CN107238547A - A kind of device and method of the solid sample of the collection liquid from raw gas - Google Patents
A kind of device and method of the solid sample of the collection liquid from raw gas Download PDFInfo
- Publication number
- CN107238547A CN107238547A CN201710568792.6A CN201710568792A CN107238547A CN 107238547 A CN107238547 A CN 107238547A CN 201710568792 A CN201710568792 A CN 201710568792A CN 107238547 A CN107238547 A CN 107238547A
- Authority
- CN
- China
- Prior art keywords
- valve
- gas
- grades
- tank
- level
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
- G01N5/045—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder for determining moisture content
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
A kind of device and method of the solid sample of collection liquid from raw gas, the collection sampling device includes one-level washing tank, two grades of washing tanks, inter cooler, refrigeration machine, knockout drum, wet gas flow meter and waste liquid tank.Appropriate organic absorbent is respectively arranged with one-level washing tank and two grades of washing tanks, the continuous trapping to tar in raw gas and dust can be achieved.Purification coal gas after inter cooler and knockout drum deep cooling, is introduced into the outer high point emptying of wet gas flow meter metering rear chamber.After sample collection terminates, the rough coal gas pipeline in device is purged using online steam, it is ensured that the long-period stable operation of device.The present invention is trapped using the selective absorbing principle of solvent to raw gas reclaimed water, tar and dust, and take the means such as filtering, extraction and rotary evaporation to separate collected absorbent, while water, tar and powder sample is obtained, the content of raw gas reclaimed water, tar and dust can be adjusted.
Description
Technical field
The present invention relates to the raw gas spin off sampling and analysing in derived energy chemical field, and in particular to a kind of from raw gas
The device and method of the solid sample of middle collection liquid.
Background technology
The pyrolysis of coal is also referred to as coal carbonization or thermal decomposition, refers to that coal is persistently heated decomposition and inversion for destructive distillation under an inert atmosphere
The burnt complex process of coal gas, coal tar and solid.As a kind of important conversion means of coal, different pyrolytic techniques are in reaction temperature
Differ from one another in terms of degree, type of reactor, heat carrier form, heating rate, such as, solid Jiao that pyrolytic process is produced is fired
Burn or can produce high-temperature gas after gasifying, the thermal source being pyrolyzed as raw coal is mixed with dry distillation gas.But during produced by
Raw gas in can be entrainment of spin offs such as tar gas, steam and dust.In order to investigate under differential responses operating mode, in raw gas
Tar gas, steam, the composition of the content of dust and tar, so as to further optimization thermal conversion process, one kind can be from raw gas
The device and method of the solid sample of middle collection liquid is most important.
The current more typically online coke-stove gas pretreatment system of coking industry, its main purpose is to remove coke-stove gas
In the impurity such as relatively small number of tar gas, steam and dust, in favor of purification coal gas, reach the purpose of compound mensuration.And be directed to
Device that tar in the raw gas that oil content is higher, dust content is higher, moisture content is higher, steam, dust content are determined and
Method rarely has open report.Compared with coke-stove gas, the spin off content in this kind of raw gas is higher, and especially coal tar contains
Amount, the coal tar and dust of high content easily block pipeline, are that the continuous acquisition of sample brings challenge.
Therefore, how on the premise of experiment or production run is not influenceed, realize that liquid is consolidated in high oil-containing, high dust-laden raw gas
The continuous acquisition of spin off, and then calculate the solid spin off of liquid and while content, obtain the production of the liquid such as coal tar in raw gas
The full fractional composition of product, as one of industry urgent problem to be solved.
The content of the invention
It is an object of the invention to overcome the difficulty for being difficult to be carried out continuously during spin off sample collection in raw gas,
There is provided a kind of high oil-containing, high dust-laden, collection liquid does not consolidate the dress of sample from raw gas on the premise of interference test or production run
Put and method, while the full fractional composition of tar can be obtained, so that the optimization for coal conversion process provides reliable basis.
To achieve the above object, dedusting and purifying device of the invention includes：Including being connected with raw gas with cooling
Bottom at the top of the one-level washing tank of chuck, one-level washing tank with two grades of washing tanks with cooling jacket is connected, two grades of washings
Tank top is connected with inter cooler tube-side inlet, and the outlet of inter cooler tube side is connected with knockout drum, knockout drum and wet type
Gas flowmeter is connected, in addition to the waste liquid tank being connected with raw gas, and successively with inter cooler shell side, two grades of washing tanks
The refrigeration machine that chuck, the chuck of one-level washing tank are connected；
One-level liquid feed valve, two grades of liquid feed valves are respectively provided with the top of described one-level washing tank, at the top of two grades of washing tanks；
Described one-level washing tank, two grades of washing tanks, the bottom of knockout drum and waste liquid tank are respectively provided with one-level row
Liquid valve, two grades of tapping valves, knockout drum condensate drain valve and waste liquid tank condensate drain valve.
