CN103018131A - Determining device and method for oil water and ash contents in gas in negative pressure state - Google Patents
Determining device and method for oil water and ash contents in gas in negative pressure state Download PDFInfo
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- CN103018131A CN103018131A CN2012105242328A CN201210524232A CN103018131A CN 103018131 A CN103018131 A CN 103018131A CN 2012105242328 A CN2012105242328 A CN 2012105242328A CN 201210524232 A CN201210524232 A CN 201210524232A CN 103018131 A CN103018131 A CN 103018131A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 113
- 238000000034 method Methods 0.000 title claims abstract description 57
- 238000001816 cooling Methods 0.000 claims abstract description 85
- 239000003921 oil Substances 0.000 claims description 81
- 239000002956 ash Substances 0.000 claims description 32
- 238000003556 assay Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 13
- 238000005259 measurement Methods 0.000 claims description 13
- 238000009833 condensation Methods 0.000 claims description 12
- 230000005494 condensation Effects 0.000 claims description 12
- 238000012360 testing method Methods 0.000 claims description 9
- 239000012530 fluid Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 239000000470 constituent Substances 0.000 claims description 6
- 230000003139 buffering effect Effects 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 235000019628 coolness Nutrition 0.000 claims description 3
- 239000000295 fuel oil Substances 0.000 claims description 3
- 238000011282 treatment Methods 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 4
- 238000004880 explosion Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 110
- 238000002474 experimental method Methods 0.000 description 15
- 238000010521 absorption reaction Methods 0.000 description 14
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 12
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 10
- 238000001354 calcination Methods 0.000 description 8
- 239000011521 glass Substances 0.000 description 6
- 229930195733 hydrocarbon Natural products 0.000 description 5
- 150000002430 hydrocarbons Chemical class 0.000 description 5
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 4
- 239000002826 coolant Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000011435 rock Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 229920000742 Cotton Polymers 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 3
- 238000010926 purge Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000010425 asbestos Substances 0.000 description 2
- 230000000740 bleeding effect Effects 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 229910052895 riebeckite Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003822 preparative gas chromatography Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
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Abstract
The invention discloses a determining device for oil water and ash contents in a gas in negative pressure state, which comprises an initial cooling bottle I, an initial cooling bottle II, a condensing coil I, a condensing coil II, a buffer bottle, an anti-explosion water ring vacuum pump, a steam-water separator, and a wet flowmeter all sequentially and hermetically connected through a connecting pipeline. The condensing coil I is placed in a low temperature cooling container I with condensate, and the outlet of the condensing coil I is provided with a receiving bottle I. The condensing coil II is placed in a low temperature cooling container II with condensate, and the outlet of the condensing coil II is provided with a receiving bottle II. The invention further discloses a determining method for oil water and ash contents in the gas in negative pressure state. The oil water and ash contents in the gas to be determined in negative pressure state are determined at the same time. The metering is more precise, the operational control is stable, the recovery rate is high, and the measuring error is small.
Description
Technical field
The present invention relates to commercial measurement device field, more particularly, the present invention relates under a kind of negative pressure state the determinator of oil, water and ash content in the device in Gas and use this device to carry out under the negative pressure state assay method of oil, water and ash content in the device in Gas.
Background technology
Oil in the methane gas, water, ash content are important indicators estimating the methane gas product quality.At energy manufacture field, the most of negative pressure that adopts of device in Gas induction system is pumped.Can oil, water, ash content in the device in Gas under the Accurate Determining negative pressure state be recycled for the calculating of commercial plant material balance, heat Balance Calculation, device improvement, device in Gas upgrading processing, device in Gas and to be had important directive significance.Composition more complicated in the methane gas under the negative pressure state, oil, water, ash concentration are not identical in the local gas, and oil content assay method, Water content determination method and dust determination method in the gas under the report negative pressure state are arranged at present.But also do not have a kind of method accurately, directly to measure simultaneously the oil in the gas, water, ash content under the negative pressure state.
