CN102156082A - Evaluation method of oil-soluble scale inhibitor and tester - Google Patents
Evaluation method of oil-soluble scale inhibitor and tester Download PDFInfo
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Abstract
The invention provides an evaluation method of an oil-soluble scale inhibitor, comprising the steps of: firstly pre-heating a test raw material and keeping the temperature at a constant value; leading the test raw material to pass through an annular space between an electric heating bar and a scale test tube at a relatively low flow speed, heating up and scaling; adjusting and stabilizing the temperature of the scale test tube by means of temperature cascade control of the electric heating bar and the scale test tube outlet; adjusting and maintaining the pressure of a scale generating part by a constant pressure valve; finally performing cycle test for the flow of returning to the original pot after being cooled, wherein the scale deposition amounts at beginning and end of blank test and agent added test are used as the evaluation standard. The method has the characteristics of easy implementation, small process parameter fluctuation, strong practicability to test raw materials, good simulation of real use working conditions of oil-soluble scale inhibitor, accurate evaluation result, and safe and reliable test procedure. Simultaneously, the flow of the tester is simplified, the volume of the tester is reduced, the constant process parameters are ensured during the evaluation procedure, and the adaptability of the tester to different raw materials is widened.
Description
Technical field
The invention belongs to the petrochemical technology field, relate generally to a kind of dynamic evaluation method and test unit of oil-soluble performance of antisludging agent.
Background technology
Antisludging agent also is called scale inhibitor, antitartar agents, anti scorching agent, is a petroleum chemical industry class chemical assistant commonly used, in order to suppress and to slow down fouling tendency in the process equipment, prolongs the even running cycle of equipment.
Petrochemical process is a continuous large-scale production run, and long-term operation has become one of important indicator of weighing its technical merit.Because process temperature height, and contain some impurity and coking precursor in the medium of processing, high temperature and the lower position of flow velocity can be assembled or be deposited on to these materials gradually, cause equipment scaling, influence heat transfer efficiency, shorten the cycle of operation of equipment, meeting occluding device when serious, cause device to stop work or the initiation security incident, bring great threat for the safety in production of petroleum chemical industry.
The formed dirt of petrochemical process mainly is made up of the inorganic scale of inorganic salts/impurity particle deposition generation and/or the organic deposition that organic coking precursor polycondensation produces.Because processing technology complexity and medium are of a great variety, the dirt that various process produced varies.Antisludging agent generally is to develop according to specific dirt, and the correct antisludging agent of selecting for use is the key of suppression equipment fouling, and therefore, antisludging agent must carry out Adaptability Evaluation in development process He before the commercial Application.Up to now, China does not also have unified evaluation of scale inhibitor standard and instrument and equipment.The evaluation of scale inhibitor method of patent and bibliographical information mainly can be divided into static method and dynamic method.Static method generally is under the static situation of test raw material, adopt constant temperature electric heating silk or incrustation testing tube, respectively blank testing with add the fouling degree of agent test raw material in the identical time, estimate the scale inhibition effect of antisludging agent with the relative value of the two, evaluation method and equipment are simple, but accuracy is relatively poor as a result.Dynamic method is to investigate the scale inhibition effect of antisludging agent under the test raw material flow state, and evaluation cycle is long, and equipment is complicated, but can simulate actual production conditions preferably, and reflect the actual usability of antisludging agent truly, therefore, dynamic method more and more comes into one's own.
In existing antisludging agent dynamic evaluation method, patent ZL95200117.9 is under certain temperature and pressure, flow through the volume of fine aperture or flow out the needed time of equal volume the fouling tendency of evaluation detected fluid or the scale-inhibiting properties of antisludging agent by measuring detected fluid; Little hole count and aperture fibrous root that different tests is selected are adjusted according to the viscosity of measured medium, lack unified adjustment standard, and certain aperture is very big because of the possibility that accidentalia is blocked in the process of the test, is difficult to reflect truly the fouling tendency of measured medium and the scale-inhibiting properties of antisludging agent.Document " petroleum refining and chemical industry " [1995,26 (5): 26～29] the catalytic slurry antisludging agent dynamic evaluation method of being introduced, be to keep under the constant condition of tested media flow velocity and furnace temp, by measuring blank and the temperature that adds agent test incrustation testing tube gateway at the whole story in the identical time period, characterize the scale inhibition effect of antisludging agent with relative temperature difference.This method can be simulated the flow state of material under actual condition preferably, but there are two obvious defects in it: the one, and evaluation procedure is a normal pressure, only is applicable to the high boiling medium as catalytic slurry etc., it is poor to adapt to; The 2nd, test is the stage of temperature fluctuation maximum at whole story, with this moment the incrustation testing tube the gateway temperature difference as evaluation criterion, be difficult to guarantee the accuracy of test data.Patent publication No. CN 1670136A is described to be a kind of evaluation method of petrochemical process process antisludging agent.This method is under certain temperature and pressure, with pump test raw material is generated between pipe and the dirt collection tube at the dirt that is one another in series and circulates; It is heating furnace that dirt generates pipe outer, and test raw material is heated to predetermined temperature; The built-in screen cloth of