CN105115848A - Reflux type oil sand oil content and moisture synchronous determination system and determination method - Google Patents
Reflux type oil sand oil content and moisture synchronous determination system and determination method Download PDFInfo
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- CN105115848A CN105115848A CN201510427563.3A CN201510427563A CN105115848A CN 105115848 A CN105115848 A CN 105115848A CN 201510427563 A CN201510427563 A CN 201510427563A CN 105115848 A CN105115848 A CN 105115848A
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Abstract
The invention discloses a reflux type oil sand oil content and moisture synchronous determination system and a determination method thereof. The device comprises a heating device, an extraction device, a reflux device and a condensation device. The extraction bottle of the extraction device comprises a bottleneck, a first bottle body, a second bottle body and a liquid channel, the second bottle body is placed inside the first bottle body, the bottleneck top of the second bottle body is just located at the bottom of the first bottle body's bottleneck, a U-shaped channel is formed between the first bottle body and the second bottle body, the second bottle body is anon-glued filter cylinder, the bottom of the first bottle body is provided with the liquid channel, a columnar adapter tube is sleeved outside the liquid channel, a gas distribution plate is also disposed between the adapter tube and the liquid channel, and the bottom of the adapter tube is connected to the heating device. The method provided by the invention can respectively determine the oil content, moisture content and solid residue content of an oil sand sample, and avoids the error brought about by direct weighing of solid residue and water mass and then acquisition of the oil content through subtraction method.
Description
Technical field
The invention belongs to the detection analysis technical field of oil-sand oil content and moisture, be specifically related to Simultaneous Determination system and the assay method of a kind of reverse-flow type oil-sand oil content and moisture.
Background technology
Oil-sand, also known as tar sand, heavy oil sand or Tar sands, is a kind of unconventional energy resource of widely distributed, rich reserves.All contain in more than 70 countries such as Canada, Venezuela, Russia, the U.S. and China and have oil-sand resource, the current world verified oil sands resource is about 3.7 trillion barrels, and folding synthesis of heavy oil is about 300-600Gt.Typical oil-sand is generally containing silt particle, You Heshui, and wherein massfraction is silt particle 70%-80%, oily 5-30%, water is less than 10%.Constantly increase along with world today's energy demand, imbalance between supply and demand worsens further, traditional fossil resources reserves gradually reduce, cost of winning progressively rises, and oil-sand progressively highlights as the advantage of the substitute of petroleum resources.
The main mining type of current oil-sand mainly contains strip mining transformation and in-situ conversion, open-pit mining techniques requirement is low, resource utilization is high, exploitation oil-sand Land use systems out has: oil-sand hot water wash technique, oil-sand organic solvent extracting taking technique and oil-sand pyrolytic process, the quality of this several technique depends on the yield of heavy oil, and the sign of heavy oil yield be unable to do without the oil content of oil sands sample.Oil content is the important indicator evaluating oil-sand quality, determine whether oil-sand ore deposit has the important evaluation index of commercial mining value, there is the feature of veto by one vote simultaneously, when China at present temporary without this metrics evaluation benchmark, the general averaged lower bound taste with reference to Canada's exploitation oil-sand is evaluated for oil content (massfraction 5%): the average oil content of GOOD TASTE is greater than 13%, the average oil content 8%-13% of middle grade, low-grade average oil content 5%-8%.