Determination method for oil content under the negative pressure state of prior art report in the gas mainly is to take solvent absorption, sorbing material absorption process or condensation enrichment absorption process to collect Oil in circulating gas.Oil content in the measurement gas such as recycling infrared spectrophotometry, ultraviolet spectrophotometry, gravimetric method, turbidimetry, vapor-phase chromatography, gas detector method.Solvent absorption: the oil in the gas can well be dissolved in the normal hexane, in venting process, be adsorbed onto again in the absorbent cotton with the air-flow entrained oil with normal hexane, with oil in normal hexane flushing, desorption absorption bottle and the absorbent cotton, use the normal hexane constant volume in the 100mL volumetric flask.According to reported in literature, normal hexane without absorption peak, be good solvent, and oil has maximum absorption band herein at the 260nm place, and its absorbance size is directly proportional with oil content, meets langbobier law, that is: A=KC.Sorbing material absorbs: a certain amount of fibrous material of filling (absorbent cotton, glass fibre, mekralon etc.), quantitative filter paper, glass fibre film or other sorbing material in stopple coupon (such as activated charcoal etc.), during sampling, allow measurement gas pass through stopple coupon with certain flow velocity, and write down the sample volume of gas with wet test meter.The condensation enrichment absorbs: the glass spiral cold-finger is immersed in the refrigerant such as liquid nitrogen, with measure gas with certain flow by condenser pipe, the oil in the gas is condensed in the spiral pipe, again with solvent with its wash-out.In addition, also can be with reference to the rock gas methods of light hydrocarbon recovery, comprising absorption method, oil-absorption process and condensation separation method.Absorption method is to utilize solid adsorbent (such as activated charcoal, silica gel and zeyssatite etc.) different to various hydro carbons adsorption capacities, and restructuring divides the method for separating with light constituent in the rock gas thereby make.Oil-absorption process, such as horse traction (Mhear) method, be based on each component in the rock gas in absorbing oil dissolubility difference and make method light, that heavy hydrocarbon component is separated.Absorb general naphtha, kerosene or the diesel oil of adopting of oil, its relative molecular weight is 100 ~ 200.According to the difference that absorbs temperature, oil-absorption process can be divided into normal temperature, middle gentle low temperature oil-absorption process; Because above-mentioned the whole bag of tricks lacks the means of preparation Oil in circulating gas standard substance, the accuracy of the whole bag of tricks, precision and repeatable relatively poor, and said method is not suitable for the mensuration of the oil content in the moisture gas under the negative pressure state; The assay method of liquid water content has two classes in the gas, and a class is instrumental method, comprises with cooling minute surface condensation hygrometer measuring the gas water dew point and directly measuring liquid water content in the rock gas with electrolytic liquid water content analyser; Another kind of is chemical method, comprises karl Fischer method, phosphorus pentoxide absorption process and colourimetry etc.But these two class methods can not be measured the industrial gasses that contain large quantity of moisture, and can not finish simultaneously oil content and ash content in the tested gas, and range of application is narrower.
Summary of the invention
Problem to be solved by this invention provides a kind of determinator of the mensuration that can finish simultaneously liquid water content, oil content and ash content in the tested device in Gas under negative pressure state and uses this device to carry out under the negative pressure state assay method of oil, water and ash content in the device in Gas.
To achieve these goals, the technical scheme that the present invention takes is: the determinator of oil, water and ash content in the device in Gas under a kind of negative pressure state that provides comprises the preliminary cooling bottle one that is tightly connected successively by connecting tube, preliminary cooling bottle two, condensing coil one, condensing coil two, surge flask, explosion-proof water ring vacuum pump, steam-water separator and wet flow indicator; Described condensing coil one places the sub-cooled container one that is contained with condensed fluid, and the exit of condensing coil one is provided with receiving bottle one; Condensing coil two places the sub-cooled container two that is contained with condensed fluid, and the exit of condensing coil two is provided with receiving bottle two.
Preferably, the preliminary cooling bottle one UNICOM porch of tentatively cooling off the pipeline of bottle two is provided with filtrator; Described preliminary cooling bottle one is placed in the frozen water mixer one, and preliminary cooling bottle two places frozen water mixer two.
Preferably, sub-cooled container one and circulating cooling pump one UNICOM; Sub-cooled container two and circulating cooling pump two UNICOMs; The outer wall of sub-cooled container one and sub-cooled container two is equipped with heat preservation sandwich layer.