dirt collection tube is collected the high molecular polymerization fouling that test raw material forms in heating process; Behind the certain hour, dirt is generated pipe and the dirt collection tube cleans, drying, weigh, the dirt general assembly (TW) that generates with blank test is a benchmark, calculate the antisludging agent of commenting to the scale inhibition performance of used test raw material, by the scale inhibition performance value performance of antisludging agent is estimated.The advantage of this method is the flow state of simulation test medium preferably, and has considered the influence of pressure to the medium form, and adaptability strengthens.Its weak point: the one, dirt is distributed in dirt respectively and generates in pipe and the dirt collection tube, makes process of the test become complicated; The 2nd, in dirt generation pipe, screen cloth is set, easily cause system jams, be not suitable for testing bituminous matter and the higher medium (as normal pressure residual oil, vacuum residuum etc.) of gum level, and the dirt that is deposited on the wall of dirt that is obtained by screen filtration and commercial unit there is very big difference; The 3rd, generate between pipe and the dirt collection tube only part of round-robin medium between the two at dirt in the test process for being deposited, can't replenish new medium from head tank, the effective internal circulating load amount of medium is few, the medium lower to some boiling points or the coking tendency is little, the dirt growing amount influences result's accuracy very little; The 4th, this invention does not have special pressure regulation facility, and it is stable to be difficult to keep system pressure; For the test raw material of high temperature, the fluctuation of system pressure may cause raw material to vaporize in a large number, and test temperature is produced bigger influence.Above-mentioned drawbacks limit the accommodation of this evaluation method.The dynamic evaluation method of described scaling tendency of patent publication No. CN 101576550A and scale inhibition effect, be to cross flux depression capillaceous with sample stream under the constant-pressure drop to characterize its scaling tendency, characterize the scale-inhibiting properties of medicament with the ratio of the cumulative flow output of sample under the identical instantaneous discharge rate attenuation amplitude and blank sample cumulative flow output.This method can be used for the evaluation of the inorganic scale of liquid medium and organic deposition prediction and scale inhibition effect, both applicable to water, also applicable to oil, obviously widens the range of application of evaluation of scale inhibitor method, the evaluating apparatus that adopts also comparatively simple.But this method exists very big drawback with the circulation and the fouling main body of kapillary as sample.Adsorption effect capillaceous is extremely strong, if sample is an organic media, the organism that is adsorbed on the capillary wall is difficult to desorption, and the rapid polymerization fouling of meeting blocks kapillary under the hot test environment; If the viscosity of medium is higher, it also is very difficult flowing through kapillary; Therefore, this method is not suitable for testing the fouling tendency of organic media under high viscosity medium and the high temperature.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of dynamic evaluation method and test unit of oil solvent performance of antisludging agent are provided, so that the actual applying working condition of simulated oil solvent antisludging agent better, the authenticity and the accuracy of the applicability of Enhancement Method, the security of process and evaluation result.The flow process of short form test device is simultaneously dwindled the volume of test unit, guarantees that technological parameter is constant in the evaluation procedure, widens the adaptability of test unit to different material.
The present invention realizes that the technical scheme that the dynamic evaluation method of above-mentioned oil solvent performance of antisludging agent is taked is: earlier with test raw material preheating and constant temperature, heat up and fouling by the annular space between electrically heated rod and the dirt testing tube then, the temperature of dirt testing tube is regulated and stablized to the mode of utilizing electrically heated rod and dirt testing tube outlet temperature tandem to control, utilize the constant pressure valve adjustment and keep the pressure of dirt generating portion, carry out cyclic test after former jar flow process is returned in cooling, with the blank and dirt deposition amount that adds agent test whole story as evaluation criterion.
The present invention realizes that the test unit of the dynamic evaluation method of above-mentioned oil solvent performance of antisludging agent comprises temperature control system, thermopair, head tank, the jar well heater, the washing oil bottle, the dirt testing tube, electrically heated rod, hydrocooler, sump oil bottle and volume pump, constant pressure valve, the inlet of described volume pump is connected with the washing oil bottle with head tank respectively by threeway, between head tank and threeway, be provided with valve, between washing oil bottle and threeway, be provided with valve, the volume pump outlet is divided into two-way, one the tunnel is used to discharge discarded test(ing) medium, and another road links to each other with the inlet of dirt testing tube; Described constant pressure valve is provided with gaging pressure table and set pressure table, its inlet is connected with described hydrocooler, outlet is divided into two-way by three-way pipe, lead up to valve with link to each other with described petroleum tank, another road links to each other with described sump oil bottle by valve, the bringing-up section of electrically heated rod bottom place described incrustation testing tube and with the inwall of incrustation testing tube between form annular space, top the circular seal face be connected with the last end in contact of dirt testing tube and be in the sealing impaction state; Exit with hydrocooler in described head tank is respectively equipped with thermopair.
Test raw material of the present invention is initial boiling point greater than 35 ℃ and can produces the oil soluble material of scale formation in process, as gasoline, diesel oil, and catalytic cracked oil pulp, vacuum residuum etc.
The preheating of test raw material of the present invention and thermostat temperature are 30～150 ℃, and test raw material is heavy more, and this temperature is high more.
