/16, B01D 53/00). The method provides for rectifying the division of purified gas flow primary kryptonxenon concentrate with getting kryptonxenon mixture and thread dump of oxygen, which is then purified by distillation with getting purity oxygen.

The disadvantage of this method is the low quality of kryptonxenon mixture of volatile against the krypton impurities, which adds cost and complexity of its further processing.

The aim of the invention is increasing the quality of kryptonxenon mix and increase profitability.

This goal is achieved by the fact that in the way of reception of the multi-component of the solution kryptonxenon and solvent mixtures of high purity, including distillation division, the distinguishing feature is that when rectification of each column receive one component (or group of components) with adjustable purity, a change which, depending on the more measurements of the composition of the steam flows in Cuba and the concentration of the column.

A device for obtaining kryptonxenon mixture and purity oxygen (see RF patent №2406047 C1, IPC F25J 3/02, SW 23/00, SW/16, 01D 53/00). The device contains a consumption booster, site physico-chemical treatment of primary concentrate from explosive and stiffening of impurities and the rectification unit, consisting of two columns, one of which receive kryptonxenon mixture, and the other with pure oxygen.

The disadvantage of this device is a low quality of kryptonxenon mixture of volatile against the krypton impurities, which adds cost and complexity of its further processing.

The aim of the invention is increasing the quality of kryptonxenon mix and increase profitability.

This goal is achieved by the fact that the device is retrieved from multicomponent solution of kryptonxenon and solvent mixtures of high purity, containing block rectification, the distinguishing feature is that the block of rectification additionally contains the column selection of intermediate particles (impurities, volatile against the krypton and non-volatile against the solvent), and distillation columns unit equipped with a sampler composition of the medium in Cuba and concentration parts.

The stated method of obtaining of multicomponent solution of kryptonxenon mixture and especially pure solvent can be implemented in the claimed device is schematically shown on the drawing.

The device includes a line 1 primary solution, node 2 physico-chemical treatment and block 3 rectification. Site physico-chemical treatment contains a recuperative heat exchanger 4, the electrical heater 5, 6 reactor, water cooler 7 and alternately operating adsorbers 8. Unit 3 distillation distillation column contains 9 receiving kryptonxenon mixture, distillation column 10 highlight interim impurities, distillation column 11 of receipt of solvent purity, multithreaded exchanger 12, cooler 13, low-temperature heat exchanger 14, filter, 15, and 16 coolant supply and line 17 feeder dry compressed gas.

Each distillation column in the head has condenser-evaporator 18-9 to 18-11, and below - cube 19-9 to 19-11, equipped with a kettle 20-94 to 20-11, the sampler A1-9 to A1-11 out of steam cavity and line 21-9 to 21-11 output bottom of a liquid. Cube 19-9 columns obtain kryptonxenon mixture additionally contains a coil 22. Oral boil all capacitors-evaporators are connected with lines 16-9 to 16-11 line 16 of supplying coolant lines 23-9 to 23-11 line 23 liquefied gas and lines 24-9 to 24-11 line 24 out of vapor. The middle part of the contact space distillation columns 9 receiving kryptonxenon mixture contains a socket, connected by a line 25 of purified solution through a low-temperature heat exchanger 14 and filter 15 with node 2 physico-chemical treatment, and the head of the column - a branch pipe, coupled line 26 with a pipe in the middle part of the contact space columns 10 highlight interim impurities. The pipe at the head of the column 10 highlight interim impurities in turn is connected by a line 27 with a pipe in the middle part of the contact space columns 11 getting solvent purity. Socket head of the column 11 of receipt of solvent purity is connected by a line 28 through the cooler 13 and multithreaded exchanger 12 exits. Columns 9 receiving kryptonxenon mixture and 10 highlight interim impurities at the top (concentration) of a part of the contact space equipped with respectively samplers A2-9 and A2-10 for predictive analysis.

The way of reception of the multi-component of the solution kryptonxenon mixture and solvent high purity on the primary example of kryptonxenon concentrate obtained for air separation plants, and use as a refrigerant liquid nitrogen, and as dry compressed gas - air is as follows.

Gaseous solution of krypton Kr and xenon Xe oxygen O 2 (solvent) with nitrogen N 2 , argon Ar, neon Ne, helium Not, hydrogen H-2 , Oscoda WITH carbon, carbon dioxide, CO2 , hydrocarbons n C H m (mainly methane CH 4 and ethane With 2 N 6 ), ozone, O 3 , water, H 2 O, TETRAFLUOROMETHANE CF 4 , freon-C 2 F 6 , monitorability (freon 11) CFCl 3 , difenilamina (freon 12) CF2Cl 2, etc. served under pressure (0,16-0,3)MPa in line 1 primary solution and later in the node 2 physico-chemical treatment. In the node physico-chemical treatment the primary flow of kryptonxenon concentrate regenerative heat exchanger 4 and electrical heater 5, carry out catalytic oxidation of hydrocarbons in the reactor 6, cooling regenerative heat exchanger 4 and water fridge 7 and absorption of water and carbon dioxide in the adsorbers 8. From node 2 physico - chemical treatment the primary flow of kryptonxenon concentrate with traces of impurities methane, water, carbon dioxide, already not dangerous from the point of view of their setting in the columns at operating temperatures, served in line 25 cleaned of mud and then through the filter 15, low-temperature heat exchanger 14 and the coil 22 in the distillation column 9 receiving kryptonxenon mixture, phlegm which is the condensate oxygen (solvent). In the process of rectification columns in the cube is going krypton, xenon and less volatile against the krypton impurities, having at the same pressure higher boiling point (2 , O 3 , H 2 O, CF4, C 2 F 6 , CFCl 3 , CF 2 Cl 2 and others). This liquid in the form of the production kryptonxenon mixture on line 21-9 is removed from the unit for further processing.