Described raw gas introduces valve, coal gas sampling valve through coal gas successively and is connected with one-level washing tank bottom inlet, gas
Liquid knockout drum top exit is connected by counterbalance valve with wet gas flow meter.
Blow-down pipe, which is picked out, between described coal gas introducing valve and coal gas sampling valve leads to waste liquid tank, and in blow-down pipe
On coal gas atmospheric valve is installed, and blow-down pipe picks out a little that distance is no more than 10cm between coal gas sample introduction valve inlet.
The level that pipe arrangement between described coal gas atmospheric valve and waste liquid tank is provided with sustained grade, i.e. waste liquid tank entrance is high
Degree is less than coal gas atmospheric valve.
Described coal gas, which is introduced, sequentially passes through steam blowing valve and steam introducing on the pipeline between valve and coal gas sampling valve
Valve is connected with steam, and be passed through valve outlet is a little introduced coal gas between distance be no more than 10cm, described steam is not low for pressure
In the saturated vapor or superheated steam of rough coal atmospheric pressure.
Described steam introduces between valve and steam blowing valve and is provided with condensate drain pipeline, and condensate drain pipeline is through steam condensate drain valve
Import the blow-down pipe that coal gas is vented valve outlet.
Described raw gas connection waste liquid tank and one-level washing tank are provided with electric tracing and heat-insulation layer along along journey pipeline,
It is provided with the refrigeration machine pipeline being connected successively with the chuck of inter cooler shell side, the chuck of two grades of washing tanks, one-level washing tank
Heat-insulation layer.
The method of the solid sample of present invention collection liquid from raw gas comprises the following steps：
1) cooling and warming starts：Refrigeration machine is opened, refrigerant temperature is set as -40~-10 DEG C, and opens refrigerant and follow
Ring；Electric tracing is opened, heat tracing temperature is set as 380~500 DEG C；
2) absorbent is filled：Coal gas sampling valve is closed, one-level tapping valve is closed, closes two grades of tapping valves, closes gas-liquid point
From tank condensate drain valve, absorbent is filled to one-level washing tank and two grades of washing tanks by one-level liquid feed valve, two grades of liquid feed valves respectively, is made
The liquid level of tank inner absorbent is higher than tank body 10~15cm of gas entry, after filling terminates, and closes one-level liquid feed valve, two grades of feed liquors
Valve；
3) replace：Treat that electric tracing feedback temperature is not less than 380 DEG C and refrigerant temperature is less than -10 DEG C, steam off is introduced
Valve, steam off blow down valve, open steam condensate drain valve, close waste liquid tank condensate drain valve, the atmospheric valve that turns on the gas-fire, turn on the gas-fire introducing
Valve is vented in the outdoor high point of waste liquid tank；
4) sample introduction：Wet gas flow meter initial reading is recorded, after coal gas introducing valve is opened and is vented 2min, coal is opened
Gas sampling valve), back pressure valve opening is adjusted, the fixed gas gas velocity for flowing through one-level washing tank is controlled with reference to wet gas flow meter
0.5~5cm/s, is sampled, after sample introduction terminates, and closes coal gas sampling valve, closes coal gas introducing valve, records wet gas flow
Meter terminates reading, and adjusts the overall accumulated amount of fixed gas；
5) liquid-solid mixture is collected：One-level liquid feed valve, two grades of liquid feed valves are opened, one-level tapping valve, two are then opened successively
Level tapping valve, knockout drum condensate drain valve collect liquid-solid mixture, open head sealing cover at the top of one-level washing tank, 50 are injected into tank
Collected in the lump after the cleaning of~500ml fresh absorbents；
6) purge：Open steam to introduce valve, open steam blowing valve, steam off condensate drain valve, after purging 2min, open coal
Gas sampling valve, closing coal gas atmospheric valve, continue to purge after 2min, and steam off introduces valve, steam off blow down valve, opens steam
Condensate drain valve, closing coal gas sampling valve, the atmospheric valve that turns on the gas-fire, closing electric tracing power supply, closing refrigeration electromechanical source；
7) mixture is separated：First, collected mixture is concentrated into 1/2~1/10 body using Rotary Evaporators
Product, secondly, suction filtration is carried out to the mixture that is concentrated from 0.1~0.8 μm of filter membrane, filter cake cleaned through fresh absorbent after
Dried in 110 DEG C of nitrogen atmosphere and obtain dust to constant weight and measure, filtrate continues to be revolved under the conditions of the bubble point temperature of absorbent
Turn evaporimeter concentration until constant weight, will be concentrated to stand after filtrate is sufficiently mixed with equal-volume extraction agent in separatory funnel and divide
Layer, the water layer isolated is weighed and measured, and finally, non-water layer solution is under the conditions of the bubble point temperature of extractant by Rotary Evaporators
Concentration is until constant weight obtains tar metering.
