A kind of determinator for viscosity in mink cell focus thermal process reactor and assay method thereof
Technical field
The present invention relates to a kind of measurement mechanism and method and technology field, especially a kind of determinator for viscosity in mink cell focus thermal process reactor and assay method thereof.
Background technology
World's crude resources is heaviness and in poor quality day by day, add the cost advantage that processing heavy crude brings, cause the whole world about to have the petrochemical industry of 42% to refine enterprise (U.S.: about have 2/3 refining enterprise) and tend to improve the ratio of middle heavy crude of processing raw material, the heavy inferior residual oil quantity of output is also inevitable thereupon increase thereupon.The latest data display that State Statistics Bureau announces, China's processing crude oil in 2013 is up to 4.79 × 10
8ton, wherein heavy crude occupies suitable ratio.The residual oil output being greater than 500 DEG C in these heavy crude is high, difficult processing, using value are low.How to greatest extent one of current significant challenge faced of petrochemical industry refining enterprise of China is the petroleum resources of these preciousnesses of processing and utilization, while meeting growing lightweight transport fuel oil demand, improves the level of resources utilization, increases Business Economic Benefit.Therefore the process technology of Efficient Conversion poor residuum becomes the focus of each large refining enterprise and the concern of international energy company.U.S.'s " petroleum times " points out that oil refining process of new generation mainly contains three kinds when commenting Residual cracking technology, i.e. RCC, delayed coking and residual hydrogenation.Wherein delay coking process, catalyzer is not used in processing, technological process is comparatively simple ripe, invests less, is particularly suitable for the poor residuum that lighting is feature with high carbon residue, high bituminous matter, high heteroatoms (sulphur, nitrogen, oxygen) and high metal (as: nickel, vanadium etc.).Become one of the most effective process of global inferior heavy (slag) oily lighting at present.In recent years simultaneously, China progressively sets up and expands the cooperation in the field of energy national with Canada of Venezuela etc.The heavy oil such as Venezuela's extra-heavy oil and Canadian oil sands bitumen probably become the important making & breaking that oil refining enterprise of following China processes raw material.These unconventional heavys/overweight matter petroleum resources viscosity is very large, gives exploitation, manages and defeatedly all bring huge challenge.
Therefore, in the area that lightweight mixing light oil is rare, obtain that viscosity is low, crude oil severe ° API is higher on the spot with the method for mild thermal cracking (or hydrogen supply thermal cracking), the upgrading of accumulating good stability oil becomes the preferred plan addressed this problem.Be that mild thermal cracking or degree of depth coking process all belong to mink cell focus thermal reaction process process, the development of current thermal reaction process process and reaction engineering design all focus on research raw material, cracking intermediate product, relation between the chemical composition of product and reactor optimum operation condition.Research and design requirement show to affect the viscosity that one of key factor of chemical reaction course in reactor is thermal response system.Reaction system viscosity can affect reaction system and relate to the performance of thermal surface contact, as heating furnace tube coking fouling etc., can also the process of hierarchy of control internal heat reaction, and affect final product characteristics (coking coking pattern).In order to understand better with rest in heterophase reactor (such as, coke drum) in the reflex action of reacting fluid, so that targetedly reactor design, regulate operation, the basic Viscosity Properties of reaction system is the data first needing quantitative measurment to obtain.
Thermal response system General reactions temperature is higher, and reaction velocity is fast, and the change of system chemical composition is also very fast, and this just requires the device heating rate very fast (in seconds) measuring viscosity, and the measurement of viscosity simultaneously wants rapidly, have instantaneity.In thermal process reactor also can generating gasification, cracking, produce a large amount of bubble, also have the high degree of carbonisation residue (such as, burnt) being insoluble to organic solvent and generate, these can change the fluid behaviour of thermal response system significantly.
The high-temperature viscosity measuring method that the feature of above-mentioned thermal response system makes some traditional, for example, disclosed in patent CN101308074A, parallel-plate flow method disclosed in rotational viscometer method, patent CN103480974A disclosed in capillary viscometer method, patent CN202735196U etc., can not be applicable to the measurement of viscosity in mink cell focus thermal process reactor.Patent CN101685058A and patent CN2852109Y discloses and relates to the similar high-temperature viscosity measurement mechanism of petrochemical complex, but equipment therefor heating rate is slower, with a minute metering, simultaneously viscosity-torque power the formula of equipment therefor must be based upon the standard substance temperature chosen and not occur on the basis of change of properties, can not meet the needs that thermal process reactor viscosity is measured.Therefore, attach most importance to the ability improving measuring system heating rate, measurement simple and fast and the complicated Phase velocity map of reply thermal response system, study a kind of new mink cell focus thermal process reactor viscosity characterizing method, the device that exploitation mink cell focus thermal process reactor viscosity is measured fast immediately has great importance.