The process of rectification in the column are the readings of measuring flow, level, pressure, temperature, hydraulic resistance (not shown)and is measured from the sampler A1-9 and maintain the minimum level (0 to 10 ppm), the methane concentration in the vapour space of the cube as substances with the closest, but low boiling points, compared with a boiling point of krypton. From the sampler A2-9 in the gas samples define and support in the steam flow concentration of column is the content of krypton, which eliminates the release of krypton in the head of the column. In my head the same columns concentrated stream of oxygen, which contains all the flying towards krypton impurities (CH 4 , N 2 , Ar, Ne, No, N 2 , and others). Its output and line 26 sent to the middle part of the distillation column 10 highlight interim impurities. In the scheme of the device there are also line 29, which will bring the flow of oxygen from the zone of possible increase of concentration of methane in the concentration of columns 9 or in the event of a failure mode of its work to prevent the ingress of krypton in the condenser-evaporator 18-9.

Flavoursome refrigerants in the device are liquid nitrogen and liquid air. Liquid nitrogen is served in the rectification unit 3 on line 16 coolant supply from an external source and forth along the lines 16-9 to 16-11 in the cavity evaporating condensers-evaporators 18-9 to 18-11. Liquid air to get the device in result of cooling and condensation to the flow of dry compressed air reverse cold streams of the evaporated refrigerant, otdelochnykh gases from the head of the column 11 of receipt of solvent purity, a production flow of solvent purity and removal of heat from the air in the boilers 20-9 to 20-11 Cuba columns. For this purpose, the flow of dry compressed air under pressure, for example, 0,57 - 0,93 MPa served in line 17 feeder dry compressed gas. A small part of the air supplied to the line 17-9 to regulate steam flow in a distillation column 9 receiving kryptonxenon mixture is cooled in the boiler 20-9 and then mixed at the entrance to the low-temperature heat exchanger 12 reverse cold-flow evaporated refrigerant. A greater part of the air is cooled in the low-temperature heat exchanger 12, along the lines 17-10 and 17-11 send respectively in boilers 20-10 and 20-11 where condense, the resulting condensate preobladayut in the cooler 13, direct in-line 23 liquefied gas and along the lines 23-9 to 23-11 drossellied respectively in the cavity evaporating condensers - evaporators 18-9 to 18-11.

Due to the fact that in the way of reception of the multi-component of the solution kryptonxenon and solvent mixtures of high purity, including distillation division, the distinguishing feature is that when rectification of each column receive one component (or group of components) with controllable cleanliness, the change of which carry depending on additional measurements of the composition of the steam flows in Cuba and concentration of columns, which improve the quality of kryptonxenon mix and profitability.

Due to the fact that the device is retrieved from multicomponent solution of kryptonxenon and solvent mixtures of high purity, including the rectification unit, the distinguishing feature is that the block of rectification additionally contains a distillation column highlight interim impurities, and distillation columns unit equipped with a sampler composition of the medium in Cuba and concentration parts, which increases the quality of kryptonxenon mix and profitability.

1. The way of reception of the multi-component of the solution kryptonxenon and solvent mixtures of high purity that includes the flow of multicomponent solution in line primary solution, pre-physical-chemical purification from hazardous and stiffening of impurities, cooling and rectifying the division into columns, equipped with samplers in the concentration of part or line Stripping and steam zone of Cuba, with the formation in the column obtain kryptonxenon the mixture kryptonxenon mixtures containing volatile impurities, and flow fraction of solvent containing volatile additives, cleaning flow fraction of solvent in a convoy of receipt of solvent purity from volatile impurities to produce solvent purity, the distinguishing feature is that the flow fraction of solvent take all volatile against the krypton impurities, volatile ingredients in relation to solvent part of which is removed into the column purification from intermediate impurities.

2. Way under item 1, characterized in that in a convoy of receiving kryptonxenon mixture in the analysis of the sampler steam space Cuba, monitor and support the minimum content of methane, and in the analysis of the sampler concentration of part - minimum content of krypton, in column purification from intermediate impurities in the analysis of the sampler steam space cube manage and keep safe methane, and in the analysis of the sampler concentration of part - the minimum content of the components of the mixture, relative to which the solvent is the least important factor in the relative volatility, in column obtain solvent-high purity in the analysis of the sampler steam space Cuba, monitor and support the minimum content of the components of the mixture with the lowest value of the coefficient of relative volatility against the solvent, and in the analysis of the sampler line Stripping - permissible content of the solvent.

3. The device receiving of multicomponent solution of kryptonxenon and solvent mixtures of high purity, line containing the primary solution, connected with the entrance to the site physico-chemical treatment, the line of purified solution with filter, low-temperature heat exchanger and coil boilers connected to the inlet nozzle in the distillation column obtain kryptonxenon mixtures containing line output kryptonxenon mixture of Cuba and the line fraction of solvent from the head of the column, which is connected with inlet nozzle power supply columns receive special solvent purity containing the output line of solvent purity of Cuba and the line of the blow-off, the distinguishing feature is that the line fraction of solvent supplied column purification from intermediate impurities with line output intermediate impurities from Cuba and the line of the pure solvent, which is connected with inlet nozzle power supply columns get solvent purity.

 

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