A detection method for the total oil content in coke oven gas

By using tetrachloroethylene absorber and infrared spectrophotometry to detect the total oil content in coke oven gas, the problems of inaccurate detection and large errors in the prior art are solved, and the total oil content in coke oven gas is achieved quickly and accurately measured.

CN114544535BActive Publication Date: 2025-07-08SHAANXI COAL & CHEM IND GRP SHENMU TIANYUAN CHEM IND
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Patent Information

Application Number
CN202210150247.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-02-18
Publication Date
2025-07-08
Estimated Expiration
2042-02-18

AI Technical Summary

Technical Problem

The existing method for detecting total oil content in coke oven gas is inaccurate, the analysis time is long and the result error is large. The use of xylene as an absorber in the prior art cannot accurately detect light component oil in coke oven gas, and moisture affects the experimental results.

Method used

Tetrachloroethylene is used as the absorber, combined with infrared spectrophotometry, the total oil content in the coke oven gas is detected, and the oil in the coke oven gas is absorbed through tetrachloroethylene, and absorbed at 0-4°C to reduce volatile losses. Multiple absorption bottles are set up to ensure the complete absorption of oil.

Benefits of technology

It improves the accuracy and speed of detection of total oil content in coke oven gas, reduces errors, and avoids the impact of moisture on detection. It is suitable for accurate measurement of light component oil in coke oven gas.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention belongs to the technical field of chemical detection, and particularly relates to a method for detecting the total oil content in coke oven gas. The method for detecting the total oil content in coke oven gas provided by the present invention comprises the following steps: absorbing the oil in the coke oven gas with tetrachloroethylene, detecting the total oil content in the tetrachloroethylene, and calculating the total oil content in the coke oven gas. The present invention selects tetrachloroethylene as the absorbent. Tetrachloroethylene has good compatibility with oil and no overlap with the components of the oil in the coke oven gas, so the test results are accurate; the absorption effect of the coke oven gas through the tetrachloroethylene absorbent is good. Tetrachloroethylene has a higher density than xylene and is not easily carried away by the gas, and the volume of the absorbent is more accurate. In addition, this absorption method is not affected by the moisture content in the coke oven gas.
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Description

Technical Field

[0001] The present invention belongs to the technical field of chemical detection, and particularly relates to a method for detecting the total oil content in coke oven gas. Background Art

[0002] The detection of the tar content in coke oven gas is an important parameter for measuring the quality of coke oven gas after purification, and is also an important indicator for ensuring the supply of coke oven gas as an energy source. Our company is a coal chemical enterprise that uses lump coal dry distillation to produce coal tar and deep-process coal tar. The obtained coke oven gas can be pretreated to produce high-purity hydrogen as an auxiliary raw material for hydrogenation. The tar content in the gas will directly affect the continuous and stable operation of the equipment in the hydrogen production section. Therefore, it is very necessary to accurately detect the total oil content in coke oven gas.

[0003] One method for measuring the tar content in coke oven gas in the prior art is the national standard method, that is, the method introduced in GB / T 12208-2008 "Determination Method for Components and Impurity Contents of Artificial Gas". This method is to pass a certain volume of coke oven gas through a filter membrane with a known mass, and calculate the contents of tar and dust based on the mass increase of the filter membrane and the sampling volume. This method has a large sampling amount, a long analysis time, a large analysis result error, and the contents of tar and dust cannot be measured separately. In addition, there is water in the gas, which forms a water seal when the gas passes through the filter membrane, making it difficult for the gas to pass through the filter membrane. The filter membrane getting wet will cause the gas pressure to increase and break through the filter membrane, resulting in the failure of the experiment.

[0004] In the prior art, there is also a detection method that uses xylene as an absorbent to dissolve the total oil in coke oven gas, and then measures the total oil content in xylene and obtains the total oil content in coke oven gas through conversion. However, the oil carried in coke oven gas is very light components, mainly benzene, toluene, xylene, etc. Using xylene as an absorbent, the xylene originally contained in the gas cannot be detected, which is theoretically unworkable and the detection result is inaccurate. Summary of the Invention

[0005] Therefore, the technical problem to be solved by the present invention is to overcome the defects of inaccurate detection method, long analysis time, large result error, etc. existing in the detection method of the total oil content in coke oven gas in the prior art, so as to provide a method for detecting the total oil content in coke oven gas.