Described absorbent is low boiling, the acetone of highly dissoluble, dichloromethane, tetrahydrofuran, benzene or toluene；
Described extractant is low boiling and the immiscible dichloromethane of water, petroleum ether, benzene or toluene.
Described raw gas is drawn from main technique gas pipeline, and temperature is 400~800 DEG C, and pressure is 0.01~10.0MPa
(G)；Described one-level washing tank, two grades of washing tanks, the operation temperature of inter cooler and knockout drum are -15~40 DEG C, behaviour
Make pressure for 0~10.0MPa (G)；The operation temperature of described waste liquid tank is 25~600 DEG C, and operating pressure is 0~1.0MPa
(G)。
Beneficial effects of the present invention are as follows：
1) solvent absorption principle is utilized, the solid spin off of liquid in raw gas can be continuously trapped, Jiao is can obtain by separation
Oil, water and solid, with reference to total tolerance of wet gas flow meter, can quantitatively calculate liquid in raw gas and consolidate containing for spin off
Amount.
2) device can be protected on the premise of not interference test or production run by electric tracing and steam blowing etc.
Measure, can be achieved the continuous sampling from operation process gas Trunk Line.
3) by the present apparatus and method, the tar sample of full cut can be obtained, is easy to tar constituent and other property
The further refinement analysis of matter.
Brief description of the drawings
Fig. 1 is overall structure diagram of the invention.
In figure：1st, one-level washing tank；2nd, two grades of washing tanks；3rd, inter cooler；4th, refrigeration machine；5th, knockout drum；6th, wet type
Gas flowmeter；7th, waste liquid tank；8th, coal gas introduces valve；9th, coal gas atmospheric valve；10th, coal gas sampling valve；11st, one-level liquid feed valve；12、
One-level tapping valve；13rd, two grades of liquid feed valves；14th, two grades of tapping valves；15th, counterbalance valve；16th, steam blowing valve；17th, steam introduces valve；
18th, steam condensate drain valve；19th, waste liquid tank condensate drain valve；20th, knockout drum condensate drain valve；21st, raw gas；22nd, steam.
Embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings.
Referring to Fig. 1, the inventive system comprises the raw gas 21 drawn from process gas Trunk Line, the raw gas is successively through coal
Gas introduces valve 8, coal gas sampling valve 10 and is connected with the bottom inlet of one-level washing tank 1 with cooling jacket, and one-level washing tank 1 is pushed up
Portion is connected with two grades of bottom inlets of washing tank 2 with cooling jacket, and two grades of tops of washing tank 2 are connected with the tube side of inter cooler 3,
The outlet of the tube side of cooler 3 is connected with knockout drum 5, and knockout drum 5 connects through counterbalance valve 15 with wet gas flow meter 6
Logical, the outlet of wet gas flow meter 6 leads to outdoor high point emptying.Steam 22 introduces valve 17 through steam and steam blowing valve 16 draws
Enter the outlet that coal gas introduces valve 8, the entrance of coal gas sampling valve 10 has branch line to lead to waste liquid tank 7 through coal gas atmospheric valve 9 after picking out,
The outlet of waste liquid tank 7 leads to outdoor high point emptying.Steam introduce have between valve 17 and steam blowing valve 16 branch line pick out after through steaming
Vapour condensate drain valve 18 leads to coal gas atmospheric valve 9 and exported.Refrigeration machine 4 is washed through the shell side of inter cooler 3, two grades successively after freezing liquid is exported
The chuck of tank 2, the chuck Posterior circle of one-level washing tank 1 return to refrigeration machine 4.One-level washing tank 1, two grades of washing tanks 2, knockout drums 5
And the bottom of waste liquid tank 7 is respectively provided with one-level tapping valve 12, two grades of tapping valves 14, knockout drum condensate drain valve 20 and waste liquid tank
Condensate drain valve 19, the top of one-level washing tank 1, two grades of tops of washing tank 2 are respectively provided with one-level liquid feed valve 11, two grades of liquid feed valves 13.
The present invention raw gas 21 connection waste liquid tank 7 and one-level washing tank 1 along journey pipeline need set electric tracing and
Insulation, steam pipe line is that the chuck successively with the shell side of inter cooler 3, the chuck of two grades of washing tanks 2, one-level washing tank 1 is connected
Heat-insulation layer is provided with the steam pipe line of refrigeration machine 4.