Preferably, also be provided with a plurality of one-way cocks on the connecting tube.
A kind of assay method that uses said apparatus to carry out under the negative pressure state oil, water and ash content in the device in Gas, the method comprises following process: the device in Gas under a certain amount of negative pressure state is extracted out from commercial plant place determinator, through tentatively cooling off, pass through again the secondary deep cooling, after three grades of subzero treatments of mistake, enter surge flask; Device in Gas in the surge flask is separated moisture after extracting out via water ring vacuum pump in steam-water separator, the device in Gas after Separation of Water divides is added up gas flow through wet flow indicator; Collecting the oil that contains a certain amount of solid impurity, aqueous mixtures that condensation gets off moves on in the ground conical flask that quartz glass makes and weighs, again the ground conical flask is connected with device for measuring moisture, residue continues heating, until there is not liquid to exist in the ground conical flask; Conical flask is transferred to is incubated 3h after being heated to 815 ℃ in the muffle furnace, cooling, its quality of weighing, and then put into muffle furnace 30min, and take out cooling, its quality of weighing namely gets ash content again, and the quality of potpourri deducts liquid water content and ash content obtains oil content; Measure the CO in surge flask and the wet test meter after gas gas
2Content records the device in Gas total amount.
Preferably, preliminary cooling is to be under 0 ℃ ~ 4 ℃ the condition flow velocity of device in Gas to be played the effect of buffering in temperature, prolongs the residence time of device in Gas in measurement mechanism, and most heavy oil fraction in the device in Gas and part water condensation are got off.
The method comprises following six processes: device in Gas is tentatively cooled off buffering course, device in Gas one-level deep cooling process, device in Gas secondary deep cooling process, the buffering course of bleeding, profit ash potpourri collection process, determination of moisture process, and ash determination process.
Preferably, device in Gas one-level deep cooling process: device in Gas enters in-20 ℃ ~-35 ℃ condensing coils and carries out the secondary deep cooling after preliminary cooling, and the light oil that cools down and water flow in the receiving bottle; Light oil constituents dew point in the device in Gas under the negative pressure state is lower, needs lower temperature it could be condensate in the condensing coil, isolates light oil constituents.
Preferably, three grades of deep cooling processes of device in Gas: device in Gas enters and carries out three grades of degree of depth coolings in-40 ~-65 ℃ of condensing coils after the secondary deep cooling, and the light oil that cools down and water flow in the receiving bottle, isolate the good remaining moisture of wherein all light oil constituents.
Preferably, the buffering course of bleeding: for the device in Gas under the negative pressure state is extracted out from commercial plant, use the larger explosion-proof vacuum water circulating pump of rate of air sucked in required, surge flask can prolong the residence time of negative pressure state device in Gas in measurement mechanism to be measured, strengthen multistage deep cooling effect, improve accuracy and the repeatability of experiment, the device in Gas under the negative pressure state is by separating the gas G﹠W in the explosion-proof water ring vacuum pump suction moisture trap.
Preferably, profit ash potpourri collection process: after closed gas gas air intake opening valve and the explosion-proof water ring vacuum pump early gate, stop explosion-proof water ring vacuum pump; All heat eliminating medium in the emptier, static 30 ~ 45min, treat that oil in the two cover condensing coils and water flow in the receiving bottle after; In the sub-cooled container of one-level deep cooling condensing coil placement, inject 30 ~ 40 ℃ warm water, use the gas purging condensing coil, oil residual in the condensing coil, water are flowed in the receiving bottle; In the sub-cooled container of secondary deep cooling condensing coil placement, inject 0 ~ 10 ℃ warm water, use the gas purging condensing coil, oil residual in the condensing coil, water are flowed in the receiving bottle, the wet flow indicator statistics gas flow of flowing through of the device in Gas after oil, water and ash content potpourri collection process are divided Separation of Water; Collect simultaneously oil, aqueous mixtures that the condensation contain solid impurity is got off, measure the quality of potpourri.The mensuration process of biodiversity: the oil in elementary cooling bottle, receiving bottle and the filtrator, water, grey potpourri are collected in the ground conical flask of quartzose quality, and the analytically pure toluene solvant of adding 300mL, conical flask is placed on above the heating furnace, and be connected with the moisture measurement pipe, install after the glass condenser pipe, open heating furnace; Constantly record the quality of the water in the moisture measurement pipe, until there is not moisture to tell; The mensuration process of ash content quality: continue the operation division box, utilize the moisture measurement pipe with after toluene solvant drains in the conical flask; Conical flask is transferred to is incubated 3h after being heated to 815 ℃ in the muffle furnace, take out and be placed on heat-resisting porcelain plate or the sheet asbestos, in air, about cooling 5min, move and be cooled to afterwards its quality of weighing of room temperature (about 20min) in people's exsiccator; Conical flask is carried out the inspectability calcination, and each 20min is until the mass change after the double calcination is no more than 0.0010g; Quality after the last calcination be as basis (when ash content is lower than 15.00%, needn't carry out the inspectability calcination), the quality that is ash content of poor quality before and after the conical flask.