At present, the oil content of domestic mensuration oil-sand generally adopts the Dean-stark toluene extraction process that soxhlet extraction methods or the fuel-efficient sand management board of Transport Model for Alberta are recommended.Soxhlet extraction methods uses Soxhlet extractor (also known as Soxhlet fat extraction apparatus), because solvent vapour directly enters condenser pipe by gas passage, again leaching extracting is carried out to solid after condensing reflux, thus cause that extract temperature is lower, extraction times is longer (generally wanting 24h).Dean-stark toluene extraction process is a lessivation of solvents upon solids, and extracting is incomplete, and experimental data accuracy, collimation are poor.CN102778409A discloses one " in working sample oil and/or the device and method of liquid water content ", extraction tube is directly placed in extraction flask by this device, the pipe diameter size of such extraction tube can be limited by the bore of extraction flask bottleneck, and the size of extraction tube directly affects the number of sample size.Due to the inequality of oil-sand itself, sample size is very few will certainly cause larger sampling error.Article " in oily sludge, 3 kinds of assay methods of profit content the compare " (Zhang Ke etc. delivered by inventor, environmental engineering journal, 2014,8 (1): 386-391) find that the sample size that it is tested only has 10g, and the Dean-stark toluene extraction process laboratory sample amount that the fuel-efficient sand management board of Transport Model for Alberta is recommended is 50g.
Summary of the invention
The object of the present invention is to provide Simultaneous Determination system and the assay method thereof of a kind of reverse-flow type oil-sand oil content and moisture thereof, by improving extraction plant, and extraction plant and heating arrangement, coordinating between reflux and condensing unit, can the oil of working sample, water and residue content accurately and rapidly.
One of task of the present invention is to provide the Simultaneous Determination system of a kind of reverse-flow type oil-sand oil content and moisture.
The Simultaneous Determination system of a kind of reverse-flow type oil-sand oil content and moisture, comprise heating arrangement, extraction plant, reflux and condensing unit, described heating arrangement is used for heating solvent making it extract oil in oil-sand, described heating arrangement is connected with described extraction plant, described reflux is between condensing unit and extraction plant, for by condensing unit reflux under liquid backflow in extraction plant, described extraction plant comprises extracting bottle and is positioned at the joint above extracting bottle, described joint is used for extracting bottle to be connected with reflux, described extracting bottle comprises bottleneck, first bottle, second bottle and fluid passage, described second bottle is placed in the first bottle, the bottleneck the top of described second bottle is positioned at the bottleneck bottom of described first bottle just, the bottom of described first bottle and the bottom of the second bottle maintain a certain distance, U is formed between described first bottle and the second bottle, described second bottle is the glue-free filter cylinder that solvent can only be made to pass through, solvent enters in described U by described glue-free filter cylinder, the sidepiece of the bottom surface of described first bottle is provided with liquid outlet channel, described fluid passage is positioned at the place of bottom center of the first bottle, and the outside of described fluid passage is arranged with the adapter of cylindricality, is also provided with gas distribution grid between described adapter and fluid passage, and the bottom of described adapter is connected with heating arrangement.
The Advantageous Effects that technique scheme is directly brought is: adopt glue-free filter cylinder as the second bottle, avoids solid particle thinner in oil-sand and enters solvent through bottle wall, and the experimental result of mensuration can be made more accurate; Gas distribution grid can make steam evenly enter extraction solvent, accelerates its violent disturbance, promotes liquid-solid mass transfer efficiency; Steam, directly through extraction solvent, improves extraction temperature, shortens extraction times; Liquid outlet channel directly can collect clean solvent after extracting completes, and avoids and again builds distilling apparatus; A large amount of sample can be held as much as possible in second bottle, and reduce the space between solid sample and the first bottle, thus decrease the accumulated amount of extracting internal solvent, save solvent;
Technique scheme combines the accuracy that can improve experimental data, shortens extraction times, can obtain purer oil-sand extractable bitumen simultaneously, again can recycling design.
As a preferred version of the present invention, described glue-free filter cylinder is made by glass fiber material.
The Advantageous Effects that technique scheme is directly brought is: directly adopt filter paper parcel sample to be difficult to avoid fine grained to enter extraction solvent, therefore add fine powder aligning step in Dean-stark toluene extractive process, adopt glue-free filter cylinder that thinner particle can be avoided to enter in extraction solvent through barrel; By distillation solvent evaporated after extracting completes and can obtain pure pitch, improve the accuracy of data, be convenient to the detection of follow-up asphaltic nature, the fine powder decreased in Dean-stark toluene extractive process corrects, by controlling the relative size of glue-free filter cylinder and the first bottle, gap (U) size to fit therebetween can be guaranteed, be unlikely to accumulate relatively large liquid in the first bottle, saved the consumption of solvent in extractive process.
