CN101576550B - Evaluation device and evaluation method for scale formation trend and scale inhibition effect - Google Patents
Evaluation device and evaluation method for scale formation trend and scale inhibition effect Download PDFInfo
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- CN101576550B CN101576550B CN2008100369928A CN200810036992A CN101576550B CN 101576550 B CN101576550 B CN 101576550B CN 2008100369928 A CN2008100369928 A CN 2008100369928A CN 200810036992 A CN200810036992 A CN 200810036992A CN 101576550 B CN101576550 B CN 101576550B
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Abstract
The invention discloses an evaluation device and an evaluation method for scale formation trend and scale inhibition effect. The principle is as follows: a sample is enabled to flow through a capillary with a constant pressure difference, and the scale formation trend of the sample is represented by the blockage condition of the capillary reflected by monitoring the attenuation of the flow rate ofthe sample in the capillary; and the scale inhibition performance of a physical measure and medicament is represented by a ratio of the accumulated outflow of a chemical or physical modified sample a nd the accumulated outflow of a bland sample under the same instantaneous outflow rate attenuating range. The evaluation device and the evaluation method for scale formation trend and scale inhibitioneffect are suitable for scale formation forecast of various liquid mediums in water treatment, petroleum exploitation, seawater desalination, petroleum processing and chemical production as well as s cale inhibition performance evaluation and selection of various physical and chemical scale inhibition measures.
Description
Technical field
The present invention relates to the dynamic evaluation method of a kind of liquid medium scaling tendency and scale inhibition effect, especially a kind ofly be used for estimating the multiple liquid medium scaling tendency of water treatment, oil exploitation, desalinization, petroleum refining and Chemical Manufacture, and the evaluating apparatus and the evaluation method thereof of various physics and chemical scale-inhibiting measure scale-inhibiting properties.
Background technology
In water treatment, oil exploitation, desalinization, petroleum refining and Chemical Manufacture, exist liquid conveying energy consumption organic because of deposition on inner-walls of duct and the heat exchange surface in a large number and/or that inorganic scale causes to increase, the problem that transport capacity descends and heat exchange efficiency descends, the economic loss highly significant that is caused.For this reason, in different industries, taked to add chemical modifications such as antisludging agent, paraffin inhibitor chemical, asphaltene dispersants respectively and handled means, and physical treatment means such as electronics, strong magnetic, ultrasound wave, electromagnetism are eliminated or alleviated the adverse effect that dirt fluid delivery and heat exchange cause at medium characteristics separately.Under this background, set up scaling tendency prediction of reliable and easy laboratory and evaluation of antisludging performance means, the scale problems that may occur for objective evaluation, preferably suitable scale inhibition agent and dosage thereof and proper physical scale inhibition means have important and practical meanings.
At present both at home and abroad used laboratory method can be divided into static state and dynamic two classes in inorganic scale prediction and evaluation of antisludging performance.
Static ratio juris is generally the scaling tendency that characterizes water sample by the loss amount of measuring calcium ions and magnesium ions in the front and back solution of aging a period of time of water sample, the scale-inhibiting properties that reflects chemical agent and physical method with the relative size of calcium ions and magnesium ions loss amount in the water sample after blank water sample and chemical modification or the physical treatment, its advantage is not for needing complicated experimental facilities, shortcoming is can not reflect from crystal to precipitate into the overall process that deposits at wall, the huge legendary turtle cooperation that particularly can only reflect antisludging agent is used, and can not reflect that it disperses and the distortion of lattice effect, and test result is subjected to impurity content in water sample and the medicament, the influence of water sample ageing process and analysis means is big, and repeatability is bad.
Dynamically ratio juris is generally with pump and makes water sample with constant rate circulation or disposable by the test pipeline section, characterize the scaling tendency of water sample by the increase amplitude of testing conduit wall thermal resistance and pipe ends pressure differential, the relative size that increases amplitude with blank water sample pipeline wall thermal resistance corresponding with chemical modification or physical treatment water sample or pressure differential reflects the scale-inhibiting properties of chemical agent and physical method, its advantage is can reflect the scaling tendency of water sample and the scale-inhibiting properties of chemical agent and physical method more reliably than static method, shortcoming is the experimental provision complex structure, involve great expense, be difficult to widespread use.
In addition, the somebody has proposed the assay method based on conductivity and pH variation, its principle is that component concentration, pH and the conductivity of aqueous solution in the crystallization process can change, speed by monitoring and relatively these variations can characterize out the scaling tendency of water sample and the scale-inhibiting properties of chemical agent and physical method, its advantage is that sense cycle is short, shortcoming is the peptizaiton that can not reflect antisludging agent, and range of application is restricted.
At present both at home and abroad used laboratory method also can be divided into static method and dynamic method two classes in organic deposition prediction and evaluation of antisludging performance.
Static ratio juris is by measuring sample sedimental amount of separating out of the change calculations of absorbance in ageing process, the particle size of particle or the scaling tendency that the sediment yield bottom the direct weighing container comes characterization sample are separated out in test, separate out and deposition with the sediment that blank sample is corresponding with sample after chemical modification or the physical treatment, the relative size of separating out the particle diameter of particle reflects the scale-inhibiting properties of chemical agent and physical method, its advantage is that required sample size is little, test period is short, shortcoming is directly to reflect sedimental actual fouling situation, needs to adopt expensive detecting instrument in the particle particle size determination.
