CN105466807A - Apparatus and method for detecting water content in coal tar - Google Patents
Apparatus and method for detecting water content in coal tar Download PDFInfo
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- CN105466807A CN105466807A CN201410437584.9A CN201410437584A CN105466807A CN 105466807 A CN105466807 A CN 105466807A CN 201410437584 A CN201410437584 A CN 201410437584A CN 105466807 A CN105466807 A CN 105466807A
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Abstract
The present invention discloses an apparatus for detecting the water content in coal tar. The apparatus comprises a closed container (1), a sample injection device (2), a first temperature measurement device (3) and a pressure measurement device (4), wherein the closed container (1) is used for placing samples 1 and 2, the sample injection device (2) is used for conveying the sample 1 and/or the sample 2 into the closed container (1), the first temperature measurement device (3) and the pressure measurement device (4) are respectively used for measuring the temperature and the pressure in the closed container (1), the sample injection device (2), the first temperature measurement device (3) and the pressure measurement device (4) are respectively connected to the closed container (1) in a sealed manner, the sample 1 is calcium carbide, and the sample 2 is coal tar. The invention further discloses a method for detecting the water content in coal tar. With the apparatus and the method of the present invention, the water content in the coal tar can be quickly, accurately and continuously detected.
Description
Technical field
The present invention relates to a kind of apparatus and method detecting water cut in coal tar.
Background technology
No matter be in laboratory, pilot-plant or suitability for industrialized production, in the coal tar that pyrolysis of coal produces, all contain a large amount of water.In coal tar, water cut has a direct impact the value of coal tar and later stage hydrogenation deep processing, so the quick and precisely detection of coal tar water cut is particularly important.
In existing patented technology file and standard, the quick detection for water cut in coal tar also has more list of references, but mostly has very strong limitation, is difficult to accomplish to detect water cut quickly and accurately.Such as patent CN102914559A discloses a kind of pick-up unit of coal tar water cut, this device improves on existing coal tar device for detecting water content, principle adopts the method that physics distills, its innovative point is the thermometer measuring gas phase temperature to be built in flask upper elbow, the working fluid of backflow separates with the steam of rising, forms closed-loop path.The amount of the sample of the method needs of physics distillation is larger, and detection time is relatively long, and accuracy is difficult to ensure, is not suitable for the Fast And Accurate Determination of water cut in a small amount of coal tar sample in laboratory.GB GB/T24214-2009 establishes the method for quick of coal tar water content in oil, the party's ratio juris adopts the moisture in calcium carbide and coal tar to react, generate acetylene, use amount tracheae measures the volume generating gas, and then obtains moisture in coal tar.But the equipment involved by device of GB coal tar high-speed moisture determination is many, and junction is more, easily leaks gas during test; And for the larger coal tar of water cut, the reaction of calcium carbide and water is very violent, the acetylene generated carries calcium carbide powder possibly and is flushed to downstream by wireway, cause accuracy and the applicability existing problems of the method, as calculated for the coal tar of water cut more than 20%, national standard method cannot Measurement accuracy; And all need again to assemble device after each test, horizontal survey cannot be carried out to same sample continuously, fast.
Therefore, need a kind of fast, accurately and can the apparatus and method of water cut in continuous detecting coal tar.
Summary of the invention
To the object of the invention is to overcome in prior art cannot fast, accurately, the defect of water cut in continuous detecting coal tar, provide a kind of scope of application wider, fast, accurately, the apparatus and method of water cut in continuous detecting coal tar or specific aqueous liquid potpourri.
The present inventor finds in an experiment, coal tar and excessive calcium carbide is reacted in closed container, and under identical temperature conditions, the pressure differential Δ P before and after reaction in closed container and the water cut in coal tar have following relation:
In formula: M is water cut in coal tar, M
h2Ofor the molal weight of water; Δ P is the pressure differential before and after reaction in closed container; V be closed container airtight time volume; m
electricityfor the quality of calcium carbide; ρ
electricityfor calcium carbide density; R is ideal gas constant; T is observed temperature; m
liquidfor the quality of coal tar.
According to above-mentioned relation formula, except Δ P, other coefficient is determined value when this system air-tight state, and the volume ratio of volume change and actual container that water and calcium carbide react the solid product generated can be ignored, so can think Δ P and m herein
waterfor linear relationship, i.e. m
water=k Δ P,
In formula: m
waterfor the water yield reacted with calcium carbide; K is slope, with the coefficient of closed container volume, calcium carbide volume, temperature correlation, can carry out linear calibration, to determine k before testing.