The method of the solid sample of collection liquid of the present invention comprises the following steps：
1) cooling and warming starts：Refrigeration machine 4, -40~-10 DEG C of setting refrigerant temperature are opened, and opens refrigerant circulation；
Open electric tracing, 380~500 DEG C of setting heat tracing temperature.
2) absorbent is filled：Coal gas sampling valve 10 is closed, one-level tapping valve 12 is closed, closes two grades of tapping valves 14, closes
Knockout drum condensate drain valve 20, respectively by one-level liquid feed valve 11, two grades of liquid feed valves 13 to one-level washing tank 1 and two grades of washing tanks
The 2 appropriate absorbents of filling, it is ensured that the liquid level of tank inner absorbent is above tank body 10~15cm of gas entry, after filling terminates, and closes
Close one-level liquid feed valve 11, close two grades of liquid feed valves 13.
3) replace：Treat that electric tracing feedback temperature is not less than 380 DEG C and refrigerant temperature is less than -10 DEG C, steam off is introduced
Valve 17, steam off blow down valve 16, steam condensate drain valve 18 is opened, waste liquid tank condensate drain valve 19, the atmospheric valve 9 that turns on the gas-fire is closed, beats
Turn on the gas introduces valve 8 and is vented in outdoor high point.
4) sample introduction：The initial reading of wet gas flow meter 6 is recorded, after coal gas introducing valve 8 is opened and is vented 2min, is opened
Coal gas sampling valve 10, then the slow regulation aperture of counterbalance valve 15, one-level washing tank 1 will be flowed through with reference to wet gas flow meter 6
Fixed gas gas velocity is controlled in the range of 0.5~5cm/s, is sampled and is kept for the regular hour.After sample introduction terminates, coal gas is closed
Sampling valve 10, closing coal gas introduce valve 8, and record wet gas flow meter 6 terminates reading, and adjusts the overall accumulated amount of fixed gas.
5) liquid-solid mixture is collected：Open one-level liquid feed valve 11, open two grades of liquid feed valves 13, one-level row is then opened successively
Liquid valve 12, two grades of tapping valves 14 are opened, knockout drum condensate drain valve 20 is opened and collects liquid-solid mixture, in order to by washing tank wall
Residue cleans up the top head sealing cover of opening one-level washing tank 1, the cleaning of 50~500ml fresh absorbents is injected into tank latter
And collect.
6) purge：Steam is opened to introduce valve 17, open steam blowing valve 16, steam off condensate drain valve 18, after purging 2min,
Turn on the gas-fire sampling valve 10, closing coal gas atmospheric valve 9, continues to purge after 2min, and steam off introduces valve 17, steam off purging
Valve 16, opening steam condensate drain valve 18, closing coal gas sampling valve 10, the atmospheric valve 9 that turns on the gas-fire, closing electric tracing power supply, closing system
The power supply of cold 4.
7) mixture is separated：First, collected mixture is concentrated into 1/2~1/10 body using Rotary Evaporators
Product, secondly, suction filtration is carried out to the mixture that is concentrated from 0.1~0.8 μm of filter membrane, filter cake cleaned through fresh absorbent after
Dried in 110 DEG C of nitrogen atmosphere and obtain dust to constant weight and measure, filtrate continues to be revolved under the conditions of the bubble point temperature of absorbent
Turn evaporimeter concentration until constant weight, again, will be concentrated quiet after filtrate is sufficiently mixed with equal-volume extraction agent in separatory funnel
Layering is put, the water layer isolated is weighed and measured, finally, non-water layer solution is steamed under the conditions of the bubble point temperature of extractant by rotation
The concentration of hair instrument is until constant weight can obtain tar, and measure.
The absorbent used is low boiling, the acetone of highly dissoluble, dichloromethane, tetrahydrofuran, benzene, toluene.
Described extractant is low boiling and the immiscible dichloromethane of water, petroleum ether, benzene or toluene.
The temperature of raw gas 21 is 400~800 DEG C, and pressure is 0.01~10.0MPa (G).
One-level washing tank 1, two grades of washing tanks 2, the operation temperature of inter cooler 3 and knockout drum 5 are -15~40 DEG C,
Operating pressure is 0~10.0MPa (G).
The operation temperature of waste liquid tank 7 is 25~600 DEG C, and operating pressure is 0~1.0MPa (G).
The present invention realizes continuous the adopting of the solid spin off of liquid in raw gas on the premise of experiment or production run is not influenceed
Collect, and then calculate the solid spin off of liquid and while content, obtain the full fractional composition of tar in raw gas, so as to be coal conversion
The optimization of technique provides reliable basis.