[0006] For this purpose, the present invention provides the following technical solutions:

[0007] The present invention provides a method for detecting the total oil content in coke oven gas, including the following steps:

[0008] Absorb the oil in coke oven gas with tetrachloroethylene, detect the total oil content in tetrachloroethylene, and calculate the total oil content in coke oven gas.

[0009] Optionally, the perchloroethylene absorbs the oil in the coke oven gas at 0 - 4°C.

[0010] Optionally, fill the perchloroethylene into an absorption bottle, introduce the coke oven gas into the absorption bottle, and the perchloroethylene absorbs the oil in the coke oven gas.

[0011] Optionally, 1 - 3 absorption bottles are provided;

[0012] Preferably, 2 absorption bottles are provided.

[0013] Optionally, the flow rate of the coke oven gas is 1 L / min - 2 L / min.

[0014] Optionally, the total oil content in the perchloroethylene is detected by infrared spectrophotometry.

[0015] Optionally, the scanning range of the infrared spectrophotometry is 3400 cm -1 ~2400 cm -1 .

[0016] Optionally, record the average temperature of the coke oven gas, the atmospheric pressure and the pressure of the coke oven gas during detection.

[0017] Optionally, the total oil content in the coke oven gas is calculated according to formula (1):

[0018]

[0019] In the formula:

[0020] c1 - the concentration of the total oil in the absorbent perchloroethylene, unit: mg / L;

[0021] V - the total volume of the absorbent perchloroethylene, unit: L;

[0022] V0 - the total volume of the coke oven gas converted to the standard state, unit: L.

[0023] The test principle of the present invention is that a certain volume of coke oven gas is passed through an absorption gas bottle filled with perchloroethylene to extract and absorb the total oil in the coke oven gas. The wet gas flowmeter accurately reads the volume of the coke oven gas, and the perchloroethylene extraction liquid is colorimetrically analyzed by infrared spectrophotometry to calculate the oil content in the perchloroethylene, and then converted to the oil content in the gas under the standard state.

[0024] Specifically, the method for detecting the total oil content in the coke oven gas provided by the present invention includes the following steps:

[0025] 1. Sampling step

[0026] a) Fill the perchloroethylene into the absorption bottle and fill the gas flowmeter with distilled water.

[0027] b) The maximum distance between the outside of the coke oven gas pipe and the absorption bottle shall not exceed 200 mm. Check the airtightness of the device. After confirming that the system is well-sealed, record the reading of the flowmeter.

[0028] c) Open the sampling valve and adjust the gas flow rate to 1 L / min - 2 L / min. Record the average gas temperature, atmospheric pressure, and gas pressure during sampling.

[0029] d) Close the sampling valve and record the reading of the flowmeter.

[0030] 2. Analysis

[0031] a) Retrieve the absorption bottle, mix the absorbents in different absorption bottles evenly, and accurately measure the volume of the absorbent.

[0032] b) Turn on the main unit and workstation of the infrared oil analyzer to make a working curve with accurate concentrations:

[0033] (1) Accurately measure 10.00 ml of the petroleum standard stock solution with a concentration of 1000 mg / L (the stock solution is a special infrared oil analyzer standard substance of tetrachloroethylene provided by the National Institute of Metrology of China) into a 100 ml volumetric flask, dilute it to the mark with tetrachloroethylene, and shake well. The concentration of the petroleum standard solution is 100 mg / L.

[0034] (2) Respectively measure 2.00 ml, 5.00 ml, 10.00 ml, and 20.00 ml of the petroleum standard solution with a concentration of 100 mg / L into 50 ml volumetric flasks, dilute them to the mark with tetrachloroethylene, and shake well to obtain standard solutions with concentrations of 4 mg / L, 10 mg / L, 20 mg / L, 40 mg / L, and 100 mg / L of petroleum;

[0035] (3) Using pure tetrachloroethylene as the blank, draw a 0 - 100 mg / L standard curve on the infrared oil analyzer, take the test samples to be measured for testing, and calculate the concentration of total oil in the absorbent through the standard curve. When the concentration of the absorbent C1 determined by colorimetry is greater than 100 mg / L; we can analyze it by dilution method; as long as the colorimetric concentration falls on our standard curve.