Summary of the invention
Object of the present invention is exactly the feature for mink cell focus thermal process reactor, overcomes the deficiency of above-mentioned existing method existence and provides a kind of determinator for viscosity in mink cell focus thermal process reactor and assay method thereof.
For achieving the above object, the present invention adopts following technical proposals: a kind of determinator for viscosity in mink cell focus thermal process reactor, is made up of reaction unit, measuring system, control system three part.
Described reaction unit comprises drive motor, electromagnetic heating system, stainless steel is withstand voltage kettle, kettle cover, urceolus, urceolus rotating shaft; Described drive motor is arranged on the bottom of the withstand voltage kettle of stainless steel; Described electromagnetic heating system, comprise electromagnetic heating coil and programmed temperature-rising controller, described electromagnetic heating coil is connected by wire with programmed temperature-rising controller, described electromagnetic heating coil adopts the temperature of reaction unit within the scope of medium/low frequency electromagnetic oscillation effect fast lifting solenoid, described programmed temperature-rising controller is for controlling temperature of reaction, and described electromagnetic heating coil is arranged at the lateral wall of the withstand voltage kettle of stainless steel; Described stainless steel is withstand voltage kettle, its one end is openend, and kettle cover and described openend are connected by bolt is airtight, and described kettle cover is provided with vacuum system and air supply system, its when viscosity is measured for reactive system provides different thermal response pressure and atmospheric condition; Described stainless steel is withstand voltage, and kettle inside is provided with a urceolus, described urceolus top end opening, and described urceolus bottom is connected by urceolus rotating shaft with described drive motor, is aggressive device; Described urceolus bottom arranges square hole, and described urceolus is connected with square hole with one end of urceolus rotating shaft, ensures the integraty of urceolus and urceolus rotating shaft, and described urceolus can take off again for charging or coke cleaning with urceolus axis of rotation easily; The other end of described urceolus rotating shaft is fixedly connected with described drive motor with electromagnetic heating coil through the withstand voltage kettle of stainless steel, and described stainless steel is withstand voltage, and kettle is connected by bearing is airtight with urceolus rotating shaft.
Described measuring system comprises inner disc, inner disc rotating shaft, speed probe and data handling system; Described inner disc is arranged at described outer barrel, coaxial and keep certain interval with described urceolus, described inner disc is connected with the speed probe above described kettle cover by inner disc rotating shaft, for slave unit, one end of inner disc rotating shaft is fixedly connected with inner disc, the other end of inner disc rotating shaft is fixedly connected with described speed probe through kettle cover, and described kettle cover is connected by bearing is airtight with inner disc rotating shaft; Described speed probe, drive motor are connected by wire with data handling system; Described speed probe, for gathering the speed discrepancy between described urceolus and inner disc, and is sent to described data handling system; Described data handling system, the speed discrepancy-viscosity correspondence table of the standard substance measured according to this measurement mechanism, is converted into corresponding k value by described speed discrepancy.
Described control system comprises infrared thermometer and gas circuit counterbalance valve, described infrared thermometer is arranged at inside kettle cover, for controlling the temperature in stainless steel cauldron, described gas circuit back pressure valve is arranged in described vacuum system, for the pressure of stable reaction unit inside, pressure is remained in pre-set range of pressure values.
Preferably, sheathed cooling jacket in the urceolus rotating shaft of kettle exterior bottom that described stainless steel is withstand voltage, the upper end of described cooling jacket is fixedly connected with the withstand voltage kettle of stainless steel, the lower end of described cooling jacket is fixedly connected with described drive motor, the inner water-filling of described cooling jacket, for cooling urceolus rotating shaft.
Preferably, described vacuum system and air supply system comprise gas inlet tube, inlet control valve, gas outlet tube, discharge control valve and tensimeter.
Preferably, described inner disc is right cylinder, and described inner disc and described outer cylinder diameter are 5-15mm to clearance distance, and end play distance is 5-15mm.
Preferably, the capacity of stainless steel cauldron is 50-500ml.
Preferably, when the air supply system of described device provides oxidizing atmosphere, gases used is oxygen; When the air supply system of described device provides reducibility gas atmosphere, gases used is hydrogen or carbon monoxide; When the air supply system of described device provides inert gas atmosphere, gases used is nitrogen.
Preferably, the pressure limit that described reaction unit provides is 0 ~ 1MPa.
Preferably, speed discrepancy-viscosity correspondence the table of described standard substance obtains by the following method: under the pressure condition of surveyed mink cell focus, select heavy oil product that viscosity is at different temperatures known as standard substance, measure its speed discrepancy under difference presets temperature of reaction with viscosity measurement mechanism in described mink cell focus thermal process reactor, and then obtain the correspondence table of speed discrepancy and k value;
The present invention also provides a kind of method using this device to carry out the measurement of mink cell focus thermal process reactor viscosity, comprises the steps:
(1) enough mink cell focuses are joined in described urceolus, guarantee that described in mink cell focus thermal process reactor, inner disc is immersed in reactant always;
(2) withstand voltage for stainless steel kettle and kettle cover are covered tightly airtight, and open vacuum system, withstand voltage for stainless steel kettle inside is evacuated to vacuum state, close vacuum system, then open air supply system, be filled with test desired gas again, be pressurized to preset value as required;
(3) set reaction by programmed temperature-rising controller temperature required, electromagnetic heating coil starts heating, opens drive motor and arranges rotating speed, open speed measuring system simultaneously;
(4) after reaction unit is warmed up to default temperature of reaction, described data handling system gathers the tachometer value of speed probe and drive motor, by the rotating speed of inner disc and the difference of drive motor rotating speed and time dependent trend thereof, speed discrepancy-viscosity correspondence the table of the standard substance measured according to this measurement mechanism, is converted into corresponding k value by described speed discrepancy.
Preferably, the rotating speed arranging drive motor is 4000rpm.
Sample mink cell focus can react at 400 DEG C under normal circumstances, and viscosity changes at any time, be difficult to directly measurement, but the speed discrepancy between inner disc and urceolus immediately to measure.Due to being not stable higher than the standard oil sample under 350 DEG C of conditions, can not react, the k value difference of its viscosity between 110 DEG C-200 DEG C is simultaneously very large, substantially can cover the region of viscosity from low to high.So can by the viscosity number of known standard oil sample, and then under same temperature condition, measure when this standard oil sample is in this viscosity and obtain speed discrepancy, standard substance viscosity under multiple temperature conditions between 110 DEG C-200 DEG C and speed discrepancy corresponding to this device are enumerated, speed discrepancy-viscosity correspondence table of this measurement mechanism standard substance can be obtained.Measured rotating speed and the drive motor rotating speed difference of sample mink cell focus inner disc by this measurement mechanism, just can convert and obtain the k value of sample mink cell focus.
General, when adopting calibrated wrench method measuring and calculating viscosity number, accurate for ensureing to measure numerical value.Torque will between 20%-85%, if moment of torsion too small or excessive time, application condition is serious, and the viscosity value obtained is inaccurate, even can not measure; And the present invention is by carrying out data processing to the speed discrepancy of urceolus and inner disc, speed discrepancy-viscosity correspondence table according to standard substance is converted into corresponding viscosity number, overcome and measure by calibrated wrench method the error produced, be also applicable to the mensuration system that range of viscosities is wider simultaneously.
The present invention adopts drive motor to drive, this is because the drive efficiency of magnetically-actuated is lower, the medium that, viscosity high for density is large, because the torque of transmission is relatively large, use critical constraints, the present invention adopts bearing countershaft to carry out the mode sealed, and improves drive efficiency, reduces maintenance cost.
In the present invention, adopt medium/low frequency electromagnetic oscillation in reaction unit, the energy of generation can act on metallic reactors inside in the short period, and temperature in maximum quick-lift attachreactor, reaches temperature of reaction as early as possible, reduces measuring error and produces.
The invention has the beneficial effects as follows, device and method of the present invention, achieve the measurement to viscosity in mink cell focus thermal process reactor and variation tendency at a certain temperature thereof; Whole device adopts Electromagnetic Heating mode, the rate of heat addition is fast, realizes in seconds, rapidly test macro can be heated to thermal response temperature required, reduce subsidiary reaction to occur, ensure that the accuracy of measurement, and can constant temperature be kept, solve the problem that conventional measuring systems is difficult to be rapidly heated, quantitative measurment can be carried out to the viscosity of Rapid Thermal course of reaction, what also can realize mink cell focus viscosity in rapid reaction is online, and continuous print, measures immediately; Measuring process simple and fast, speed discrepancy-viscosity correspondence the table of the standard substance measured in advance by device, the system viscosity in the complicated Phase velocity map situation of mink cell focus thermal response can be measured rapidly, measurement numerical value is accurate, measurement range of viscosities is wide, and assurance device is applicable in thermal process the reaction system generating gas phase and solid product; Measure speed discrepancy-viscosity correspondence table in advance to adopt the mink cell focus of known viscosity distribution as standard substance, ensure that metering system measuring process is convenient, Applicable temperature scope is comparatively large, especially also can be suitable under the hot conditions of mink cell focus thermal response; Measurement atmospheric condition is wide, and under oxidisability (as oxygen), reducibility gas (as hydrogen, carbon monoxide), inert conditions, (as nitrogen) all can use; Measurement pressure limit is wide, can carry out under 0 ~ 1MPa condition.
Accompanying drawing explanation
Fig. 1 is the structural representation of measurement mechanism of the present invention;
Wherein 1. drive motor, the 2. withstand voltage kettle of stainless steel, 3. kettle cover, 4. gas circuit counterbalance valve, 5. electromagnetic heating coil, 6. programmed temperature-rising controller, 7. bolt, 8. gas inlet tube, 9. inlet control valve, 10. gas outlet tube, 11. discharge control valves, 12. tensimeters, 13. urceolus, 14. urceolus rotating shafts, 15. inner discs, 16. inner disc rotating shafts, 17. speed probes, 18. data handling systems, 19. wires, 20. mink cell focuses, 21. cooling jackets, 22. infrared thermometers.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further described.
For a determinator for viscosity in mink cell focus thermal process reactor, be made up of reaction unit, measuring system, control system three part.
Described reaction unit comprises drive motor 1, electromagnetic heating system, stainless steel is withstand voltage kettle 2, kettle cover 3, urceolus 13, urceolus rotating shaft 14; Described drive motor 1 is arranged on the bottom of the withstand voltage kettle 2 of stainless steel; Described electromagnetic heating system, comprises electromagnetic heating coil 5 and programmed temperature-rising controller 6, and described electromagnetic heating coil 5 is connected by wire 19 with programmed temperature-rising controller 6; Described electromagnetic heating coil 5 adopts the temperature of reaction unit within the scope of medium/low frequency electromagnetic oscillation effect fast lifting solenoid, and control temperature of reaction by programmed temperature-rising controller 6, described electromagnetic heating coil 5 is arranged at the lateral wall of the withstand voltage kettle 2 of stainless steel; The capacity of described stainless steel is withstand voltage kettle 2 is 50-500ml, its one end is openend, kettle cover 3 is connected by bolt 7 is airtight with described openend, described kettle cover 3 is provided with described vacuum system and air supply system, described vacuum system and air supply system comprise gas inlet tube 8, inlet control valve 9, gas outlet tube 10, discharge control valve 11 and tensimeter 12, its when viscosity is measured for reactive system provides the pressure limit of 0 ~ 1MPa, and when needs provide oxidizing atmosphere, gases used is oxygen; When needs provide reducibility gas atmosphere, gases used is hydrogen or carbon monoxide; When needs provide inert gas atmosphere, gases used is nitrogen; Described stainless steel is withstand voltage, and kettle 2 inside is provided with a urceolus 13, described urceolus 13 top end opening, and described urceolus 13 bottom is connected by urceolus rotating shaft 14 with described drive motor 1, is aggressive device; Described urceolus 13 bottom arranges square hole, and described urceolus 13 is connected with square hole with one end of urceolus rotating shaft 14, ensures the integraty of urceolus 13 and urceolus rotating shaft 14, and described urceolus 13 can rotate with urceolus rotating shaft 14 and can take off easily for charging or coke cleaning; The other end of described urceolus rotating shaft 14 is fixedly connected with described drive motor 1 with electromagnetic heating coil 5 through the withstand voltage kettle of stainless steel 2, and described stainless steel is withstand voltage, and kettle 2 is connected by bearing is airtight with urceolus rotating shaft 14; Sheathed cooling jacket 21 in the urceolus rotating shaft 14 of described stainless steel the is withstand voltage outer side-lower of kettle 2, the upper end of described cooling jacket 21 is fixedly connected with the withstand voltage kettle 2 of stainless steel, the lower end of described cooling jacket 21 is fixedly connected with described drive motor 1, the inner water-filling of described cooling jacket, for cooling urceolus rotating shaft 14.