Dynamically ratio juris makes sample contact with heat exchange surface for adopting pump recycle design or rotational shear mode, come the scaling tendency of characterization sample by the amount of scale buildup on the weighing heat exchange surface, reflect the scale-inhibiting properties of chemical agent and physical method with the relative size of the blank sample amount of scale buildup corresponding with chemical modification or physical treatment sample.In addition, also the someone has proposed to reflect the sample scaling tendency by measuring sample by the increase speed that heat exchange pipeline section pressure falls, and the relative size of the increase speed of falling with the blank sample heat exchange pipeline section pressure corresponding with chemical modification or physical treatment sample reflects the method for the scale-inhibiting properties of chemical agent and physical method.The advantage of dynamic method is the scaling tendency that can reflect sample reliably, and the scale-inhibiting properties of chemical agent and physical method, and shortcoming is that required sample size is big, and test period is long, and the experimental provision complex structure involves great expense.
Summary of the invention
In view of this, the purpose of this invention is to provide brief appraisal device and method of testing thereof that prediction of a kind of suitable inorganic scale and organic deposition and scale inhibition effect are estimated, under the prerequisite of damage appraisement result reliability not, reduce its complexity as far as possible, the restriction that reduces to use.
The present invention is that to solve the problems of the technologies described above the technical scheme that adopts be a kind of scaling tendency and scale inhibition effect evaluating apparatus, comprises that liquid provides container, liquid reception and measuring container and at least one kapillary.Liquid provides container that liquid sample is provided; Liquid receives and measuring container receives and the volume and/or the weight of measurement liquid sample; The kapillary entrance point is communicated with this liquid provides container, and endpiece is communicated with this liquid and receives and measuring container, to provide container to receive and measuring container conveying liquid to this liquid from this liquid under a constant pressure difference.
In above-mentioned scaling tendency and scale inhibition effect evaluating apparatus, also comprise a constant pressure difference holdout device, with so that described liquid provides in the container under the sample liquid level first pressure in somewhere to be constantly equal to that described liquid receives and second pressure of measuring container, wherein this first pressure is less than the 3rd pressure at described at least one entrance point capillaceous place, thereby keeps a constant pressure difference that equals the difference of the 3rd pressure and first pressure between described at least one two ends capillaceous.
In above-mentioned scaling tendency and scale inhibition effect evaluating apparatus, the constant pressure difference holdout device can comprise a gas equalizing line, the one end inserts sample liquid level that described liquid provides container down and be higher than described entrance point capillaceous, its other end is communicated with described liquid and receives and measuring container, and wherein said liquid provides container and described liquid to receive and measuring container is closed container.
In above-mentioned scaling tendency and scale inhibition effect evaluating apparatus, one of them is communicated with described gas equalizing line and atmosphere, source of the gas and vacuum system.
In above-mentioned scaling tendency and scale inhibition effect evaluating apparatus, described constant pressure difference holdout device comprises an air communicating pipe, the one end inserts sample liquid level that described liquid provides container down and be higher than described entrance point capillaceous, its other end is communicated with atmosphere, it is closed container that wherein said liquid provides container, and described liquid reception and measuring container are communicated with atmosphere.
In above-mentioned scaling tendency and scale inhibition effect evaluating apparatus, also comprise one first temperature regulating device, be constant temperature in order to keep described liquid that the fluid temperature in the container is provided.
In above-mentioned scaling tendency and scale inhibition effect evaluating apparatus, also comprise a stirring apparatus, in order to provide the liquid sample in the container to stir to described liquid.
In above-mentioned scaling tendency and scale inhibition effect evaluating apparatus, also comprise one second temperature regulating device, be constant temperature in order to keep the fluid temperature in the described kapillary.
The present invention also proposes a kind of scaling tendency and scale inhibition effect evaluation method, uses above-mentioned scaling tendency and scale inhibition effect evaluating apparatus to measure, and this method comprises: make described kapillary two ends set up constant pressure difference; And when described kapillary two ends reach constant pressure difference, begin to test and write down the sample size of different time capillary flow, and calculate the pairing discharge rate of variant sample size to liquid reception and measuring container; Wherein, come the scaling tendency of characterization sample with the instantaneous discharge rate attenuation under the difference accumulative total sample stream output, with chemistry or physical modification sample accumulative total discharge under the identical instantaneous discharge rate attenuation amplitude and the ratio sign physical measure of a reference coupon cumulative flow output and the scale-inhibiting properties of medicament.
In above-mentioned scaling tendency and scale inhibition effect evaluation method, the method that makes described kapillary two ends reach constant pressure difference comprises: utilize a gas equalizing line one end to insert sample liquid level that described liquid provides container down and be higher than described entrance point capillaceous, the other end is communicated with described liquid and receives and measuring container, and provide at described liquid under the condition of container and reception of described liquid and measuring container sealing, make liquid sample provide container to pass through described kapillary and flow into described liquid and receive and measuring container, a end under the liquid sample of the container bubble of emerging is provided described liquid and provides up to described gas equalizing line from described liquid.
In above-mentioned scaling tendency and scale inhibition effect evaluation method, the method that makes described kapillary two ends reach constant pressure difference comprises: utilize an air communicating pipe one end to insert liquid sample that described liquid provides container down and be higher than described kapillary and provide entrance point in the container at described liquid, the air communicating pipe other end is communicated with atmosphere, and under described liquid provides seal of vessel and described liquid reception and measuring container and condition that atmosphere is communicated with, make liquid sample provide container to pass through described kapillary and flow into described liquid and receive and measuring container, a end under the liquid sample of the container bubble of emerging is provided described liquid and provides up to described air communicating pipe from described liquid.