[0036] c) Calculation:

[0037] The total oil content in the coke oven gas is calculated by mass concentration, and the value is expressed in milligrams per cubic meter (mg / m 3 ) and is calculated according to formula (1):

[0038]

[0039] In the formula:

[0040] c1——The concentration of total oil in the absorbent tetrachloroethylene, in milligrams per liter (mg / L);

[0041] V—the total volume of the absorbent perchloroethylene, in liters (ml);

[0042] V0—the volume of the sampled gas converted to standard conditions, in liters (m 3 ).

[0043] The calculation result should be rounded to two decimal places.

[0044] The technical solution of the present invention has the following advantages:

[0045] The method for detecting the total oil content in coke oven gas provided by the present invention includes the following steps: absorbing the oil in coke oven gas with perchloroethylene, detecting the total oil content in perchloroethylene, and calculating the total oil content in coke oven gas. The present invention selects perchloroethylene as the absorbent, which does not overlap with the components of the oil in coke oven gas, and the test results are accurate; the absorption effect of coke oven gas through the perchloroethylene absorbent is good. Perchloroethylene has a higher density than xylene and is not easily carried away by the gas, and the volume of the absorbent is more accurate. In addition, this absorption method is not affected by the moisture content in coke oven gas.

[0046] In the method for detecting the total oil content in coke oven gas provided by the present invention, the perchloroethylene absorbs the oil in coke oven gas at 0 - 4°C. This is because, firstly, the oil in the gas will condense at low temperature and is easy to absorb; secondly, the absorbent is not easily volatilized at low temperature, and the volume (accurate) volatilization loss is small.

[0047] In the method for detecting the total oil content in coke oven gas provided by the present invention, multiple absorption bottles are provided, which can make the oil in coke oven gas be absorbed more thoroughly and further improve the accuracy of the test results.

[0048] In the method for detecting the total oil content in coke oven gas provided by the present invention, the infrared spectrophotometry is selected to detect the total oil content in perchloroethylene. The absorption data is stable, the adjustable range of the infrared wave region is wider, and it is more suitable for experimental analysis. This is because the contents of total oil and petroleum are calculated from the absorbances A -1 (stretching vibration of the C—H bond in the CH2 group), A -1 (stretching vibration of the C—H bond in the CH3 group), and A -1 (stretching vibration of the C—H bond in the aromatic ring) at the wavenumbers of 2930 cm 2930 , A 2960 , A 3030 . This wavelength range is exactly the infrared wavelength region. Description of the Drawings

[0049] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the following will briefly introduce the drawings required for the description of the specific embodiments or the prior art. Obviously, the drawings in the following description are some embodiments of the present invention. For those of ordinary skill in the art, without creative work, other drawings can be obtained based on these drawings.

[0050] Figure 1 It is a schematic structural diagram of the sampling device used in the embodiments and comparative examples of the present invention;

[0051] Figure 2 It is the standard infrared spectrophotometry curve graph used in the test process of the present invention;

[0052] Reference numerals:

[0053] 1. Sampling valve; 2. Absorption bottle; 3. Ice-water bath; 4. Empty bottle; 5. Thermometer; 6. U-shaped manometer; 7. Wet gas flowmeter. Specific embodiments

[0054] The following embodiments are provided to better further understand the present invention. It is not limited to the best embodiment, and does not limit the content and protection scope of the present invention. Any product that is the same as or similar to the present invention obtained by anyone under the inspiration of the present invention or by combining the features of the present invention with other prior art features falls within the protection scope of the present invention.

[0055] For those not specifying specific experimental steps or conditions in the embodiments, the operations or conditions of the conventional experimental steps described in the literature in this field can be followed. For reagents or instruments not specifying the manufacturer, they are all conventional reagent products that can be obtained through commercial purchase.

[0056] Example 1

[0057] This example provides a method for detecting the total oil content in coke oven gas, specifically including the following steps:

[0058] 1. In this example, the source of the coke oven gas is Shenmu Tianyuan Chemical Co., Ltd. Using the sampling device as shown in Figure 1 , the specific sampling steps are as follows:

[0059] a) Accurately measure two portions of 50 ml of tetrachloroethylene (analytical grade) and separately pour them into two absorption bottles 2 placed in the ice-water bath 3. The wet gas flowmeter 7 is filled with distilled water.

