CN107238547B - Device and method for collecting liquid-solid sample from crude gas - Google Patents
Device and method for collecting liquid-solid sample from crude gas Download PDFInfo
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- CN107238547B CN107238547B CN201710568792.6A CN201710568792A CN107238547B CN 107238547 B CN107238547 B CN 107238547B CN 201710568792 A CN201710568792 A CN 201710568792A CN 107238547 B CN107238547 B CN 107238547B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- 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
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The device for collecting the liquid-solid sample from the crude gas comprises a primary washing tank, a secondary washing tank, an intercooler, a refrigerator, a gas-liquid separation tank, a wet gas flowmeter and a waste liquid tank. The primary washing tank and the secondary washing tank are respectively provided with a proper amount of organic absorbent, so that the continuous collection of tar and dust in the crude gas can be realized. The purified gas after being subjected to deep cooling by the intercooler and the gas-liquid separation tank is introduced into a wet gas flowmeter for metering and then is discharged at an outdoor high point. After the sample collection is finished, the online steam can be utilized to sweep a raw gas pipeline in the device, so that the long-period stable operation of the device is ensured. The invention uses the selective absorption principle of solvent to collect water, tar and dust in crude gas, and adopts the means of filtration, extraction, rotary evaporation and the like to separate the collected absorbent, thus obtaining water, tar and dust samples and simultaneously accounting the content of water, tar and dust in the crude gas.
Description
Technical Field
The invention relates to the sampling and analysis of crude gas incidental matters in the field of energy and chemical industry, in particular to a device and a method for collecting a liquid-solid sample from crude gas.
Background
Pyrolysis of coal is also known as carbonization or thermal decomposition of coal, and refers to a complex process in which coal is continuously decomposed by heating under an inert atmosphere to be converted into carbonization gas, coal tar and solid coke. As an important conversion means of coal, different pyrolysis technologies have various characteristics in terms of reaction temperature, reactor type, heat carrier form, heating rate and the like, for example, solid coke generated in the pyrolysis process can generate high-temperature gas after being burnt or gasified, and the high-temperature gas can be used as a heat source for pyrolysis of raw coal to be mixed with carbonization gas. But the crude gas produced in the process is entrained with tar gas, water vapor, dust and other accessory substances. In order to examine the contents of tar gas, water vapor and dust and the composition of tar in raw gas under different reaction conditions so as to further optimize the thermal conversion process, a device and a method for collecting liquid-solid samples from the raw gas are important.
At present, an online coke oven gas pretreatment system in the coking industry is more common, and the main purpose of the online coke oven gas pretreatment system is to remove relatively less tar gas, water vapor, dust and other impurities in the coke oven gas, so that the gas can be purified, and the purpose of component determination can be achieved. The device and the method for measuring the tar, the water vapor and the dust content in the crude gas with higher oil content, higher dust content and higher water vapor content are freshly reported. Compared with coke oven gas, the crude gas has higher content of incidental matters, especially coal tar, and the high content of coal tar and dust is easy to block the pipeline, thus providing challenges for continuous collection of samples.
Therefore, on the premise of not influencing the test or production operation, the continuous collection of liquid-solid incidental matters in the high-oil-content and high-dust-content crude gas is realized, so that the total fraction composition of liquid products such as coal tar oil is obtained while the content of the liquid-solid incidental matters in the crude gas is calculated, and the method becomes one of the problems to be solved in the industry.
Disclosure of Invention
The invention aims to overcome the difficulty that the continuous process is difficult in the process of collecting the incidental sample in the crude gas, and provides the device and the method for collecting the liquid-solid sample from the crude gas with high oil content and high dust content on the premise of not interfering the test or production operation, and meanwhile, the full fraction composition of tar can be obtained, so that a reliable basis is provided for optimizing the coal conversion process.