Therefore, above-mentioned relation formula can be reduced to:
Therefore, to achieve these goals, on the one hand, the invention provides a kind of device detecting water cut in coal tar, described device comprises closed container, sample introduction equipment, first temperature measuring equipment and pressure instrumentataion, closed container is for placing sample 1 and sample 2, sample introduction equipment is used in closed container, carry sample 1 and/or sample 2, first temperature measuring equipment and pressure instrumentataion are respectively used to measure the temperature and pressure in closed container, sample introduction equipment, first temperature measuring equipment and pressure instrumentataion are tightly connected with closed container respectively, wherein, sample 1 is calcium carbide, sample 2 is coal tar.
Preferably, mixing plant is provided with in closed container.
Preferably, the wall of closed container is provided with exhausr port and air intake opening, exhausr port is for discharging air in closed container and inert gas, and air intake opening is used for being filled with inert gas in closed container.
Preferably, described device also comprises the well heater for heating closed container.
Preferably, described closed container is provided with and allows the injection port that passes of described sample introduction equipment, and described injection port is provided with packoff, and make described sample introduction equipment in closed container during sample introduction, closed container still keeps leakproofness.
Second aspect, the invention provides a kind of method detecting water cut in coal tar, described method comprises:
(1) in confined conditions, sample 1 and sample 2 are reacted in closed container, and wherein, sample 1 is calcium carbide, and sample 2 is coal tar;
(2) after question response terminates, the pressure differential Δ P under identical temperature conditions before and after assaying reaction in closed container, and calculate the water cut in coal tar by pressure differential Δ P.
Preferably, calcium carbide is excessive relative to the water in coal tar.
Preferably, the mode of described identical temperature conditions is provided to comprise: described closed container is placed in water bath with thermostatic control.
Preferably, the reaction in closed container is made to carry out under an inert atmosphere.
Preferably, the reaction in closed container is made under agitation to carry out.
Preferably, the water cut through type (I) in coal tar calculates,
Wherein, M is water cut in coal tar, M
h2Ofor the molal weight of water; Δ P is the pressure differential before and after reaction in closed container; V be closed container airtight time volume; m
electricityfor the quality of calcium carbide; ρ
electricityfor calcium carbide density; R is ideal gas constant; T is observed temperature; m
liquidfor the quality of coal tar.
Preferably, the water cut through type (II) in coal tar calculates,
Wherein, M is water cut in coal tar; K is slope; Δ P is the pressure differential before and after reaction in closed container; m
liquidfor the quality of coal tar.
Preferably, described method is carried out as above detection in the device of water cut in coal tar.
Apparatus and method of the present invention, calculate the water cut in coal tar by the change of pressure in closed container, fast, accurately; Because reaction unit is airtight, even if the coal tar larger to water cut, also can detect fast and accurately, namely be applicable to the mensuration of various water cut; Apparatus structure of the present invention is simple, only need take a breath at every turn and can carry out test next time, can realize continuous detecting after having tested; These apparatus and method can be widely used in the mensuration of water cut in all aqueous liquid potpourris do not reacted with calcium carbide.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Accompanying drawing explanation
Fig. 1 is the structural representation of a kind of preferred implementation of the device of water cut in detection coal tar of the present invention.
Description of reference numerals
1 closed container; 2 sample introduction equipment; 3 first temperature measuring equipments; 4 pressure instrumentataions; 5 second temperature measuring equipments; 6 injection ports; 7 mixing plants; 8 exhausr ports; 9 air intake openings; 10 guide cylinders; 11 water baths; 12 supports.
Embodiment
Below the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
On the one hand, as shown in Figure 1, the invention provides a kind of device detecting water cut in coal tar, this device comprises closed container 1, sample introduction equipment 2, first temperature measuring equipment 3 and pressure instrumentataion 4, closed container 1 is for placing sample 1 and sample 2, sample introduction equipment 2 for carrying sample 1 and/or sample 2 in closed container 1, first temperature measuring equipment 3 and pressure instrumentataion 4 are respectively used to measure the temperature and pressure in closed container 1, sample introduction equipment 2, first temperature measuring equipment 3 and pressure instrumentataion 4 are tightly connected with closed container 1 respectively, wherein, sample 1 is calcium carbide, sample 2 is coal tar.
In the present invention, for the size and shape of closed container 1 without particular/special requirement, can adopt those skilled in the art the structure of thinkable various applicable gas diffusion and gas displacement, be preferably cube or cylindrical shape, in order to operate with easy to carry, such as, closed container 1 can be cylindrical, volume can be 10-50L, and internal diameter can be 10-20cm, and height can be 30-40cm.
In the present invention, sample introduction equipment 2, for carrying sample 1 and/or sample 2 in closed container 1, has namely referred to three kinds of input modes, first in closed container 1, loads sample 1, carries sample 2 by sample introduction equipment 2 in closed container 1; Or first in closed container 1, load sample 2, in closed container 1, carry sample 1 by sample introduction equipment 2; Or by sample introduction equipment 2 successively respectively to carrying sample 1 and sample 2 in closed container 1, can first carry sample 1, then carrying sample 2, also can first carry sample 2, then carry sample 1.Be preferably first kind of way.