[0060] b) The longest distance between the outside of the coke oven gas pipe and the absorption bottle does not exceed 200 mm. In this example, the distance is 198 mm. Check the airtightness of the device. After confirming that the system is airtight, record the reading of the wet gas flowmeter as 8559 L.

[0061] c) Open the sampling valve 1 and adjust the flow rate of the coke oven gas to 1.5 L / min. Record the average gas temperature of 15 °C, the atmospheric pressure of 89875 Pa during sampling through the thermometer 5, and record the coke oven gas pressure of 30 Pa through the U-shaped manometer 6.

[0062] d) Close the sampling valve 1 and record the reading of the wet gas flowmeter 7 as 8768 L.

[0063] 2. Analysis

[0064] a) Retrieve the absorption bottles, mix the absorbents in the two absorption bottles evenly, and accurately measure the recovered volume of the absorbent as 96.6 ml.

[0065] b) Turn on the main unit and workstation of the infrared oil analyzer, select the infrared standard curve range of 0 - 100 mg / L, and draw the standard curve according to the method in the instruction manual:

[0066] (1) Accurately measure 10.00 ml of the petroleum standard stock solution with a concentration of 1000 mg / L (the stock solution is a standard reference material for the infrared oil analyzer provided by the National Institute of Metrology of China) into a 100 ml volumetric flask, dilute to the mark with tetrachloroethylene, and shake well. The concentration of the petroleum standard solution is 100 mg / L.

[0067] (2) Measure 2.00 ml, 5.00 ml, 10.00 ml, and 20.00 ml of the petroleum standard solution with a concentration of 100 mg / L into 50 ml volumetric flasks respectively, dilute to the mark with tetrachloroethylene, and shake well to obtain petroleum standard solutions with concentrations of 4 mg / L, 10 mg / L, 20 mg / L, 40 mg / L, and 100 mg / L;

[0068] (3) Using pure tetrachloroethylene as the blank, draw a 0 - 100 mg / L standard curve on the infrared oil analyzer.

[0069] 3. Analyze with pure tetrachloroethylene as the blank, then pour the sample to be measured into a 4 cm quartz cuvette for colorimetry, and obtain the concentration of total oil in the absorbent according to the standard curve.

[0070] c) Calculation:

[0071] The total oil content in the coke oven gas is calculated by mass concentration, and the value is expressed in milligrams per liter (mg / m 3 ) and calculated according to the following formula:

[0072]

[0073]

[0074] In the formula:

[0075] Standard state: temperature: 273.15K; atmospheric pressure: 101.325KPa.

[0076] ρ —— Total oil content in coke oven gas, unit: milligram per cubic meter (mg / m 3 );

[0077] c1 —— Concentration of total oil in the absorbent tetrachloroethylene, unit: milligram per liter (mg / L);

[0078] V —— Total volume of the absorbent tetrachloroethylene, unit: liter (m 3 );

[0079] V0 —— Volume of the sampled gas converted to the standard state, unit: liter (L).

[0080] V1 —— Reading of the flowmeter before sampling, unit: liter (L);

[0081] V2 —— Reading of the flowmeter after sampling, unit: liter (L);

[0082] f —— Correction factor of the wet gas flowmeter;

[0083] t1 —— Value of the average temperature of the gas during sampling, unit: degree Celsius (℃);

[0084] P —— Value of the atmospheric pressure during sampling, unit: kilopascal (KPa);

[0085] P1 —— Value of the gas pressure during sampling, unit: kilopascal (KPa);

[0086] P2 —— Value of the saturated water vapor pressure at the gas temperature during sampling, unit: kilopascal (KPa);

[0087] The calculation result should be rounded to two decimal places.

[0088] Actual measured data of the example:

[0089]

[0090]

[0091] Example 2

[0092] This example provides a method for detecting the total oil content in coke oven gas, which specifically includes the following steps:

[0093] 1. In this example, the source of the coke oven gas is Shenmu Tianyuan Chemical Co., Ltd., and the sampling device as shown in Figure 1 is used. The specific sampling steps are as follows:

[0094] a) Accurately measure two portions of 50 mL of perchloroethylene (analytical reagent grade) and transfer them into two absorption bottles 2 placed in an ice-water bath 3. Fill the wet gas flowmeter 7 with distilled water.