Adopt the device of technical scheme of the present invention, the preliminary cooling bottle one that under negative pressure state, is tightly connected successively, preliminary cooling bottle two, condensing coil one, condensing coil two, surge flask, explosion-proof water ring vacuum pump, steam-water separator and wet flow indicator; Described condensing coil one places the sub-cooled container one that is contained with condensed fluid, and the exit of condensing coil one is provided with receiving bottle one; Condensing coil two places the sub-cooled container two that is contained with condensed fluid, and the exit of condensing coil two is provided with the proving installation that receiving bottle two consists of, and can finish simultaneously the mensuration of liquid water content, oil content and ash content in the tested gas under negative pressure state.Use proving installation provided by the present invention, under negative pressure state to device in Gas in oil, water, the ash content assay method, what the method adopted is the method for multistage cooling, its principle is to utilize under negative pressure state the different characteristics of each hydrocarbon component condensing temperature in the unstripped gas, in the process of progressively cooling with the hydrocarbon component condensation separation of higher out, compare with the additive method of prior art, this method metering more is applicable to detect under the negative pressure state oily in the industrial methane gas, water, ash content, and measure more accurate, operation control is stable, the recovery is high, measuring error is little, the characteristics that repeatability is high are so that test result is more accurate.
Description of drawings
Fig. 1 is the synoptic diagram of the determinator of oil, water and ash content in the device in Gas under a kind of negative pressure state of the present invention;
Fig. 2 is the determinator division box synoptic diagram of oil, water and ash content in the device in Gas under a kind of negative pressure state of the present invention;
Among the figure: 1, preliminary cooling bottle one; 2, preliminary cooling bottle two; 3, the circulating cooling pump one; 4, the sub-cooled container one; 5, receiving bottle one; 51, receiving bottle two; 6, the sub-cooled container two; 7, the circulating cooling pump two; 8, surge flask; 9, explosion-proof water ring vacuum pump; 10, steam-water separator; 11, wet flow indicator; 12, valve one; 13, filtrator; 14, valve two; 15, valve three; 16, valve four; 17, valve five; 18, valve six; 19, valve seven; 20, valve eight; 21, valve ten; 22, valve 11; 23, valve 13; 24, three-way interface; 25, rain glass and thermometer, 26, condensing coil two; 27, condensing coil one; 28, plug; 29, glass condenser pipe; 30, moisture measurement pipe; 31, the ground conical flask of quartzy quality; 32, heating furnace; 33, the frozen water mixer one; 34, the frozen water mixer two.
Embodiment
The below contrasts accompanying drawing, by the description to embodiment, effect and principle of work, manufacturing process and operation using method etc. to the mutual alignment between the shape of the specific embodiment of the present invention such as related each member, structure, the each several part and annexation, each several part, be described in further detail, to help those skilled in the art inventive concept of the present invention, technical scheme had more complete, accurate and deep understanding.