In above-mentioned scaling tendency and scale inhibition effect evaluation method, be included in also in the measuring process that to keep described liquid generator and described kapillary be constant temperature.
The present invention is owing to adopt above technical scheme, make it compared with prior art, has following beneficial effect: the invention provides brief appraisal device and method of testing thereof that prediction of a kind of suitable inorganic scale and organic deposition and scale inhibition effect are estimated, can dope the scaling tendency of multiple liquid medium reliably, and the scale-inhibiting properties of physical measure and medicament, under the prerequisite of damage appraisement result reliability not, the structure of proving installation is simplified significantly, but range of application is wider.
Description of drawings
For above-mentioned purpose of the present invention, feature and advantage can be become apparent, below in conjunction with accompanying drawing the specific embodiment of the present invention is elaborated, wherein:
Fig. 1 is Prediction of Fouling and scale inhibition effect evaluating apparatus synoptic diagram according to an embodiment of the invention.
Fig. 2 is Prediction of Fouling and scale inhibition effect evaluating apparatus synoptic diagram in accordance with another embodiment of the present invention.
Embodiment
Principle of the present invention flows through kapillary for making sample with constant pressure difference, by the scaling tendency of the kapillary stopping state characterization sample that decay reflected of sample flow in the monitoring kapillary; In addition, characterize the scale-inhibiting properties of physical measure and medicament with the ratio of chemistry or physical modification sample accumulative total discharge and blank sample cumulative flow output under the identical instantaneous discharge rate attenuation amplitude.
With reference to shown in Figure 1, scaling tendency of the present invention and scale inhibition effect evaluating apparatus comprise that the kapillary 5 (shown in the figure one) and a liquid of a container 2 of storing and provide liquid 21, one first temperature regulating device 1, a gas equalizing line 4, one or more circulating liquids receive and measuring container 6.Container 2 bottoms have the adapter 20 of flowing out for sample, and kapillary 5 is installed in it, and kapillary 5 inlet end 5a are positioned at liquid sample 21, and endpiece 5b is communicated to liquid and receives and measuring container 6.
In the container 2 stirring apparatus 3 can be set, it is mainly used in and prevents to separate out in the sample 21 deposition of particle at container bottom, also can play simultaneously sample mixed is acted on uniformly.
As an example, it is poor that gas equalizing line 4 is used to provide the constant pressure at kapillary 5 two ends.Gas equalizing line 4 one end 4a are deep under the liquid level of sample, other end 4b places in liquid reception and the measuring container 6, connection can one of them be connected gas equalizing line 4 with atmosphere, source of the gas and vacuum system, its difference is to control different gaseous pressures and gas phase atmosphere, and test condition and actual production or natural process are consistent.When gas equalizing line 4 is connected with atmosphere, turn down by the duct that will be communicated with atmosphere, can reduce sample volatilization loss.
The liquid that has inserted gas equalizing line 4 provides container 2 can entire body transparent, also can be local transparent, as long as can clearly observe the lower end of inserting the gas equalizing line in the sample.
Under the constant condition of pressure at two ends difference, the main effect of kapillary 5 is for the sample circulation and the deposition surface of foulant in the sample is provided, and the scaling tendency of the metering function reflection sample that dwindling of kapillary 5 internal diameters caused of the deposition by foulant.Liquid receives and measuring container 6 also is a closed container, it mainly acts on is to store and measure by sample size capillaceous, liquid receives and measuring container 6 both can adopt the volume mode to measure sample size (as marking scale thereon), also can adopt the mass metrology mode.
In addition, second temperature regulating device 7 can be set outside kapillary 5, it is mainly used in the temperature of sample in the control kapillary 5.Under need the situation for the evaluation of the fouling that is caused by thermograde, second temperature regulating device 7 also can be used for the thermograde that provides required.
Compare with the scale inhibition effect evaluation method with existing scaling tendency, the remarkable difference of scaling tendency among the present invention and scale inhibition effect evaluation method and device is to remain in the test process constant pressure differential at kapillary two ends.
Illustrate at first that below gas equalizing line makes kapillary 5 two ends have the principle of constant pressure difference.When initial, there is fluid pressure in gas equalizing line 4 end 4a in sample, there is liquid to flow out in kapillary 5 exits, because container 2 is airtight (except kapillary and gas equalizing lines), after capillary outlet has liquid to flow out, volume in debt can only discharge gas by gas equalizing line 4 end in sample 21 and replenish, begin to have bubble to discharge up to gas equalizing line 4 end 4a in sample 21, so just make gas equalizing line 4 in sample one section all be full of (certain vacuum is formed at container 2 tops) by gas.Under this state, the gas equilibrium intraductal atmospheric pressure equates with the fluid pressure at one end 4a place.According to the hydrostatics principle, the gaseous tension that is interconnected equates everywhere.In addition, liquid receiving vessel 6 only is communicated with container 2 by gas equalizing line 4, and other parts are airtight.So the liquid receiving vessel 6 interior pressure (being called second pressure at this) that gas equalizing line 4 other end 4b are connected equate with the fluid pressure (being called first pressure at this) at an end 4a place.