In the present invention, sample introduction equipment 2, first temperature measuring equipment 3 and pressure instrumentataion 4 are tightly connected with closed container 1 respectively, for the mode be tightly connected without particular/special requirement, the thinkable various mode of those skilled in the art can be adopted to be connected and sealed.
In the present invention, in order to make calcium carbide and water more fully react faster, namely in order to make test result more quick and precisely, in closed container 1, be preferably provided with mixing plant 7.It will be understood by those skilled in the art that mixing plant 7 is to stir material accelerated reaction, therefore, mixing plant 7 is preferably arranged on the bottom in closed container 1, as shown in Figure 1.
In the present invention, in order to prevent the water vapor in air, test result is impacted, the wall of closed container 1 is preferably provided with exhausr port 8 and air intake opening 9, exhausr port 8 is for discharging the gas in closed container 1, and air intake opening 9 for being filled with inert gas in closed container 1.When operative installations detects, react again after the air displacement in closed container 1 being gone out by exhausr port 8 and air intake opening 9.After one-time detection completes, exhausr port 8 and air intake opening 9 also can be used for being replaced away by the acetylene gas of generation, to detect next time.For the particular location of exhausr port 8 and air intake opening 9 without particular/special requirement, if can substitution gas be played and do not affect bottom calcium carbide stir effect, such as can be arranged on the sidewall of closed container 1, in order to substitution gas better, the position of exhausr port 8 is preferably higher than air intake opening 9 and closer to closed container top.In order to better ensure the impermeability of exhausr port 8 and air intake opening 9, and in order to manipulate the open and close of exhausr port 8 and air intake opening 9 more easily, exhausr port 8 and air intake opening 9 are preferably provided with valve.
In the present invention, in order to make temperature when measuring pressure before and after reaction identical, device of the present invention preferably also comprises the well heater for heating closed container 1.Conveniently regulate the temperature in closed container 1, well heater is preferably water bath 11, and closed container 1 is placed in water bath 11, and water bath 11 is for regulating the temperature in closed container 1.Water bath with thermostatic control can be filled with identical to ensure the temperature of reacting in the closed container 1 of front and back in water bath 11.In order to make whole confined space temperature consistent, the sidewall of water bath 11 preferably higher than the height of the confined space of closed container 1, with the water bath with thermostatic control making the whole confined space of closed container 1 all can be placed in water bath 11.
In the present invention, in order to make the temperature of the whole confined space of closed container 1 more consistent, the bottom of closed container 1 does not preferably contact the bottom of water bath 11, is namely preferably provided with support 12 in water bath 11, closed container 1 is placed in water bath 11 by support 12, as shown in Figure 1.
In the present invention, in order to measure the temperature of water bath with thermostatic control, this device preferably also comprises the second temperature measuring equipment 5, second temperature measuring equipment 5 for measuring the temperature of water-bath in water bath 11, as shown in Figure 1.
In the present invention, for the first temperature measuring equipment 3 and the second temperature measuring equipment 5 without particular/special requirement, the various temperature measuring equipments that this area is conventional can be adopted, such as thermometer; For pressure instrumentataion 4 also without particular/special requirement, the various pressure instrumentataions can commonly used for this area, such as U-shaped differential manometer.
Type selecting scope for differential manometer can need to select according to different measuring precision and measurement range, such as, for the closed container 1 that volume is 10L, 5mL water and calcium carbide react, under the condition of 25 DEG C, pressure increase is about 35Kpa, when surveyed liquid water content is 0.05mL, container inner pressure is changed to 0.344Kpa, when surveyed liquid water content is 0.005mL, container inner pressure is changed to 0.0344Kpa, therefore, for the closed container 1 that volume is 10L, sample introduction is the liquid of 5mL, under the condition of 25 DEG C, the type selecting scope of differential manometer can be 0.01-50Kpa.
In order to make sample introduction equipment 2 convenient and hermetically to sample introduction in closed container 1, preferably, closed container 1 is provided with the injection port 6 allowing sample introduction equipment 2 to pass, and injection port 6 is provided with packoff, make sample introduction equipment 2 in closed container 1 during sample introduction, closed container 1 still keeps leakproofness.In order to more convenient to operate, sample introduction equipment 2 preferably includes needle tubing and syringe needle, and packoff is preferably the rubber plug closing injection port 6, makes syringe needle penetrate rubber plug to be pushed in closed container 1 by the sample in needle tubing when carrying sample.
In the present invention, do not splash on the sidewall of closed container 1 to make sample introduction, can completely and calcium carbide react, namely in order to more stably keep the direction of sample introduction, preferably, closed container 1 is provided with guide cylinder 10 in the position of the corresponding injection port 6 of external container, guide cylinder 10 for guaranteeing the sample introduction direction of sample introduction equipment 2, as shown in Figure 1.