In order to achieve the above object, a dust-removing purification device of the present invention includes: the system comprises a first-stage washing tank with a cooling jacket, which is communicated with raw coal, wherein the top of the first-stage washing tank is connected with the bottom of a second-stage washing tank with a cooling jacket, the top of the second-stage washing tank is connected with an intercooler pipe side inlet, an intercooler pipe side outlet is communicated with a gas-liquid separation tank, the gas-liquid separation tank is communicated with a wet gas flowmeter, and the system also comprises a waste liquid tank communicated with raw coal, and a refrigerator which is sequentially communicated with an intercooler shell side, the jacket of the second-stage washing tank and the jacket of the first-stage washing tank;
the top of the primary washing tank and the top of the secondary washing tank are respectively provided with a primary liquid inlet valve and a secondary liquid inlet valve;
the bottoms of the primary washing tank, the secondary washing tank, the gas-liquid separation tank and the waste liquid tank are respectively provided with a primary liquid discharge valve, a secondary liquid discharge valve, a gas-liquid separation tank condensation valve and a waste liquid tank condensation valve.
The crude gas is communicated with the inlet at the bottom of the primary washing tank through a gas introducing valve and a gas sampling valve in sequence, and the outlet at the top of the gas-liquid separation tank is communicated with a wet gas flowmeter through a back pressure valve.
And a vent pipeline is connected between the gas inlet valve and the gas sample injection valve to be led to the waste liquid tank, the gas vent valve is arranged on the vent pipeline, and the distance between the vent pipeline connection point and the gas sample injection valve inlet is not more than 10cm.
The piping between the gas vent valve and the waste liquid tank is provided with continuous gradient, namely the level of the inlet of the waste liquid tank is lower than that of the gas vent valve.
The pipeline between the gas introducing valve and the gas sampling valve is connected with steam through the steam purging valve and the steam introducing valve in sequence, the distance between the inlet point and the outlet of the gas introducing valve is not more than 10cm, and the steam is saturated steam or superheated steam with the pressure not lower than the pressure of the raw gas.
And a condensate draining pipeline is arranged between the steam introducing valve and the steam purging valve, and the condensate draining pipeline is converged into a vent pipeline of the gas vent valve outlet through the steam condensate draining valve.
The crude gas is communicated with the waste liquid tank and the primary washing tank, electric tracing and heat insulation layers are arranged on the along-path pipelines, and the heat insulation layers are arranged on the refrigerator pipeline which is sequentially communicated with the intercooler shell side, the jacket of the secondary washing tank and the jacket of the primary washing tank.
The method for collecting the liquid-solid sample from the crude gas comprises the following steps:
1) And (3) refrigerating and heating starting: starting a refrigerator, setting the temperature of the refrigerant to be-40 to-10 ℃, and starting the refrigerant circulation; starting electric tracing, and setting the temperature of the tracing to 380-500 ℃;
2) Filling an absorbent: closing a gas sample injection valve, a primary liquid discharge valve, a secondary liquid discharge valve and a gas-liquid separation tank condensation discharge valve, filling absorbent into a primary washing tank and a secondary washing tank through the primary liquid inlet valve and the secondary liquid inlet valve respectively, enabling the liquid level of the absorbent in the tank to be 10-15 cm higher than the gas inlet of the tank body, and closing the primary liquid inlet valve and the secondary liquid inlet valve after filling is finished;
3) Replacement: when the electric tracing feedback temperature is not lower than 380 ℃ and the refrigerant temperature is lower than-10 ℃, closing a steam introducing valve, closing a steam purging valve, opening a steam condensing valve, closing a waste liquid tank condensing valve, opening a gas emptying valve, and opening the gas introducing valve to empty at an outdoor high point of the waste liquid tank;
4) And (3) sample injection: recording initial readings of a wet gas flowmeter, opening a gas sampling valve after the gas introducing valve is opened and is emptied for 2 min), adjusting the opening of a back pressure valve, controlling the gas speed of noncondensable gas flowing through a primary washing tank to be 0.5-5 cm/s by referring to the wet gas flowmeter, sampling, closing the gas sampling valve after sampling is finished, closing the gas introducing valve, recording the termination readings of the wet gas flowmeter, and accounting the total volume of noncondensable gas;
5) And (3) collecting a liquid-solid mixture: opening a first-stage liquid inlet valve and a second-stage liquid inlet valve, sequentially opening a first-stage liquid discharge valve, a second-stage liquid discharge valve and a gas-liquid separation tank condensation discharge valve to collect liquid-solid mixture, opening a sealing cover at the top of a first-stage washing tank, injecting 50-500 ml of fresh absorbent into the tank, cleaning and collecting;
6) And (3) purging: opening a steam introducing valve, opening a steam purging valve, closing a steam condensing valve, opening a gas sampling valve, closing a gas emptying valve after purging for 2min, and closing the steam introducing valve, closing the steam purging valve, opening the steam condensing valve, closing the gas sampling valve, opening the gas emptying valve, closing an electric tracing power supply and closing a refrigerator power supply after continuing purging for 2 min;
7) Separating the mixture: firstly, concentrating the collected mixture to 1/2-1/10 of the volume by using a rotary evaporator, secondly, selecting a filter membrane of 0.1-0.8 mu m to carry out suction filtration on the concentrated mixture, cleaning a filter cake by using a fresh absorbent, drying the filter cake in a nitrogen atmosphere at 110 ℃ until the constant weight is obtained, metering, continuously concentrating filtrate by using the rotary evaporator under the condition of the bubble point temperature of the absorbent until the constant weight is obtained, fully mixing the concentrated filtrate with an equal volume of extractant in a separating funnel, standing and layering, weighing and metering a separated water layer, and finally concentrating a non-water layer solution by using the rotary evaporator under the condition of the bubble point temperature of the extractant until the constant weight is obtained, and metering tar.