The following is the specific embodiment of the present invention：It include cooling and warming startup, absorbent filling, displacement, sample introduction,
Liquid-solid mixture is collected, purging, mixture separate seven key steps.First, refrigeration machine 4, setting refrigerant temperature -20 are opened
DEG C, and refrigerant circulation is opened, open electric tracing, 400 DEG C of setting heat tracing temperature.Secondly, close coal gas sampling valve 10, close one
Level tapping valve 12, close two grades of tapping valves 14, close knockout drum condensate drain valve 20, respectively by one-level liquid feed valve 11, two grades
Liquid feed valve 13 fills appropriate absorbent to one-level washing tank 1 and two grades of washing tanks 2, it is ensured that the liquid level of tank inner absorbent is above tank
Body 10~15cm of gas entry, after filling terminates, closes one-level liquid feed valve 11, closes two grades of liquid feed valves 13.Treat that electric tracing feeds back
Temperature is not less than 380 DEG C and refrigerant temperature is less than -10 DEG C, and steam off introduces valve 17, steam off blow down valve 16, opens and steam
Vapour condensate drain valve 18, closing waste liquid tank condensate drain valve 19, the atmospheric valve 9 that turns on the gas-fire, the introducing valve 8 that turns on the gas-fire are vented in outdoor high point.
Again, the initial reading of wet gas flow meter 6 is recorded, after coal gas introducing valve 8 is opened and is vented 2min, turn on the gas-fire sampling valve
10, then the slow regulation aperture of counterbalance valve 15, the fixed gas gas velocity of one-level washing tank 1 will be flowed through with reference to wet gas flow meter 6
Control is sampled and kept for the regular hour in the range of 0.5~5cm/s.After sample introduction terminates, closing coal gas sampling valve 10,
Close coal gas and introduce valve 8, record wet gas flow meter 6 terminates reading, and adjusts the overall accumulated amount of fixed gas.Then, carry out
Liquid-solid mixture is collected, and is opened one-level liquid feed valve 11, is opened two grades of liquid feed valves 13, and one-level tapping valve 12 is then opened successively, is beaten
Open two grades of tapping valves 14, open the collection liquid-solid mixture of knockout drum condensate drain valve 20, open the top end socket of one-level washing tank 1
Lid, is collected in the lump after the cleaning of 50~500ml fresh absorbents is injected into tank.Purging cleaning is then carried out again, is opened steam and is drawn
Enter valve 17, open steam blowing valve 16, steam off condensate drain valve 18, after purging 2min, the sampling valve 10 that turns on the gas-fire, closing coal gas
Atmospheric valve 9, continues to purge after 2min, and steam off introduces valve 17, steam off blow down valve 16, opens steam condensate drain valve 18, closes
Coal gas sampling valve 10, the atmospheric valve 9 that turns on the gas-fire are closed, electric tracing power supply is closed, closes the power supply of refrigeration machine 4.Finally, mixture is carried out
Separation：Collected mixture is concentrated into 1/2~1/10 volume using Rotary Evaporators, from 0.1~0.8 μm of filter membrane
Suction filtration is carried out to the mixture being concentrated, filter cake is dried to constant weight after being cleaned through fresh absorbent in 110 DEG C of nitrogen atmosphere
And measure, filtrate is continued by Rotary Evaporators concentration under the conditions of the bubble point temperature of absorbent up to constant weight, in separatory funnel
Filtrate will be concentrated and be sufficiently mixed rear stratification with equal-volume extraction agent, the water layer isolated is weighed and measured, and non-water layer is molten
Liquid is under the conditions of the bubble point temperature of extractant by Rotary Evaporators concentration until constant weight can obtain tar, and measure.
Claims (10)
1. a kind of device of the solid sample of collection liquid from raw gas, it is characterised in that：Including the band being connected with raw gas (21)
There is the bottom with two grades of washing tanks (2) with cooling jacket at the top of the one-level washing tank (1) of cooling jacket, one-level washing tank (1)
Portion is connected, and is connected at the top of two grades of washing tanks (2) with inter cooler (3) tube-side inlet, the outlet of inter cooler (3) tube side and knockout drum
(5) it is connected, knockout drum (5) is connected with wet gas flow meter (6), in addition to the waste liquid being connected with raw gas (21)
Tank (7), and be connected successively with the chuck of inter cooler (3) shell side, the chuck of two grades of washing tanks (2), one-level washing tank (1)
Refrigeration machine (4)；
One-level liquid feed valve (11), two grades of feed liquors are respectively provided with the top of described one-level washing tank (1), at the top of two grades of washing tanks (2)
Valve (13)；
Described one-level washing tank (1), two grades of washing tanks (2), the bottom of knockout drum (5) and waste liquid tank (7) are filled respectively
There are one-level tapping valve (12), two grades of tapping valves (14), knockout drum condensate drain valve (20) and waste liquid tank condensate drain valve (19).