Learn easily by said process, the constant compression force difference is to be determined by gas equalizing line 4 lower ends and the difference in height Δ H between the kapillary entrance point that are inserted among Fig. 1 in the sample between the two ends of kapillary 5: if do not consider the capillarity at capillary outlet place, according to the hydrostatics principle, the fluid pressure that is inserted into the gas equalizing line lower end in the sample equates that with the fluid pressure at capillary outlet place then the fluid pressure (being called the 3rd pressure at this) at place, capillary inlet and the pressure differential Δ P of capillary outlet place liquid are under capillary water placing flat situation:
Δ P=ρ
SampleG Δ H (1)
ρ wherein
Sample---the density of sample, unit is kg/m
3
G---acceleration of gravity, its value is 9.80665m/s
2
Difference in height between Δ H-gas equalizing line one end 4a and the capillary inlet 5a, unit is m.
Under horizontal with capillary tube or non-horizontal mode placement situation, the relational expression that all can be obtained between sample discharge rate and the capillary size by the Bernouli equation is as follows:
Q=π ρ
SampleG Δ Hd
In 4/ 128 η
SampleL (2)
Wherein Q-is by sample flow capillaceous, and unit is m
3/ s;
d
In-internal diameter capillaceous, unit is m;
η
SampleThe dynamic viscosity of sample in the-kapillary, unit is Pas;
L-length capillaceous, unit is m.
By (2) formula as seen, be directly proportional with 4 powers of capillary inner diameter by snap sample flow capillaceous, thus capillary inner diameter reduce slightly just can be reflected in the decay of instantaneous delivery.For example, the attenuation amplitude of instantaneous delivery just can reach 34.39% when capillary inner diameter reduces 10%, and the attenuation amplitude of instantaneous delivery just can reach 82.15% when capillary inner diameter reduces 35%.
In the above embodiments, be to describe as the constant pressure difference holdout device, yet this is not construed as limiting with gas equalizing line 4.In the present invention, essence is to make the pressure of liquid reception and measuring container 6 be constantly equal to the pressure that liquid provides a certain position that is higher than kapillary entrance point 5a place in the container 2, thereby the differential water pressures that the difference in height Δ H between this position and the entrance point 5a is caused then provides the constant pressure difference at kapillary two ends.The principle that the above embodiment of following basis is disclosed is described for an embodiment again.
Fig. 2 be another embodiment of the present invention the device synoptic diagram, wherein identical with last embodiment label is represented components identical, does not repeat them here.Difference is, replace above-mentioned gas equalizing line 4 as the constant pressure difference holdout device by air communicating pipe 8, the one end 8a insertion liquid of air communicating pipe 8 provides the sample liquid level of container 2 to descend and be higher than the entrance point 5a of kapillary 5, other end 8b directly is communicated with atmosphere, and liquid provide container 2 still with isolated from atmosphere (promptly airtight).In addition, liquid receiving vessel 6a also directly is communicated with atmosphere.Therefore the pressure at other end 8b place is constantly equal to liquid receiving vessel 6a internal pressure.The higher liquid that makes of fluid pressure flows to liquid receiving vessel 6a through kapillary 5 in the container 2 because of liquid provides in the early stage, after the other end 8b of air communicating pipe 8 is emerged bubble, promptly can set up constant pressure difference at kapillary 5 two ends.
Present embodiment is compared last embodiment, and structure is more simple, thereby easier realization.Lose under not serious or the acceptable situation at sample evaporation, present embodiment is compared last embodiment and is had superiority.
After understanding spirit of the present invention, those skilled in the art also can design other structure and set up constant pressure difference, as long as it is contained within the scope of the invention.
With description embodiment illustrated in fig. 1 scaling tendency of the present invention and scale inhibition effect evaluation method, it comprises following concrete steps below:
In the adapter of transparent vessel bottom, kapillary is installed, add sample to be evaluated therein, one end of gas equalizing line is inserted into liquid level top in the transparent vessel, its other end is inserted into liquid to be received and measuring apparatus top, gas equalizing line is communicated with atmosphere, vacuum system or source of the gas, starts stirring apparatus and temperature regulating device;
When specimen temperature reaches predetermined value, one end of gas equalizing line is inserted into the correct position of liquid level below in the transparent vessel, explanation according to preamble, capillary outlet end 5b begins trickle, outflow along with liquid, the liquid that gas equalizing line 4 is inserted in the sample 21 is discharged from gradually, all discharges back one end 4a to liquid and has bubble release.This end 4a begins to discharge bubble and is actually the signal that gas equalizing line 4 is all occupied by gas, the signal of kapillary 5 two ends constant-pressure drops foundation just.
After constant-pressure drop is set up, one end 4a begins to discharge bubble start of record to start with gas equalizing line, begin to test and write down the sample size that the different time capillary end flows out, calculating capillary end outflow sample size obtains the pairing discharge rate of various sample discharge to the first order derivative of time.
Come the scaling tendency of characterization sample with the instantaneous discharge rate attenuation under the difference accumulative total sample stream output, with chemistry or physical modification sample accumulative total discharge under the identical instantaneous discharge rate attenuation amplitude and the ratio sign physical measure of reference coupon (as blank sample) cumulative flow output and the scale-inhibiting properties of medicament.
Below in conjunction with specific embodiment evaluation method and device of the present invention are described further, in the following embodiments, embodiment 1 and embodiment 2 are according to structure evaluating apparatus embodiment illustrated in fig. 2, embodiment 3 and embodiment 4 are according to structure evaluating apparatus embodiment illustrated in fig. 1, please refer to following each embodiment of reading illustrated in figures 1 and 2.