As another preferred version of the present invention, the sidepiece of the bottom surface of described first bottle is provided with liquid outlet channel, liquid outlet channel is provided with valve.
The Advantageous Effects that technique scheme is directly brought is: take out the second bottle after extracting terminates, the second bottle is accumulated in inner after continuing heated solvent volatilization condensation, open valve can between reclaim pure solvent, avoid the operation of again building distilling apparatus.
As another preferred version of the present invention, have the body of rod in the inner side of described first bottle near bottle bottom lateral arrangement, described second bottle is placed on the described body of rod.
The Advantageous Effects that technique scheme is directly brought is: fix the second bottle, ensures to there is uniform space between the first bottle and the second bottle.
Preferably, the described body of rod is furnished with four uniformly along the bottle wall circumference interval of the first bottle, and the vertical range of each body of rod and the first bottle bottle bottom is 3-5mm.
The Advantageous Effects that technique scheme is directly brought is: both can avoid second bottle of bottom blocking fluid passage and gas distribution grid, be reserved with again the relative height that sufficient space ensure that the second bottle.
Preferably, described gas distribution grid is uniform-distribution with eight pores.
The Advantageous Effects that technique scheme is directly brought is: gas enters the inner violent bubbling of extractor by the pore on gas distribution grid, and disturbance liquid, promotes the carrying out of solid-liquid mass transfer, reduces extraction times.
Preferably, described joint is for falling funnel-form.
The Advantageous Effects that technique scheme is directly brought is: the resistance decreasing gas uphill process, is convenient to solvent vapour and enters condenser through water trap.
Preferably, described solvent is aromatic hydrocarbons, naphthenic hydrocarbon or halogenated hydrocarbons.
The Advantageous Effects that technique scheme is directly brought is: solvent is better to the heavy constituent in oil sands bitumen especially asphaltene dissolution effect, ensure that the accuracy of experimental result.
Two of task of the present invention is to provide the assay method of the Simultaneous Determination system of reverse-flow type oil-sand oil content and moisture, comprises the following steps successively:
A, measure appropriate solvent, be added in the solvent bottle of heating arrangement, take 50 ~ 100g oil sands sample and put into the second bottle, the second bottle filling oil sands sample is placed in the first bottle, assembles Analytical system successively in order;
B, condenser system and water are connected, and open heating arrangement and be heated to solvent boiling to make it circulating reflux extracting, stop heating to during solvent water white transparency in extracting bottle;
The volume of water in c, reading reflux, then take out the second bottle, and put it into electric drying oven with forced convection inner drying 1h, after drying completes, taking-up is put into exsiccator cooling, is weighed, by the way of distillation, the solvent in solvent bottle is evaporated, thus can oil sands bitumen be obtained;
The content of the water in d, oil-sand, solid residue and oil presses following formula (1), (2), (3) calculating successively:
Y
water=ρ V/m
0(1)
In formula (1): m
0-oil sands sample quality, the density of ρ-water, the volume of V-water;
Y
residue=(m
0-m
1-ρ V)/m
0(2)
In formula (2), m
0-oil sands sample quality, m
1the quality of residue after-oven dry, the density of ρ-water, the volume of V-water;
Y
oil=(m
3– m
2)/m
0(3)
In formula (3), m
0-oil sands sample quality, m
3the quality sum of solvent bottle and oil sands bitumen after the volatilization of-solvent is clean, m
2the quality of-solvent bottle.
The Advantageous Effects that the present invention brings is:
First, in Analytical system of the present invention, the structure of extraction plant is improved, extraction plant after improvement compared with prior art, especially compared with CN102778409A, the loss of thinner solid particle can be avoided by arranging the first bottle and the second bottle in the present invention, solvent containing solute in CN102778409A directly enters bottom flask by spout hole, the thinner solid particle that part can be caused like this to mix in a solvent enters flask, thus cause producing larger experimental error, the present invention adopts glue-free filter cylinder to solve this problem; Be provided with gas distribution grid at the first bottle body bottom, steam, to the violent disturbance of liquid, facilitates solid-liquid mass transport process, shortens the reaction time, and apparatus structure is simple, is convenient to the assembling with other commercial instruments.
Secondly, assay method of the present invention, increases the amount of oil sands sample, avoids the accidental error brought because sample size is very few; The oil content of oil sands sample, water percentage and solid residue can be measured respectively containing rate, avoid the quality directly weighing solid residue and water and then obtain by minusing the error that oil content brings, and because solid residue exists loss in CN102778409A, make the oil content that records higher; And the oil-sand extractable bitumen sample that can obtain cleaning is so that the detection analysis of follow-up physical property, pure solvent can be reclaimed simultaneously.
In addition, the inventive method not only directly can record oil content and the water percentage (not needing indirect calculation to obtain) of oil-sand, and can be used to measure most of solid particle (such as: resinous shale, oily sludge etc.); Avoid solid-liquor separation after extracting terminates, save laboratory operating procedures and time; According to azeotropic distillation principle, suitable solvent is selected also to can be used to extracting heat-sensitive substance.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, explanation clear, complete is further done to the present invention:
Fig. 1 is the structural representation of determinator of the present invention;
Fig. 2 is extraction plant decomposed figure of the present invention;
Fig. 3 is the A-A sectional view at Fig. 2 first bottle place;
In figure, 1, condensing unit, 2, reflux, 3, joint, 4, extraction plant, 5, solvent bottle, 6, heating plant, the 41, first bottle, the 42, second bottle, 43, the body of rod, 44, fluid passage, 45, adapter, 46, gas distribution grid, 47, pore, 48, liquid outlet channel.
Embodiment
Below in conjunction with specific embodiment, the present invention is elaborated.
As shown in Figure 1, determinator of the present invention comprises condensing unit 1, reflux 2, extraction plant 4 and heating arrangement (solvent bottle 5 and heating plant 6 are as heating arrangement), what be positioned at bottom is heating arrangement, extraction plant 4 is positioned at above heating arrangement, reflux is between condensing unit and extraction plant, condensing unit 1 can select spherical condensation tube, serpentine condenser or other specification, the present invention is preferably spherical condensation tube or straight cold finger, and serpentine condenser resistance is not considered comparatively greatly herein, the pipeline connecting condenser pipe can select common emulsion tube or rubber tube, for reflux 2, conventional water trap can be selected, the optional electric heating cover of heating arrangement or oil bath pan heat round-bottomed flask, level land flask or ground conical flask (as solvent bottle).
Annexation those skilled in the art for above-mentioned four kinds of devices all can assemble according to knowwhy, for this extraction plant 4 with the use of condensing unit 1, reflux 2 and heating arrangement do not elaborate at this.
The solvent can put in solvent bottle 5 is aromatic hydrocarbons, naphthenic hydrocarbon or halogenated hydrocarbons, the principle that the present invention measures oil-sand oil content and moisture thereof is: according to the similar principle that mixes, evaporate when solvent is heated, enter extraction plant 4 to contact with extract with oil-sand, violent bubbling and stirring, make soluble constituent be dissolved in extraction solvent; Part uncondensed gas enters in the condensing reflux system of top through water trap, and the solvent of condensation passes back into extraction system after water trap.Extract containing soluble constituent is back in the solvent bottle of bottom under gravity, and extraction solvent is evaporated again, and process is carried out continuously repeatedly, until stop when solvent in extraction system is transparent.Final soluble constituent is stayed in solvent bottle, and can not be stayed in filter paper groove by extraction solvent dissolved solid gravel.