Fig. 1 is oil, water and the determinator of ash content and the synoptic diagram of assay method thereof in the device in Gas under a kind of negative pressure state of the present invention; Fig. 2 is the determinator division box synoptic diagram of oil, water and ash content in the device in Gas under a kind of negative pressure state of the present invention; The determinator of oil, water and ash content in the device in Gas under a kind of negative pressure state of the present invention as shown in the figure comprises the preliminary cooling bottle 1 that is tightly connected successively by pipeline, preliminary cooling bottle 22, condensing coil 1, condensing coil 2 26, surge flask 8, explosion-proof water ring vacuum pump 9, steam-water separator 10 and wet flow indicator 11; Condensing coil 1 places the sub-cooled container 1 that is contained with condensed fluid, and the exit of condensing coil 1 is provided with receiving bottle 1; Condensing coil 2 26 places the sub-cooled container 26 that is contained with condensed fluid, and the exit of condensing coil 2 26 is provided with receiving bottle 2 51; The porch that the pipeline of bottle 22 tentatively cools off in preliminary cooling bottle one 1 UNICOMs is provided with filtrator 13; Preliminary cooling bottle 1 is placed in the frozen water mixer 1, and preliminary cooling bottle 22 places frozen water mixer 2 34; Sub-cooled container 1 and circulating cooling pump one 3 UNICOMs; Sub-cooled container 26 and circulating cooling pump 27 UNICOMs; Also be provided with one-way cock on the pipeline; Adopt the device of technical scheme of the present invention, carry out under the negative pressure state assay method of oil, water and ash content in the device in Gas, device in Gas to be measured enters preliminary cooling bottle 1 through valve 1, the device in Gas inlet is by valve 1 and valve 10 controls, through higher heavy oil fraction and the part water of boiling range under the condensation after 0 ~ 5 ℃ of preliminary cooling; Filter device in Gas afterwards through filter 13 and enter the again cooling of preliminary cooling bottle 22; Device in Gas enters-20 ~-35 ℃ of condensing coils 1 and carries out the cooling of the secondary degree of depth after the cooling of twice preliminary cooling bottle, and the light oil that cools down and water flow in the receiving bottle 1; The device in Gas of process secondary degree of depth cooling enters again carries out three grades of degree of depth coolings in-40 ~-65 ℃ of condensing coils 2 26; Through the device in Gas of three grades of degree of depth cooling by entering surge flask 8, again by explosion-proof water ring vacuum pump 9 after surge flask 8 is extracted out, enter in the moisture trap 10 with device in Gas and water separately; Device in Gas after the separation enters metered volume in the wet flow indicator 11 by valve 13 and three-way interface 24, measures temperature T, pressure P through rain glass and thermometer 25 again; In the logical device in Gas process, the situation of cold oil water slug pipeline can occur in condensing coil 1 and condensing coil 2 26 at set intervals, this moment shut-off valve 1 and valve 10, close again explosion-proof water ring pump 9, heat eliminating medium in sub-cooled container 1 and the sub-cooled container 25 is discharged, and the heat preservation sandwich layer of sub-cooled container 1 and sub-cooled container 25 outsides laid down, treat that profit in condensing coil 1 and the condensing coil 2 26 is melted into after liquid enters in receiving bottle 1 and the receiving bottle 2 51, open first coolant circulation pump 1 and coolant circulation pump 27, reopen again explosion-proof water ring pump 9, open valve 10 and valve 1, running gear is proceeded determination test; When there being the gas tolerance by cooling device to surpass 3Nm
3And when the quality of collecting oil surpasses 30g, shut-off valve 1 and valve valve 10, stop explosion-proof water ring vacuum pump 9, coolant circulation pump 1 and coolant circulation pump 27, discharge the heat eliminating medium in sub-cooled container 1 and the sub-cooled container 26, and the heat preservation sandwich layer of sub-cooled container 1 and sub-cooled container 26 outsides is laid down; Treat that condensing coil 1 and condensing coil 2 26 rise to room temperature, unload explosion-proof water ring vacuum pump 9, steam-water separator 10, wet test meter 11; The accumulative total reading of record wet flow indicator 11; After 30 ~ 45min, 30 ~ 40 ℃ hot water are injected sub-cooled container 1; In sub-cooled container 25, inject 0 ~ 10 ℃ water, in cooling system, inject purging air by valve 1 with inflator, oil residual in condensing coil 1 and the condensing coil 2 26, water, grey potpourri are purged in receiving bottle 1 and the receiving bottle 2 51; Oil, water, grey potpourri in tentatively cooling bottle 1, elementary cooling bottle 22, receiving bottle 1, receiving bottle 2 51 and the filtrator 13 are measured its quality and collect in the ground conical flask 31 of quartzy quality, and add the analytically pure toluene solvant of 300mL; Ground conical flask 31 is placed on above the heating furnace 32, and is connected with moisture measurement pipe 30, install after the glass condenser pipe 29 that the end is plugged with plug 28, open heating furnace 32; Constantly record the quality of the water in the moisture measurement pipe 30, until there is not moisture to tell; Continue the operation division box, utilize the moisture measurement pipe with after toluene solvant drains in the ground conical flask 31; Conical flask is transferred to is incubated 3h after being heated to 815 ℃ in the muffle furnace, cooling, its quality of weighing, and then put into muffle furnace 30min, taking-up is placed on heat-resisting porcelain plate or the sheet asbestos, in air, about cooling 5min, move and be cooled to its quality of weighing after the room temperature in people's exsiccator, cool time about 20min; Ground conical flask 31 is carried out the inspectability calcination, and each 20min is until the mass change after the double calcination is no more than 0.0010g; Quality after the last calcination when ash content is lower than 15.00%, needn't be carried out the inspectability calcination as basis, and the quality of the device in Gas volume by recording, the quality of water, oil, the Mass Calculation of ash obtain oil, water, ash content in the device in Gas; In the middle of the device operation, collect behind the wet flow indicator 11 and the device in Gas sample in the surge flask 8, and measure the CO in the sample
2And H
2S.
The device in Gas volume calculates under the standard state, behind the reading of the wet flow indicator before and after record is measured, temperature T, pressure P, the analysis wet flow indicator 11 and the CO in the device in Gas sample in the surge flask 8
2, H
2S content; Computing formula is suc as formula (1):
In the formula:
L-device in Gas volume (under the standard state), unit is (Nm
3);
V
1, V
2 Wet test meter 11 readings before the-experiment, unit is (L);
V
3, V
4 Wet test meter 11 readings after the-experiment, unit is (L);
Atmospheric pressure under P-experimental state, unit are (Pa);
1atm-standard atmospheric pressure, unit are (Pa);
Temperature behind T-air deep-cooling, unit be (℃);
C
1The CO of device in Gas sample in the-surge flask
2Volumetric concentration;
C
2The H of device in Gas sample in the-surge flask
2The S volumetric concentration;
C
3The CO of-wet flow indicator after gas gas sample
2Volumetric concentration;
C
4The H of-wet flow indicator after gas gas sample
2The S volumetric concentration.
Water in the device in Gas, light oil and ash content quality and calculating, the quality of the preliminary cooling bottle 1 before and after record is measured, preliminary cooling bottle 22, receiving bottle 1, receiving bottle 2 51, filtrator 13; Computing formula is suc as formula (2):
M
1=(m
1-m’
1)+(m
2-m’
2)+(m
3-m’
3)+(m
4-m’
4)+(m
5-m’
5)
…………………（2）
In the formula:
m
1The quality of preliminary cooling bottle 1 after the-experiment, unit is (g);
m
2The quality of preliminary cooling bottle 22 after the-experiment, unit is (g);
m
3The quality of receiving bottle 1 after the-experiment, unit is (g);
m
4The quality of receiving bottle 2 51 after the-experiment, unit is (g);
m
5The quality of-experiment after-filter 13, unit is (g);
M '
1The quality of preliminary cooling bottle 1 after the-experiment, unit is (g);
M '
2The quality of preliminary cooling bottle 22 after the-experiment, unit is (g);
m
3The quality of receiving bottle 1 after the-experiment, unit is (g);
M '
4The quality of-experiment receiving bottle 2 51, unit is (g);
M '
5The quality of-experiment after-filter 13, unit is (g);
Ash content Mass Calculation in the device in Gas, the quality of the ground conical flask 31 of quartzy quality before and after record is measured; Computing formula is suc as formula (3):
M
4=(m
6-m’
6) …………………（3）
In the formula:
m
6The quality of corresponding ground conical flask 31 after the-experiment, unit is (g);
M '
6The quality of ground conical flask 31 before the-experiment, unit is (g).
Oil quality in the device in Gas is calculated, and it is characterized in that: by water, light oil and ash content quality with deduct biodiversity and the ash content quality obtains; Computing formula is suc as formula (4):
M
3=M
1-M
2-M
4 …………………（4）
In the formula:
M
1-by water, light oil and ash content quality and, unit is (g);
M
2-biodiversity, unit are (g);
M
4-ash content quality, unit is (g).
Device in Gas (1Nm
3) in liquid water content calculate, with quality divided by device in Gas volume (standard state); Computing formula is suc as formula (5):
In the formula:
M
2The quality of-water, unit is (g);
L-device in Gas volume (standard state), unit is (Nm
3).
Device in Gas (1Nm
3) in oil content calculate with oil quality divided by the device in Gas volume; Computing formula is suc as formula (6):
In the formula:
M
3The quality of-oil, unit is (g);
L-device in Gas volume (standard state), unit are (Nm
3).
Device in Gas (1Nm
3) in ash content calculate with grey quality divided by the device in Gas volume; Computing formula is suc as formula (7):
In the formula:
M
4-ash content quality, unit is (g);
L-device in Gas volume (standard state), unit are (Nm
3).
Adopt the device of technical scheme of the present invention, with under the negative pressure state to the assay method of oil, water, ash content in the device in Gas, what the method adopted is the method for multistage cooling, under negative pressure state, can finish simultaneously the mensuration of liquid water content, oil content and ash content in the tested device in Gas, the metering of this method more is applicable to detect under the negative pressure state oil, water, ash content in the industrial methane gas, and measure more accurate, the characteristics that operation control is stable, the recovery is high, measuring error is little, repeatability is high are so that test result is more accurate.
Above-described embodiment is described preferred implementation of the present invention; be not that scope of the present invention is limited; design under the prerequisite of spirit not breaking away from the present invention; various distortion and improvement that the common engineering technical personnel in this area make technical scheme of the present invention all should fall in the definite protection domain of claims of the present invention.
Claims (10)
1. the determinator of oil, water and ash content in the device in Gas under the negative pressure state is characterized in that: comprise the preliminary cooling bottle one that is tightly connected successively by connecting tube, preliminary cooling bottles two, condensing coil one, condensing coil two, surge flask, explosion-proof water ring vacuum pump, steam-water separator and wet flow indicator; Described condensing coil one places the sub-cooled container one that is contained with condensed fluid, and the exit of condensing coil one is provided with receiving bottle one; Condensing coil two places the sub-cooled container two that is contained with condensed fluid, and the exit of condensing coil two is provided with receiving bottle two.
2. according to the determinator of oil, water and ash content in the device in Gas under the negative pressure state claimed in claim 1, it is characterized in that: the porch that the pipeline of bottle two tentatively cools off in described preliminary cooling bottle one UNICOM is provided with filtrator; Described preliminary cooling bottle one is placed in the frozen water mixer one, and preliminary cooling bottle two places frozen water mixer two.
3. according to the determinator of oil, water and ash content in the device in Gas under the negative pressure state claimed in claim 1, it is characterized in that: described sub-cooled container one and circulating cooling pump one UNICOM; Sub-cooled container two and circulating cooling pump two UNICOMs; The outer wall of sub-cooled container one and sub-cooled container two is equipped with heat preservation sandwich layer.
4. according to the determinator of oil, water and ash content in the device in Gas under the negative pressure state claimed in claim 1, it is characterized in that: also be provided with a plurality of one-way cocks on the described connecting tube.
5. a right to use requires under the 1 described negative pressure state in the device in Gas determinator of oil, water and ash content to carry out under the negative pressure state assay method of oil, water and ash content in the device in Gas, it is characterized in that: the method comprises following process: the device in Gas under a certain amount of negative pressure state is extracted out from commercial plant place described determinator, through tentatively cooling off, pass through again the secondary deep cooling, after three grades of subzero treatments of mistake, enter surge flask; Device in Gas in the surge flask is separated moisture after extracting out via water ring vacuum pump in steam-water separator, the device in Gas after Separation of Water divides is added up gas flow through wet flow indicator; Collecting the oil that contains a certain amount of solid impurity, aqueous mixtures that condensation gets off moves on in the ground conical flask that quartz glass makes and weighs, again the ground conical flask is connected with device for measuring moisture, residue continues heating, until there is not liquid to exist in the ground conical flask; Conical flask is transferred to is incubated 3h after being heated to 815 ℃ in the muffle furnace, cooling, its quality of weighing is put into muffle furnace 30min again, takes out cooling, and its quality of weighing namely gets ash content again, and the quality of potpourri deducts liquid water content and ash content obtains oil content; Measure the CO in surge flask and the wet test meter after gas gas
2Content records the device in Gas total amount.
6. according to the assay method of oil, water and ash content in the device in Gas under the negative pressure state claimed in claim 5, it is characterized in that: described preliminary cooling is to be under 0 ℃ ~ 4 ℃ the condition flow velocity of device in Gas to be played the effect of buffering in temperature, prolong the residence time of device in Gas in measurement mechanism, condensation goes out heavy oil fraction and the part water in the device in Gas.
7. according to the assay method of oil, water and ash content in the device in Gas under the negative pressure state claimed in claim 5, it is characterized in that: described device in Gas is-20 ℃ ~-35 ℃ in temperature and carries out the secondary deep cooling, isolates light oil constituents.
8. according to the assay method of oil, water and ash content in the device in Gas under the negative pressure state claimed in claim 5, it is characterized in that: described three grades of deep coolings are will further cool off through the device in Gas behind the secondary deep cooling under temperature is-40 ℃～-65 ℃ condition, isolate wherein all light oil constituents and remaining moisture.
9. according to the assay method of oil, water and ash content in the device in Gas under the negative pressure state claimed in claim 5, it is characterized in that: the device in Gas under the described negative pressure state is by separating the gas G﹠W in the explosion-proof water ring vacuum pump suction moisture trap.
10. according to the assay method of oil, water and ash content in the device in Gas under the negative pressure state claimed in claim 5, it is characterized in that: the wet flow indicator statistics gas flow of flowing through of the device in Gas after described oil, water and ash content potpourri collection process are divided Separation of Water; Collect simultaneously oil, aqueous mixtures that the condensation contain solid impurity is got off, measure the quality of potpourri.
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| CN2012105242328A CN103018131A (en) | 2012-12-07 | 2012-12-07 | Determining device and method for oil water and ash contents in gas in negative pressure state |
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| CN2012105242328A CN103018131A (en) | 2012-12-07 | 2012-12-07 | Determining device and method for oil water and ash contents in gas in negative pressure state |
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| CN105065912A (en) * | 2015-08-10 | 2015-11-18 | 珠海优特电力科技股份有限公司 | Work method of liquid metering equipment and liquid metering equipment |
| CN108426801A (en) * | 2018-04-23 | 2018-08-21 | 西南石油大学 | A kind of method of the easy precipitate content of low temperature in measurement natural gas |
| CN108507901A (en) * | 2018-06-21 | 2018-09-07 | 河南省煤气(集团)有限责任公司义马气化厂 | The analysis method of trace carbinol in a kind of purified gas |
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| CN105065912A (en) * | 2015-08-10 | 2015-11-18 | 珠海优特电力科技股份有限公司 | Work method of liquid metering equipment and liquid metering equipment |
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| CN110243720A (en) * | 2019-07-31 | 2019-09-17 | 海德里希(厦门)真空机械制造有限公司 | A kind of embedded residual gas content measuring method of liquid material and pasty material |
| CN113567055A (en) * | 2021-06-30 | 2021-10-29 | 黔西县黔希煤化工投资有限责任公司 | Method for measuring leakage amount of process gas in steam heat exchanger |
| CN113567055B (en) * | 2021-06-30 | 2024-05-28 | 黔西县黔希煤化工投资有限责任公司 | Method for measuring leakage amount of process gas in steam heat exchanger |
| CN114739858A (en) * | 2022-04-26 | 2022-07-12 | 张玲 | System and method for detecting content of tar and ash in gas |
| CN115300941A (en) * | 2022-08-17 | 2022-11-08 | 青岛科技大学 | A kind of method for separating heavy oil and light oil from oil-water mixture |
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Application publication date: 20130403 |