The absorbent is acetone, methylene dichloride, tetrahydrofuran, benzene or toluene with low boiling point and high solubility;
the extractant is dichloromethane, petroleum ether, benzene or toluene which has low boiling point and is not mutually soluble with water.
The crude gas is led out from a main process gas pipeline, the temperature is 400-800 ℃, and the pressure is 0.01-10.0 MPa (G); the operating temperature of the primary washing tank, the secondary washing tank, the intercooler and the gas-liquid separation tank is-15-40 ℃, and the operating pressure is 0-10.0 MPa (G); the operating temperature of the waste liquid tank is 25-600 ℃, and the operating pressure is 0-1.0 MPa (G).
The beneficial effects of the invention are as follows:
1) By utilizing the solvent absorption principle, liquid-solid incidental matters in the raw gas can be continuously captured, tar, water and solids can be obtained through separation, and the content of the liquid-solid incidental matters in the raw gas can be quantitatively calculated by combining the total gas quantity of the wet gas flowmeter.
2) The device can realize continuous sampling of the main pipeline of the secondary operation process gas through protection measures such as electric tracing and steam purging on the premise of not interfering with test or production operation.
3) By the device and the method, a tar sample of the whole fraction can be obtained, and further refinement analysis of tar composition and other properties is facilitated.
Drawings
Fig. 1 is a schematic diagram of the overall structure of the present invention.
In the figure: 1. a first-stage washing tank; 2. a second-stage washing tank; 3. an intercooler; 4. a refrigerating machine; 5. a gas-liquid separation tank; 6. a wet gas flow meter; 7. a waste liquid tank; 8. a gas introduction valve; 9. a gas vent valve; 10. a gas sample injection valve; 11. a primary liquid inlet valve; 12. a primary drain valve; 13. a secondary liquid inlet valve; 14. a secondary drain valve; 15. a back pressure valve; 16. a steam purge valve; 17. a steam introduction valve; 18. a steam purge valve; 19. a waste liquid tank condensation valve; 20. a gas-liquid separation tank discharge valve; 21. raw gas; 22. steam.
Detailed Description
The invention is described in further detail below with reference to the accompanying drawings.
Referring to fig. 1, the device of the invention comprises a raw gas 21 led out from a main process gas pipeline, the raw gas is sequentially communicated with an inlet at the bottom of a primary washing tank 1 with a cooling jacket through a gas inlet valve 8 and a gas injection valve 10, the top of the primary washing tank 1 is connected with an inlet at the bottom of a secondary washing tank 2 with the cooling jacket, the top of the secondary washing tank 2 is connected with a tube side of an intercooler 3, an outlet of the tube side of the intercooler 3 is communicated with a gas-liquid separation tank 5, the gas-liquid separation tank 5 is communicated with a wet gas flowmeter 6 through a back pressure valve 15, and an outlet of the wet gas flowmeter 6 is led to outdoor high-point venting. Steam 22 is introduced into the outlet of the gas introducing valve 8 through the steam introducing valve 17 and the steam purging valve 16, the inlet of the gas sampling valve 10 is branched and connected, and then is led to the waste liquid tank 7 through the gas emptying valve 9, and the outlet of the waste liquid tank 7 is led to outdoor high-point emptying. The steam is led to the outlet of the gas emptying valve 9 through the steam condensation discharging valve 18 after being led out by a branch line between the steam inlet valve 17 and the steam purging valve 16. The refrigerating machine 4 outputs the refrigerating fluid, and the refrigerating fluid is circulated back to the refrigerating machine 4 after passing through the shell side of the intercooler 3, the jacket of the secondary washing tank 2 and the jacket of the primary washing tank 1 in sequence. The bottoms of the primary washing tank 1, the secondary washing tank 2, the gas-liquid separation tank 5 and the waste liquid tank 7 are respectively provided with a primary liquid discharge valve 12, a secondary liquid discharge valve 14, a gas-liquid separation tank condensation discharge valve 20 and a waste liquid tank condensation discharge valve 19, and the tops of the primary washing tank 1 and the secondary washing tank 2 are respectively provided with a primary liquid inlet valve 11 and a secondary liquid inlet valve 13.