Capacity is on the glass tubualted bottle outlet valve rear tube of 2500ml emulsion tube to be installed, and plugs the stainless steel capillary that 5 sizes are respectively φ 2.0mm * 215mm, φ 1.6mm * 100mm, φ 0.9mm * 82mm, φ 0.6mm * 28mm, φ 0.5mm * 28mm on emulsion tube simultaneously; It is on the magnetic stirring apparatus of 25 ℃ of air baths that the glass tubualted bottle is placed temperature, adds the magnetic stir bar that is of a size of φ 8mm * 50mm therein, respectively places a glass cylinder below each stainless steel capillary end; With deionized water, concentration is that 1% aqueous sodium carbonate and mass concentration are that to place water temperature be 25 ℃ water-bath preheating 30min for 1% calcium chloride water; Add the 25ml mass concentration successively and be 1% aqueous sodium carbonate in the glass tubualted bottle, 2425ml deionized water and 50ml mass concentration are 1% calcium chloride water, start magnetic stirring apparatus and begin to stir with the rotating speed of 300r/min; The 16# plug that will be inserted with φ 7mm * 400mm glass tube covers on the glass tubualted bottle; Open the switch of glass tubualted bottle, wait 5 capillary ends all to have and fall behind the insertion depth of regulating plug upper glass pipe under the water droplet, the difference in height that makes glass tube lower end and stainless steel capillary end is 140mm; After treating that the glass tube lower end begins to discharge bubble, pick up counting and write down the initial water yield in 5 graduated cylinders; Water yield during beginning in glass cylinder of 5min record, after the water yield in the glass cylinder surpasses 100ml, every the 100ml capacity is once each instantaneous the rate of output water capillaceous of the graduated cylinder of 5ml and stopwatch test, after test is finished the water sample in the graduated cylinder is poured in the graduated cylinder under the kapillary.
The instantaneous the rate of output water of each kapillary by the above-mentioned steps test sees Table 1 with the attenuation that the water outlet volume increases.
Table 1: the instantaneous delivery of blank sample in kapillary is with flowing out the attenuation that volume of sample increases.
By the test data in the table 1 as seen, there is the difference of highly significant in the kapillary of different-diameter to the sensitivity of dirt deposition thing, diameter is that 3 above kapillaries of 0.9mm are very low to the susceptibility that is deposited on dirt deposition thing wherein, and the attenuation amplitude that reaches momentary rate under the situation of 200ml at kapillary water outlet volume is all less than 15%; Just reach 91% and diameter is the momentary rate attenuation amplitude of kapillary when aquifer yield just reaches 4.6ml of 0.5mm, the test duration is 30min, the dirt deposition thing is crossed be sensitivity; Diameter is that the momentary rate attenuation amplitude of kapillary when aquifer yield is 58.3ml of 0.6mm is 81%, and the test duration is 75min.Consideration reduces with capillary diameter, although its susceptibility to the dirt deposition thing is remarkable, but when capillary diameter is separated out 6 times of particle diameter in less than sample, test result is subjected to some stochastic factor will be excessive, cause the collimation of test result significantly to descend, therefore under sample size and test duration can received situations, should select large diameter kapillary for use as far as possible.3 kapillaries of diameter more than 0.9mm in this example are because internal diameter is too big, too little to wherein dirt deposition thing susceptibility, the sample size of testing significant momentary rate attenuation amplitude needs is too big, diameter is that the kapillary of 0.5mm is because too small dirt deposition thing is wherein then crossed of internal diameter is sensitivity, aquifer yield is too small, having only diameter is that the internal diameter capillaceous of 0.6mm is the most suitable, only consuming the momentary rate attenuation amplitude that just can test under 58ml sample and the 75min situation consuming time above 80%, can ensure that also the sample discharge rate is only low simultaneously.
Be on the glass tubualted bottle outlet valve rear tube of 2500ml emulsion tube to be installed at capacity, on emulsion tube, plug the stainless steel capillary that is of a size of φ 0.6mm * 28mm; It is on the magnetic stirring apparatus of 25 ℃ of air baths that the glass tubualted bottle is placed temperature, adds the magnetic stir bar that is of a size of φ 8mm * 50mm therein, places a glass cylinder below the stainless steel capillary end; With deionized water, concentration is that 1% aqueous sodium carbonate and mass concentration are that to place water temperature be 25 ℃ water-bath preheating 30min for 1% calcium chloride water; In the glass tubualted bottle, add the 25ml mass concentration successively and be 1% aqueous sodium carbonate, 1.25ml mass concentration and be 1% ATMP (ATMP) aqueous solution, 2424ml deionized water and 50ml mass concentration and be 1% calcium chloride water, start magnetic stirring apparatus and begin to stir with the rotating speed of 300r/min; The 16# plug that will be inserted with φ 7mm * 400mm glass tube covers on the glass tubualted bottle; Open the switch of glass tubualted bottle, wait capillary end to have and fall behind the insertion depth of regulating plug upper glass pipe under the water droplet, the difference in height that makes glass tube lower end and stainless steel capillary end is 140mm; After treating that the glass tube lower end begins to discharge bubble, pick up counting and write down the initial water yield in the graduated cylinder; Water yield during beginning in glass cylinder of 5min record, after the water yield in the glass cylinder surpasses 100ml, every the 100ml capacity is once each instantaneous the rate of output water capillaceous of the graduated cylinder of 5ml and stopwatch test, after test is finished the sample in the graduated cylinder is poured in the graduated cylinder under the kapillary.
The instantaneous the rate of output water of kapillary by the above-mentioned steps test sees Table 2 with the attenuation that the water outlet volume increases.
Table 2: the instantaneous delivery of dosing sample in kapillary is with flowing out the attenuation that volume of sample increases
| Accumulated outflow ml | Instantaneous the rate of output water ml/min | Instantaneous the rate of output water attenuation amplitude % |
| 0 | 1.4 | 0.0 |
| 7 | 1.4 | 0.0 |
| 14 | 1.4 | 0.0 |
| 21 | 1.38 | 1.4 |
| 27.9 | 1.34 | 4.3 |
| 34.6 | 1.36 | 2.9 |
| 41.4 | 1.34 | 4.3 |
| 48.1 | 1.35 | 3.6 |
| 100 | 1.35 | 3.6 |
| 200 | 1.35 | 3.6 |
| 300 | 1.33 | 5.0 |
| 400 | 1.35 | 3.6 |
| 500 | 1.33 | 5.0 |
| Accumulated outflow ml | Instantaneous the rate of output water ml/min | Instantaneous the rate of output water attenuation amplitude % |
| 600 | 1.36 | 2.9 |
As seen test data by the stainless steel capillary of φ 0.6mm * 28mm in data in the table 2 and the table 1 contrasts, increase 5mg/l antisludging agent ATMP (ATMP) in the sample in embodiment 1, can significantly reduce the scaling tendency of sample, not adding the momentary rate attenuation amplitude of agent sample when the sample stream output is 58.3ml among the embodiment 1 is 81%, have only 2.9% and add the momentary rate attenuation amplitude of agent sample when discharge reaches 600ml among the embodiment 2, show in sample, to add 5mg/l antisludging agent ATMP (ATMP) can to make it be that 80% o'clock cumulative flow output reaches more than 10 times of blank sample by momentary rate attenuation amplitude capillaceous.
Test data among embodiment 1 and the embodiment 2 and contrast thereof show that the scaling tendency and the scale inhibition effect evaluation method that provide among the present invention are applicable to that inorganic scale is predicted and the evaluation of scale inhibition effect.
With one kind of 2500ml dewater gas-free oil in 80 ℃ water-bath airtight heating 48h (hour) be placed in 60 ℃ of water-baths and leave standstill 12h; Be on the glass tubualted bottle outlet valve rear tube of 2500ml silicone tube to be installed with capacity, on silicone tube, plug the stainless steel capillary that is of a size of φ 2.0mm * 215mm; It is on the magnetic stirring apparatus that has heating function of 36 ℃ of air baths that the glass tubualted bottle is placed temperature, add the magnetic stir bar that is of a size of φ 8mm * 50mm therein, the stainless steel capillary end is passed the top that a capacity is the plastic cylinder of 10ml, the plug that is inserted with φ 7mm glass tube is covered on plastic cylinder; Oil sample is poured in the glass tubualted bottle, started magnetic stirring apparatus and begin to stir with the rotating speed of 300r/min; The 16# plug that will be inserted with φ 7mm * 400mm glass tube and magnetic stirring apparatus temperature probe covers on the glass tubualted bottle, and setting the control temperature is 55 ℃; With emulsion tube connect be inserted in the glass tubualted bottle and plastic cylinder in φ 7mm glass tube; Treat to open when the oil sample temperature is reduced to 55 ℃ in the glass tubualted bottle switch of glass tubualted bottle, the insertion depth that falls behind adjusting plug upper glass pipe under the oil droplet is arranged and its end tightly is posted on the tubualted bottle wall Deng capillary end, the difference in height that makes glass tube lower end and stainless steel capillary end is 140mm; After treating that the glass tube lower end begins to discharge bubble, pick up counting and write down initial oil mass in the plastic cylinder, the oil mass in plastic cylinder of 5min record.
The instantaneous fuel-displaced speed of kapillary by the above-mentioned steps test sees Table 3 with the attenuation that goes out the oil volume increase.
Table 3: the attenuation that the instantaneous delivery of blank oil sample in kapillary increases with the oil sample elution volume
| Accumulation output ml | Instantaneous fuel-displaced speed ml/min | Instantaneous fuel-displaced speed attenuation amplitude % |
| 0.0 | 0.33 | 0.0 |
| 1.7 | 0.33 | 0.0 |
| 3.3 | 0.32 | 3.0 |
| Accumulation output ml | Instantaneous fuel-displaced speed ml/min | Instantaneous fuel-displaced speed attenuation amplitude % |
| 4.9 | 0.28 | 15.2 |
| 6.3 | 0.20 | 39.4 |
| 7.3 | 0.14 | 57.6 |
| 8.0 | 0.10 | 69.7 |
| 8.5 | 0.06 | 81.8 |
| 8.8 | 0.04 | 87.9 |
| 9.0 | 0.02 | 93.9 |
By in the table 3 as seen, very fast in the wax deposition speed under 36 ℃ of its GB freezing point temperatures through 80 ℃ of heat treated crude oil, the throughput in φ 2.0mm * 215mm kapillary only is that the attenuation amplitude of its instantaneous discharge rate just reaches 81.8% under the situation of 8.5ml.
It is that 80 ℃ the airtight heating of water-bath 48h is placed on 60 ℃ of water-baths and leaves standstill 12h that 2460ml embodiment 3 described dehydration gas-free oils are placed water temperature; Be on the glass tubualted bottle outlet valve rear tube of 2500ml silicone tube to be installed with capacity, on silicone tube, plug the stainless steel capillary that is of a size of φ 2.0mm * 215mm; It is on the magnetic stirring apparatus that has heating function of 36 ℃ of air baths that the glass tubualted bottle is placed temperature, add the magnetic stir bar that is of a size of φ 8mm * 50mm therein, the stainless steel capillary end is passed the top that a capacity is the plastic cylinder of 250ml, the plug that is inserted with φ 7mm glass tube is covered on plastic cylinder; Oil sample is poured in the glass tubualted bottle, and adding 40ml concentration again is the xylene solution of poly-acetic acid-vinyl acetate (EVA, the trade mark are 28/3) of 1% (m/v); Starting magnetic stirring apparatus begins to stir; The 16# plug that will be inserted with φ 7mm * 400mm glass tube and magnetic stirring apparatus temperature probe covers on the glass tubualted bottle, and setting the control temperature is 55 ℃; Connect the φ 7mm glass tube that is inserted in glass tubualted bottle and the plastic cylinder with emulsion tube; Treat to open when the oil sample temperature is reduced to 55 ℃ in the glass tubualted bottle switch of glass tubualted bottle, the insertion depth that falls behind adjusting plug upper glass pipe under the oil droplet is arranged and its end tightly is posted on the tubualted bottle wall Deng capillary end, the difference in height that makes glass tube lower end and stainless steel capillary end is 140mm; After treating that the glass tube lower end begins to discharge bubble, pick up counting and write down initial oil mass in the plastic cylinder, the oil mass in plastic cylinder of 5min record.
The instantaneous fuel-displaced speed of kapillary by the above-mentioned steps test sees Table 4 with the attenuation that goes out the oil volume increase.
Table 4: add the attenuation that the instantaneous delivery of agent oil sample in kapillary increases with the oil sample elution volume
| Accumulation output ml | Instantaneous fuel-displaced speed ml/min | Instantaneous fuel-displaced speed attenuation amplitude % |
| 0.0 | 1.65 | 0.00 |
| 8.2 | 1.63 | 1.21 |
| 16.4 | 1.62 | 1.82 |
| 24.5 | 1.62 | 1.82 |
| 32.6 | 1.62 | 1.82 |
| 40.7 | 1.60 | 3.03 |
| 48.7 | 1.60 | 3.03 |
| 56.7 | 1.58 | 4.24 |
| 64.6 | 1.58 | 4.24 |
| 72.5 | 1.60 | 3.03 |
| 80.5 | 1.58 | 4.24 |
| 88.4 | 1.58 | 4.24 |
| 96.3 | 1.56 | 5.45 |
By the contrast of the test data in table 4 and the table 3 as seen, in through 80 ℃ of heat treated crude oil, add the poly-acetic acid-vinyl acetate (EVA of 200mg/l, the trade mark is 28/3) can significantly weaken its wax deposition trend, not adding the momentary rate attenuation amplitude of agent sample when discharge only is 8.5ml among the embodiment 3 is 81.8%, have only 4.24% and add the momentary rate attenuation amplitude of agent sample when discharge reaches 88.4ml among the embodiment 4, show and in sample, add the poly-acetic acid-vinyl acetate (EVA, the trade mark are 28/3) of 160mg/l paraffin inhibitor chemical can to make it be that 80% o'clock cumulative flow output reaches more than 10 times of blank sample by momentary rate attenuation amplitude capillaceous.
Test data among embodiment 3 and the embodiment 4 and contrast thereof show that the scaling tendency and the scale inhibition effect evaluation method that provide among the present invention are applicable to that organic deposition is predicted and the evaluation of scale inhibition effect.
In sum, the invention provides brief appraisal device and method of testing thereof that prediction of a kind of suitable inorganic scale and organic deposition and scale inhibition effect are estimated, liquid integrated flow capillaceous by two ends being applied constant pressure difference and moment flow velocity measurement, can dope the scaling tendency of multiple liquid medium reliably, and the scale-inhibiting properties of physical measure and medicament, under the prerequisite of damage appraisement result reliability not, the structure of proving installation is simplified significantly, but range of application is wider.
Though the present invention discloses as above with preferred embodiment; right its is not in order to qualification the present invention, any those skilled in the art, without departing from the spirit and scope of the present invention; when can doing a little modification and perfect, so protection scope of the present invention is when with being as the criterion that claims were defined.
Claims (11)
1. scaling tendency and scale inhibition effect evaluating apparatus comprise:
Liquid provides container, and liquid sample is provided;
Liquid receives and measuring container, receives and measure the volume and/or the weight of liquid sample;
At least one kapillary, its entrance point is communicated with this liquid provides container, and its endpiece is communicated with this liquid and receives and measuring container, to provide container to receive and measuring container conveying liquid to this liquid from this liquid under a constant pressure difference;
Also comprise a constant pressure difference holdout device, with so that described liquid provides in the container under the sample liquid level first pressure in somewhere to be constantly equal to that described liquid receives and second pressure of measuring container, wherein this first pressure is less than the 3rd pressure at described at least one entrance point capillaceous place, thereby keeps a constant pressure difference that equals the difference of the 3rd pressure and first pressure between described at least one two ends capillaceous.
2. scaling tendency as claimed in claim 1 and scale inhibition effect evaluating apparatus, it is characterized in that: described constant pressure difference holdout device comprises a gas equalizing line, the one end inserts sample liquid level that described liquid provides container down and be higher than described entrance point capillaceous, its other end is communicated with described liquid and receives and measuring container, and wherein said liquid provides container and described liquid to receive and measuring container is closed container.
3. scaling tendency as claimed in claim 2 and scale inhibition effect evaluating apparatus is characterized in that: one of them is communicated with described gas equalizing line and atmosphere, source of the gas and vacuum system.
4. scaling tendency as claimed in claim 1 and scale inhibition effect evaluating apparatus, it is characterized in that: described constant pressure difference holdout device comprises an air communicating pipe, the one end inserts sample liquid level that described liquid provides container down and be higher than described entrance point capillaceous, its other end is communicated with atmosphere, it is closed container that wherein said liquid provides container, and described liquid reception and measuring container are communicated with atmosphere.
5. scaling tendency as claimed in claim 1 and scale inhibition effect evaluating apparatus is characterized in that: also comprising one first temperature regulating device, is constant temperature in order to keep described liquid that the fluid temperature in the container is provided.
6. scaling tendency as claimed in claim 1 and scale inhibition effect evaluating apparatus is characterized in that: also comprise a stirring apparatus, in order to provide the liquid sample in the container to stir to described liquid.
7. scaling tendency as claimed in claim 1 and scale inhibition effect evaluating apparatus is characterized in that: also comprising one second temperature regulating device, is constant temperature in order to keep the fluid temperature in the described kapillary.
8. scaling tendency and scale inhibition effect evaluation method use described scaling tendency of claim 1 and scale inhibition effect evaluating apparatus to measure, and this method comprises:
Make described kapillary two ends set up constant pressure difference; And
When described kapillary two ends reach constant pressure difference, begin to test and write down the sample size of different time capillary flow, and calculate the pairing discharge rate of variant sample size to liquid reception and measuring container;
Wherein, come the scaling tendency of characterization sample with the instantaneous discharge rate attenuation under the difference accumulative total sample stream output, with chemistry or physical modification sample accumulative total discharge under the identical instantaneous discharge rate attenuation amplitude and the ratio sign physical measure of reference coupon accumulative total discharge and the scale-inhibiting properties of medicament.
9. scaling tendency as claimed in claim 8 and scale inhibition effect evaluation method, it is characterized in that, the method that makes described kapillary two ends reach constant pressure difference comprises: utilize a gas equalizing line one end to insert sample liquid level that described liquid provides container down and be higher than described entrance point capillaceous, the other end is communicated with described liquid and receives and measuring container, and provide at described liquid under the condition of container and reception of described liquid and measuring container sealing, make liquid sample provide container to pass through described kapillary and flow into described liquid and receive and measuring container, a end under the liquid sample of the container bubble of emerging is provided described liquid and provides up to described gas equalizing line from described liquid.
10. scaling tendency as claimed in claim 8 and scale inhibition effect evaluation method, phase is characterised in that, the method that makes described kapillary two ends reach constant pressure difference comprises: utilize an air communicating pipe one end to insert liquid sample that described liquid provides container down and be higher than described kapillary and provide entrance point in the container at described liquid, the air communicating pipe other end is communicated with atmosphere, and under described liquid provides seal of vessel and described liquid reception and measuring container and condition that atmosphere is communicated with, make liquid sample provide container to pass through described kapillary and flow into described liquid and receive and measuring container, a end under the liquid sample of the container bubble of emerging is provided described liquid and provides up to described air communicating pipe from described liquid.
11. scaling tendency as claimed in claim 8 and scale inhibition effect evaluation method is characterized in that, are included in also in the measuring process that to keep described liquid generator and described kapillary be constant temperature.
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| CN104023545A (en) * | 2011-12-22 | 2014-09-03 | 利乐拉瓦尔集团及财务有限公司 | A method for monitoring the operation of a liquid food processing system |
| CN104237455B (en) * | 2013-06-18 | 2017-09-08 | 中国石油天然气股份有限公司 | Flue Gas Expander Fouling in Fcc Unit is predicted and evaluation of anti-scale experimental facilities |
| CN104343427B (en) * | 2013-07-24 | 2016-11-09 | 中国石油化工股份有限公司 | A kind of prediction CO2the method of oil reservoirs inorganic scaling trend |
| US11125735B2 (en) * | 2017-03-30 | 2021-09-21 | Championx Usa Inc. | Dynamic wax deposition testing systems and methods |
| CN108732304A (en) * | 2018-04-12 | 2018-11-02 | 西南石油大学 | A kind of non-metallic pipe pipe water delivery dynamic scale formation experiment circuit and method |
| CN109342258A (en) * | 2018-11-27 | 2019-02-15 | 上海电力学院 | A kind of evaluation method of heat exchange metal surface scale-inhibiting properties |
| CN110376337A (en) * | 2019-08-19 | 2019-10-25 | 兖矿水煤浆气化及煤化工国家工程研究中心有限公司 | A kind of capillary dynamic pressure difference scale inhibition instrument |
| CN110793878A (en) * | 2019-10-24 | 2020-02-14 | 江门联福广科新材料科技有限公司 | Method for testing performance of scale-inhibiting filter material |
| CN113340762B (en) * | 2020-03-02 | 2023-10-31 | 中国石油天然气股份有限公司 | Corrosion and scaling detection device and method |
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| DE3933798C2 (en) * | 1989-10-10 | 1999-02-04 | Dietrich Dr Rer Nat Frahne | Arrangement for testing the effectiveness of physical measures to prevent scale deposits in water-bearing systems |
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