If device of the present invention needs to carry out signal output, thermometer usable thermocouple replaces, U-shaped differential manometer can use suitable pressure transducer differential pressure transmitter to replace, sensor can connect on computers by control system, automatically can be calculated the water cut of surveyed coal tar by pressure change.Device of the present invention can also repack a set of online detection instrument into.
According to one of the present invention preferred embodiment, as shown in Figure 1, in detection coal tar of the present invention, the device of water cut comprises closed container 1, sample introduction equipment 2, first temperature measuring equipment 3, pressure instrumentataion 4, injection port 6, mixing plant 7, exhausr port 8, air intake opening 9, guide cylinder 10, water bath 11, support 12 and the second temperature measuring equipment 5.Closed container 1 is cylindrical, and volume is 10-50L, and internal diameter is 10-20cm, and height is 30-40cm; Sample introduction equipment 2 comprises needle tubing and syringe needle; First temperature measuring equipment 3 and the second temperature measuring equipment 5 are thermometer; Pressure instrumentataion 4 is U-shaped differential manometer; Closed container 1 is provided with the injection port 6 allowing sample introduction equipment 2 to pass, and injection port 6 is provided with packoff, and packoff is the rubber plug of closed injection port 6; Mixing plant 7 is arranged on the bottom centre in closed container 1; Exhausr port 8 and air intake opening 9 are separately positioned on the both sides sidewall of closed container 1, and the position of exhausr port 8 is higher than air intake opening 9; Guide cylinder 10 is arranged on the position of the outside corresponding injection port 6 of closed container 1 upper container, sample introduction equipment 2 by guide cylinder 10 to sample introduction in closed container 1; Closed container 1 is placed in water bath 11 by support 12, and the sidewall of water bath 11 is higher than the height of the confined space of closed container 1; Second temperature measuring equipment 5 is for measuring the temperature of water-bath in water bath 11.
Second aspect, the invention provides a kind of method detecting water cut in coal tar, the method comprises:
(1) in confined conditions, sample 1 and sample 2 are reacted in closed container 1, and wherein, sample 1 is calcium carbide, and sample 2 is coal tar;
(2) after question response terminates, the pressure differential Δ P under identical temperature conditions before and after assaying reaction in closed container 1, and calculate the water cut in coal tar by pressure differential Δ P.
The present invention's pressure differential be intended to by reacting front and back under temperature conditions identical in closed container 1 calculates the water cut in coal tar, therefore, what those skilled in the art should understand that is, react completely to make the water in coal tar, namely in order to make test result more accurate, calcium carbide is excessive relative to the water in coal tar.
In the present invention, for the amount of calcium carbide without particular/special requirement, as long as excessive relative to the water in coal tar, namely ensure the water complete reaction in coal tar.For the cylindrical closed vessel 1 of 10-50L, after the addition of calcium carbide can add for making calcium carbide, form the calcium carbide layer of 4-6cm in the bottom of closed container 1.
In order to make the water in calcium carbide and coal tar react better, calcium carbide preferably adopts calcium carbide powder.The gas forming amount of calcium carbide powder is preferably greater than 300L/kg, is more preferably 300-500L/kg; Granularity is preferably 0.1-1cm, is more preferably 0.2-0.5cm.
In the present invention, for the amount of the coal tar reacted with excessive calcium carbide without particular/special requirement, as long as relative to the water in coal tar, calcium carbide is excessive.Such as, relative to volume be 10-50L, internal diameter is 10-20cm, the high cylindrical closed vessel 1 for 30-40cm, when the addition of calcium carbide is the calcium carbide layer forming 4-6cm after calcium carbide is added in the bottom of closed container 1, the amount of the coal tar added during each detection can be 3-8mL.
When the employing closed container 1 of above-mentioned specification, the calcium carbide of above-mentioned amount and coal tar, as calculated, the calcium carbide amount that each test uses is no more than 4g, with the bulk density of calcium carbide in container for 1g/cm
3calculate, the calcium carbide in container can at least 300 tests.
It will be understood by those skilled in the art that the temperature conditions that identical temperature conditions refers to when reacting front and back mensuration pressure is identical.Identical for the temperature made when measuring pressure before and after reaction, the thinkable various mode of those skilled in the art can be adopted, such as, well heater can be adopted to regulate, provide the mode of identical temperature conditions to preferably include: closed container 1 is placed in water bath with thermostatic control.In order to make whole confined space temperature consistent, preferably the whole confined space of closed container 1 is all placed in water bath with thermostatic control.For the temperature of water bath with thermostatic control without particular/special requirement, can be the ordinary temperature that calcium carbide and water react, such as, can be 25-40 DEG C.