The crude gas 21 of the invention is communicated with a waste liquid tank 7 and an along-path pipeline of a primary washing tank 1, electric tracing and heat preservation are required to be arranged, and a steam pipeline is provided with a heat preservation layer on a steam pipeline of a refrigerator 4 which is sequentially communicated with a shell side of an intercooler 3, a jacket of a secondary washing tank 2 and a jacket of the primary washing tank 1.
The method for collecting the liquid-solid sample comprises the following steps:
1) And (3) refrigerating and heating starting: starting the refrigerator 4, setting the temperature of the refrigerant to-40 to-10 ℃, and opening the refrigerant circulation; and starting electric heat tracing, and setting the temperature of the heat tracing to 380-500 ℃.
2) Filling an absorbent: closing the gas injection valve 10, closing the primary liquid discharge valve 12, closing the secondary liquid discharge valve 14 and closing the gas-liquid separation tank condensation discharge valve 20, respectively filling a proper amount of absorbent into the primary washing tank 1 and the secondary washing tank 2 through the primary liquid inlet valve 11 and the secondary liquid inlet valve 13, ensuring that the liquid level of the absorbent in the tank is 10-15 cm higher than the gas inlet of the tank body, and closing the primary liquid inlet valve 11 and the secondary liquid inlet valve 13 after filling.
3) Replacement: when the electric tracing feedback temperature is not lower than 380 ℃ and the refrigerant temperature is lower than-10 ℃, closing the steam introducing valve 17, closing the steam purging valve 16, opening the steam condensing valve 18, closing the waste liquid tank condensing valve 19, opening the gas emptying valve 9, and opening the gas introducing valve 8 to empty at an outdoor high point.
4) And (3) sample injection: recording the initial reading of the wet gas flowmeter 6, opening the gas sampling valve 10 after the gas introducing valve 8 is opened and is emptied for 2min, then slowly adjusting the opening of the back pressure valve 15, controlling the non-condensable gas velocity flowing through the primary washing tank 1 within the range of 0.5-5 cm/s by referring to the wet gas flowmeter 6, sampling and maintaining for a certain time. After the sample injection is finished, the gas sample injection valve 10 is closed, the gas introduction valve 8 is closed, the reading of the wet gas flowmeter 6 is recorded, and the total volume of the non-condensable gas is calculated.
5) And (3) collecting a liquid-solid mixture: opening a primary liquid inlet valve 11, opening a secondary liquid inlet valve 13, sequentially opening a primary liquid discharge valve 12, opening a secondary liquid discharge valve 14 and opening a gas-liquid separation tank condensation discharge valve 20 to collect a liquid-solid mixture, and injecting 50-500 ml of fresh absorbent into the tank for cleaning in order to clean the residue on the wall surface of the washing tank, and collecting the residue together.
6) And (3) purging: opening the steam introducing valve 17, opening the steam purging valve 16, closing the steam condensing valve 18, opening the gas sampling valve 10, closing the gas venting valve 9 after 2 minutes of purging, closing the steam introducing valve 17, closing the steam purging valve 16, opening the steam condensing valve 18, closing the gas sampling valve 10, opening the gas venting valve 9, closing the electric tracing power supply, and closing the power supply of the refrigerator 4 after 2 minutes of purging.