Shown in composition graphs 2 and Fig. 3, extraction plant 4 comprises extracting bottle and is positioned at the joint 3 above extracting bottle, joint 3 is for being connected extracting bottle with reflux, extracting bottle comprises bottleneck, first bottle 41, second bottle 42 and fluid passage 44, wherein the second bottle 42 is placed in the first bottle 41, the bottleneck the top of the second bottle 42 is positioned at the bottleneck bottom of the first bottle 41 just, in order to stablizing of the second bottle, also the bottleneck bottom of the bottleneck the top of the second bottle and the first bottle slightly can be bonded together, when can prevent bubbling like this, the second bottle is unstable, the distance of 3-5mm is kept in the bottom of the bottom of the first bottle and the second bottle, U is formed between first bottle and the second bottle, the body of rod 43 is had near bottle bottom lateral arrangement in the inner side of the first bottle, the body of rod 43 interval is furnished with four uniformly, being placed on the body of rod 43 of second bottle Absorbable organic halogens.
Above-mentioned second bottle is the glue-free filter cylinder that solvent can only be made to pass through, solvent enters in U by glue-free filter cylinder, and the sidepiece of the bottom surface of the first bottle is provided with liquid outlet channel 48, and this liquid outlet channel 48 is for recycling design, this liquid outlet channel 48 is also provided with valve, facilitates recycling design; Fluid passage is positioned at the bottom of the first bottle, the outside of fluid passage is arranged with the adapter 45 of cylindricality, also gas distribution grid is provided with between adapter and fluid passage, gas distribution grid 46 is laid with pore 47, pore can be arranged in annular on gas distribution grid, and the bottom of adapter 45 is connected by ground with between solvent bottleneck.
Above-mentioned glue-free filter cylinder is made up of glass fiber material, and solvent can freely pass through, and solid particle then can not be through, and the external diameter of glue-free filter cylinder is slightly less than the internal diameter of the first bottle so that install.
The Simultaneous Determination method of reverse-flow type oil-sand oil content of the present invention and moisture, comprises the following steps:
The first step, measure appropriate solvent, pour in flask.Take 50g oil sands sample and put into glue-free filter cylinder, then glue-free filter cylinder is put into the first bottle, according to flask, extraction plant, joint, water trap and condenser pipe successively erecting equipment, finally open condensate water and be heated to solvent boiling and make it circulating reflux extracting, stop to during solvent water white transparency in extraction plant.By controlling the rate of heat addition in experimentation, extraction plant inside liquid level is made to remain on proper height;
Wherein said solvent can select aromatic hydrocarbons (benzene,toluene,xylene), naphthenic hydrocarbon (cyclohexane, cycloheptane) or halogenated hydrocarbons (methenyl choloride, phenixin).
After second step, extracting terminate, first the volume of water in water trap is read, then glue-free filter cylinder is taken out, put into electric drying oven with forced convection (temperature setting is than the boiling point height 5-10 DEG C of solvent), take out after dry 1h and put into exsiccator cooling 30min weighing, finally by distillation, the solvent in flask is evaporated, thus can oil sands bitumen be obtained;
The oil of the 3rd step, oil-sand, water and solid residue cubage method:
The water percentage of oil-sand calculates by formula (1):
Y
water=ρ V/m
0(1) in formula: m
0-sample quality; The density of ρ-water; The volume of V-water
The slag-containing rate of oil-sand calculates by formula (2):
Y
slag=(m
0-m
1-ρ V)/m
0(2) in formula: m
0-sample quality; m
1the quality of residue after-oven dry; The density of ρ-water; The volume of V-water
The oil content rate of oil-sand calculates by formula (3):
Y
oil=(m
3– m
2)/m
0(3) in formula: m
0-sample quality; m
3the quality sum of flask and oil sands bitumen after the volatilization of-solvent is clean; m
2the quality of-flask.
Embodiment 1:
With oil-sand S
1for testing sample, said apparatus and method is utilized to measure its oil, water and solid residue content, the residue of sample complete for extracting is dry under 145 DEG C of conditions, dimethylbenzene is volatilized and to sample constant weight, weighs the amount of solid residue, flask internal solvent is distilled, weigh the amount of oil sands bitumen after constant weight, calculate the content of oil, water and solid residue respectively.Measurement result is listed in the table below.
Oil sands sample S
1oil content measurement result is shown in Table 1:
Table 1
| Measure number of times | 1 | 2 | 3 | 4 | Mean value | Standard deviation |
| Oil content | 30.11 | 29.06 | 30.09 | 30.23 | 29.8725 | 0.5452 |
Oil sands sample S
1measurement of water-content coefficient the results are shown in Table shown in 2:
Table 2
| Measure number of times | 1 | 2 | 3 | 4 | Mean value | Standard deviation |
| Water percentage | 2.22 | 2.43 | 2.09 | 2.67 | 2.3525 | 0.2538 |
Oil sands sample S
1slag-containing rate measurement result is shown in Table 3:
Table 3
| Measure number of times | 1 | 2 | 3 | 4 | Mean value | Standard deviation |
| Slag-containing rate | 68.33 | 68.01 | 67.35 | 66.86 | 67.6375 | 0.6597 |
Embodiment 2:
With oil-sand S
2for testing sample, apparatus of the present invention and method is utilized to measure its oil, water and solid residue content, the residue of sample complete for extracting is dry under 145 DEG C of conditions, dimethylbenzene is volatilized and to sample constant weight, weighs the amount of solid residue, flask internal solvent is distilled, weigh the amount of oil sands bitumen after constant weight, calculate the content of oil, water and solid residue respectively:, measurement result is listed in the table below.
Oil sands sample S
2oil content measurement result is shown in Table 4:
Table 4
| Measure number of times | 1 | 2 | 3 | 4 | Mean value | Standard deviation |
| Oil content | 13.74 | 14.03 | 14.83 | 14.17 | 14.1925 | 0.4612 |
Oil sands sample S
2oil content measurement result is shown in Table 5:
Table 5
| Measure number of times | 1 | 2 | 3 | 4 | Mean value | Standard deviation |
| Water percentage | 31.52 | 31.43 | 32.31 | 32.67 | 31.9825 | 0.6053 |
Oil sands sample S
2slag-containing rate measurement result is shown in Table 6:
Table 6
| Measure number of times | 1 | 2 | 3 | 4 | Mean value | Standard deviation |
| Slag-containing rate | 84.13 | 84.85 | 83.81 | 84.06 | 84.2125 | 0.4466 |
Embodiment 3:
With oil-sand S
2for testing sample, apparatus of the present invention and method is utilized to measure its oil, water and solid residue content, the residue of sample complete for extracting is dry under 145 DEG C of conditions, dimethylbenzene is volatilized and to sample constant weight, weighs the amount of solid residue, flask internal solvent is distilled, weigh the amount of oil sands bitumen after constant weight, calculate the content of oil, water and solid residue respectively.Measurement result is listed in the table below.
Oil sands sample S
2oil content measurement result is as shown in table 7:
Table 7
| Measure number of times | 1 | 2 | 3 | 4 | Mean value | Standard deviation |
| Oil content | 22.71 | 21.56 | 21.83 | 22.17 | 22.0675 | 0.4957 |
Oil sands sample S
2oil content measurement result is as shown in table 8:
Table 8
| Measure number of times | 1 | 2 | 3 | 4 | Mean value | Standard deviation |
| Water percentage | 31.52 | 31.43 | 32.31 | 32.67 | 31.9825 | 0.6053 |
Oil sands sample S
2slag-containing rate measurement result is as shown in table 9:
Table 9
| Measure number of times | 1 | 2 | 3 | 4 | Mean value | Standard deviation |
| Slag-containing rate | 45.63 | 45.03 | 45.81 | 46.26 | 45.6825 | 0.5093 |
Embodiment 4
With oil-sand S
3for testing sample, apparatus of the present invention and method is utilized to measure its oil, water and solid residue content, the residue of sample complete for extracting is dry under 145 DEG C of conditions, dimethylbenzene is volatilized and to sample constant weight, weighs the amount of solid residue, flask internal solvent is distilled, weigh the amount of oil sands bitumen after constant weight, calculate the content of oil, water and solid residue respectively.
