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    • 专利摘要:
    1471561 Sampling a polyphasic mixture of compounds ENTREPRISE DE RECHERCHES ET D'ACTIVITES PETROLIERES ELF 17 Sept 1974 [21 Sept 1973] 40483/74 Heading G1B A method for continuously sampling a polyphasic mixture of compounds having a monotonic, as defined, relationship between boiling point and molecular weight for the analysis of gaseous compounds of said mixture which have a mass, i.e. molecular weight, below a selected value, comprises continuously sampling, within a sampling by-pass passage connected in parallel to a main flow passage for the mixture to be analyzed, a fraction of said mixture, passing the said fraction via traced, as defined, pipes through at least one dust remover, then through at least one heat exchanger in which a heat-transporting fluid circulates at an adjustable temperature T 1 condensing gaseous compounds having greater mass than said selected value in a housing placed within an enclosure at an adjustable temperature T 2 greater than T 1 and which housing is maintained under stable pressure and temperature conditions and passing to an analytical instrument the gaseous output from said housing. The analytical instrument may be a mass spectrometer. The sampling flow-rate may be adjusted downstream of said housing.
    公开号:SU831088A3
    申请号:SU742062432
    申请日:1974-09-20
    公开日:1981-05-15
    发明作者:Жаньи Жан；Франсуаз Ги；Тевене Даниэль
    申请人:Антреприз Де Решерш Э Д Активитепетрольер Елф (Фирма)；
    IPC主号:
    专利说明:

    (54) DEVICE FOR THE SELECTION OF GAS SAMPLES FROM A MULTIPHASE MIXTURE
    measuring the amounts of products detected relative to the total mass. A convenient way to limit the mass of gas products sent to the mass spectrometer is to control the temperature of the gas mixture sent to the mass spectrometer. The boiling point of the substance is directly dependent on the molecular weight of the substance indicated. By setting the temperature of the mixture and sending to the measuring instrument only gaseous products at this temperature, limit the area of the studied substances that are in the gaseous state at this temperature, when substances with large molecular weights correspond to condensed substances.
    The condensation products obtained by continuous selection of the gas mixture is collected in a vessel called an evaporation vessel, the temperature and pressure in which can be controlled. For the reliability of the analysis, it is important to accurately determine the temperature and pressure conditions in this vessel, as well as to ensure its continuity. Strict quantitative analysis of gaseous products in multiphase samples, in particular steam cracking, is impossible when using conventional evaporation columns, which are not stable enough for the analysis to reflect the composition of the gaseous phases. The selection circuit runs parallel to the main circulation circuit of the mixture, the fraction of which is selected under pressure conditions such that the criteria (numbers) of the Reynolds in the main circuit and in the selection circuit would be OK. The analyzed mixture is sent to the heating pipes, then at least through one dust collector and one heat exchanger, where the heat transfer fluid circulates at a controlled temperature T. the condensed and gaseous fractions of the mixture are then collected in an evaporation vessel placed in a chamber with controlled temperature. The components of the mixture are sent to the analyzer, the molecular weight of which is such that they are in a gaseous state at temperature T. The nozzles are heated throughout their length due to the circulation of superheated steam in a cylindrical pipe coaxial with Pervol (which prevents the formation of kryyLensatov, as well as the danger of blocking these plugs at certain points in the channel (at the lowest point, in narrow places, etc.). The heat exchanger is designed to lower the temperature of the mixture circulating in the nozzles to cause the formation of condensation of heavy components, for example, after an evaporation vessel in a heated line opening to the analyzer Usually, the temperature of the heat exchanger Tj. T is maintained in the evaporating vessel, so that the temperature along the pipes through which the mixture circulates from the heat exchanger ensures that the steam sent to the analyzer, after leaving the evaporator There was no condensate in the vessel. When analyzing vapor cracking, the dust collector is mainly designed to remove most of the carbonaceous
    particles. The gaseous mixture from the outlet of the evaporation vessel is sent to the mass spectrometer, the temperature T and Tj of the first heat exchanger and the evaporation vessel are automatically controlled, based on the difference in the molecular weight of the components, analyzed in a mass spectrometer, and the outputs of the gaseous components 5 after the evaporation vessel are controlled to get the allowable travel time on the line. Temperature regulation T and T2. allows for the creation of rigorous and stable working conditions for the evaporation vessel and is carried out automatically. On the other hand, a valve restricting the flow of gas to the analyzer and provided after the evaporating vessel is at the end of the extraction device, so that the pressure is controlled as precisely as possible inside the evaporation vessel.
    The drawing schematically shows the proposed device.
    The device contains a bleed loop that runs parallel to the main circulation loop of the analyzed mixture and is equipped with two valves at the inlet and the exit of this bleed loop, and a vacuum device after the triple valve, the latter connecting at the open position 0 of Selection with heated pipe; dust collector; temperature-controlled heat exchanger T; evaporative vessel placed in a temperature-controlled chamber heated sockets making the connection: triple valve — dust collector — heat exchanger — evaporative vessel — analyzer, valve after the evaporative vessel, regulating the pressure in the latter; automatic
    means for adjusting the temperatures T- (and T, and the pressure in the inspection vessel, namely, at the indicated points; means for ensuring the circulation of the coolant in
    heat exchanger; heating means for adjusting the temperature in the chamber enclosing the evaporation vessel; means for controlling the level of liquid obtained from condensation products in the evaporation vessel and for removing liquid condensation products and solid particles from the evaporation vessel.
    The device has a valve, called a grinder, capable of breaking a coke crust (deposited grandchild) during actuation due to the deposition of particles of solid carbon. This triple valve continuously passes gaseous products into the secondary circuit, and the opening of the valve triggers the third channel, i.e. allows to take part of the feed substance to the dust collector and to the selection device. In the latter, there is a steam jet ejector arranged so as to facilitate the circulation of the streams in the pipe, creating an artificially rarefied before the point of injection of steam into the circuit. The steam jet ejector is designed so that Reynol-sa criteria are the same in both pipes. The dust collector is formed by a metal sieve with a fine mesh. When analyzing vapor cracking, the function of the dust collector is to remove carbon particles as it passes through the metal sieve.
    The chamber in which the evaporating vessel is placed contains a tank filled with the liquid surrounding the evaporating vessel; insulated resistors, immersed in the specified, liquid and through which an electric current of a regulated value flows; mixing means that allow the temperature of the liquid in the tank to be uniform and the means for measuring the temperature of this liquid The liquid enclosed in the tank is silicone oil, and as the mixing means, the agitators are immersed in it. Silicone oil is more commonly used than water, since its boiling point is higher, which allows temperature adjustment for higher values and without excessive evaporation. The evaporating vessel contains a container, the bottom of which is inclined relative to the horizontal, and the lowest part of the bottom of the evaporating vessel is connected to the outlet pipe of a periodic drain, equipped with a valve; a vertical nozzle passing into the evaporation vessel through the bottom of the latter, open at the upper end and equipped with a pneumatic valve with automatic control, provided in the part of the nozzle for rejecting the chamber; a device for measuring the pressure drop between two points in the evaporation vessel lying on the vertical; a vertical wall dividing the internal volume of the evaporation vessel into two parts communicating at the base and a metal filter near the top of the evaporation vessel in front of the branch pipe for the gas phase.
    The control of the valve connected to the outlet may be
    0 manual, since this release is rarely used. Measuring the differential pressure allows the water level to be controlled by affecting the automatic selection valve. The current enters the evaporation vessel in the part where there is a level detector for condensation of light hydrocarbons here.
    The selection of the fraction of the mixture for quantitative analysis is carried out continuously, limiting the number of gaseous components to those whose molecular weight is less than a given molecular weight. This upper limit of the molecular weight of the gaseous gases of the various components is fixed by the stability of the temperature in front of the evaporating vessel, and the products with high molecular weight are condensed. are in an evaporation vessel.
    0
    In the main pipeline, a two-phase mixture circulates, the analysis of which is produced. In parallel with pipeline 1, a mixture extraction circuit 2 is provided with an inlet valve 3 and an exhaust valve 4, an ejector 5 connected to a steam pipeline where the pressure is higher than the pressure in circuit 2, and a valve 6, called a grinder, with a manual control connected to the filter 7 by a heated pipe 8, while the filter 7 is connected to the inlet of the heat exchanger 9 by a heated pipe 10. The heat exchanger 9 has a pipe 11 through which the refrigerant circulates temperature controlled. The output of the heat exchanger is connected by a heated pipe 12 to a coil, which first passes outside the evaporating vessel and then 0; inside the latter. The evaporating vessel 13 is enclosed in the chamber 14, of which there is a silicone bath with new oil. The internal volume of the evaporating vessel is divided into two
    5 parts by a metal wall 15, the flow through the nozzle 12 is performed in the left part of the evaporating vessel, where a level 16 detector is provided. Evaporating vessel
    0 is equipped with a metal filter 17. Resistors 18 and 19, fed through temperature controller 20, maintain a constant temperature in a bath of silicone oil, which is measured using a thermostat 21. Stirring the bath with silicone oil is performed by a stirrer 22. Pipe 23, equipped with a valve 24, serves to discharge very heavy condensates and solid particles periodically formed. precipitated at the bottom of the evaporating vessel. Liquid components (hydrocarbons and water) and solid particles 25 flow along an inclined wall 26 forming the bottom of the evaporation vessel 13 relative to the pipe 23. The C-shaped pipe 16 has two branches that enter the evaporation vessel, it encloses the device 27 for measuring the differential pressure. between two points; on the basis of this measurement, control is performed by means of a regulator by opening the pneumatic valve. at 28, - the control of the level of liquid in the evaporation vessel provided at the port 29. The gases in the evaporating vessel are led out to the measuring instrument via the heated nozzle 30, in which there is an inlet valve 31, the opening of which is controlled by the regulator 32 (automatic) pressure while the pressure is measured by the sensor 33.
    Under operating conditions, the liquid level in the evaporation vessel is fixed at a fixed point lying between both points and reference points of the differential pressure sensor. The water level is maintained at the upper end of the pipe. The internal surface of the evaporating vessel is made of stainless steel, because it contacts directly with hydrocarbons. The volume between the two walls (the evaporation vessel and the enclosing chamber) is filled with silicone oil, into which several heating resistors 18 and 19 are immersed, which allow the temperature of the oil in the bath to be regulated using a known regulator (not shown in the drawing) associated with bath temperature sensor 21 (graduated thermocouple or thermometer).
    In the analysis, vapor phase cracking effluents from the heat exchanger at a temperature close to 75 ° C. The fluid passing through the exchanger is water at. Temperature with silicone oil 95 ° C. Thus, the temperature increases
    in an evaporation vessel, but this is not enough to re-evaporate water. The bath temperature is maintained so as to select the end point of the gas phase, i.e. molecular weight limit for the components to be analyzed in the meter. This point is determined depending on subsequent loads, i.e. substances whose concentration is desired to be measured in a mass spectrometer. The gas phase is directed to the mass spectrometer via a nozzle 30 heated by water vapor at a pressure of 8 bar (175 ° C). Thus, with
    At this temperature there are no condensates that would enter the mass spectrometer, which is detrimental to its action. Taking into account the conditions of temperature, pressure and supply, set exactly in the evaporating vessel, it is possible to experimentally determine the transfer matrix, which, when multiplied by the vector composition of the vapor phase, whose components were measured by analysis, determine the composition before the evaporator.
    权利要求:
    Claims (2)
    [1]
    1.Tkhorzhevsky V.P. Automatic analysis of the chemical composition of gases. M., 1969, p. 195.
    [2]
    2. In the same place 197 (prototype).
    V-.
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    同族专利:
    公开号 | 公开日
    BE819700A|1974-12-31|
    FR2245245A5|1975-04-18|
    JPS5060290A|1975-05-24|
    DE2444201A1|1975-04-10|
    NL7412014A|1975-03-25|
    IT1030059B|1979-03-30|
    DE2444201B2|1978-07-27|
    GB1471561A|1977-04-27|
    US3944824A|1976-03-16|
    CA1021175A|1977-11-22|
    DE2444201C3|1979-04-05|
    引用文献:
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    US2412359A|1943-12-01|1946-12-10|Stanolind Oil & Gas Co|Ionic analysis|
    BE582035A|1958-08-30|GB1501903A|1975-04-18|1978-02-22|British Petroleum Co|Sampling device|
    DE2950658A1|1979-12-15|1981-06-19|Krupp Polysius Ag, 4720 Beckum|Gas sample extraction appts. - using injector for recycling and pump for branch sample to analyser|
    US5621161A|1995-04-11|1997-04-15|Leyse; Robert H.|Method for monitoring for the presence of dissolved gas in a fluid under pressure|
    DE19857776C1|1998-12-04|2000-07-06|Schering Ag|Arrangement for extracting specimens from product line carrying liquid has specimen extraction block with removable container immediately after valve in flow direction in branch line|
    US7629177B2|2004-01-21|2009-12-08|Siemens Industry, Inc.|Method and apparatus for introduction of high boiling point streams at low temperature|
    RU2372981C2|2004-10-12|2009-11-20|Акцо Нобель Коатингс Интернэшнл Бв|Method and system for monitoring in online mode|
    US20060078843A1|2004-10-12|2006-04-13|Akzo Nobel Coatings International B.V.|System|
    CN102636368B|2012-04-18|2014-09-24|华东理工大学|Multiphase online sampling device and multiphase online sampling method suitable for high-temperature hydrocarbon gas |
    CN104849106A|2015-04-03|2015-08-19|中国石油天然气股份有限公司|Industrial catalytic cracking stripping section oil gas online sampling and detecting method, and apparatus thereof|
    JP6476340B1|2018-09-28|2019-02-27|東芝プラントシステム株式会社|By-product gas measurement system|
    CN113184936A|2021-03-25|2021-07-30|宣化钢铁集团有限责任公司|Efficient and energy-saving ammonia distillation deacidification system and method for recycling ammonia nitrogen|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    FR7333933A|FR2245245A5|1973-09-21|1973-09-21|
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