7) Separating the mixture: firstly, concentrating the collected mixture to 1/2-1/10 of the volume by using a rotary evaporator, secondly, selecting a filter membrane of 0.1-0.8 mu m to carry out suction filtration on the concentrated mixture, cleaning a filter cake by using a fresh absorbent, drying the filter cake in a nitrogen atmosphere at 110 ℃ until the constant weight is obtained, metering, continuously concentrating filtrate by using the rotary evaporator under the condition of the bubble point temperature of the absorbent until the constant weight, thirdly, fully mixing the concentrated filtrate with an equal volume of extractant in a separating funnel, standing and layering, weighing and metering a separated water layer, and finally concentrating a non-water layer solution by using the rotary evaporator until the constant weight is obtained under the condition of the bubble point temperature of the extractant, and metering.
The absorbent used is acetone, methylene dichloride, tetrahydrofuran, benzene and toluene with low boiling point and high solubility.
The extractant is dichloromethane, petroleum ether, benzene or toluene which has low boiling point and is not mutually soluble with water.
The temperature of the raw gas 21 is 400-800 ℃ and the pressure is 0.01-10.0 MPa (G).
The operating temperature of the primary washing tank 1, the secondary washing tank 2, the intercooler 3 and the gas-liquid separation tank 5 is-15 to 40 ℃ and the operating pressure is 0 to 10.0MPa (G).
The operating temperature of the waste liquid tank 7 is 25-600 ℃, and the operating pressure is 0-1.0 MPa (G).
The invention realizes the continuous collection of liquid-solid incidental matters in the raw gas on the premise of not influencing the test or production operation, and further obtains the total fraction composition of tar while accounting the content of the liquid-solid incidental matters in the raw gas, thereby providing a reliable basis for optimizing the coal conversion process.
The following is one embodiment of the present invention: the method comprises seven main steps of refrigeration and heating starting, absorbent filling, replacement, sample injection, liquid-solid mixture collection, purging and mixture separation. First, the refrigerator 4 is turned on, the refrigerant temperature is set to-20 ℃, the refrigerant cycle is turned on, the electric heat tracing is turned on, and the heat tracing temperature is set to 400 ℃. And secondly, closing the gas injection valve 10, closing the primary liquid discharge valve 12, closing the secondary liquid discharge valve 14 and closing the gas-liquid separation tank condensation discharge valve 20, respectively filling a proper amount of absorbent into the primary washing tank 1 and the secondary washing tank 2 through the primary liquid inlet valve 11 and the secondary liquid inlet valve 13, ensuring that the liquid level of the absorbent in the tank is 10-15 cm higher than the gas inlet of the tank body, and closing the primary liquid inlet valve 11 and the secondary liquid inlet valve 13 after filling. When the electric tracing feedback temperature is not lower than 380 ℃ and the refrigerant temperature is lower than-10 ℃, closing the steam introducing valve 17, closing the steam purging valve 16, opening the steam condensing valve 18, closing the waste liquid tank condensing valve 19, opening the gas emptying valve 9, and opening the gas introducing valve 8 to empty at an outdoor high point. And recording the initial reading of the wet gas flowmeter 6, opening the gas injection valve 10 after the gas introduction valve 8 is opened and is emptied for 2min, then slowly adjusting the opening of the back pressure valve 15, controlling the non-condensable gas velocity flowing through the primary washing tank 1 within the range of 0.5-5 cm/s by referring to the wet gas flowmeter 6, and sampling and maintaining for a certain time. After the sample injection is finished, the gas sample injection valve 10 is closed, the gas introduction valve 8 is closed, the reading of the wet gas flowmeter 6 is recorded, and the total volume of the non-condensable gas is calculated. Then, collecting the liquid-solid mixture, opening a primary liquid inlet valve 11 and a secondary liquid inlet valve 13, sequentially opening a primary liquid discharge valve 12, opening a secondary liquid discharge valve 14, opening a gas-liquid separation tank condensation discharge valve 20, collecting the liquid-solid mixture, opening a top sealing cover of the primary washing tank 1, injecting 50-500 ml of fresh absorbent into the tank, cleaning, and collecting. Then purging and cleaning are carried out, the steam introducing valve 17 is opened, the steam purging valve 16 is opened, the steam condensing valve 18 is closed, after purging for 2min, the gas sampling valve 10 is opened, the gas discharging valve 9 is closed, after purging is continued for 2min, the steam introducing valve 17 is closed, the steam purging valve 16 is closed, the steam condensing valve 18 is opened, the gas sampling valve 10 is closed, the gas discharging valve 9 is opened, the electric tracing power supply is closed, and the power supply of the refrigerator 4 is closed. Finally, the mixture was separated: concentrating the collected mixture to 1/2-1/10 of the volume by using a rotary evaporator, filtering the concentrated mixture by using a filter membrane of 0.1-0.8 mu m, cleaning a filter cake by using a fresh absorbent, drying the filter cake in a nitrogen atmosphere at 110 ℃ until the constant weight is achieved, continuously concentrating the filtrate by using the rotary evaporator under the condition of the bubble point temperature of the absorbent until the constant weight is achieved, fully mixing the concentrated filtrate with an equal volume of the extractant in a separating funnel, standing and layering the mixture, weighing and metering a separated water layer, concentrating a non-water layer solution by using the rotary evaporator under the condition of the bubble point temperature of the extractant until the constant weight is achieved, and metering the tar.