In the present invention, in order to prevent the water vapor in closed container 1 in air from impacting test result, the reaction in closed container 1 is preferably made to carry out under an inert atmosphere.Namely in closed container 1, be filled with inert gas air displacement is gone out.For inert gas without particular/special requirement, only otherwise affect the reaction of calcium carbide and water, such as, can be nitrogen.
In the present invention, in order to make calcium carbide and water more fully react faster, namely in order to make test result more quick and precisely, the reaction in closed container 1 is preferably made under agitation to carry out.For the speed stirred without particular/special requirement, such as, can be 2-5rpm.
In the present invention, the water cut in coal tar calculates preferably by formula (I),
Wherein, M is water cut in coal tar, M
h2Ofor the molal weight of water; Δ P is the pressure differential before and after reaction in closed container 1; V be closed container 1 airtight time volume; m
electricityfor the quality of calcium carbide; ρ
electricityfor calcium carbide density; R is ideal gas constant 8.314J/ (mol*k); T is observed temperature; m
liquidfor the quality of coal tar.
As described in summary of the invention, according to above-mentioned relation formula, except Δ P, other coefficient is determined value when this system air-tight state, and the volume ratio of volume change and actual container that water and calcium carbide react the solid product generated can be ignored, so can think Δ P and m herein
waterfor linear relationship, i.e. m
water=k Δ P,
In formula: m
waterfor the water yield reacted with calcium carbide; K is slope, with the coefficient of closed container volume, calcium carbide volume, temperature correlation, can carry out linear calibration, to determine k before testing.
Therefore, the water cut in coal tar also calculates preferably by formula (II),
Wherein, M is water cut in coal tar; K is slope; Δ P is the pressure differential before and after reaction in closed container (1); m
liquidfor the quality of coal tar.
In the present invention, for slope k, linear calibration can be carried out before testing to determine k, for the method for linear calibration without particular/special requirement, the thinkable various method of those skilled in the art can be adopted, such as, the computing method of k can comprise: by the water of known difference amount and excessive calcium carbide being reacted in closed container 1 respectively, the pressure under identical temperature conditions before and after assaying reaction in closed container 1, calculating pressure difference Δ P', and through type (III) calculates
M
water=k Δ P'(III)
Wherein, m
waterfor the quality of water, Δ P' is the pressure differential before and after water and calcium carbide react in closed container 1.Such as, be 10-20cm, the high cylindrical closed vessel 1 for 30-40cm relative to 10-50L, internal diameter, bottom is covered with the calcium carbide layer of 4-6cm, can add 0.1,0.5,1,2,3,4 and 5ml water respectively, and record the reading of pressure instrumentataion 4 before and after every secondary response, calculate Δ P
1'-Δ P
7'.According to water weight m
waterwith the relation of Δ P', according to formula (III) slope calculations k.Also can according to m
watermap with Δ P', ask the slope of figure center line, i.e. slope k.
It will be understood by those skilled in the art that and should according to circumstances regular k be calibrated, and affect test result according to access times replacing calcium carbide to prevent calcium carbide and water from cannot react completely.
The inventive method is preferably carried out as above detection in the device of water cut in coal tar.
As mentioned above, after one-time detection completes, exhausr port 8 and air intake opening 9 also can be used for being replaced away by the acetylene gas of generation, to detect next time.Namely the inventive method also comprises after pressure measurement completes, first open after the pressure of closed container 1 reduced to normal pressure by exhausr port 8, then open air intake opening 9, utilize the acetylene produced in inert gas replacement closed container 1, replace rear air intake opening 9 of first closing and closed exhausr port 8 again, can start to test next time.
It will be understood by those skilled in the art that method and apparatus of the present invention not only can be used for the detection of water cut in coal tar, also can be used for the detection of water cut in all aqueous mixtures do not reacted with calcium carbide.
According to one of the present invention preferred embodiment, the inventive method specifically comprises:
By closed container 1 dry 6-10 hour at 80-100 DEG C before detection starts, to guarantee that its inside surface does not have water, then closed container 1 is placed on the support 12 of water bath 11, calcium carbide is added in closed container 1, water bath with thermostatic control is injected in water bath 11, the height of water-bath makes the whole confined space of closed container 1 all be placed in water-bath, open exhausr port 8 and air intake opening 9, the nitrogen of temperature identical with water-bath is used to purge in container, observe the first temperature measuring equipment 3, the reading of the second temperature measuring equipment 5 and pressure instrumentataion 4, to treat in closed container 1 temperature and constant temperature identical with bath temperature, after constant voltage 30min, first close air intake opening 9, treat temperature in closed container 1, pressure does not change rear closedown exhausr port 8, closed container 1 is made to enter air-tight state.
0.1,0.5,1,2,3,4 and 5mL water is got respectively with sample introduction equipment 2, then sample introduction equipment 2 is prolonged guide cylinder 10 and vertically insert injection port 6, start sample introduction, open mixing plant 7 subsequently, after temperature in closed container 1 is identical with bath temperature and pressure no longer changes, the reading of record pressure instrumentataion 4, and the pressure differential Δ P calculating the pressure instrumentataion of each test
1'-Δ P
7'.According to formula (III) m
water=k Δ P', obtains slope k.