Oil sands sample S
3oil content measurement result is as shown in table 10:
Table 10
| Measure number of times | 1 | 2 | 3 | 4 | Mean value | Standard deviation |
| Oil content | 18.98 | 19.09 | 20.06 | 19.03 | 19.2675 | 0.5349 |
Oil sands sample S
3oil content measurement result is as shown in table 11:
Table 11
| Measure number of times | 1 | 2 | 3 | 4 | Mean value | Standard deviation |
| Water percentage | 57.32 | 56.93 | 57.71 | 57.47 | 57.3575 | 0.3271 |
Oil sands sample S
2slag-containing rate measurement result is as shown in table 12:
Table 12
| Measure number of times | 1 | 2 | 3 | 4 | Mean value | Standard deviation |
| Slag-containing rate | 23.26 | 23.81 | 23.03 | 23.63 | 23.4325 | 0.3527 |
Also alternate manner can be adopted between the present invention first bottle and the second bottle to connect, as arranged the dimple of accommodation second bottle at the first bottle body bottom.
It should be noted that, those skilled in the art under enlightenment of the present invention, to the simple replacement of the connected mode of extraction plant specification and the first bottle and the second bottle, all should within protection scope of the present invention.
Claims (9)
1. the Simultaneous Determination system of a reverse-flow type oil-sand oil content and moisture, comprise heating arrangement, extraction plant, reflux and condensing unit, described heating arrangement is used for heating solvent and utilizing the oil in described solvent extraction oil-sand, described heating arrangement is connected with described extraction plant, described reflux is between condensing unit and extraction plant, for by the liquid backflow under condensing unit condensation in extraction plant, it is characterized in that: described extraction plant comprises extracting bottle and is positioned at the joint above extracting bottle, described joint is used for extracting bottle to be connected with reflux, described extracting bottle comprises bottleneck, first bottle, second bottle and fluid passage, described second bottle is placed in the first bottle, the bottleneck the top of described second bottle is positioned at the bottleneck bottom of described first bottle just, the bottom of described first bottle and the bottom of the second bottle maintain a certain distance, U is formed between described first bottle and the second bottle, described second bottle is the glue-free filter cylinder that solvent can only be made to pass through, solvent enters in described U by described glue-free filter cylinder, the sidepiece of the bottom surface of described first bottle is provided with liquid outlet channel, described fluid passage is positioned at the place of bottom center of the first bottle, and the outside of described fluid passage is arranged with the adapter of cylindricality, is also provided with gas distribution grid between described adapter and fluid passage, and the bottom of described adapter is connected with heating arrangement.
2. the Simultaneous Determination system of reverse-flow type oil-sand oil content according to claim 1 and moisture, is characterized in that: described glue-free filter cylinder is made by glass fiber material.
3. the Simultaneous Determination system of reverse-flow type oil-sand oil content according to claim 1 and moisture, is characterized in that: described liquid outlet channel is provided with valve.
4. the Simultaneous Determination system of reverse-flow type oil-sand oil content according to claim 1 and moisture, is characterized in that: have the body of rod in the inner side of described first bottle near bottle bottom lateral arrangement, and described second bottle is placed on the described body of rod.