[0095] b) The maximum distance between the external part of the coke oven gas pipe and the absorption bottle does not exceed 200 mm. In this embodiment, the distance is 195 mm. Check the airtightness of the device. After confirming that the system is highly airtight, record the reading of the wet gas flowmeter as 8442 L.

[0096] c) Open the sampling valve 1 and adjust the coke oven gas flow rate to 1.5 L / min. Record the average temperature of the gas during sampling as 16 °C and the atmospheric pressure as 89873 Pa through the thermometer 5, and record the coke oven gas pressure as 45 Pa through the U-shaped manometer 6.

[0097] d) Close the sampling valve 1 and record the reading of the wet gas flowmeter 7 as 8957 L.

[0098] 2. Analysis

[0099] a) Retrieve the absorption bottles, mix the absorbents in the two absorption bottles evenly, and accurately measure the recovered volume of the absorbent as 94 ml.

[0100] b) Turn on the main unit and workstation of the infrared oil analyzer. Set the curve range to 0 - 100 mg / L and draw the standard curve according to the method in Example 1.

[0101] 3. Use pure perchloroethylene as the blank for analysis, then pour the sample to be measured into a 4 cm quartz cuvette for colorimetry, and obtain the concentration of total oil in the absorbent according to the standard curve.

[0102] c) Calculation:

[0103] The total oil content in the coke oven gas is calculated in terms of mass concentration and is expressed in milligrams per cubic meter (mg / m3). The calculation method is the same as that in Example 1. The measured data in this embodiment:

[0104]

[0105]

[0106] Example 3

[0107] This embodiment provides a method for detecting the total oil content in coke oven gas, which specifically includes the following steps:

[0108] 1. In this embodiment, the source of the coke oven gas is Shenmu Tianyuan Chemical Co., Ltd., and the sampling device shown as Figure 1 is used. The specific sampling steps are as follows:

[0109] a) Accurately measure two portions of 50 mL of perchloroethylene (analytical reagent grade) and transfer them into two absorption bottles 2 placed in an ice-water bath 3. The wet gas flowmeter 7 is filled with distilled water.

[0110] b) The maximum distance between the outer part of the coke oven gas pipe and the absorption bottle does not exceed 200 mm. In this embodiment, the distance is 194 mm. Check the airtightness of the device. After confirming that the system is well-sealed, record the reading of the wet gas flowmeter as 9842 L.

[0111] c) Open the sampling valve 1 and adjust the coke oven gas flow rate to 1.6 L / min. Record the average gas temperature during sampling as 14 °C and the atmospheric pressure as 89684 Pa through the thermometer 5, and record the coke oven gas pressure as 54 Pa through the U-shaped manometer 6.

[0112] d) Close the sampling valve 1 and record the reading of the wet gas flowmeter 7 as 9957.

[0113] 2. Analysis

[0114] a) Retrieve the absorption bottles, mix the absorbents in the two absorption bottles evenly, and accurately measure the recovered volume of the absorbent as 98 ml.

[0115] b) Turn on the infrared oil analyzer main unit and the workstation, set the curve range to 0 - 100 mg / L, and draw a standard curve according to the method in Example 1.

[0116] 3. Use pure perchloroethylene as the blank for analysis, then pour the sample to be measured into a 4-cm quartz cuvette for colorimetry, and obtain the total oil concentration in the absorbent according to the standard curve.

[0117] c) Calculation:

[0118] The total oil content in coke oven gas is calculated in terms of mass concentration, and the value is expressed in milligrams per liter (mg / m 3 ) as shown. The specific calculation method is the same as that in Example 1. The measured data in this embodiment are:

[0119]

[0120]

[0121] Example 4

[0122] This embodiment provides a method for detecting the total oil content in coke oven gas, which specifically includes the following steps:

[0123] 1. In this embodiment, the source of the coke oven gas is Shenmu Tianyuan Chemical Co., Ltd., and the sampling device as shown is used. The specific sampling steps are as follows: Figure 1 As shown, the specific sampling steps are:

[0124] a) Accurately measure two portions of 50 mL of perchloroethylene (analytical reagent grade) and separately transfer them into two absorption bottles 2 placed in an ice-water bath 3. The wet gas flowmeter 7 is filled with distilled water.