After each detection completes, first open exhausr port 8, after pressure reduces to normal pressure in closed container 1, then open air intake opening 9, utilize nitrogen to replace the acetylene produced in container.When in closed container 1, temperature is identical with bath temperature, after pressure is identical with atmospheric pressure, first closes air intake opening 9 and close exhausr port 8 again and can start to test next time.
Coal tar sample to be detected is got with sample introduction equipment 2, sample introduction reacting in a manner described, after temperature in closed container 1 is identical with bath temperature and pressure no longer changes, the reading of record pressure instrumentataion 4, and calculate the pressure differential Δ P of pressure instrumentataion, according to formula (II)
obtain the water cut M in solution.
In the present invention, sampling can sample with reference to GB/T1999-2008.
Embodiment
The present invention is further illustrated for following embodiment, but therefore do not limit the present invention.
In the following Examples and Comparative Examples:
Sampling samples according to GB/T1999-2008.
All adopt Fig. 1 shown device to detect, device is specially: be made up of closed container 1, sample introduction equipment 2, first temperature measuring equipment 3, pressure instrumentataion 4, injection port 6, mixing plant 7, exhausr port 8, air intake opening 9, guide cylinder 10, water bath 11, support 12 and the second temperature measuring equipment 5.Closed container 1 is cylindrical; Sample introduction equipment 2 comprises needle tubing and syringe needle; First temperature measuring equipment 3 and the second temperature measuring equipment 5 are thermometer; Pressure instrumentataion 4 is U-shaped differential manometer; Injection port 6 is arranged on closed container 1, and injection port 6 is provided with packoff, and packoff is the rubber plug of closed injection port 6; Mixing plant 7 is arranged on the bottom centre in closed container 1; Exhausr port 8 and air intake opening 9 are separately positioned on the both sides sidewall of closed container 1, and the position of exhausr port 8 is higher than air intake opening 9; Guide cylinder 10 is arranged on the position of the outside corresponding injection port 6 of closed container 1 upper container, sample introduction equipment 2 by guide cylinder 10 to sample introduction in closed container 1; Closed container 1 is placed in water bath 11 by support 12, and the sidewall of water bath 11 is higher than the height of the confined space of closed container 1; Second temperature measuring equipment 5 is for measuring the temperature of water-bath in water bath 11.
Detection starts front and is all handled as follows after completing:
By closed container 1 at 80 DEG C dry 8 hours before detection starts, to guarantee that its inside surface does not have water, then closed container 1 is placed on the support 12 of water bath 11, calcium carbide is added in closed container 1, water bath with thermostatic control is injected in water bath 11, the height of water-bath makes the whole confined space of closed container 1 all be placed in water-bath, open exhausr port 8 and air intake opening 9, the nitrogen of temperature identical with water-bath is used to purge in container, observe the first temperature measuring equipment 3, the reading of the second temperature measuring equipment 5 and pressure instrumentataion 4, to treat in closed container 1 temperature and constant temperature identical with bath temperature, after constant voltage 30min, first close air intake opening 9, treat temperature in closed container 1, pressure does not change rear closedown exhausr port 8, closed container 1 is made to enter air-tight state.
After each detection completes, first open exhausr port 8, after pressure reduces to normal pressure in closed container 1, then open air intake opening 9, utilize nitrogen to replace the acetylene 10min produced in container.When in closed container 1, temperature is identical with bath temperature, after pressure is identical with atmospheric pressure, first closes air intake opening 9 and close exhausr port 8 again and test next time.
The computing method of slope k are:
0.1,0.5,1,2,3,4 and 5mL water is got respectively with sample introduction equipment 2, then sample introduction equipment 2 is prolonged guide cylinder 10 and vertically insert injection port 6, start sample introduction, open mixing plant 7 subsequently, after temperature in closed container 1 is identical with bath temperature and pressure no longer changes, the reading of record pressure instrumentataion 4, and the pressure differential Δ P calculating the pressure instrumentataion of each test
1'-Δ P
7'.According to formula (III) m
water=k Δ P', obtains slope k.
Embodiment 1
The volume of closed container 1 is 25L, and internal diameter is 15cm, and height is 35cm.The temperature of water bath with thermostatic control is 30 DEG C, 5mL coal tar sample (known moisture content is 0.5 % by weight) is got with sample introduction equipment 2, then sample introduction equipment 2 is prolonged guide cylinder 10 and vertically insert injection port 6, start sample introduction, open mixing plant 7 subsequently, after temperature in closed container 1 is identical with bath temperature and pressure no longer changes, the reading of record pressure instrumentataion 4, and calculate the pressure differential Δ P of pressure instrumentataion before and after reaction, according to formula (II)
the water cut M obtained in coal tar is 0.499 % by weight.