2. the harvester of the solid sample of liquid in raw gas according to claim 1, it is characterised in that：Described raw gas
(21) introduce valve (8), coal gas sampling valve (10) through coal gas successively with one-level washing tank (1) bottom inlet to be connected, gas-liquid separation
Tank (5) top exit is connected by counterbalance valve (15) with wet gas flow meter (6).
3. the harvester of the solid sample of liquid in raw gas according to claim 2, it is characterised in that：Draw in described coal gas
Enter to pick out blow-down pipe between valve (8) and coal gas sampling valve (10) and lead to waste liquid tank (7), and coal gas is installed on blow-down pipe
Atmospheric valve (9), and blow-down pipe pick out a little between coal gas sampling valve (10) entrance distance be no more than 10cm.
4. the harvester of the solid sample of liquid in raw gas according to claim 3, it is characterised in that：Described coal gas emptying
Pipe arrangement between valve (9) and waste liquid tank (7) is provided with sustained grade, i.e. the level height of waste liquid tank (7) entrance is put less than coal gas
Empty valve (9).
5. the harvester of the solid sample of liquid in raw gas according to claim 2, it is characterised in that：Described coal gas is introduced
Steam blowing valve (16) is sequentially passed through on pipeline between valve (8) and coal gas sampling valve (10) and steam introduces valve (17) and steam
(22) be connected, and be passed through a little introduce valve (8) outlet with coal gas between distance no more than 10cm, described steam (22) be pressure not
Less than the saturated vapor or superheated steam of raw gas (21) pressure.
6. the harvester of the solid sample of liquid in raw gas according to claim 5, it is characterised in that：Described steam is introduced
Condensate drain pipeline is provided between valve (17) and steam blowing valve (16), condensate drain pipeline imports coal gas through steam condensate drain valve (18) and put
The blow-down pipe of empty valve (9) outlet.
7. the harvester of the solid sample of liquid in raw gas according to claim 1, it is characterised in that：Described raw gas
(21) connection waste liquid tank (7) and one-level washing tank (1) are provided with electric tracing and heat-insulation layer along along journey pipeline, cold with successively
Set on refrigeration machine (4) pipeline that device (3) shell side, chuck, the chuck of one-level washing tank (1) of two grades of washing tanks (2) are connected
There is heat-insulation layer.
8. the method for the solid sample of a kind of collection liquid from raw gas, it is characterised in that comprise the following steps：
1) cooling and warming starts：Refrigeration machine (4) is opened, refrigerant temperature is set as -40~-10 DEG C, and opens refrigerant circulation；
Electric tracing is opened, heat tracing temperature is set as 380~500 DEG C；
2) absorbent is filled：Coal gas sampling valve (10) is closed, one-level tapping valve (12) is closed, closes two grades of tapping valves (14), closes
Close knockout drum condensate drain valve (20), respectively by one-level liquid feed valve (11), two grades of liquid feed valves (13) to one-level washing tank (1) and
Two grades of washing tanks (2) fill absorbent, the liquid level of tank inner absorbent is higher than tank body 10~15cm of gas entry, filling terminates
Afterwards, one-level liquid feed valve (11), two grades of liquid feed valves (13) are closed；
3) replace：Treat that electric tracing feedback temperature is not less than 380 DEG C and refrigerant temperature is less than -10 DEG C, steam off introduces valve
(17), steam off blow down valve (16), open steam condensate drain valve (18), close waste liquid tank condensate drain valve (19), turn on the gas-fire emptying
Valve (9), the introducing valve (8) that turns on the gas-fire are vented in the outdoor high point of waste liquid tank 7；
4) sample introduction：Wet gas flow meter (6) initial reading is recorded, after coal gas introduces valve (8) unlatching and is vented 2min, is opened
Coal gas sampling valve (10), adjusts counterbalance valve (15) aperture, one-level washing tank (1) will be flowed through with reference to wet gas flow meter (6)
Fixed gas gas velocity is controlled in 0.5~5cm/s, is sampled, after sample introduction terminates, and is closed coal gas sampling valve (10), closing coal gas and is drawn
Enter valve (8), record wet gas flow meter (6) terminates reading, and adjusts the overall accumulated amount of fixed gas；
5) liquid-solid mixture is collected：One-level liquid feed valve (11), two grades of liquid feed valves (13) are opened, one-level tapping valve is then opened successively
(12), two grades of tapping valves (14), knockout drum condensate drain valves (20) collect liquid-solid mixture, open at the top of one-level washing tank (1)
Head sealing cover, is collected in the lump after the cleaning of 50~500ml fresh absorbents is injected into tank；
6) purge：Open steam to introduce valve (17), open steam blowing valve (16), steam off condensate drain valve (18), purge 2min
Afterwards, turn on the gas-fire sampling valve (10), closing coal gas atmospheric valve (9), continues to purge after 2min, and steam off introduces valve (17), closed
Steam blowing valve (16) is closed, steam condensate drain valve (18) is opened, closes coal gas sampling valve (10), the atmospheric valve that turns on the gas-fire (9), closes
Electric tracing power supply, closing refrigeration machine (4) power supply；
7) mixture is separated：First, collected mixture is concentrated into 1/2~1/10 volume using Rotary Evaporators, its
It is secondary, carry out suction filtration to the mixture that is concentrated from 0.1~0.8 μm of filter membrane, filter cake cleaned through fresh absorbent after at 110 DEG C
Nitrogen atmosphere in dry and obtain dust to constant weight and measure, filtrate is continued by rotary evaporation under the conditions of the bubble point temperature of absorbent
Instrument concentration will be until constant weight, will be concentrated stratification after filtrate is sufficiently mixed with equal-volume extraction agent, separation in separatory funnel
The water layer gone out is weighed and measured, finally, and non-water layer solution is concentrated straight under the conditions of the bubble point temperature of extractant by Rotary Evaporators
Tar metering is obtained to constant weight.