5. the Simultaneous Determination system of reverse-flow type oil-sand oil content according to claim 4 and moisture, it is characterized in that: the described body of rod is furnished with four uniformly along the bottle wall circumference interval of the first bottle, and the vertical range of each body of rod and the first bottle bottle bottom is 3-5mm.
6. the Simultaneous Determination system of reverse-flow type oil-sand oil content according to claim 1 and moisture, is characterized in that: described gas distribution grid is distributed with eight pores.
7. the Simultaneous Determination system of reverse-flow type oil-sand oil content according to claim 1 and moisture, is characterized in that: described joint is for falling funnel-form.
8. the Simultaneous Determination system of reverse-flow type oil-sand oil content according to claim 1 and moisture, is characterized in that: described solvent is aromatic hydrocarbons, naphthenic hydrocarbon or halogenated hydrocarbons.
9. the assay method of the reverse-flow type oil-sand oil content according to any one of claim 1-8 and the Simultaneous Determination system of moisture, is characterized in that: comprise the following steps successively:
A, measure appropriate solvent, be added in the solvent bottle of heating arrangement, take 50 ~ 100g oil sands sample and put into the second bottle, the second bottle filling oil sands sample is placed in the first bottle, assembles Analytical system successively in order;
B, condenser system and water are connected, and open heating arrangement and be heated to solvent boiling to make it circulating reflux extracting, stop heating to during solvent water white transparency in extracting bottle;
The volume of water in c, reading reflux, then take out the second bottle, and put it into electric drying oven with forced convection inner drying 1h, after drying completes, taking-up is put into exsiccator cooling, is weighed, by the way of distillation, the solvent in solvent bottle is evaporated, thus can oil sands bitumen be obtained;
The content of the water in d, oil-sand, solid residue and oil presses following formula (1), (2), (3) calculating successively:
Y
water=ρ V/m
0(1)
In formula (1): m
0-oil sands sample quality, the density of ρ-water, the volume of V-water;
Y
residue=(m
0-m
1-ρ V)/m
0(2)
In formula (2), m
0-oil sands sample quality, m
1the quality of residue after-oven dry, the density of ρ-water, the volume of V-water;
Y
oil=(m
3– m
2)/m
0(3)
In formula (3), m
0-oil sands sample quality, m
3the quality sum of solvent bottle and oil sands bitumen after the volatilization of-solvent is clean, m
2the quality of-solvent bottle.
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|---|---|---|---|
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|---|---|---|---|
| CN201510427563.3A CN105115848B (en) | 2015-07-20 | 2015-07-20 | The Simultaneous Determination system and assay method of reverse-flow type oil-sand oil content and moisture |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN108918324A (en) * | 2018-06-04 | 2018-11-30 | 中国石油化工股份有限公司 | The separator and method for quantitatively determining of oil, Free water, irreducible water in rock |
| CN108918324B (en) * | 2018-06-04 | 2024-04-12 | 中国石油化工股份有限公司 | Separation device for oil, free water and bound water in rock and quantitative determination method |
| CN109187262A (en) * | 2018-09-19 | 2019-01-11 | 常州大学 | A kind of measuring method of oil-sand oil content |
| CN109682713A (en) * | 2019-02-21 | 2019-04-26 | 吉林大学 | A kind of oil content of oil shale apparatus for automatically measuring and measuring method |
| CN109682713B (en) * | 2019-02-21 | 2024-04-19 | 吉林大学 | Automatic determination device and determination method for oil content of oil shale |
| CN110286054A (en) * | 2019-07-09 | 2019-09-27 | 山东俊富非织造材料有限公司 | A kind of detection method of hydrophilic emulsion concentration |
| CN113970500A (en) * | 2021-10-27 | 2022-01-25 | 北京新风航天装备有限公司 | Method for rapidly measuring oil content of oil stain solid waste |
| CN113970500B (en) * | 2021-10-27 | 2023-08-29 | 北京新风航天装备有限公司 | Rapid determination method for oil content of greasy dirt solid waste |
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