WO2017052399A1 - Réacteur haute pression à action périodique à géométrie de taylor-couette - Google Patents

Réacteur haute pression à action périodique à géométrie de taylor-couette Download PDF

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Publication number
WO2017052399A1
WO2017052399A1 PCT/RU2015/000593 RU2015000593W WO2017052399A1 WO 2017052399 A1 WO2017052399 A1 WO 2017052399A1 RU 2015000593 W RU2015000593 W RU 2015000593W WO 2017052399 A1 WO2017052399 A1 WO 2017052399A1
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WO
WIPO (PCT)
Prior art keywords
reactor
reactor according
taylor
liquid
flange
Prior art date
Application number
PCT/RU2015/000593
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English (en)
Russian (ru)
Inventor
Маркос МИЛЛАН-АГОРИО
Джонатан БЭЛЛ
Original Assignee
Общество с ограниченной ответственностью "Уникат"
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Publication date
Application filed by Общество с ограниченной ответственностью "Уникат" filed Critical Общество с ограниченной ответственностью "Уникат"
Priority to PCT/RU2015/000593 priority Critical patent/WO2017052399A1/fr
Publication of WO2017052399A1 publication Critical patent/WO2017052399A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/26—Oils; Viscous liquids; Paints; Inks

Definitions

  • the invention relates to the field of deposits formed from fossil oil and other liquids on heated surfaces, inside a Taylor-Couette device that can operate in a fully turbulent fluid flow.
  • the invention relates to devices and methods for producing solid deposits from various organic liquids for studying the phenomenon of thermally initiated sedimentation process.
  • paraffin waxes and inorganic salts contained in fossil oil can also be deposited on preheater heat exchangers in the early stages of processing. Paraffin waxes are called normal alkanes with more than 20 carbon atoms.
  • Part of this fraction contains derivatives of porphyrin molecules resulting from the decomposition of organic life forms. It is assumed that they can act as centers of destabilization of fossil oil at elevated temperatures.
  • an important parameter in the formation of precipitation is the type of liquid, its composition and flow rate.
  • the use of reactors with a small working volume allows precise control of the composition of the liquid and, as a result, makes it possible to study the effect of the composition on the deposition process.
  • the present invention includes a single-phase batch phase Taylor-Couette fluid reactor in which the outer cylinder is fixed and the inner cylinder can rotate, a sample of the test fluid fills the volume between these cylinders.
  • a Taylor-Couette cell consists of an inner cylinder of radius Ri and an outer cylinder of radius R2 and length 1.
  • the liquid fills an annular cavity, the volume of which is defined as; t / (R2-Ri) 2 .
  • the inner cylinder rotates at a frequency ⁇ , causing fluid movement.
  • a fluid sample consists of an organic fluid placed in an annular cavity using a pump or compressed gas.
  • the source gas in the cell exits through the outlet until it is completely removed from the system.
  • the length and ratio of Ri and R 2 can be varied by replacing the outer cylinder and / or the inner rotating cylinder. A greater shear stress and a smaller reactor volume are achieved with a narrow gap between the cylinders, then with a wider gap the rector will operate in a flow mode, which is more similar to a pipe in the casing and a tubular heat exchanger.
  • the Taylor-Couette cell is heated externally using a cylindrical furnace.
  • the linear flow velocity of fossil oil in industrial heat exchangers is usually in the range of 1 - 3 m / s, and the flow is turbulent in all heat exchangers, with the exception of the earliest on the production line (when the feed has a low temperature); in this regard, the reactor was designed to operate in turbulent mode.
  • An important requirement for its design is the ability to achieve a rotation speed of the inner cylinder greater than 1 m / s, which is identical to the speed of the fluid in the pipe.
  • the number of revolutions per minute (rpm) for a known circumferential speed is calculated as follows:
  • the main dynamic variable is the rotation speed of the inner cylinder: the rotation speed ( ⁇ ) can be calculated as follows: ⁇ - rpm V
  • V circumferential rotation speed (m / s)
  • the tangential Reynolds number (Re t ) on the surface of the inner cylinder is defined as:
  • FIG. 13 A preferred design is shown in FIG. 13.
  • the Taylor-Couette geometry batch high pressure reactor in the form of a module (Fig. 2) consists of an upper flange 1 made of stainless steel, a cylindrical body 2 made of various possible materials, and a lower flange 3 consisting from stainless steel.
  • the inner cylinder 4 consists of stainless steel and is a rotor coaxially connected to the stainless rod 5 with an external cylinder, and also provided with a countersunk bolt 6.
  • the volume of the annular space for a liquid is determined by the dimensions of the inner cylinder, the outer cylinder, as well as the upper and lower flanges.
  • the upper and lower flanges are attached to the outer wall using six steel bolts 7 and are sealed with a gasket 8.
  • a commercial DC motor and a magnetically coupled drive are connected coaxially with the upper flange of the reactor in position 9 and are connected by a cylindrical rotor 4 controlled by an alternating current source.
  • the upper flange 1 is connected to the inlet 10 and the outlet 12 crimp fittings using threaded connections 11 and 13, respectively.
  • the fittings are screwed into the upper head through the threaded port 17 and connected to a K-type thermocouple to measure the temperature of the liquid, then the hole 18 drilled in the joints of the upper part allows the insertion of another K-type thermocouples to wall 2 to measure its temperature.
  • the support frame 19 also mounts the Taylor-Couette cell to the lifting mechanism on the threaded holes 20.
  • the flange base 3 described above has a threaded port 14 for discharging liquid through a stainless pressure relief valve 15 and bolts for connecting to the flange.
  • the above-described wall 2 may consist of carbon-containing steel, stainless steel, titanium, copper or brass, and also contains an opening for a K-type thermocouple and bolts for connecting to the flange.
  • the Taylor-Couette reactor described above is heated by a vertical cylindrical furnace with an insulating ceramic pipe 23 coated with ceramic wool to prevent heat loss.
  • the temperature of the surface of the wall of the reactor (T w ) is kept constant, and the temperature of the liquid inside the reactor (Th) is not more than 4 ° C lower than the temperature of the wall (T w - Th ⁇ 4 ° C)
  • the above Taylor-Couette reactor can be increased, reduced, removed from the furnace by means of a lifting mechanism, can also be fixed using the support frame 16.
  • the inlet to cell 10 is associated with cleaning / loading the system of FIG. 4 inlet with a flexible stainless steel hose.
  • the pressure above the liquid is measured using a sensor in the outlet port 12, the system is protected against overpressure by the graduated pressure relief valve RV.B during the operation, the needle valve V6 connected to the liquid supply reactor remains open.
  • Excessive fluid is present in the inlet-outlet lines and in the Vesl supply vessel. Thermal expansion of the liquid during heating allows the excess volume to return back to the vessel. For safety reasons, the pre-calculated minimum gas volume is always present in the supply vessel before heating so that when heated, the liquid fills the entire space during expansion.
  • the Ves2 liquid product container is connected to the liquid port of the product via the flange base 3 of the reactor through a detachable tube when the reactor is raised at the end of the experiment.
  • the purge / load process allows the user to degass the system using an inert gas supply under pressure, repeatedly increasing / decreasing the pressure in the system. If necessary, the system can be pre-dried by passing an inert gas through it for a long period of time.
  • a sample of liquid is introduced into the cylinder and gently injected into the reactor by means of a pressure gradient created by the inert gas inlet system during slow rotation of the inner cylinder.
  • a qualified operator can fill the reactor without bubbles, a single-phase system can be achieved by removing gas from the outlet, until the entire line is filled with liquid. Increasing the pressure in the system to full working will further lead to the destruction of the remaining bubbles that could be trapped.
  • the sedimentation research reactor can be moved higher or lower into or out of the furnace electrically (FIG. 4) without the need for connecting / disconnecting or fitting pipe connections. This provides added safety since the reactor can be remotely removed from the furnace in the event of a leak or other technical problems.
  • the flexible hose maintains pressure above the liquid and therefore prevents the evaporation of high boiling liquids.
  • the reactor operates at a wall body temperature between 150 and 350 ° C.
  • the pressure on the liquid in the preferred embodiment of the reactor is in the range of 20-50 bar.
  • the fluid turbulence in the above embodiment corresponds to the tangential Reynolds number on the surface of the rotor in the range from 8,000 to 200,000.
  • the wall may also contain a removable inner sleeve, consisting of various materials for inspection and analysis after sedimentation experiments.
  • a removable inner sleeve consisting of various materials for inspection and analysis after sedimentation experiments.
  • Such a wall allows the user to analyze the surface topology of oil deposition and other spatially resolved methods such as EDX, IR Fourier imaging, and cross-polarized optical microscopy.
  • the reactor can be easily dismantled for cleaning and collecting deposits, the wall of the reactor can be easily replaced with other material.
  • the fluid dynamics in a single-phase Taylor-Couette cell is well understood and can be easily predicted. This is confirmed by high-speed visualization of fluid dynamics and computer simulations.
  • the reactor operates in a highly turbulent mode.
  • This invention is in a stable state with a small temperature difference between the liquid and the wall of the reactor, which avoids boiling.
  • the reactor contains a small volume of liquid, which makes it possible to use synthetic and semi-synthetic mixtures together with fossil oil and products of its processing with strong heating of the walls of the reactor, which allows increasing the growth rate of deposits to the rate of their growth on industrial equipment.
  • the use of a cylindrical furnace and ceramic pipes isolated from convective heat loss ensures uniform heat distribution within the reactor.
  • the reactor configuration can be easily modified, and in the CSTR configuration, it can be operated continuously.
  • FIG. 1 The lateral cross section of a cylindrical Taylor reactor -
  • FIG. 2 Cross-section from top to bottom of the upper wall of the flange
  • FIG. 3 Cross-section from top to bottom of decomposition-deposition equipment together with the furnace
  • FIG. 4 The decomposition-deposition reactor with a furnace and connected lines for cleaning, loading and collecting products. Valve numbers V #, T # tees, A # adapters, V # tanks, P # pressure transmitters, RV # safety valves
  • FIG. 5 General scheme of the Taylor-Couette cell