Claims (8)
1. A device for collecting a liquid-solid sample from raw gas, which is characterized in that: the device comprises a first-stage washing tank (1) with a cooling jacket, which is communicated with raw gas (21), wherein the top of the first-stage washing tank (1) is connected with the bottom of a second-stage washing tank (2) with the cooling jacket, the top of the second-stage washing tank (2) is connected with a tube side inlet of an intercooler (3), a tube side outlet of the intercooler (3) is communicated with a gas-liquid separation tank (5), the gas-liquid separation tank (5) is communicated with a wet gas flowmeter (6), and the device further comprises a waste liquid tank (7) which is communicated with the raw gas (21), and a refrigerator (4) which is sequentially communicated with the shell side of the intercooler (3), the jacket of the second-stage washing tank (2) and the jacket of the first-stage washing tank (1);
the top of the primary washing tank (1) and the top of the secondary washing tank (2) are respectively provided with a primary liquid inlet valve (11) and a secondary liquid inlet valve (13);
the bottoms of the primary washing tank (1), the secondary washing tank (2), the gas-liquid separation tank (5) and the waste liquid tank (7) are respectively provided with a primary liquid discharge valve (12), a secondary liquid discharge valve (14), a gas-liquid separation tank condensation discharge valve (20) and a waste liquid tank condensation discharge valve (19);
the raw gas (21) is communicated with the bottom inlet of the primary washing tank (1) sequentially through a gas introduction valve (8) and a gas injection valve (10), and the top outlet of the gas-liquid separation tank (5) is communicated with the wet gas flowmeter (6) through a back pressure valve (15);
the crude gas (21) is communicated with a waste liquid tank (7) and an on-line pipeline of a primary washing tank (1), an electric tracing and heat-insulating layer is arranged on a pipeline of a refrigerator (4) which is sequentially communicated with a shell side of an intercooler (3), a jacket of a secondary washing tank (2) and a jacket of the primary washing tank (1).
2. The device for collecting liquid-solid samples from raw gas according to claim 1, wherein: and a vent pipeline is led to the waste liquid tank (7) from the gas inlet valve (8) to the gas sampling valve (10), a gas vent valve (9) is arranged on the vent pipeline, and the distance between the vent pipeline connecting point and the inlet of the gas sampling valve (10) is not more than 10cm.
3. The device for collecting liquid-solid samples from raw gas according to claim 2, characterized in that: the piping between the gas vent valve (9) and the waste liquid tank (7) is provided with continuous gradient, namely the level of the inlet of the waste liquid tank (7) is lower than that of the gas vent valve (9).
4. The device for collecting liquid-solid samples from raw gas according to claim 1, wherein: the pipeline between the gas introducing valve (8) and the gas sampling valve (10) is connected with steam (22) through a steam purging valve (16) and a steam introducing valve (17) in sequence, the distance between the inlet point and the outlet of the gas introducing valve (8) is not more than 10cm, and the steam (22) is saturated steam or superheated steam with the pressure not lower than the pressure of the raw gas (21).
5. The device for collecting a liquid-solid sample from raw gas as claimed in claim 4, wherein: a condensate draining pipeline is arranged between the steam introducing valve (17) and the steam purging valve (16), and the condensate draining pipeline is connected to an outlet of the gas emptying valve (9) through a steam condensate draining valve (18).