[0125] b) The maximum distance between the external part of the coke oven gas pipe and the absorption bottle does not exceed 200 mm. In this embodiment, the distance is 195 mm. Check the airtightness of the device. After confirming that the system is airtight, record the reading of the wet gas flowmeter as 8798 L.

[0126] c) Open the sampling valve 1 and adjust the coke oven gas flow rate to 1.1 L / min. Record the average gas temperature during sampling as 16 °C and the atmospheric pressure as 89873 Pa through the thermometer 5, and record the coke oven gas pressure as 45 Pa through the U-shaped manometer 6.

[0127] d) Close the sampling valve 1 and record the reading of the wet gas flowmeter 7 as 8829 L.

[0128] 2. Analysis

[0129] a) Retrieve the absorption bottles, mix the absorbents in the two absorption bottles evenly, and accurately measure the recovered volume of the absorbent as 94 ml.

[0130] b) Turn on the infrared oil analyzer main unit and the workstation. Set the curve range to 0 - 100 mg / L and draw a standard curve according to the method in Example 1.

[0131] 3. Use pure perchloroethylene as the blank for analysis, then pour the sample to be measured into a 4-cm quartz cuvette for colorimetry, and obtain the total oil concentration in the absorbent according to the standard curve.

[0132] c) Calculation:

[0133] The total oil content in coke oven gas is calculated in terms of mass concentration, with the value expressed in milligrams per liter (mg / m 3 ). The specific calculation method is the same as that in Example 1. The measured data in this example are:

[0134]

[0135]

[0136]

[0137] Example 5

[0138] This example provides a method for detecting the total oil content in coke oven gas, which specifically includes the following steps:

[0139] 1. In this example, the source of the coke oven gas is Shenmu Tianyuan Chemical Co., Ltd. The sampling device shown is used, and the specific sampling steps are as follows: Figure 1 As shown,

[0140] a) Accurately measure two portions of 50 mL of perchloroethylene (superior grade pure) and separately pour them into two absorption flasks 2 placed in an ice-water bath 3. Fill the wet gas flowmeter 7 with distilled water.

[0141] b) The maximum distance between the external part of the coke oven gas pipe and the absorption flask does not exceed 200 mm. In this embodiment, the distance is 194 mm. Check the airtightness of the device. After confirming that the system is highly airtight, record the reading of the wet gas flowmeter as 8842 L.

[0142] c) Open the sampling valve 1 and adjust the coke oven gas flow rate to 2 L / min. Record the average gas temperature during sampling as 14 °C and the atmospheric pressure as 89684 Pa through the thermometer 5, and record the coke oven gas pressure as 54 Pa through the U-shaped manometer 6.

[0143] d) Close the sampling valve 1 and record the reading of the wet gas flowmeter 7 as 9692 L.

[0144] 2. Analysis

[0145] a) Retrieve the absorption flasks, mix the absorbents in the two absorption flasks evenly, and accurately measure the recovered volume of the absorbent as 98 ml.

[0146] b) Turn on the main unit and workstation of the infrared oil analyzer, set the curve range to 0 - 100 mg / L, and draw the standard curve according to the method in Example 1.

[0147] 3. Use pure perchloroethylene as the blank for analysis, then pour the sample to be measured into a 4-cm quartz cuvette for colorimetry, and obtain the concentration of total oil in the absorbent according to the standard curve.

[0148] c) Calculation:

[0149] The total oil content in the coke oven gas is calculated by mass concentration, and the value is expressed in milligrams per liter (mg / m 3 ), and the specific calculation method is the same as that in Example 1. The measured data in this example are as follows:

[0150]

[0151] The absorbent is diluted to a 500-ml volumetric flask with perchloroethylene, and the colorimetry result is 43.52 mg / L, so the absorbent concentration is 231.49 mg / L

[0152]

[0153] Comparative Example 1

[0154] This comparative example provides a method for detecting the total oil content in coke oven gas, which specifically includes the following steps:

[0155] 1. In this comparative example, the source of the coke oven gas is Shenmu Tianyuan Chemical Co., Ltd. The sampling device shown in Figure 1 is used. The specific sampling steps are as follows:

[0156] a) Accurately measure two portions of 50 ml of xylene (analytical reagent grade) and place them separately into two absorption bottles 2 placed in an ice-water bath 3. The wet gas flowmeter 7 is filled with distilled water.

[0157] b) The longest distance between the outside of the coke oven gas pipe and the absorption bottle does not exceed 200 mm. In this example, the distance is 198 mm. Check the airtightness of the device. After confirming that the system is airtight, record the reading of the wet gas flowmeter as 9195 L.

[0158] c) Open the sampling valve 1 and adjust the flow rate of the coke oven gas to 2.0 L / min. Record the average gas temperature during sampling as 15 °C and the atmospheric pressure as 89875 Pa through the thermometer 5, and record the pressure of the coke oven gas as 30 Pa through the U-shaped manometer 6.

[0159] d) Close the sampling valve 1 and record the reading of the wet gas flowmeter 7 as 9405 L.

[0160] 2. Analysis

[0161] a) Retrieve the absorption bottles, mix the absorbents in the two absorption bottles evenly, and accurately measure the recovered volume of the absorbent as 92 ml.

[0162] b) Turn on the main unit and workstation of the ultraviolet oil analyzer, select the ultraviolet standard curve range of 0 - 50 mg / L, configure the petroleum standard solution according to the method in the instruction manual, make the volume constant with xylene, use xylene as the blank analysis, then pour it into a 1 cm quartz cuvette for colorimetry to measure the total oil concentration in the absorbent.

[0163] c) Calculation:

[0164] The total oil content in the coke oven gas is calculated by mass concentration, and the value is expressed in milligrams per cubic meter (mg / m 3 ). The data processing method is the same as that in Example 1. The measured data in this comparative example are as follows:

[0165]

[0166]

[0167] From the test results of the above examples and comparative examples, it can be seen that for the analysis by tetrachloroethylene absorption and infrared spectrophotometry colorimetry, the analysis range is wide and the data are stable and accurate; for the analysis by xylene absorption and ultraviolet spectrophotometry colorimetry, the absorbance of the reagent blank is large during colorimetry, the analysis data are on the small side, and the accuracy is poor. This is because xylene is a component in the gas itself, and there is a large difference between it as an absorbent and the actual total oil content, so it is inaccurate.

[0168] Obviously, the above embodiments are merely examples given for clear illustration and are not limitations on the implementation manners. For those of ordinary skill in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to enumerate all the implementation manners here. And the obvious changes or modifications derived therefrom still fall within the protection scope of the present invention.

Claims

1. A detection method for the total oil content in coke oven gas, characterized in that, It includes the following steps: Absorb the oil in the coke oven gas with tetrachloroethylene, detect the total oil content in the tetrachloroethylene, and calculate the total oil content in the coke oven gas; The tetrachloroethylene absorbs the oil in the coke oven gas at 0-4°C; the flow rate of the coke oven gas is 1 L / min to 2 L / min.

2. The detection method for the total oil content in coke oven gas according to claim 1, characterized in that, Load the tetrachloroethylene into the absorption bottle, introduce the coke oven gas into the absorption bottle, and the tetrachloroethylene absorbs the oil in the coke oven gas.

3. The detection method for the total oil content in coke oven gas according to claim 2, wherein One to three absorption bottles are provided.

4. The detection method for the total oil content in coke oven gas according to claim 3, wherein Two absorption bottles are provided.

5. The detection method for the total oil content in coke oven gas according to any one of claims 1-4, characterized in that, The infrared spectrophotometry is used to detect the total oil content in the tetrachloroethylene.

6. The detection method for the total oil content in coke oven gas according to claim 5, characterized in that, The scanning range of the infrared spectrophotometry is 3400 cm -1 ~2400 cm -1 .

7. The detection method for the total oil content in coke oven gas according to any one of claims 1-6, characterized in that, Record the average temperature of the coke oven gas, the atmospheric pressure and the pressure of the coke oven gas during the detection.

8. The detection method for the total oil content in coke oven gas according to claim 7, characterized in that, The total oil content in the coke oven gas is calculated according to formula (1): In the formula: c1 - the concentration of the total oil in the absorbent tetrachloroethylene, unit: mg / L; V - the total volume of the absorbent tetrachloroethylene, unit: L; V0 - the total volume of the coke oven gas converted to the standard state, unit: L.