9. the method for the solid sample of the collection liquid according to claim 8 from raw gas, it is characterised in that：Described absorbent
For low boiling, the acetone of highly dissoluble, dichloromethane, tetrahydrofuran, benzene or toluene；Described extractant is low boiling and water
Immiscible dichloromethane, petroleum ether, benzene or toluene.
10. the method for the solid sample of the collection liquid according to claim 8 from raw gas, it is characterised in that：Described rough coal
Gas (21) is drawn from main technique gas pipeline, and temperature is 400~800 DEG C, and pressure is 0.01~10.0MPa (G)；Described one-level is washed
The operation temperature for washing tank (1), two grades of washing tanks (2), inter cooler (3) and knockout drum (5) is -15~40 DEG C, operation pressure
Power is 0~10.0MPa (G)；The operation temperature of described waste liquid tank (7) is 25~600 DEG C, and operating pressure is 0~1.0MPa
(G)。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710568792.6A CN107238547B (en) | 2017-07-13 | 2017-07-13 | Device and method for collecting liquid-solid sample from crude gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710568792.6A CN107238547B (en) | 2017-07-13 | 2017-07-13 | Device and method for collecting liquid-solid sample from crude gas |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107238547A true CN107238547A (en) | 2017-10-10 |
| CN107238547B CN107238547B (en) | 2023-06-27 |
Family
ID=59991595
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710568792.6A Active CN107238547B (en) | 2017-07-13 | 2017-07-13 | Device and method for collecting liquid-solid sample from crude gas |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107238547B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108008656A (en) * | 2017-12-28 | 2018-05-08 | 陕西延长石油（集团）有限责任公司 | A kind of alternating pressure coke discharging control device and method of gas purifier |
| CN108303395A (en) * | 2018-02-01 | 2018-07-20 | 农业部规划设计研究院 | The method for fast measuring of tar content during a kind of biomass continuous pyrolysis |
| CN112857937A (en) * | 2021-01-25 | 2021-05-28 | 吉林省吉科软信息技术有限公司 | Automatic pesticide residue detection system based on food safety |
| CN113893637A (en) * | 2021-10-09 | 2022-01-07 | 陕西延长石油（集团）有限责任公司 | Device and method for on-line sampling of multi-phase components in high-temperature gas |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3138439A (en) * | 1960-04-12 | 1964-06-23 | Exxon Research Engineering Co | Apparatus and process for heatless fractionation of gaseous constituents |
| CN101183056A (en) * | 2007-12-20 | 2008-05-21 | 眉山麦克在线设备有限公司 | Coal gasification device on-line analysis sample pretreatment system |
| CN104155326A (en) * | 2014-07-17 | 2014-11-19 | 北京神雾环境能源科技集团股份有限公司 | Multifunctional carbon-containing substance pyrolysis evaluation device and method |
| CN106701202A (en) * | 2017-01-05 | 2017-05-24 | 东华工程科技股份有限公司 | Apparatus and method used for mixing reaction of synthetic gas and coal and gas-solid-liquid grading separation of product |
| CN207147914U (en) * | 2017-07-13 | 2018-03-27 | 陕西延长石油（集团）有限责任公司 | A kind of device of the solid sample of the collection liquid from raw gas |
-
2017
- 2017-07-13 CN CN201710568792.6A patent/CN107238547B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3138439A (en) * | 1960-04-12 | 1964-06-23 | Exxon Research Engineering Co | Apparatus and process for heatless fractionation of gaseous constituents |
| CN101183056A (en) * | 2007-12-20 | 2008-05-21 | 眉山麦克在线设备有限公司 | Coal gasification device on-line analysis sample pretreatment system |
| CN104155326A (en) * | 2014-07-17 | 2014-11-19 | 北京神雾环境能源科技集团股份有限公司 | Multifunctional carbon-containing substance pyrolysis evaluation device and method |
| CN106701202A (en) * | 2017-01-05 | 2017-05-24 | 东华工程科技股份有限公司 | Apparatus and method used for mixing reaction of synthetic gas and coal and gas-solid-liquid grading separation of product |