6. A method for collecting a liquid-solid sample from raw gas, comprising the steps of:
1) And (3) refrigerating and heating starting: starting a refrigerator (4), setting the temperature of the refrigerant to be-40 to-10 ℃, and starting the refrigerant circulation; starting electric tracing, and setting the temperature of the tracing to 380-500 ℃;
2) Filling an absorbent: closing a gas injection valve (10), a primary liquid discharge valve (12), a secondary liquid discharge valve (14) and a gas-liquid separation tank condensation discharge valve (20), filling absorbent into a primary washing tank (1) and a secondary washing tank (2) through a primary liquid inlet valve (11) and a secondary liquid inlet valve (13) respectively, so that the liquid level of the absorbent in the tank is 10-15 cm higher than a tank gas inlet, and closing the primary liquid inlet valve (11) and the secondary liquid inlet valve (13) after filling;
3) Replacement: when the electric tracing feedback temperature is not lower than 380 ℃ and the refrigerant temperature is lower than-10 ℃, closing a steam introducing valve (17), closing a steam purging valve (16), opening a steam condensing valve (18), closing a waste liquid tank condensing valve (19), opening a gas emptying valve (9), and opening a gas introducing valve (8) to empty at an outdoor high point of the waste liquid tank 7;
4) And (3) sample injection: recording initial readings of a wet gas flowmeter (6), opening a gas sampling valve (10) after a gas introducing valve (8) is opened and is emptied for 2min, adjusting the opening of a back pressure valve (15), controlling the gas speed of noncondensable gas flowing through a primary washing tank (1) to be 0.5-5 cm/s by referring to the wet gas flowmeter (6), sampling, closing the gas sampling valve (10) after sampling is finished, closing the gas introducing valve (8), recording the end readings of the wet gas flowmeter (6), and accounting the total volume of the noncondensable gas;
5) And (3) collecting a liquid-solid mixture: opening a primary liquid inlet valve (11) and a secondary liquid inlet valve (13), then sequentially opening a primary liquid outlet valve (12), a secondary liquid outlet valve (14) and a gas-liquid separation tank condensation valve (20) to collect a liquid-solid mixture, opening a top sealing cover of a primary washing tank (1), injecting 50-500 ml of fresh absorbent into the tank, cleaning and collecting;
6) And (3) purging: opening a steam introducing valve (17), opening a steam purging valve (16), closing a steam condensing valve (18), opening a gas sampling valve (10) after purging for 2min, closing a gas emptying valve (9), closing the steam introducing valve (17), closing the steam purging valve (16), opening the steam condensing valve (18), closing the gas sampling valve (10), opening the gas emptying valve (9), closing an electric tracing power supply, and closing a power supply of a refrigerator (4) after purging for 2 min;
7) Separating the mixture: firstly, concentrating the collected mixture to 1/2-1/10 of the volume by using a rotary evaporator, secondly, selecting a filter membrane of 0.1-0.8 mu m to carry out suction filtration on the concentrated mixture, cleaning a filter cake by using a fresh absorbent, drying the filter cake in a nitrogen atmosphere at 110 ℃ until the constant weight is obtained, metering, continuously concentrating filtrate by using the rotary evaporator under the condition of the bubble point temperature of the absorbent until the constant weight is obtained, fully mixing the concentrated filtrate with an equal volume of extractant in a separating funnel, standing and layering, weighing and metering a separated water layer, and finally concentrating a non-water layer solution by using the rotary evaporator under the condition of the bubble point temperature of the extractant until the constant weight is obtained, and metering tar.
7. The method for collecting a liquid-solid sample from raw gas according to claim 6, wherein: the absorbent is acetone, methylene dichloride, tetrahydrofuran, benzene or toluene with low boiling point and high solubility; the extractant is dichloromethane, petroleum ether, benzene or toluene which has low boiling point and is not mutually soluble with water.
8. The method for collecting a liquid-solid sample from raw gas according to claim 6, wherein: the raw gas (21) is led out from a main process gas pipeline, the temperature is 400-800 ℃, and the pressure is 0.01-10.0 MPa (G); the operating temperature of the primary washing tank (1), the secondary washing tank (2), the intercooler (3) and the gas-liquid separation tank (5) is-15-40 ℃, and the operating pressure is 0-10.0 MPa (G); the operation temperature of the waste liquid tank (7) is 25-600 ℃, and the operation pressure is 0-1.0 MPa (G).
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