Embodiment 2
The volume of closed container 1 is 12L, and internal diameter is 10cm, and height is 40cm.The temperature of water bath with thermostatic control is 25 DEG C, 5mL coal tar sample (known moisture content is 1 % by weight) is got with sample introduction equipment 2, then sample introduction equipment 2 is prolonged guide cylinder 10 and vertically insert injection port 6, start sample introduction, open mixing plant 7 subsequently, after temperature in closed container 1 is identical with bath temperature and pressure no longer changes, the reading of record pressure instrumentataion 4, and calculate the pressure differential Δ P of pressure instrumentataion before and after reaction, according to formula (II)
the water cut M obtained in coal tar is 1.01 % by weight.
Embodiment 3
The volume of closed container 1 is 38L, and internal diameter is 20cm, and height is 30cm.The temperature of water bath with thermostatic control is 40 DEG C, 5mL coal tar sample (known moisture content is 0.1 % by weight) is got with sample introduction equipment 2, then sample introduction equipment 2 is prolonged guide cylinder 10 and vertically insert injection port 6, start sample introduction, open mixing plant 7 subsequently, after temperature in closed container 1 is identical with bath temperature and pressure no longer changes, the reading of record pressure instrumentataion 4, and calculate the pressure differential Δ P of pressure instrumentataion before and after reaction, according to formula (II)
the water cut M obtained in coal tar is 0.098 % by weight.
As can be seen from the above embodiments, the inventive method and device can detect the water cut in coal tar exactly.
Apparatus and method of the present invention, calculate the water cut in coal tar by the change of pressure in closed container, fast, accurately; Because reaction unit is airtight, even if the coal tar larger to water cut, also can detect fast and accurately, namely be applicable to the mensuration of various water cut; Apparatus structure of the present invention is simple, only need take a breath at every turn and can carry out test next time, can realize continuous detecting after having tested; These apparatus and method can be widely used in the mensuration of water cut in all aqueous liquid potpourris do not reacted with calcium carbide.
Below the preferred embodiment of the present invention is described in detail by reference to the accompanying drawings; but; the present invention is not limited to the detail in above-mentioned embodiment; within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out combination in any between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (19)
1. one kind is detected the device of water cut in coal tar, it is characterized in that, described device comprises closed container (1), sample introduction equipment (2), first temperature measuring equipment (3) and pressure instrumentataion (4), closed container (1) is for placing sample 1 and sample 2, sample introduction equipment (2) is for conveying sample 1 and/or sample 2 in closed container (1), first temperature measuring equipment (3) and pressure instrumentataion (4) are respectively used to measure the temperature and pressure in closed container (1), sample introduction equipment (2), first temperature measuring equipment (3) and pressure instrumentataion (4) are tightly connected with closed container (1) respectively, wherein, sample 1 is calcium carbide, sample 2 is coal tar.
2. device according to claim 1, wherein, is provided with mixing plant (7) in closed container (1).
3. device according to claim 1, wherein, the wall of closed container (1) is provided with exhausr port (8) and air intake opening (9), exhausr port (8) is for discharging air in closed container (1) and inert gas, and air intake opening (9) for being filled with inert gas in closed container (1).
4. device according to claim 1, wherein, described device also comprises the well heater for heating closed container (1).
5. device according to claim 4, wherein, described well heater is water bath (11), and closed container (1) is placed in water bath (11), and water bath (11) is for regulating the temperature in closed container (1).
6. device according to claim 5, wherein, be provided with support (12) in water bath (11), closed container (1) is placed in water bath (11) by support (12).
7. the device according to claim 5 or 6, wherein, described device also comprises the second temperature measuring equipment (5), and the second temperature measuring equipment (5) is for measuring the temperature of water-bath in water bath (11).
8. device according to claim 1, wherein, described closed container (1) is provided with the injection port (6) allowing described sample introduction equipment (2) to pass, described injection port (6) is provided with packoff, make described sample introduction equipment (2) in closed container (1) during sample introduction, closed container (1) still keeps leakproofness.
9. device according to claim 8, wherein, described sample introduction equipment (2) comprises needle tubing and syringe needle, described packoff is the rubber plug closing described injection port (6), makes syringe needle penetrate described rubber plug to be pushed in closed container (1) by the sample in needle tubing when carrying sample.
10. device according to claim 8 or claim 9, wherein, closed container (1) is provided with guide cylinder (10) in the position of the corresponding injection port (6) of external container, and guide cylinder (10) is for guaranteeing the sample introduction direction of sample introduction equipment (2).
11. 1 kinds of methods detecting water cut in coal tar, it is characterized in that, described method comprises:
(1) in confined conditions, sample 1 and sample 2 are reacted in closed container (1), and wherein, sample 1 is calcium carbide, and sample 2 is coal tar;
(2) after question response terminates, the pressure differential Δ P under identical temperature conditions before and after assaying reaction in closed container (1), and calculate the water cut in coal tar by pressure differential Δ P.
12. methods according to claim 11, wherein, calcium carbide is excessive relative to the water in coal tar.
13. methods according to claim 11, wherein, provide the mode of described identical temperature conditions to comprise: described closed container (1) is placed in water bath with thermostatic control.
14. methods according to claim 11, wherein, make the reaction in closed container (1) carry out under an inert atmosphere.
15. methods according to claim 11, wherein, make the reaction in closed container (1) under agitation carry out.
16. according to the method in claim 11-15 described in any one, and wherein, the water cut through type (I) in coal tar calculates,
Wherein, M is water cut in coal tar, M
h2Ofor the molal weight of water; Δ P is the pressure differential before and after reaction in closed container (1); V be closed container (1) airtight time volume; m
electricityfor the quality of calcium carbide; ρ
electricityfor calcium carbide density; R is ideal gas constant; T is observed temperature; m
liquidfor the quality of coal tar.
17. according to the method in claim 11-15 described in any one, and wherein, the water cut through type (II) in coal tar calculates,
Wherein, M is water cut in coal tar; K is slope; Δ P is the pressure differential before and after reaction in closed container (1); m
liquidfor the quality of coal tar.
18. methods according to claim 17, wherein, the computing method of k comprise: by the water of known difference amount and excessive calcium carbide being reacted in described closed container (1) respectively, pressure under described identical temperature conditions before and after assaying reaction in closed container (1), calculating pressure difference Δ P', and through type (III) calculates
M
water=k Δ P'(III)
Wherein, m
waterfor the quality of water, Δ P' is the pressure differential before and after water and calcium carbide react in closed container (1).
19. according to the method in claim 11-15 described in any one, wherein, in the detection coal tar of described method in claim 1-10 described in any one water cut device in carry out.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106442210A (en) * | 2016-06-21 | 2017-02-22 | 江苏南水水务科技有限公司 | Gasometric-method soil water content detection device and method |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87101213A (en) * | 1987-12-25 | 1988-06-08 | 中国农业科学院仪器厂 | Measure the method and the instrument of water content for relaxed matter |
| CN2042967U (en) * | 1989-01-16 | 1989-08-16 | 北京市建筑工程研究所 | Portable determination instrument for detemining water content of sand |
| CN2277297Y (en) * | 1996-09-09 | 1998-04-01 | 中国科学院成都有机化学研究所 | Automatic temp. control high-pressure reactor |
| CN101008600A (en) * | 2007-01-23 | 2007-08-01 | 同济大学 | Quick determination method of water content of block |
| JP2008096256A (en) * | 2006-10-11 | 2008-04-24 | Onsui:Kk | Analysis method of gas component, separation device of gas component, and discrimination method |
| CN102914559A (en) * | 2012-11-15 | 2013-02-06 | 山东泰德新能源有限公司 | Device for detecting water content of coal tar |
| CN203069541U (en) * | 2013-02-28 | 2013-07-17 | 长沙理工大学 | Methanol gas static detection device |
| CN103868817A (en) * | 2014-03-27 | 2014-06-18 | 济钢集团有限公司 | Device and method for rapidly measuring water content of coal tar |
-
2014
- 2014-08-29 CN CN201410437584.9A patent/CN105466807A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87101213A (en) * | 1987-12-25 | 1988-06-08 | 中国农业科学院仪器厂 | Measure the method and the instrument of water content for relaxed matter |
| CN2042967U (en) * | 1989-01-16 | 1989-08-16 | 北京市建筑工程研究所 | Portable determination instrument for detemining water content of sand |
| CN2277297Y (en) * | 1996-09-09 | 1998-04-01 | 中国科学院成都有机化学研究所 | Automatic temp. control high-pressure reactor |
| JP2008096256A (en) * | 2006-10-11 | 2008-04-24 | Onsui:Kk | Analysis method of gas component, separation device of gas component, and discrimination method |
| CN101008600A (en) * | 2007-01-23 | 2007-08-01 | 同济大学 | Quick determination method of water content of block |
| CN102914559A (en) * | 2012-11-15 | 2013-02-06 | 山东泰德新能源有限公司 | Device for detecting water content of coal tar |
| CN203069541U (en) * | 2013-02-28 | 2013-07-17 | 长沙理工大学 | Methanol gas static detection device |
| CN103868817A (en) * | 2014-03-27 | 2014-06-18 | 济钢集团有限公司 | Device and method for rapidly measuring water content of coal tar |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106442210A (en) * | 2016-06-21 | 2017-02-22 | 江苏南水水务科技有限公司 | Gasometric-method soil water content detection device and method |
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