Annular cross-sectional area between incrustation testing tube of the present invention and the electrically heated rod: the circulation area of associated line=2.0～10.0: 1.0, preferred 4.0～7.0: 1.0, the flow velocity of test raw material in the reduction incrustation testing tube.
The band splenium of evaluation method of the present invention divides between volume pump and constant pressure valve, promptly mainly concentrates on dirt and generates the position; Its test pressure is by the constant pressure valve adjustment and keep.Test pressure can determine that generally the high 0.05～2.0MPa of saturated vapor pressure than test raw material under this temperature gets final product preferred 0.1～1.5MPa by the saturated vapor pressure of raw material under the test temperature; Also can simulate the on-stream pressure that antisludging agent uses the position commercial plant.
Flushing oil of the present invention is the sherwood oil of 60～90 ℃ of boiling ranges.This sherwood oil is a petrochemical industry cleaning solvent commonly used, its stable in properties, be difficult for residual, cheap, free from extraneous odour, toxic and side effect is little, cleaning experiment system apace, and reduce the harmful effect that the experimenter is brought.
The flow process of evaluation of scale inhibitor method provided by the present invention can make a large amount of fresh feeds enter the dirt testing tube, has created advantageous conditions for increasing the dirt growing amount; Simultaneously, raw material in the dirt testing tube is in the condition of high temperature and helps the dirt generation, can further improve the dirt growing amount, the circulation that makes the lower test raw material of fouling tendency pass through certain hour also can generate the dirt of capacity, improves the adaptability of the present invention to the different tests raw material.With test raw material temperature heating and constant temperature to 30～150 ℃, can make test raw material have good flowability all the time, prevent the influence of material temperature fluctuation to evaluation result; Simultaneously, raw material preheating temperature is not higher than 150 ℃, does not reach into dirty condition as yet, can prevent test raw material in cyclic process in position foulings such as pipeline, valve, volume pumps, protect evaluating apparatus well.Adopt the form of electrically heated rod and dirt testing tube subassembly that test raw material is heated, and allow raw material pass through the incrustation testing tube with lower flow velocity, dwindle the volume of high-temperature part widely, the flow process and the dirt generating mode of antisludging agent dynamic evaluation method have been simplified, improve the heating rate of raw material, increased the area and the incrustation amount of dirt deposition; And the mode of this heavy coalescent dirt of inside surface at electrically heated rod outside surface and incrustation testing tube, identical with the dirt deposition mode in the commercial unit, can reflect the fouling ability of test raw material and the scale inhibition ability of antisludging agent to be measured more truly, simulate the fouled condition of production equipment under the actual condition better, improve the authenticity of evaluation result.Electrically heated rod has temperature control system, and controls with the material temperature employing tandem of incrustation testing tube outlet, can improve the stability of test material temperature in the incrustation testing tube and the accuracy of test figure.And utilize the constant pressure valve adjustment and keep the pressure of dirt generating portion of the present invention, easy to use, regulate flexibly, pressure stability.Adopt pressurization and constant voltage operation, can keep raw material under test temperature, to be in liquid condition all the time, avoid raw material to undergo phase transition, improve the security of the present invention the adaptability and the process of the test of different tests raw material to having a strong impact on that evaluation result produces.The adaptability of this evaluation method can be effectively widened in the combination of above-mentioned factors, avoids the technological parameter fluctuation phenomenon, improves the security of precision of test result and process of the test.
Description of drawings
Fig. 1 is an evaluation of scale inhibitor schematic representation of apparatus provided by the present invention.
Fig. 2 a-c is the unitized construction synoptic diagram of dirt testing tube of the present invention and electrically heated rod.
Fig. 3 influences chart for the ratio of the annular cross-sectional area between incrustation testing tube of the present invention and the electrically heated rod and the circulation area of associated line changes to scale inhibition effect.
Fig. 4 is the property list of catalytic cracked oil pulp of the present invention.
Fig. 5 is the property list of mixed diesel of the present invention.
Fig. 6 is the property list of coker gasoline of the present invention.
Among the figure, 1, power supply and temperature control system, 2, thermopair, 3, head tank, 4, the head tank well heater, 5, the washing oil bottle, 6, volume pump, 7～9, valve, 10, the detachable heat-insulating cover, 11, the dirt testing tube, 12, electrically heated rod; 13, thermopair, 14, valve, 15, hydrocooler, 16, thermopair, 17, constant pressure valve, 18～22, valve, 23, the sump oil bottle, 24, pad, 25, gland, P1, gaging pressure table, P2, set pressure table.
Embodiment
The present invention realizes by following steps:
(1) will test selected raw material metering back and add head tank, heating makes it have good flowability, and keeps this raw material temperature constant in process of the test.Test raw material is sent into the incrustation testing tube with the volume pump constant speed, annular space between incrustation testing tube and electrically heated rod flows through, the temperature and pressure for the treatment of test raw material picks up counting when reaching predetermined value, after circulation a period of time, close heating power supply, continue to be cooled to the test raw material temperature and the preheat temperature basically identical of incrustation testing tube outlet with the test raw material circulation; With flushing oil washing test system and cooling once more, reduce to then, unload electrically heated rod and incrustation testing tube, dry up the flushing oil on surface near after the room temperature, dry and steady.Calculate the general assembly (TW) difference Δ G of test front and back electrically heated rod and incrustation testing tube
1
(2) in the test raw material of equivalent, add a certain amount of antisludging agent to be measured, after stirring, with identical test method of step (1) and condition, the general assembly (TW) difference Δ G of electrically heated rod and incrustation testing tube before and after the determination test
2With (Δ G
1-Δ G
2)/Δ G
1Percentage characterize the antisludging agent tested scale inhibition effect to test raw material.
The invention will be further described in conjunction with the accompanying drawings: as shown in Figure 1, as shown in Figure 1, a kind of evaluation experimental device that is applicable to the oil-soluble antisludging agent, on head tank 3, be provided with head tank well heater 4, thermopair 2 and temperature control system 1, head tank well heater 4 places head tank 3 outsides, what head tank well heater 4 adopted is barrel-like structure, and heating element is placed between insulator and the shell.Head tank 3 can be taken out from well heater 4 easily.One end of thermopair 2 is positioned at head tank 3, and the other end is connected with temperature control system 1.The inlet of volume pump 6 is connected with washing oil bottle 5 with head tank 3 respectively by threeway, be provided with valve 20 between head tank 3 and the threeway, be provided with valve 21 between washing oil bottle 5 and the threeway, can realize switching between head tank 3 and the washing oil bottle 5 by controlled valve 20 and 21; The outlet of volume pump 6 through valve 7 be divided into two-way after threeway links to each other, the one tunnel is used to efflux discarded test(ing) medium, is provided with valve 8 in its exit, another road links to each other with dirt testing tube 11 by valve 9.Dirt testing tube 11 is " U " shape pipe, and inner wall smooth which is provided with entry and exit; Electrically heated rod 12 is "T"-shaped structure, and outer wall is smooth, and the vertical portion, bottom is divided into bringing-up section, and upper level partly is the circular seal face; The bringing-up section of electrically heated rod 12 bottoms place incrustation testing tube 11 and with the inwall of incrustation testing tube between form annular space, top the circular seal face be connected with the last end in contact of dirt testing tube 11 and be in the sealing impaction state, in the contact site of electrically heated rod 12 and dirt testing tube 11 pad 24 is set and makes the electrically heated rod 12 and the contact site of dirt testing tube 11 reach excellent sealing.The effect of electrically heated rod 12 has two: bottom vertically part is stretched in the dirt testing tube 11, plays heat effect; Top is the sealing surface of a circle, and fundamental purpose is the sealing that realizes between electrically heated rod 12 and the dirt testing tube 11, prevents that test raw material is from leaking between the two; Simultaneously, this structure will be easy to dismounting, because after will pulling down subassembly weighing, scale removal, oven dry after each experiment, just can test next time.The sealing of electrically heated rod 12 and dirt testing tube 11 compresses mode can be had multiple, as interconnected: promptly the outside, the bottom of the circular seal face of electrically heated rod 12 has external thread, dirt testing tube 11 upper inner have internal thread, electricity is added rod 12 screw within the dirt testing tube 11, realize that by pad 24 sealing compresses connection (shown in the 2a among Fig. 2) between the two; Connect formula outward: promptly the lower inside of the circular seal face of electrically heated rod 12 has internal thread, the upper outside of dirt testing tube 11 has external thread, dirt testing tube 11 is screwed in the circular seal face of electrically heated rod 12, realize that by pad 24 sealing compresses connection (shown in the 2b among Fig. 2) between the two; Gland-type: promptly the inboard of gland 25 has internal thread, the upper outside of dirt testing tube 11 has external thread, electrically heated rod 12 directly embeds in the gland 25, electrically heated rod 12 is sealed to compress with dirt testing tube 11 with pad 24 by gland 25 to be connected (shown in the 2c among Fig. 2).These three kinds of connected modes provided by the present invention are not limited only to this only as an example.Adopting above-mentioned connected mode purpose is for flexible dismounting, is convenient to operations such as weigh in the test front and back, scale removal, cleaning.After dirt testing tube 11 and electrically heated rod 12 seal combination, be connected on the evaluating apparatus, be enclosed with detachable heat-insulating cover 10 in its outside.Detachable heat-insulating cover 10 uses to be made as soft insulation materials such as glass fibre, its profile is consistent with the profile of dirt testing tube 11 and electrically heated rod 12 seal assemblies, one side opening, after being wrapped on dirt testing tube 11 and electrically heated rod 12 seal assemblies, can carry out opening part is connected with mode commonly used such as hasp, shackle, to realize insulation and to avoid the burn purpose of testing crew of high temperature.Electrically heated rod 12 has temperature controller, and this temperature controller can be independently, also can integrate with other control section.The material temperature that the thermopair 13 that the surface temperature of electrically heated rod 12 and dirt testing tube 11 exits are provided with is detected adopts conventional tandem control.The outlet of dirt testing tube 11 successively with valve 14, hydrocooler 15, constant pressure valve 17 connects.Constant pressure valve 17 is that valve (as the YTY-4 type fluid pressure regulator of Jiangsu Province Valve Factory, Funing County production) is set and kept to a kind of pressure, which is provided with gaging pressure table P1 and set pressure table P2, when the pressure of gaging pressure table P1 was lower than the pressure of set pressure table P2, constant pressure valve 17 was in closed condition; When the pressure of gaging pressure table P1 during a little more than the pressure of set pressure table P2, constant pressure valve 17 is in conducting state.The discharge pipe of constant pressure valve 17 is divided into two-way, and the valve 18 of leading up to links to each other with petroleum tank 3 with 19, and another road links to each other with sump oil bottle 23 by valve 22.When being communicated with petroleum tank 3, valve-off 22 is opened valve 18 and 19 and is got final product; When being communicated with sump oil bottle 23, valve-off 19 is opened valve 18 and 22 and is got final product.Be provided with thermopair 16 in the exit of hydrocooler 15, purpose is to control the amount of chilled water by the test raw material temperature behind the detection hydrocooler 15, guarantee can not cause system jams when test heavy test raw material, thermopair 13 all links to each other with temperature control system 1 with thermopair 16.
Described each temperature detection of present embodiment, control and power supply can separate work, in order to reduce the volume of test unit, present embodiment is integrated in one with all temperature detection, control and power unit system, be referred to as power supply and temperature control system 1, yet this is not the restriction that the present invention is made.What relate to detection, control and power circuit employing in the temperature control system 1 is conventional circuit.
The evaluation of general antisludging agent is divided into twice test, once is blank test, and another time is for adding the agent test.
Test for the first time is blank test, promptly under the situation that does not add antisludging agent, only carries out the fouling test with selected test raw material.Detailed process is as follows:
Accurately the dirt testing tube 11 of weighing clean dried and the general assembly (TW) of electrically heated rod 12 are designated as G
1, be accurate to 0.01g.Annular cross-sectional area between incrustation testing tube and the electrically heated rod: the circulation area of associated line=2.0～10.0: 1.0, preferred 4.0～7.0: 1.0.Assemble dirt testing tube 11 and electrically heated rod 12, then it properly is connected on the evaluating apparatus, detachable heat-insulating cover 8 is arrived surely the outside of dirt testing tube 11 and electrically heated rod 12 subassemblies together.The sherwood oil that in washing oil bottle 5, adds capacity.Quantitatively add test raw material in head tank 3, the power supply preheating of opening head tank well heater 4 is also constant in 30～150 ℃, and test raw material is heavy more, and this temperature is high more, so that test raw material has good flowability.Valve-off 8,21 and 22, open valve 7,9,14,18,19 and 20, open volume pump 6, test raw material returns head tank according to the order of head tank 3 → valve 20 → volume pump 6 → valve 7 → valve 9 → dirt testing tube 11 → valve 14 → hydrocooler 15 → constant pressure valve 17 → valve 18 → valve 19 → head tank 3.After head tank 3 return ports have test raw material to flow out, the set pressure table P2 and dirt testing tube 11 outlet temperatures of constant pressure valve 17 are set to predetermined value, after the pressure of tensimeter P1 to be measured reached predetermined value, the power supply of opening electrically heated rod 12 began heating.The fetch boiling water chilled water of refrigeratory 15, the amount of regulating chilled water, the temperature that thermopair 16 is surveyed show and the preheat temperature basically identical of test raw material.Electrically heated rod and dirt testing tube outlet temperature are carried out tandem control, when temperature that the thermopair 13 of dirt testing tube outlet is detected with pick up counting after test temperature is consistent; After test raw material circulation a period of time, cut off the power supply of electrically heated rod 12, continue to stop volume pump 6 when circulation cools to preheat temperature basically identical with test raw material, open valve 8, bleed off the test raw material in dirt testing tube 11 and the pipeline.Valve-off 8,19 and 20 is opened valve 21 and 22, with the pressure zero setting of the set pressure table P2 of constant pressure valve 17, opens volume pump 6, and with the petroleum ether system in the washing oil bottle 5, sump oil returns sump oil bottle 23.When the flushing oil of sump oil return port is colourless, stop volume pump 6, open valve 8, put the flushing oil in clean dirt testing tube 11 and the pipeline.Close the general supply of this evaluating apparatus, take down detachable heat-insulating cover 10, unload dirt testing tube 11 and electrically heated rod 12 subassemblies, dry up the inside surface of dirt testing tube 11 and the outside surface of electrically heated rod 12 with nitrogen, in 120 ℃ baking oven dry 1 hour then, the two gross weight of weighing behind the cool to room temperature in exsiccator, note is made G
2, be accurate to 0.01g.Calculate the incrustation amount Δ G of blank test
1, Δ G
1=G
2-G
1
Test for the second time is for adding the agent test.The test raw material of the same race of adding and blank test equivalent in head tank 3, to wherein adding a certain amount of antisludging agent to be evaluated, after stirring, process conditions and the test method identical with blank test add the agent test.Add the dirt testing tube 11 of agent test front and back and the general assembly (TW) of electrically heated rod 12 and be designated as G respectively
3And G
4, add the incrustation amount Δ G that agent is tested
2=G
4-G
3
The scale inhibition performance of the antisludging agent of estimating=(Δ G
1-Δ G
2)/Δ G
1* 100%.
The scale inhibition performance of antisludging agent is big more, illustrates that its scale inhibition effect is good more.
The present invention is further elaborated by the following examples.Its purpose is content of the present invention is described better, but protection scope of the present invention is not limited by the cases cited.
The operating condition of catalytic slurry is estimated the performance of two kinds of slurry oil antisludging agents at the bottom of the simulation catalytic fractionator.
Test raw material is a catalytic cracked oil pulp, is a kind of heavy test raw material of easy coking/fouling, and its character is seen Fig. 4.
(a), blank test:
Select the annular cross-sectional area between bar incrustation testing tube and the electrically heated rod: the circulation area of associated line=5.0: 1.0, the dirt testing tube 11 of weighing clean dried and the general assembly (TW) of electrically heated rod 12 properly are connected to it on evaluating apparatus then.In head tank 3, add the 2Kg catalytic slurry, be warmed up to 110 ℃, and keep this temperature constant.In washing oil bottle 5, add the sherwood oil that accounts for its volume 80%.Valve-off 8,21 and 22 is opened valve 7,9,14,18,19 and 20, opens volume pump 6, after head tank 3 return ports have catalytic slurry to flow out, the pressure of the set pressure table P2 of constant pressure valve 17 is made as 0.5MPa (pressure at the bottom of the simulation catalytic fractionator).Dirt testing tube 11 outlet temperatures are set at 380 ℃, and electrically heated rod 12 and dirt testing tube 11 outlet temperatures are carried out tandem control.After the pressure for the treatment of the gaging pressure table P1 of constant pressure valve 17 reached 0.5MPa, the power supply of opening electrically heated rod 12 began heating.Regulate cooling water inflow, make that the temperature of catalytic slurry remains on about 105 ℃ after hydrocooler 15 coolings.The temperature that thermopair 13 is detected picks up counting when reaching 380 ℃, behind the circulation 5.0h, cuts off the power supply of electrically heated rod 12, continue the about 26min of circulation, the temperature that thermopair 13 is detected reaches 117 ℃, stops the amount of allowing pump 6, open valve 8, bleed off the catalytic slurry in dirt testing tube 11 and the pipeline.Shut-off valve 8,19 and 20 is opened valve 21 and 22, with the pressure zero setting of the set pressure table P2 of constant pressure valve 17.Open volume pump 6, with the petroleum ether system in the washing oil bottle 5, behind the 21min, the return port flushing oil of sump oil bottle 23 is colourless, stops volume pump 6, opens valve 8, puts the flushing oil in clean dirt testing tube 11 and the pipeline.Close the general supply of this evaluating apparatus, take down detachable heat-insulating cover 10, unload dirt testing tube 11 and electrically heated rod 12 subassemblies, dry up the inside surface of dirt testing tube 11 and the outside surface of electrically heated rod 12 with nitrogen, in 120 ℃ baking oven dry 1 hour then, cool to room temperature in exsiccator, weighing.The incrustation amount Δ G of blank test
1=14.38g.
(b), add the agent test:
In head tank 3, add catalytic slurry 2Kg shown in Figure 4, add antisludging agent A 0.32g, after stirring, by testing with poly-(a) identical process conditions of step and test method.Record the incrustation amount Δ G2A=6.81g that adds behind the antisludging agent A.
In head tank 3, add catalytic slurry 2Kg shown in Figure 4, add antisludging agent B 0.32g, after stirring, by testing with identical process conditions of step (a) and test method.Record the incrustation amount Δ G that adds behind the antisludging agent B
2B=2.54g.
The scale inhibition performance of antisludging agent is big more, illustrates that its scale inhibition effect is good more.That is to say that for the catalytic cracked oil pulp shown in the table 1, the scale inhibition effect of antisludging agent B is better than antisludging agent A.
The operating condition of simulation diesel oil hydrogenation raw material heat interchanger, C estimates to the diesel oil hydrogenation antisludging agent.
Test is a straight-run diesel oil with diesel oil: the compound sample of catalytic diesel oil=1: 1 is the less middle matter test raw material of a kind of coking/fouling tendency, and its character is seen Fig. 5.
(c), blank test:
Select the annular cross-sectional area between incrustation testing tube and the electrically heated rod: the circulation area of associated line=5.0: 1.0, the dirt testing tube 11 of weighing clean dried and the general assembly (TW) of electrically heated rod 12 properly are connected to it on evaluating apparatus then.In head tank 3, add the 2Kg mixed diesel, the temperature of head tank is remained on 60 ℃.In washing oil bottle 5, add the sherwood oil that accounts for its volume 80%.Valve-off 8,21 and 22, open valve 7,9,14,18,19 and 20, open volume pump 6, after head tank 3 return ports have mixed diesel to flow out, the pressure of the set pressure table P2 of constant pressure valve 17 is made as 9.0MPa (pressing the pressure of diesel oil hydrofining device in the simulation).The outlet temperature of dirt testing tube 11 is set at 320 ℃ when pressure diesel hydrotreating unit (middle reaction product temperature), and the outlet temperature of electrically heated rod 12 and dirt testing tube 11 is carried out tandem control.After the pressure for the treatment of the gaging pressure table P1 of constant pressure valve 17 reached 9.0MPa, the power supply of opening electrically heated rod 12 began heating.Regulate cooling water inflow, the mixed diesel temperature through hydrocooler 15 coolings is remained on about 55 ℃.The temperature that thermopair 13 is detected picks up counting when reaching 320 ℃, behind the circulation 8.0h, cuts off the power supply of electrically heated rod 12, continue the about 20min of circulation, the temperature that thermopair 13 is detected reaches 68 ℃, stops volume pump 6, open valve 8, bleed off the mixed diesel in dirt testing tube 11 and the pipeline.Valve-off 8,19 and 20 is opened valve 21 and 22, with the pressure zero setting of the set pressure table P2 of constant pressure valve 17, opens volume pump 6, with the petroleum ether system in the washing oil bottle 5.The flushing oil at sump oil bottle 23 return port places is colourless behind the 14min, stops volume pump 6, opens valve 8, puts the flushing oil in clean dirt testing tube 11 and the pipeline.Close the general supply of this evaluating apparatus, take down detachable heat-insulating cover 10, unload dirt testing tube 11 and electrically heated rod 12 subassemblies, dry up the inside surface of dirt testing tube 11 and the outside surface of electrically heated rod 12 with nitrogen, in 120 ℃ baking oven dry 1 hour then, cool to room temperature in exsiccator, weighing.The incrustation amount Δ G of blank test
1=7.65g.
(d), add the agent test:
In head tank 3, add mixed diesel 2Kg shown in Figure 5, add diesel oil hydrogenation antisludging agent C 0.40g, after stirring, by testing with identical process conditions of step (c) and test method.Record the incrustation amount Δ G that adds behind this antisludging agent
2=1.94g.
The operating condition of simulation coker gasoline hydrogenating materials heat interchanger, D estimates to the gasoline hydrogenation antisludging agent.
Test the used bigger lightweight test raw material of coker gasoline coking/fouling ability, its character is seen Fig. 6.
(e), blank test:
Select the annular cross-sectional area between incrustation testing tube and the electrically heated rod: the circulation area of associated line=5.0: 1.0, the dirt testing tube 11 of weighing clean dried and the general assembly (TW) of electrically heated rod 12 properly are connected to it on evaluating apparatus then.In head tank 3, add the 2Kg coker gasoline, the temperature of head tank is remained on 30 ℃.In washing oil bottle 5, add the sherwood oil that accounts for its volume 80%.Valve-off 8,21 and 22 is opened valve 7,9,14,18,19 and 20, opens volume pump 6, after head tank 3 return ports have coker gasoline to flow out, the pressure of the set pressure table P2 of constant pressure valve 17 is made as 3.2MPa (pressure of gasoline hydrogenation device).The outlet temperature of dirt testing tube 11 is set at 280 ℃ (reaction product temperature in gasoline hydrogenation device some time), and the outlet temperature of electrically heated rod 12 and dirt testing tube 11 is carried out tandem and is regulated.After the pressure for the treatment of the gaging pressure table P1 of constant pressure valve 17 reached 3.2MPa, the power supply of opening electrically heated rod 12 began heating.Regulate cooling water inflow, make through hydrocooler 15 cooled coker gasoline temperature to remain on about 30 ℃.The temperature that thermopair 13 is detected picks up counting when reaching 280 ℃, behind the circulation 6.0h, cuts off the power supply of electrically heated rod 12, continue the about 22min of circulation, the temperature that thermopair 13 is detected reaches 36 ℃, stops volume pump 6, open valve 8, bleed off the coker gasoline in dirt testing tube 11 and the pipeline.Valve-off 8,19 and 20 is opened valve 21 and 22, with the pressure zero setting of the set pressure table P2 of constant pressure valve 17, opens volume pump 6, with the petroleum ether system in the washing oil bottle 5.Behind the 12min, the flushing oil at sump oil bottle 23 return port places is colourless, stops volume pump 6, opens valve 8, puts the flushing oil in clean dirt testing tube 11 and the pipeline.Close the general supply of this evaluating apparatus, take down detachable heat-insulating cover 10, unload dirt testing tube 11 and electrically heated rod 12 subassemblies, dry up the inside surface of dirt testing tube 11 and the outside surface of electrically heated rod 12 with nitrogen, in 120 ℃ baking oven dry 1 hour then, cool to room temperature in exsiccator, weighing.The incrustation amount Δ G of blank test
1=10.39g.
(f), add the agent test:
In head tank 3, add coker gasoline 2Kg shown in Figure 6, add gasoline hydrogenation antisludging agent D 0.36g, after stirring, by testing with identical process conditions of step (e) and test method.Record the incrustation amount Δ G that adds behind this antisludging agent
2=1.64g.
Annular cross-sectional area between investigation incrustation testing tube and the electrically heated rod changes the influence to evaluation result with the ratio of the circulation area of associated line (hereinafter to be referred as the area ratio).As test raw material, except that the area ratio changed, remaining test procedure was identical with embodiment 2 with condition with mixed diesel shown in Figure 5.
Fig. 3 is seen in the influence of different area comparison test findings.As can be seen from Figure 3, when the area ratio is between 4.0: 1.0～7.0: 1.0 the time, the scale inhibition performance of the antisludging agent of being estimated changes little, substantially be one section straight line, that is to say, area is than between 4.0～7.0: 1.0 o'clock, test findings more accurately and reliably, this also is that the preferred area ratio of the present invention is 4.0～7.0: 1.0 reason.
Claims (10)
1. the evaluation method of an oil-soluble antisludging agent, it is characterized in that: earlier with test raw material preheating and constant temperature, heat up and fouling by the annular space between electrically heated rod and the dirt testing tube then, the temperature of dirt testing tube is regulated and stablized to the mode of utilizing electrically heated rod and dirt testing tube outlet temperature tandem to control, utilize the constant pressure valve adjustment and keep the pressure of dirt generating portion, carry out cyclic test after former jar flow process is returned in cooling, with the blank and dirt deposition amount that adds agent test whole story as evaluation criterion.
2. a test unit of realizing the evaluation method of the described oil-soluble antisludging agent of claim 1 comprises temperature control system [1], thermopair [2], head tank [3], jar well heater [4], washing oil bottle [5], dirt testing tube [11], electrically heated rod [12], hydrocooler [15], thermopair [16] and sump oil bottle [23], it is characterized in that: also be provided with volume pump [6] and constant pressure valve [17], the inlet of described volume pump [6] is connected with washing oil bottle [5] with head tank [3] respectively by threeway, between head tank and threeway, be provided with valve [20], between washing oil bottle [5] and threeway, be provided with valve [21], volume pump [6] outlet is divided into two-way, one the tunnel is used to discharge discarded test(ing) medium, and another road links to each other with the inlet of dirt testing tube [11]; Described constant pressure valve [17] is provided with gaging pressure table [P1] and set pressure table [P2], its inlet is connected with described hydrocooler [15], outlet is divided into two-way by three-way pipe, the valve [18] of leading up to links to each other with described petroleum tank [3] with [19], and another road links to each other with described sump oil bottle [23] by valve [22]; The bringing-up section of described electrically heated rod [12] bottom place described incrustation testing tube [11] and with the inwall of incrustation testing tube between form annular space, top the circular seal face be connected with the last end in contact of dirt testing tube and be in the sealing impaction state; In described head tank [3] and the exit of hydrocooler [15] be respectively equipped with thermopair [2] and thermopair [16].
3. the evaluation method of oil-soluble antisludging agent according to claim 1 is characterized in that: described test raw material is initial boiling point greater than 35 ℃ and can produces the oil-soluble constitents of scale formation in process.
4. the evaluation method of oil-soluble antisludging agent according to claim 1, it is characterized in that: described test pressure is set and is kept by constant pressure valve, its set pressure can be selected the high 0.05～2.0MPa of saturated vapor pressure than raw material under the test temperature, also can simulate the on-stream pressure that antisludging agent uses the position commercial plant.
5. the evaluation method of oil-soluble antisludging agent according to claim 1 is characterized in that: the preheating of described test raw material and thermostat temperature are 30～150 ℃.
6. the test unit of the evaluation method of oil-soluble antisludging agent according to claim 2 is characterized in that: described incrustation testing tube [11] and electrically heated rod [12] are removable subassembly.
7. the test unit of the evaluation method of oil-soluble antisludging agent according to claim 2, it is characterized in that: described electrically heated rod [12] has temperature control system, and the material temperature that its surface temperature and incrustation testing tube exit thermopair [13] are detected adopts tandem control.
8. the test unit of the evaluation method of oil-soluble antisludging agent according to claim 2 is characterized in that: when the pressure of the gaging pressure table [P1] on the described constant pressure valve [17] was lower than the pressure of set pressure table [P2], constant pressure valve [17] was in closed condition; When the pressure of gaging pressure table [P1] was higher than the pressure of set pressure table [P2], constant pressure valve [17] was in conducting state.
9. the test unit of the evaluation method of oil-soluble antisludging agent according to claim 2, it is characterized in that: the annular cross-sectional area between described incrustation testing tube [11] and the electrically heated rod [12]: the circulation area of associated line=2.0～10.0: 1.0, preferred 4.0～7.0: 1.0.
10. according to the test unit of the evaluation method of claim 2 or 6 or 9 described oil-soluble antisludging agents, it is characterized in that: described described dirt testing tube [11] is " U " shape pipe, electrically heated rod [12] is "T"-shaped structure, the lower heating of electrically heated rod partly places the incrustation testing tube, top is connected with the last end in contact of dirt testing tube and is in the sealing impaction state, is provided with pad [24] in the contact site.
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| CN103969152A (en) * | 2014-04-17 | 2014-08-06 | 广州特种承压设备检测研究院 | Scale and corrosion inhibitor performance testing device and detection method of scale and corrosion inhibitor performances |
| CN104267147A (en) * | 2014-09-02 | 2015-01-07 | 中国石油天然气股份有限公司 | Simulation device for evaluating deposition characteristic of polymer in oil field polymer-containing produced water heating furnace |
| CN104698124A (en) * | 2013-12-06 | 2015-06-10 | 中国石油天然气股份有限公司 | A dynamic scale inhibition rate tester |
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| CN113820241A (en) * | 2021-11-01 | 2021-12-21 | 中国石油化工股份有限公司 | Scale inhibitor performance evaluation device and method |
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Application publication date: 20110817 |