CN2896281Y - Preise testing device for pour point of petroleum product - Google Patents

Abstract

The utility model relates to an accurate pour point testing device for the test not included in the other type and the petroleum products pertaining to the field of petroleum industry technology which is composed by an out-wrapped circulation water jacket [2] connected with a hot water inlet [1], a hot water outlet [6] and a program-controlled water bath and the bottom center of the oil tank [30] is provided with a pipe section that is connected to the miniature measuring pump [26] through the oil tank outlet valve [29]. The outlet of the miniature measuring pump [26] is connected to the ring pipeline [27] and communicated with the pipeline at the top of the oil tank [30]. At the outlet of the miniature measuring pump [26] on the ring pipeline [27], a plurality of orifices are opened up and is connected with a plurality of sample container valves [25], [24], [23], [22] and [21] in series. After entering the cold bath [8], the orifices are connected by the hose [11] respectively to the bottom of a sample container [10] in the cold/hot bath [8]. One side of the cold/hot bath [8] is connected with a cold/hot coil [7] that is connected with a temperature-control water bath, is filled with the cold/hot liquid therein and is provided with a thermometer [4] on the top. The device is characterized in that the operation is easy and convenient, the testing oil sample has not history of structural damage, the precision is high and the repeatability is good.

Description

The accurate proving installation of petroleum products pour point

Technical field

The utility model is the accurate proving installation of the petroleum products pour point of test petroleum products pour point, relates to test not to be covered of other class and petroleum industry technical field.

Background technology

Pour point be petroleum products under regulation test apparatus and condition, be cooled to slowly be warmed to the minimum temperature that begins to flow after liquid does not flow.For industrial pipe laying, the petroleum sneeze-point temperature is meant that the crude oil that solidifies attitude in the pipeline begins to melt mobile minimum temperature.For scientific experiment, the crude oil modified pour point is to embody the crucial technical indicator of oil product different disposal effect, and what its was represented is after crude oil modified is cooled to uniform temperature, heats up the minimum temperature that can flow under rated condition.And crude oil modified is meant the crude oil after methods such as bakingout process and adding pour-point depressant or pour-point depressant change its original rheological characteristics, and its test result will directly instruct oil transportation production.Test procedure requires will judge and thermometric its mobility status every 2 ℃ in the world, but because the oil transport line is very long, the every intensification of crude oil just needs a large amount of energy for 1 ℃, so the precision that pour point temperature is measured is of great importance to oil field energy saving.

According to State Standard of the People's Republic of China " petroleum sneeze-point determination method " GB/T3535-83 (91), the assay method of petroleum sneeze-point is defined as: will clean sample and pour test tube into to the groove place, clog test tube with the cork that is inserted with cloud point and pour point temperature meter, then the sample in the test tube is carried out pre-service, make sample under the situation of not stirring, be heated to above certain temperature of sample expection pour point, if the expection pour point is higher than 33 ℃, then will heat the back sample and in air or about 25 ℃ of water-baths, be cooled to 36 ± 1 ℃, if the expection pour point is between 33～-33 ℃, then need not cooling processing, if the expection pour point is lower than-33 ℃, then needs to use the water-bath of relatively lower temp to be about to sample earlier and be cooled to 15 ± 1 ℃.Through after the above pre-service, dry test-tube is put into sleeve pipe, and stably be contained on the upright position of cryostat, make sleeve pipe expose the heat eliminating medium liquid level and be not more than 25 millimeters, sample is through enough coolings, keep 5 seconds of horizontal level and sample does not have when mobile up to test tube, write down observed test temperature meter reading, this reading is added 3 ℃ of results as pour point on the sample.Following pour point then is heating sample to 105 under condition of stirring ± 1 ℃, and pours test tube into, is cooled to be higher than certain temperature of sample expection pour point then, and the method for testing of pour point obtains down the test result of pour point in the employing.But there are some researches show that the relation of condensation point and pour point neither has parallel consistance, " the differing 3 ℃ " of stipulating in neither standard is so simple, so the pour point of crude oils method of testing of existing national Specification lacks scientific.And according to People's Republic of China's oil and gas industry standard " crude oil modified pour point measurement fusion method " (SY7516-92), its crude oil modified pour point measurement method is defined as: sample is poured in vitro to annular graticule place, clog test tube with the cork that has the condensation point thermometer, thermometer is fixed on test tube central authorities, makes mercury bulb apart from the pipe end 8～10mm.Two test tubes of each specimen preparation.If the pour point of sample is at-5～10 ℃, the cold-trap with two test tube vertical putting into-12 that sample and thermometer be housed ℃ when treating that specimen temperature arrives-10 ℃, takes out test tube, dries outer wall and adds sleeve pipe immediately, is placed on the casing support that can make sleeve pipe inclination miter angle.Connect adjustable electric furnace, sample is heated up with the speed of 1 ℃/min, when specimen temperature be raised to estimate pour point before 5～10 ℃ the time, every interval is alternately taken out test tube for 2 ℃ and is observed, and keeps the upright position to observe 5 seconds in test tube, if the not mobile sign in oil sample surface, can be with the tube back original position, continue to heat up, mobile if the oil sample surface has, then this temperature spot is pour point.Standard is judged with the Repeatability and Reproducibility of test result result's reliability, test the same operator that is defined as of repeatability, in same laboratory, use same instrument, step by the method regulation, in continuous time, same sample is carried out replication, gained result's difference should be above 2 ℃; The person that is defined as the different operating to repeatability in the different experiments chamber, uses instrument of the same type, by the step of method regulation, same sample is measured, and gained result's difference should be above 5 ℃.As seen, the error of existing pour point method of testing is very big, is difficult to satisfy scientific research and produces actual needs.

No matter be national standard or industry standard, all have very big defective.Particularly the test to last pour point does not have strict scientific basis, and the test process of pour point also lacks rationality down, is unacceptable because oil sample is heated to 105 ± 1 ℃ to some light oil.In addition,, under temperature rate faster, be difficult to guarantee that the oil sample central temperature is consistent with the edge, and be difficult to guarantee that the oil sample liquid level is smooth and give and observe liquid level move making troubles because the two all adopts circular test tube.In the test tube moving process, also be difficult to avoid shaking or temperature variation does not impact the structure that forms under the crude oil low temperature.Like this, the test result of final pour point is difficult to the accuracy and the degree of accuracy that reach higher.

Summary of the invention

The purpose of this utility model be design a kind of simple to operate, save time, the accurate proving installation of the oil sample non-structure destroys history, accuracy and accuracy are high petroleum products pour point.

The petroleum products that the inclination 45 is positioned in the vessel with reference to existing industry standard regulation is cooled to-20 ℃, slow heat temperature raising, until container being adjusted to vertical placement through 5s, obtain oil sample liquid level in the container and begin minimum oil sample temperature when mobile, be the regulation of pour point, the technical scheme of the utility model realization above-mentioned purpose is the oil tank 30 of outsourcing cyclic water jacket 2 is made of oil sample 3 annulus line 27 of miniature volume pump 26 and insulation a circulation line, on circulation oil sample pipeline, pick out many pipeline sections side by side to 8 li of cold and hot baths, termination one sample holder 10 on the every pipeline section.Concrete formation as shown in Figure 1, be exactly outsourcing cyclic water jacket 2 and have the bottom center of the oil tank 30 that hot water inlet 1 and hot water outlet 6 be connected with the controllable temperature water-bath to have pipeline section to connect miniature volume pump 26 through valve 29, miniature volume pump 26 outlet T-Ring shape pipelines 27 also are communicated with it to oil tank 30 tops, outside miniature volume pump 26 outlets of annulus line 27, open a plurality of mouthfuls and upwards connect a plurality of sample holder valves 25 side by side, 24,23,22,21 enter cold and hot bath 8 backs are respectively connect a sample holder 10 in cold and hot bath 8 respectively by flexible pipe 11 bottom, cold and hot bath 8 one sides have the cold and hot coil pipe 7 that is connected the temperature control bath by cold-heated plate tube inlet 31 with cold and hot coil pipe outlet 32, in the cold and hot bath 8 cold and hot liquid are arranged.Wherein cold and hot bath 8 is cuboid containers, the forward plane of structure of a row sample holder 10 is clear glass or organic glass observation window or can installs magnifier again additional in the cold and hot bath 8, and make oil sample graticule 36 in the sample holder 10 in the visual range of observation window, cold and hot coil pipe 7 is installed on the opposite of observation window, between cold and hot coil pipe 7 and the sample holder 10 background light is installed, cold and hot bath inlet 9 and the rectangular mouth 14 of a plurality of cold and hot bath are arranged at cold and hot bath 8 tops, and cold and hot bath 8 tops are equipped with thermometer 4.Sample holder 10 is cuboid containers of clear glass or organic glass material, and its bottom center has oil sample 3 to import and export pipe, and sample holder 10 is laterally little at observation window direction size ratio backward.And sample holder frame 13 is by support plate 33, adjuster bar 34, bracket 35 and hinge axis 12 are formed, become flute profile and merge the porose bracket of bottom land central authorities 35 and be connected by hinge axis 12 hinges with the top of rectangle support plate 33 on one side with sample holder 10 close-fittings, the bottom of support plate 33 and cold and hot bath 8 inner bottom parts are connected, bracket 35 is connected at the hinge place and one stretches out adjuster bar 34 outside the cold and hot bath 8 vertically upward and from cold and hot bath rectangular mouthful 14 with bracket 35, cooperate with adjuster bar 34, the cold and hot bath that cold and hot bath 8 top adjuster bars 34 stretch out rectangular mouthfuls 14 liang correct make sample holder 10 be in 45 ° and with the position of horizontal vertical, and in the inboard of rectangular mouthful 14 of cold and hot bath or the outside post flexible heat-insulating layer with mouthful isometric joint-cutting.

This device is when testing, earlier the oil sample in the oil tank 30 3 is heated to 50 ± 1 ℃, open miniature volume pump 26 and oil sample 3 is circulated in circulation line and enter sample holder 10, regulate temperature controlled water bath and make cold and hot bath 8 be cooled to-20 ℃, oil samples solidify fully in the sample holder 10.Then, regulate temperature controlled water bath again, in cold and hot coil pipe 7, feed the higher fluid of temperature, make cold and hot bath 8 temperature be warmed up to first observed temperature point of expection pour point with the speed that is not higher than 0.5 ℃/min, keep constant temperature, first sample holder 10 is become the upright position from pulling with level with level angle at 45, observe whether oil sample 3 surfaces have mobile in this sample holder 10.If obviously do not move, then abandon observing this sample holder 10.Continue to be warmed up to second observed temperature point, keep constant temperature, second sample holder 10 pulled with level become the upright position, observe whether oil sample 3 surfaces have mobile in this sample holder 10.By that analogy, till the liquid level that can observe at some observed temperature point discoveries moves.At this moment, satisfy the requirement of measuring accuracy as the difference of this temperature spot observed temperature point last with it, then this temperature spot is the pour point of the oil sample of testing 3; Do not satisfy the requirement of measuring accuracy as the difference of this temperature spot observed temperature point last with it, then oil sample 3 in the oil tank 30 must be warmed up to 50 ± 1 ℃ again, change oil sample 3 in the sample holder 10, and adjust expection observed temperature point, again test by initial step, up to move at some observed temperature point oil sample 3 liquid levels and with it on till the difference of an observed temperature point satisfies the requirement of measuring accuracy.At some observed temperature points, usually only allow to pull a sample holder 10, and in case pull some sample holders 10, find that its liquid level does not move, then suggestion each temperature observation point that raises is gradually afterwards no longer proceeded observation, because can't judge its inner structure whether damaging influence is arranged, its data will be as final testing result.If all sample holder 10 is all pulled and is not found the sign that liquid level moves, then must test again by initial step, heighten each observation station temperature to proper range, till moving at some observed temperature point discovery liquid levels.It is prudent that the selection of expection pour point and observed temperature point is wanted, and not so, the number of times of test will be many, will increase the time of test.If the closing to reality pour point that the expection pour point is selected and the quantity of sample holder 10 are abundant, so from the expection pour point first observed temperature point, the order of magnitude that just can claimed accuracy is the difference between each observed temperature point, observed temperature point time several sample holders 10 that quantity begins for first observed temperature point that rises to the expection condensation point from oil sample 3 temperature are set, and sample holder 10 that just can be less and less repeated test number of times are finished whole tests.For example, requiring test accuracy is 0.5 °, and the difference between the observed temperature point is also selected 0.5 °, as long as the selection of expection pour point is good, so just can reduce the number of times of repeated test.Certainly, if the actual pour point difference of distance that the expection pour point is selected is bigger, this is common occurrence in test job, can with the observed temperature point difference choosing in when beginning greatly, the order of magnitude that promptly selects claimed accuracy subsequently is the difference of observed temperature point, so also can reduce the number of times of repeated test,, should avoid the number of times of repeated test as far as possible because repeated test is more time-consuming.In fact because the unlikely too many sample holder 10 that is provided with, also only repeated test is repeatedly under the certain situation of sample holder 10 numbers sometimes.The accuracy of test result and degree of accuracy are to show that by temperature control accuracy and degree of accuracy, temperature accuracy and degree of accuracy, human eye may observe liquid level move the limit of sign and sample holder 10 numbers or the test multiplicity under sample holder 10 numbers one stable condition and determine.

Description of drawings

The accurate proving installation pie graph of Fig. 1 petroleum products pour point

Fig. 2 sample holder shelf structure figure

Fig. 3 sample holder structural drawing

Wherein

1-hot water inlet 2-cyclic water jacket

3-oil sample 4-temperature juice

5-stirrer 6-hot water outlet

The cold and hot bath of the cold and hot coil pipe 8-of 7-

The cold and hot bath inlet of 9-10-sample holder

11-flexible pipe 12-hinge axis

Rectangular mouthful of the cold and hot bath of 13-sample holder frame 14-

15-heat-insulation layer 16-pipeline rebound valve

17-recycling can inlet valve 18-recycling can

19-recycling can outlet valve 20-cryostat tapping valve

21-sample holder valve 22-sample holder valve

23-sample holder valve 24-sample holder valve

The miniature volume pump of 25-sample holder valve 26-

27-annulus line 28-valve

29-oil tank outlet valve 30-oil tank

The cold and hot coil pipe outlet of 31-cold-heated plate tube inlet 32-

33-support plate 34-adjuster bar

35-bracket 36-oil sample graticule

Embodiment

Embodiment. concrete enforcement of the present utility model is described and the utility model is further described with this example.The formation of this example as shown in Figure 1, from the oil tank 30 bottom center openings that are surrounded by cyclic water jacket 2 to external oil tank outlet valve 29, after threeway connects valve 28 downwards, another connects annulus line 27, miniature volume pump 26, pipeline rebound valve 16 turns back to oil tank 30 tops and constitutes the oil sample circulation line of test, behind miniature volume pump 26, upwards connect 5 sample holder valves 25,24,23,22,21 respectively connect respectively in the cold and hot liquid level of a sample holder 10 to the cold and hot bath 8, cold and hot bath 8 rear sides are equipped with the cold and hot coil pipe 7 of cold-heated plate tube inlet 31 and cold and hot coil pipe outlet 32, the front is the clear glass observation window, background light is installed behind, and circulation line connects recycling can 18 through recycling can inlet valve 17.Wherein oil tank 30 volumes are 1 liter, and annulus line 27 is a Φ 10mm steel pipe, the poly-ethylbenzene pipe that outsourcing 10mm is thick; Miniature volume pump 26 models are selected MS-CA ISMATEC wriggling volume pump for use; The model of pipeline rebound valve 16, recycling can inlet valve 17, recycling can outlet valve 19, sample holder valve 21,22,23,24,25, oil tank outlet valve 29 and valve 28 is the manual stainless steel through type of Q41F ball valves; Cold and hot bath 8 is 600 * 200 * 100mm cuboid container, the high 80mm of cold and hot liquid level in the cold and hot bath 8; Sample holder 10 (see figure 3)s are cuboid glass containers of high 100mm, wide 20mm, thick 5m, and the top is airtight, and bottom center has outside Φ 10mm, the long 10mm mouth of pipe; Flexible pipe 11 is Φ 15mm, long 50mm rubber tube, and an end is enclosed within outside the mouth of pipe under the sample holder 10, and the other end is enclosed within on the outlet of each sample holder valve; The structure of sample holder frame 13 as shown in Figure 2, wherein bracket 35 is converted into 5 * 5mm flute profile and is made a call to a Φ 4mm hole in bottom land central authorities by thick 2mm steel plate, so that the mouth of pipe at 10 ends of sample holder stretches out, support plate 33 is the steel plate of wide 5mm, high 70mm, thick 3mm, its following and cold and hot bath 8 inner bottom platings welding, the top is connected with bracket 35 hinges by the hinge axis 12 of Φ 3mm, up vertically welds the adjuster bar 34 of Φ 3mm, long 160mm at bracket 35 hinge places; The cold and hot bath at cold and hot bath 8 tops is wide 3mm, long 130mm for rectangular mouthful 14.4 one in thermometer also is equipped with at cold and hot bath 8 tops.In oil tank 30, insert 0.5 liter of Daqing crude oil, starting temperature controlled water bath heats to 50 ± 1 ℃ to oil tank 30, shut-off valve 28, recycling can inlet valve 17, open oil tank outlet valve 29, pipeline rebound valve 16, starting miniature volume pump 26 makes oil sample 3 enter circulation oil sample pipeline to circulate, open 25,24,23,22,21 and 5 sample holders 10 of sample holder valve then, make oil sample enter the sample holder 10 that the inclination 45 is placed.Starting temperature controlled water bath starts working cold and hot coil pipe 7, make that the oil sample temperature drops to-20 ℃ in the sample holder 10, test beginning starts well heater in the cold and hot bath 8 earlier makes that oil sample 3 is warming up to 25 ℃ of first observed temperatures of expection pour point in the sample holder 10, keep constant temperature 2min, first sample holder 10 is adjusted to the upright position, keep 5s, observing oil sample 3 liquid levels does not move, continuation is with 0.5 ℃ of gradient increased temperature, constant temperature, step before repeating, after being adjusted to upright position 5s to the 5th sample holder 10, observing the oil sample liquid level has had and has moved, and illustrates that the oil sample pour point is 27.0 ℃.This routine test result error is less than 0.5 ℃, and is taller as claimed accuracy, if increase sample holder 10 numbers and (or) dwindle heating gradient.This test is successively shared just to be finished smoothly less than 2 hours.Tested twice again as stated above, test result is respectively 27.5 ℃, 27.0 ℃, and repeatability is no more than 1 ℃.With same device and same method, same Daqing crude oil is tested in another laboratory, and the difference of different experiments chamber test result is no more than 1.5 ℃.

As seen, the utility model is easy and simple to handle, quick, and the device assembling is easy to realize that the test oil sample does not have the repeated measures process, degree of accuracy height, good reproducibility easily.

Claims (5)

1. accurate proving installation that is used to test a kind of petroleum products pour point of petroleum products pour point, it is characterized in that the oil tank (30) of outsourcing cyclic water jacket (2) is made of the annulus line (27) of miniature volume pump (26) and insulation the circulation line of oil sample (3), on circulation line, pick out many pipeline sections side by side to cold and hot bath (8) lining, termination one sample holder (10) on the every pipeline section.

2. the accurate proving installation of petroleum products pour point according to claim 1, it is characterized in that at outsourcing cyclic water jacket (2) and have the bottom center of the oil tank (30) that hot water inlet (1) and hot water outlet (6) be connected with the controllable temperature water-bath to have pipeline section to connect miniature volume pump (26) through valve (29), miniature volume pump (26) outlet T-Ring shape pipeline (27) also is communicated with it to oil tank (30) top, begin out a plurality of mouthfuls of a plurality of sample holder valves (25) that connect upwards arranged side by side from miniature volume pump (26) exit of annulus line (27), (24), (23), (22), (21), enter cold and hot bath (8) back is respectively connect the sample holder (10) in cold and hot bath (8) respectively by flexible pipe (11) bottom, cold and hot bath (8) one sides have the cold and hot coil pipe (7) of the temperature controlled water bath of connecing, thermometer (4) is equipped with on top, and cold and hot bath has cold and hot liquid in (8).

3. the accurate proving installation of petroleum products pour point according to claim 1 and 2, it is characterized in that described cold and hot bath (8) is the cuboid closed container, the forward plane of structure of a row sample holder (10) is clear glass or organic glass observation window or installs magnifier again additional in the cold and hot bath (8), and make the interior pasta of sample holder (10) in the visual range of observation window, cold and hot coil pipe (7) is installed on the opposite of observation window, between cold and hot coil pipe (7) and the sample holder (10) background light is installed, cold and hot bath inlet (9) and rectangular mouthful of a plurality of cold and hot bath (14) are arranged at cold and hot bath (8) top.

4. the accurate proving installation of petroleum products pour point according to claim 1 and 2, it is characterized in that described sample holder (10) is the cuboid container of clear glass or organic glass material, its bottom center has oil sample (3) to import and export pipe, and sample holder (10) is laterally little at observation window direction size ratio backward.

5. the accurate proving installation of petroleum products pour point according to claim 1 and 2, it is characterized in that described sample holder frame (13) is by support plate (33), adjuster bar (34), bracket (35) and hinge axis (12) are formed, become flute profile and merge the porose bracket (35) of bottom land central authorities and be connected by hinge axis (12) hinge with the top of rectangle support plate (33) on one side with sample holder (10) close-fitting, the bottom of support plate (33) and cold and hot bath (8) inner bottom part are connected, bracket (35) is connected at the hinge place and one stretches out adjuster bar (34) cold and hot bath (8) outside vertically upward and from cold and hot bath rectangular mouthful (14) with bracket (35), and in the inboard of cold and hot bath rectangular mouthful (14) or the outside post flexible heat-insulating layer with the isometric joint-cutting of mouth.

Images