Described measuring system comprises inner disc 15, inner disc rotating shaft 16, speed probe 17 and data handling system 18; Described inner disc 15 is right cylinder, and it is inner that it is arranged at described urceolus 13, coaxial with described urceolus 13, and described inner disc 15 is 5-15mm with described urceolus 13 radial play distance, and end play distance is 5-15mm.Described inner disc 15 is connected with the speed probe 17 above described kettle cover 3 by inner disc rotating shaft 16, for slave unit, one end of inner disc rotating shaft 16 is fixedly connected with inner disc 15, the other end of inner disc rotating shaft 16 is fixedly connected with described speed probe 17 through kettle cover 3, and described kettle cover 3 is connected by bearing is airtight with inner disc rotating shaft 16; Described speed probe 17, drive motor 1 are connected by wire 19 with data handling system 18; Described speed probe 17, for gathering the speed discrepancy between described urceolus 13 and inner disc 15, and is sent to described data handling system 18; Described data handling system 18, is converted into corresponding k value for the speed discrepancy according to viscosity measurement mechanism in the described mink cell focus thermal process reactor preset-viscosity correspondence table by described speed discrepancy.
Described control system comprises infrared thermometer 22 and gas circuit counterbalance valve 4, described infrared thermometer 22 is arranged at inside kettle cover 3, for controlling the temperature in stainless steel cauldron, described gas circuit counterbalance valve 4 is arranged on kettle cover 3 gas outlet tube 10, for the pressure of stable reaction unit inside, pressure is remained in pre-set range of pressure values.
Utilize said apparatus to measure a method for mink cell focus thermal process reactor viscosity, comprise the steps:
(1) enough mink cell focuses 20 are joined in described urceolus 13, guarantee that inner disc 15 described in thermal process reactor is immersed in reaction product mink cell focus 20 always;
(2) withstand voltage for stainless steel kettle 2 and kettle cover 3 are covered tightly airtight, and open discharge control valve 11, withstand voltage for stainless steel kettle 2 inside is evacuated to vacuum state, close discharge control valve 11 again, open inlet control valve 9, be filled with test desired gas again, be pressurized to preset value as required;
(3) set desired reaction temperature by programmed temperature-rising controller 6, electromagnetic heating coil 5 starts heating, and open described speed measuring system, the rotating speed arranging drive motor 1 is 4000rpm simultaneously;
(4) after reaction unit is warmed up to default temperature of reaction, described data handling system 18 gathers the tachometer value of speed probe 17 and drive motor 1.Under the pressure condition of surveyed mink cell focus 20, select mink cell focus 20 product that viscosity under different temperatures is known as standard substance, with the speed discrepancy of viscosity measurement mechanism measurement standard material under difference presets temperature of reaction in described mink cell focus thermal process reactor, obtain the correspondence table of speed discrepancy and k value, in table 1.By measuring the rotating speed of inner disc 15 of mink cell focus 20 gained and the difference of drive motor 1 rotating speed and time dependent trend thereof, speed discrepancy-viscosity of establishing criteria material is corresponding to be shown, and described speed discrepancy is converted into corresponding k value.
Table 1 pressure is 0.2Mpa, the speed discrepancy-viscosity correspondence table of the heavy oil product that under the different temperatures obtained by viscosity measurement mechanism in mink cell focus thermal process reactor, viscosity is known
1. speed discrepancy |
Viscosity |
2. speed discrepancy |
Viscosity |
3989rmp |
13140mm·s
-1(110℃)
|
168rmp |
502mm·s
-1(140℃)
|
2534rmp |
6768mm·s
-1(115℃)
|
58rmp |
230mm·s
-1(150℃)
|
1187rmp |
3679mm·s
-1(120℃)
|
30rmp |
118mm·s
-1(160℃)
|
675rmp |
2100mm·s
-1(125℃)
|
11rmp |
40mm·s
-1(180℃)
|
362rmp |
1254mm·s
-1(130℃)
|
3rmp |
18mm·s
-1(200℃)
|
Embodiment one
Under 0.2MPa, 400 DEG C of reaction conditionss (mitigation thermal response), reaction time records certain heavy crude oil residue oil sample thermal process reactor speed discrepancy numerical value when being 30min be 43rmp, and it is 141mms that the speed discrepancy-viscosity correspondence table conversion through table 1 can obtain system viscosity
-1.
Embodiment two
Under 0.2MPa, 450 DEG C of reaction conditionss (fierce thermal response), reaction time records certain heavy crude oil residue oil sample thermal process reactor speed discrepancy numerical value when being 30min be 1789rmp, and it is 5890mms that the speed discrepancy-viscosity correspondence table conversion through table 1 can obtain system viscosity
-1.
The above is only preferred embodiment of the present invention, but not does any pro forma restriction to the present invention.When not exceeding technical solution of the present invention scope, any those skilled in the art all can slightly change according to above-mentioned technology contents or be modified to the Equivalent embodiments of equivalent variations.Every technical spirit according to the present invention above embodiment is done any simple change, modification and equivalent variations, all still belong to the scope of technical solution of the present invention.