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Food Science & Technology (AREA)
  • Medicinal Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

L'invention concerne des équipements et des méthodes de transformation de pétroles fossiles, d'autres produits pétroliers, de mélanges synthétiques ou semi-synthétiques et de milieux organiques visant à obtenir des dépôts solides sur les surfaces chauffées typiques dans le cas des échangeurs de chaleur utilisés dans des équipements de transformation de pétrole. L'invention décrit également une méthode pour obtenir le liquide indiqué ici ainsi que la substance de sédimentation pour une analyse physico-chimique ultérieure.
PCT/RU2015/000593 2015-09-21 2015-09-21 Réacteur haute pression à action périodique à géométrie de taylor-couette WO2017052399A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/RU2015/000593 WO2017052399A1 (fr) 2015-09-21 2015-09-21 Réacteur haute pression à action périodique à géométrie de taylor-couette

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/RU2015/000593 WO2017052399A1 (fr) 2015-09-21 2015-09-21 Réacteur haute pression à action périodique à géométrie de taylor-couette

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114870765A (zh) * 2022-05-24 2022-08-09 清华大学 多环隙式泰勒反应器

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6535796B1 (en) * 1997-12-04 2003-03-18 Rheocontrol Method for characterizing complex fluids and appliances resulting from said method
US7150183B2 (en) * 2003-06-19 2006-12-19 Schlumberger Technology Corporation Compositional characterization and quantification of solid deposits from hydrocarbon fluids
US7523648B2 (en) * 2007-02-14 2009-04-28 Schlumberger Technology Corporation Apparatus and methods for solids deposition and analysis
RU2431827C2 (ru) * 2005-11-30 2011-10-20 Энвироникс Ой Способ и устройство для измерения подвижности ионов

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6535796B1 (en) * 1997-12-04 2003-03-18 Rheocontrol Method for characterizing complex fluids and appliances resulting from said method
US7150183B2 (en) * 2003-06-19 2006-12-19 Schlumberger Technology Corporation Compositional characterization and quantification of solid deposits from hydrocarbon fluids
RU2431827C2 (ru) * 2005-11-30 2011-10-20 Энвироникс Ой Способ и устройство для измерения подвижности ионов
US7523648B2 (en) * 2007-02-14 2009-04-28 Schlumberger Technology Corporation Apparatus and methods for solids deposition and analysis

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114870765A (zh) * 2022-05-24 2022-08-09 清华大学 多环隙式泰勒反应器

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