| CN207147914U (en) * | 2017-07-13 | 2018-03-27 | 陕西延长石油（集团）有限责任公司 | A kind of device of the solid sample of the collection liquid from raw gas |
Non-Patent Citations (2)
| Title |
|---|
| 周夏: "三流道内外混水煤浆气化工艺烧嘴浅析", 《化肥设计》, no. 02 * |
| 孟祥清: "鲁奇炉煤气出口提取油含量实验研究", 《化工技术与开发》, no. 10 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108008656A (en) * | 2017-12-28 | 2018-05-08 | 陕西延长石油（集团）有限责任公司 | A kind of alternating pressure coke discharging control device and method of gas purifier |
| CN108008656B (en) * | 2017-12-28 | 2023-06-27 | 陕西延长石油（集团）有限责任公司 | Alternating pressure coke discharging control device and method for gas purifier |
| CN108303395A (en) * | 2018-02-01 | 2018-07-20 | 农业部规划设计研究院 | The method for fast measuring of tar content during a kind of biomass continuous pyrolysis |
| CN112857937A (en) * | 2021-01-25 | 2021-05-28 | 吉林省吉科软信息技术有限公司 | Automatic pesticide residue detection system based on food safety |
| CN112857937B (en) * | 2021-01-25 | 2022-07-01 | 吉林省吉科软信息技术有限公司 | Automatic pesticide residue detection system based on food safety |
| CN113893637A (en) * | 2021-10-09 | 2022-01-07 | 陕西延长石油（集团）有限责任公司 | Device and method for on-line sampling of multi-phase components in high-temperature gas |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107238547B (en) | 2023-06-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107238547A (en) | A kind of device and method of the solid sample of the collection liquid from raw gas | |
| CN102010729B (en) | Multifunctional fluidized bed type biomass pyrolysis conversion device | |
| CN207147914U (en) | A kind of device of the solid sample of the collection liquid from raw gas | |
| CN201864688U (en) | Multifunctional fluidized bed type biomass pyrolysis converter | |
| CN101649226A (en) | Method for preparing fuel gas by gasifying biomass materials and device thereof | |
| CN105692551B (en) | The method and apparatus that a kind of biomass efficient produces hydrogen-rich gas | |
| CN205620407U (en) | Coke oven tedge smoke and dust gas sampling analysis device | |
| CN107586550A (en) | A kind of organic matter automatically cleaning gasification and pyrolysis coupling activation prepares the device and method that high quality heat is vented one's spleen with activated carbon | |
| CN104155326B (en) | Multi-functional carbonaceous material pyrolytic model device and evaluation method | |
| CN105295968B (en) | A kind of device and method for improving low-order coal pyrolytic tar yield | |
| CN105905895A (en) | Preparation device and preparation method of nitrogen-containing activated carbon | |
| WO2014198180A1 (en) | Organic material dry distillation pyrolysis gasifier, treatment system and method | |
| CN105018121B (en) | Gas, tar and activated carton co-production system | |
| CN107655926A (en) | A kind of Pyrolysis Experiment device and its method for pyrolysis | |
| CN1404974A (en) | Method for obtaining high-temp. bamboo charcoal and fine bamboo-wax from bamboo material | |
| CN103131453B (en) | Pyrolytic evaluation device for carbon-containing substances | |
| CN108994050A (en) | A kind of rubbish processing to be harmless device and method | |
| CN107794064A (en) | A kind of disturbance formula inner member rotary kiln pyrogenation reactor and biomass pyrolytic carbonize method | |
| CN112816361B (en) | System and method for evaluating thermal conversion of organic matter-containing solid | |
| CN201598271U (en) | Decoking and dust removing equipment utilizing garbage microwave pyrolysis gas to prepare fuel gas | |
| CN208700990U (en) | A kind of gasification of biomass reformate upgrading pilot system | |
| CN101477130A (en) | Gas analysis pretreatment system | |
| CN205710599U (en) | A kind of system for mixed coal character is analyzed comprehensively | |
| CN108977212B (en) | Straw carbomorphism device | |
| CN201632174U (en) | Device for purifying, collecting and utilizing biomass gas |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |