A device for improving the detection accuracy of oily sludge water and oil content

Abstract

The present invention belongs to the technical field of experimental detection methods, and specifically relates to a device for improving the detection accuracy of water and oil content in oily sludge, which specifically comprises a thermal extraction module, a liquid phase separation module is connected to the top of the thermal extraction module, the liquid phase separation module is connected to a circulating condensation module, and a detection and analysis module; the integrated device is used to achieve effective separation of oil and water in the oily sludge, and can perform accurate quantitative calculations, thereby solving the problems of complicated oil and water detection steps in the oily sludge in the prior art, large errors in detection results, poor repeatability due to imperfect detection methods, and improving the detection accuracy.

Description

Technical Field

[0001] The invention belongs to the technical field of experimental detection methods, and in particular relates to a device for improving the detection accuracy of oily sludge water and oil content. Background Art

[0002] Oily sludge refers to discarded oily solids and muddy substances. Oily sludge is mainly composed of a large number of by-products composed of water, oil and solid particles. Oily sludge mainly comes from human production and consumption of oil. It is mainly oil sludge and oil sands produced in the production process of oil exploration and development industry and petrochemical industry. It has the characteristics of large production volume, high oil content, high heavy oil components, high water content, few comprehensive utilization methods, and great difficulty in treatment. In addition to a large amount of residual oil and petroleum hydrocarbons, oily sludge also contains benzene, phenols, anthracene, pyrene and other toxic substances with foul odors.

[0003] Oily sludge, depending on its source, generally has a water content of 30%-85%, an oil content of 15%-50%, and a solid content of 5%-46%. Among them, water mainly exists in the form of a stable oil-in-water emulsion. Since the oily sludge contains a high content of petroleum hydrocarbons and heavy metals, it is a hazardous waste and therefore needs to be harmlessly treated; at the same time, due to the high content of petroleum hydrocarbons, different methods can be used to recover the crude oil in it. In order to evaluate the economic efficiency of different recovery methods and the recovery value of oily sludge, it is necessary to establish a rapid and accurate analysis method for the water content, oil content and solid content of oily sludge samples. At present, the commonly used methods for analyzing the water content of oily sludge samples are: ① drying method; ② azeotropic distillation method; ③ Karl Fischer titration method; ④ thermal analysis method; the commonly used methods for analyzing the oil content are: ① Soxhlet extraction method; ② infrared spectroscopy scanning method; ③ ultraviolet spectrophotometry, etc. In actual use, since the analysis of moisture content generally adopts the weight method, the analysis of oil content requires re-sampling, solidification through anhydrous sodium sulfate, and then extraction of oil in the oily sludge with a Soxhlet extractor and solvent for analysis. The above method for determining the moisture content and oil content of oily sludge has cumbersome detection steps, time-consuming analysis process, and imperfect detection methods, resulting in errors in the detection results. For example: the water content in oily sludge is relatively high, and the distribution of oil, water and solid content is uneven. There is uneven sampling during the analysis process, which leads to large deviations in the analysis results and cannot clearly reflect the true content of the oily sludge. During the drying method for determining the water content, light hydrocarbon components will volatilize, superimposing the losses of water and light oil components, and the measured water content will be greater than the true value. When determining the oil content of oily sludge, it is necessary to add acid to break the emulsion, add anhydrous sodium sulfate to solidify it, crush it at room temperature, wrap it with filter paper, and use a Soxhlet extractor. A small amount of sample will fall during the crushing process, resulting in a reduction in the sample and inaccurate measurement results. The above problems will affect the accuracy of the measurement results of the water content and oil content of the oily sludge, affect the subsequent on-site production and engineering technology guidance, and cause deviations in environmental pollution assessments. Summary of the invention

[0004] The purpose of the present invention is to provide a device for improving the detection accuracy of water and oil content in oily sludge, so as to solve the problems of complicated detection steps and imperfect detection methods in the detection process of oily sludge, resulting in large errors in detection results and poor repeatability.

[0005] To achieve the above object, the present invention provides the following technical solutions:

[0006] A device for improving the detection accuracy of oily sludge water and oil content, comprising a thermal extraction module and a detection and analysis module, wherein the top of the thermal extraction module is connected to a liquid phase separation module, and the liquid phase separation module is connected to a circulating condensation module, wherein the thermal extraction module comprises a bottle body, a bottle mouth is arranged on the top of the bottle body, a sample rack is connected to the inner thread of the bottle mouth, and the outer thread of the bottle mouth is connected to the liquid phase separation module, wherein the liquid phase separation module comprises an extraction chamber, which is in the shape of an inverted "mountain", the interior of the extraction chamber is a hollow chamber, and both sides of the bottom of the extraction chamber are connected to U-shaped tubes , one end of the U-shaped tube is connected to the bottom of the extraction chamber and a stop valve is arranged on the U-shaped tube, the other end of the U-shaped tube is higher than the bottom of the extraction chamber and a knob air release valve is arranged at the end, a lower liquid channel is connected to the U-shaped tube between the bottom of the extraction chamber and the stop valve, the lower liquid channel is an inverted U-shape, a fixed sleeve is arranged at the protruding end of the lower liquid channel, frosted openings are opened at both ends of the upper part of the extraction chamber, the frosted openings are connected to condensing tubes, and the condensing tubes are connected to a circulating condenser; a gas phase channel is arranged in the middle of the bottom of the extraction chamber, and the gas phase channel is plugged into the bottle mouth and communicates with the bottle body;

[0007] The top of the fixing sleeve is a solid ring platform, the interior of the fixing sleeve is hollow and the inner wall is provided with an internal thread of the fixing sleeve, and the internal thread of the fixing sleeve is threadedly connected with the external thread of the bottle mouth;

[0008] The bottom of the bottle body is provided with a bottle bottom fixing plate, the bottom of the bottle bottom fixing plate is provided with a heating device, the bottle body is a round bottom flask, and explosion-proof beads are placed at the bottom of the bottle body;

[0009] The test includes the following steps:

[0010] Step 1: Extraction Preparation

[0011] Add extraction liquid and explosion-proof beads to the bottle and place it on the heating device for standby use. Put the oily sludge sample into the bottom of the sample rack, connect the liquid phase separation module to the bottle, close the stop valve, connect the condenser to the liquid phase separation module, then connect the circulating condensation module and the liquid phase separation module, and start the circulating condenser;

[0012] Step 2: Circular extraction, condensation and liquefaction to obtain water content

[0013] Start the heating device to heat the bottle body, record the start time of the test, open the stop valve, let the liquid water at the bottom of the extraction chamber slowly enter the U-shaped tube, close the stop valve, continue to cycle the above operations, and read the scale value on the U-shaped tube after the extraction is completed;

[0014] During the above operation, the oil in the upper layer of the extraction chamber flows into the bottle body through the lower liquid channel for cyclic extraction. After extraction, the organic solvent in the bottle body is fixed to volume in a volumetric flask, and filtered through an anhydrous sodium sulfate filling column dried at 550°C to remove residual moisture. After that, the oil content in the organic solvent can be quantitatively analyzed with the help of analytical equipment to obtain the oil content in the oily sludge, and the end time of the test is recorded at this time.

[0015] Step 3: Calculation of water content, oil content, solid content and test time

[0016] The grams of oily sludge sample and the grams of water content and oil content obtained in the experiment are used to obtain the grams of solid content. The water content, oil content and solid content in the oily sludge are further calculated by subtracting the grams of water content and oil content obtained in the experiment from the grams of oily sludge sample.

[0017] Preferably, an adjusting frame hook is provided at the upper end of the sample rack, and an annular frame is overlapped at the upper end of the adjusting frame hook. The annular frame is a double-layer ring, and the upper ring of the annular frame is fixedly connected with a threaded barrel. The threaded barrel is a hollow barrel and is provided with an external thread on the outside. A threaded barrel cap is provided at the top of the threaded barrel, and a through hole for two lower liquid channels to pass through is provided on the threaded barrel cap. The outer wall of the threaded barrel cap is provided with a thread and is threadedly connected with the inner thread of the fixed sleeve. The outer diameter of the threaded barrel cap is the same as the outer diameter of the bottle mouth, and a sample net is suspended at the lower part of the sample rack.

[0018] Preferably, the outlet of the circulating condenser is connected to the liquid inlet hose of the left condenser tube, the liquid outlet of the left condenser tube is connected to the liquid inlet hose of the right condenser tube, and the liquid outlet of the right condenser tube is connected to the inlet hose of the circulating condenser.

[0019] Preferably, the detection and analysis module includes a volumetric flask and an analysis device, and the analysis device can be an infrared photometer, an ultraviolet photometer or a chromatograph.

[0020] Preferably, the detection and analysis module further comprises an anhydrous sodium sulfate filling column, and the anhydrous sodium sulfate filling column needs to be dried at 550°C.

[0021] Preferably, the U-shaped tube is provided with a scale, the bottle mouth is provided with an internal thread, and the internal thread of the bottle mouth is threadedly connected to the sample holder.

[0022] The beneficial technical effects of the present invention compared with the prior art are as follows:

[0023] The present invention provides a device for improving the detection accuracy of water and oil content in oily sludge, comprising a thermal extraction module, a liquid phase separation module connected to the top of the thermal extraction module, and a circulating condensation module connected to the liquid phase separation module; the integrated device is used to effectively separate oil and water in the oily sludge, and can perform accurate quantitative calculations, thereby solving the problems of complicated oil and water detection steps in the oily sludge, large errors in detection results, poor repeatability due to imperfect detection methods, and improving the detection accuracy. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 It is a schematic diagram of the structure of the device for detecting the oil content in oily sludge water and oil content of the present invention;

[0025] Figure 2This is a sample diagram of the sample rack structure of the present invention.

[0026] In the figure, 1-bottle body, 1a-bottom fixing plate, 1b-bottle mouth, 2-extraction liquid, 2a-explosion-proof beads, 3-sample rack, 4-sample net, 5-ring rack, 5a-adjustment rack hook, 5b-threaded cylinder, 5c-threaded cylinder screw cap, 6-U-shaped tube, 7-knob air release valve, 8-extraction chamber, 9-extraction sample, 10-stop valve, 11-gas phase channel, 12-lower liquid channel, 13-frosted mouth, 14-condenser, 15-circulating condenser, 16-heating device, 17-fixing sleeve, 18-fixing sleeve internal thread. DETAILED DESCRIPTION

[0027] In order to make the technical means, creative features, objectives and effects achieved by the present invention easy to understand, the present invention is further explained below in conjunction with specific implementation methods.

[0028] See also Figure 1-2 As shown, the present invention provides a device for improving the detection accuracy of oily sludge water and oil content, comprising a thermal extraction module and a detection and analysis module, the top of the thermal extraction module is connected to a liquid phase separation module, and the liquid phase separation module is connected to a circulation condensation module;

[0029] The hot extraction module comprises a bottle body 1, a bottle mouth 1b with inner and outer double threads is arranged on the top of the bottle body 1, the inner threads of the bottle mouth 1b are connected to the sample rack 3, and the outer side of the bottle mouth 1b is connected to the liquid phase separation device;

[0030] Specifically, the liquid phase separation module includes an extraction chamber 8, which is in the shape of an inverted "mountain", and a gas phase channel 11 is provided in the middle of the bottom of the extraction chamber 8, and the gas phase channel 11 is communicated with the bottle body 1. The inside of the extraction chamber 8 is a hollow chamber. The inverted "mountain"-shaped extraction chamber 8 is convenient for separating and collecting the gas phase and liquid phase generated during the extraction process. The gas phase rises from the middle channel to the circulation condensation module, and after being cooled and turned into liquid, it will gather at the bottom of both ends of the extraction chamber 8, which is convenient for subsequent water-oil stratification and collection;

[0031] Both sides of the bottom of the extraction chamber 8 are connected to U-shaped tubes 6, and scales are set on the U-shaped tubes 6. One end of the U-shaped tube 6 is connected to the bottom of the extraction chamber 8 and a stop valve 10 is set on the U-shaped tube 6. The other end of the U-shaped tube 6 is higher than the bottom of the extraction chamber 8 and a knob air release valve 7 is set at the end. Due to the density difference, the water-oil solution in the extraction chamber 8 will form layers. The bottom aqueous solution can be collected through the U-shaped tube 6 first, and the knob air release valve 7 is used to facilitate liquid water to enter the U-shaped tube 6. The volume of the aqueous solution can be intuitively read through the scales on the U-shaped tube 6; the U-shaped tube 6 between the bottom of the extraction chamber 8 and the stop valve 10 is connected to a lower liquid channel 12, and the lower liquid channel 12 is an inverted U-shape. The extended end of the liquid channel 12 is inserted into the bottle body 1 through the fixed sleeve 17. The top of the fixed sleeve 17 is a solid ring platform. The interior of the fixed sleeve 17 is hollow and the inner wall is provided with a fixed sleeve internal thread 18. The fixed sleeve internal thread 18 is threadedly connected with the external thread of the bottle mouth 1b. Both ends of the upper part of the extraction chamber 8 are provided with frosted openings 13, which are connected to the condenser 14, and the condenser 14 is connected to the circulating condenser 15; the outlet of the circulating condenser 15 is connected to the liquid inlet hose of the left condenser 14, the liquid outlet of the left condenser 14 is connected to the liquid inlet hose of the right condenser 14, and the liquid outlet of the right condenser 14 is connected to the inlet hose of the circulating condenser 15;

[0032] Meanwhile, a bottom fixing plate 1a is arranged at the bottom of the bottle body 1 , a heating device 16 is arranged at the bottom of the bottom fixing plate 1a , the bottle body 1 is a round bottom flask, and explosion-proof beads 2a are placed at the bottom of the bottle body 1 .

[0033] The oily sludge sample is placed in the bottle body 1 through the sample rack 3, and the oil in the oily sludge is extracted under heating conditions by using the principle of similar dispersibility. The oil and water are vaporized at high temperature, and rise to the circulating condensation module through the liquid phase separation module to condense and liquefy into small droplets. In the liquid phase separation module, the water and oil are separated, and the volume of the aqueous solution is read. The oil phase flows into the bottle body through the liquid phase separation device for cyclic extraction. After the extraction, the organic solvent is removed from the bottle body and fixed to a volumetric flask of a certain volume, and the oil phase content is analyzed with the help of the detection and analysis module. The present invention uses an integrated device to simultaneously detect the water and oil contents in the oily sludge by taking only one sample, thereby simplifying the problem of complicated traditional detection steps, and at the same time overcoming the problem of large errors and poor repeatability in the detection results caused by the imperfections of traditional detection methods, thereby improving the overall detection efficiency and detection accuracy.

[0034] Specifically, an adjusting frame hook 5a is provided at the upper end of the sample rack 3, and an annular frame 5 is overlapped at the upper end of the adjusting frame hook 5a. The annular frame 5 is a double-layer ring, and a threaded barrel 5b is fixedly connected to the upper ring of the annular frame 5. The threaded barrel 5b is a hollow cylinder and is provided with an external thread on the outside. A threaded barrel cap 5c is provided on the top of the threaded barrel 5b. A through hole for two lower liquid channels 12 to pass through is provided on the threaded barrel cap 5c, and a thread is provided on the outer wall of the threaded barrel cap 5c and is threadedly connected with the inner thread 18 of the fixed sleeve. The outer diameter of the threaded barrel cap 5c is the same as the outer diameter of the bottle mouth 1b, and a sample net 4 is suspended at the lower part of the sample rack 3; the hanging height of the sample rack 3 in the bottle body 1 is conveniently adjusted through the threaded barrel 5b to ensure that the sample can enter the extraction liquid 2 to ensure the sufficiency of the reaction. At the same time, the threaded connection enhances the sealing effect of the bottle mouth, and the threaded barrel cap 5c not only realizes the ingenious connection between the thermal extraction module and the liquid phase separation module, but also improves the sealing of the device as a whole to ensure the accuracy of the detection.

[0035] When in use, add a certain amount of extract 2 to the bottle body 1, then add the explosion-proof beads 2a that have been treated and dried by the extract 2, and place it on the heating device 16 for standby use. Then put the oily sludge into the sample net 4, and then put the sample net 4 into the sample rack 3. The sample rack 3 is suspended on the annular rack 5 through the adjustment rack hook 5a, and the threaded barrel cap 5c is slowly rotated to make the threaded barrel 5b and the bottle mouth 1b threadedly connected and the sample rack 3 extends into the bottle body 1 at a suitable height position. Then, the gas phase channel 11 is threadedly connected with the bottle mouth 1b and the threaded barrel cap 5c through the fixing sleeve 17. When connecting, the lower liquid channel 12 passes through the through hole on the threaded barrel cap 5c, the stop valve 10 is closed, the knob vent valve 7 is opened, the condenser 14 is connected to the extraction chamber 8 through the frosted port 13, and then the outlet of the circulating condenser 15 is connected. The bottle 1 is connected to the liquid inlet hose of the left condenser 14, the liquid outlet of the left condenser 14 is connected to the liquid inlet hose of the right condenser 14, and the liquid outlet of the right condenser 14 is connected to the inlet hose of the circulating condenser 15; during extraction, the heating device 16 and the circulating condenser 15 are turned on, the organic solvent or water in the bottle 1 is vaporized by high temperature, rises to the condenser 14 through the gas phase channel 11, and liquefies, and becomes small droplets in the extraction chamber 8. The water phase and the oil phase are separated, and the stop valve 10 is opened to allow the separated water to slowly enter the U-shaped tube 6 until the liquid phase water level is level with the bottom of the extraction chamber 8, and then the stop valve 10 is closed, the volume of the aqueous solution in the U-shaped tube 6 is read, and then the stop valve 10 is opened to allow the water phase to completely pass through the stop valve 10, and then the stop valve 10 is closed, and the oil phase flows into the bottle 1 through the lower liquid channel 12 for circulation extraction.

[0036] The test includes the following steps:

[0037] Step 1: Extraction Preparation

[0038] Add the extracting liquid 2 and the explosion-proof beads 2a to the bottle 1 and place it on the heating device 16 for standby use. Take m (g) of the oily sludge sample and put it into the bottom of the sample rack 3 so that the sample is immersed in the extracting liquid 2 in the bottle 1. Connect the liquid phase separation module to the bottle 1, close the stop valve 10, connect the condensing pipe 14 to the liquid phase separation module, then connect the circulating condensing module and the liquid phase separation module, and start the circulating condenser 15.

[0039] Step 2: Circular extraction, condensation and liquefaction to obtain water content

[0040] Start the heating device 16 to heat the bottle 1. At this time, record the start time of the test as t1. Using the similarity-compatible principle, extract the oil in the oily sludge under heating conditions. The oil and water are vaporized at high temperature and enter the condenser 14 through the gas phase channel 11 to condense and liquefy into small droplets. The water and oil gathered in the extraction chamber 8 form layers. Open the stop valve 10 to allow the liquid water at the bottom of the extraction chamber 8 to slowly enter the U-shaped tube 6. Close the stop valve 10 and continue to cycle the above operations. After the extraction is completed, read the scale value v (ml) on the U-shaped tube 6, which is the water content m1 (g) in the oily sludge.

[0041] During the above operation, the oil in the upper layer of the extraction chamber 8 will flow into the bottle body 1 through the lower liquid channel 12 for cyclic extraction. After extraction, the organic solvent in the bottle body 1 is fixed to volume in a volumetric flask and filtered through an anhydrous sodium sulfate filling column dried at 550°C to remove residual moisture. After that, the oil content in the organic solvent can be quantitatively analyzed with the help of analytical equipment to obtain the oil content m2(g) in the m(g) oily sludge. At this time, the end time of the test is recorded as t2.

[0042] Step 3: Calculation of water content, oil content and solid content

[0043] The solid content m3 is calculated by the weight m of the oily sludge sample, the water content m1 and the oil content m2 obtained in the experiment. The water content, oil content and solid content in m grams of oily sludge can be further calculated. The specific calculation formula is as follows:

[0044] m(g) Water content in oily sludge = m1 / m×100%;

[0045] m(g) Oil content in oily sludge = m2 / m×100%;

[0046] m(g) solid content in oily sludge = m-m1-m2 / m×100%;

[0047] It should also be noted that the time t used to complete the detection of water content and oil content in oily sludge by adopting the technical solution of the present invention is calculated by the start and end time of the test, t=t2-t1.

[0048] The detection and analysis module includes a volumetric flask and analysis equipment. The analysis equipment can be an infrared photometer, an ultraviolet photometer or a chromatograph. The detection and analysis module also includes an anhydrous sodium sulfate filling column, which needs to be dried at 550°C. After extraction, the organic solvent is removed from the bottle body and fixed to a volumetric flask of a certain volume. In order to remove a small amount of water in the organic solvent, it can be filtered through an anhydrous sodium sulfate filling column dried at 550°C, and the oil phase content is analyzed with the help of analysis equipment such as an infrared photometer, an ultraviolet photometer or a chromatograph.

[0049] In order to better reflect the technical scheme and technical effects of the present invention, the technical effects achieved by this scheme are reflected by comparing the specific implementation steps:

[0050] The oily sludge samples from the oil sludge pool in an oilfield operating area were taken as the analysis objects. Indoor test analysis was carried out according to two different methods: the traditional method and the present technology. The water content can be determined according to CJ / T221-2023, and the oil content can be determined according to the traditional method CJ / T221-2023. The traditional method uses Soxhlet extraction and then infrared spectrophotometry to determine the total oil, mineral oil, animal and vegetable oil in urban sludge. The sample measurement wavenumber selection range is 3400 cm~2400 cm. The total oil substances in the sludge are extracted with tetrachloroethylene, and the total oil is determined. Then the extract is adsorbed with magnesium silicate, and the polar substances such as animal and vegetable oils are eluted before the mineral oil is determined.

[0051] The data analysis results are summarized as follows:

[0052] (1) The oil content, water content and solid content of oily sludge were tested by using a traditional Soxhlet extractor, oven, electronic balance and infrared spectrophotometer, and compared with this technical method:

[0053] Data verification is to use different sampling amounts for the same sample of oily sludge, and to test it in the same laboratory using the traditional method and the method of the technical solution of the present invention. The main test parameters are water content, oil content and solid content. The test results are compared based on repeatability, accuracy, total value, etc. The test results are shown in Table 1;

[0054] Table 1 Comparison test data of different methods for determining oily sludge

[0055]

[0056] It can be seen from the data in Table 1 that when the sample size is about 5 g, the relative standard deviations of the oil content and solid content determined by the traditional method are 27.58%, 11.08% and 5.97% respectively. There is a large experimental error in the determination of data accuracy. Under the same sampling volume, the method in this case is used for single injection. The device is used to achieve small volatility and good repeatability. The relative standard deviations of water content, oil content and solid content are 1.9%, 0.23% and 2.36% respectively.

[0057] When the sample size is about 10g, the relative standard deviations of the water content, oil content and solid content determined by the traditional method are 16.3%, 25.13% and 5% respectively. Under the same sampling volume, the single injection method of this case is adopted. The application of this device achieves small volatility and good repeatability. The relative standard deviations of the water content, oil content and solid content are 0.18%, 2.08% and 0.17% respectively; at the same time, it can save time costs 3~3.2 times and improve work efficiency.

[0058] Therefore, the experimental data show that in the specific implementation of the control variable test data, the traditional method has large data volatility, poor repeatability, low accuracy, and great limitations. It cannot accurately detect the moisture content, oil content and solid content of oily sludge, and cannot guide on-site production needs. The test data in this case has small volatility, good repeatability, low standard deviation, and a total content close to 100%, which fully meets the requirements of analytical data accuracy.

[0059] (2) The oil content, water content and solid content of oily sludge were tested and compared with the technical method using traditional gas chromatography, solid-liquid extraction instrument and electronic balance.

[0060] Table 2 Comparison test data of different methods for determining oily sludge

[0061]

[0062] From the data in Table 2, it can be detected that the errors and fluctuations of multiple sampling measurements are large, and the relative standard deviations of oil content, water content and solid content are 16.48%, 18.23% and 1.43% respectively; in this case, the relative standard deviations of oil content, water content and solid content measured three times in a row are 6.41%, 2.98% and 0.001% respectively; at the same time, it can save time costs by 2.6 times and improve work efficiency.

[0063] The present invention discloses a device for improving the detection accuracy of water and oil content in oily sludge, aiming to solve the problems of complicated detection steps and imperfect detection methods in the detection process of oily sludge, resulting in large errors in detection results and poor repeatability; an integrated device is used to effectively separate oil and water in oily sludge, and accurate quantitative calculation can be performed, thereby improving the accuracy of the detection results of water content and oil content in oily sludge.

[0064] The above shows and describes the basic principles, main features and advantages of the present invention. It should be understood by those skilled in the art that the present invention is not limited by the above embodiments, and the above embodiments and descriptions are only preferred examples of the present invention, and are not intended to limit the present invention. Various changes and improvements may be made without departing from the scope of the present invention, and these changes and improvements fall within the scope of the invention to be protected, and the scope of the present invention to be protected is defined by the attached claims and their equivalents.

Claims

1. A device for improving the detection accuracy of oily sludge water and oil content, comprising a thermal extraction module and a detection and analysis module, wherein the top of the thermal extraction module is connected to a liquid phase separation module, and the liquid phase separation module is connected to a circulation condensation module, wherein the thermal extraction module comprises a bottle body (1), wherein a bottle mouth (1b) is arranged at the top of the bottle body (1), a sample rack (3) is connected inside the bottle mouth (1b), and the outside of the bottle mouth (1b) is connected to the liquid phase separation module, wherein: The liquid phase separation module comprises an extraction chamber (8), the extraction chamber (8) is in the shape of an inverted "mountain", the interior of the extraction chamber (8) is a hollow chamber, both sides of the bottom of the extraction chamber (8) are connected to U-shaped tubes (6), one end of the U-shaped tube (6) is connected to the bottom of the extraction chamber (8) and a stop valve (10) is provided on the U-shaped tube (6), the other end of the U-shaped tube (6) is higher than the bottom of the extraction chamber (8) and a knob air release valve (7) is provided at the end, and the bottom of the extraction chamber (8) and the stop valve (10) are connected to each other. The U-shaped tubes (6) are connected to a lower liquid channel (12), the lower liquid channel (12) is an inverted U-shape, a fixing sleeve (17) is provided at the protruding end of the lower liquid channel (12), both ends of the upper part of the extraction chamber (8) are provided with frosted openings (13), the frosted openings (13) are connected to a condenser (14), the condenser (14) is connected to a circulating condenser (15), and a gas phase channel (11) is provided in the middle of the bottom of the extraction chamber (8), and the gas phase channel (11) is communicated with the bottle body (1); The top of the fixing sleeve (17) is a solid ring platform, the interior of the fixing sleeve (17) is hollow and the inner wall is provided with a fixing sleeve internal thread (18), and the fixing sleeve internal thread (18) is threadedly connected to the external thread of the bottle mouth (1b); The bottom of the bottle body (1) is provided with a bottle bottom fixing plate (1a), the bottom of the bottle bottom fixing plate (1a) is provided with a heating device (16), the bottle body (1) is a round-bottom flask, and explosion-proof beads (2a) are placed at the bottom of the bottle body (1); The test includes the following steps: Step 1: Extraction Preparation The bottle (1) is added with an extracting liquid (2) and explosion-proof beads (2a) and placed on a heating device (16) for standby use. The oily sludge sample is placed at the bottom of the sample rack (3). The liquid phase separation module is connected to the bottle (1). The stop valve (10) is closed. The condensation pipe (14) is connected to the liquid phase separation module. The circulating condensation module and the liquid phase separation module are then connected. The circulating condenser (15) is started to work. Step 2: Circulate extraction and condense to obtain water content The heating device (16) is started to heat the bottle body (1), and the test start time is recorded at this time. The stop valve (10) is opened to allow the liquid water at the bottom of the extraction chamber (8) to slowly enter the U-shaped tube (6). The stop valve (10) is closed and the above operation is continued to be circulated. After the extraction is completed, the scale value on the U-shaped tube (6) is read; During the above operation, the oil in the upper layer of the extraction chamber (8) flows into the bottle body (1) through the lower liquid channel (12) for cyclic extraction. After extraction, the organic solvent in the bottle body (1) is fixed to a volumetric flask and filtered through an anhydrous sodium sulfate column dried at 550° C. to remove residual water. After that, the oil content in the organic solvent can be quantitatively analyzed with the aid of an analytical device to obtain the oil content in the oily sludge. At this time, the end time of the test is recorded. Step 3: Calculation of water content, oil content, solid content and test time The grams of oily sludge sample and the grams of water content and oil content obtained in the experiment are used to obtain the grams of solid content. The water content, oil content and solid content in the oily sludge are further calculated by subtracting the grams of water content and oil content obtained in the experiment from the grams of oily sludge sample.

2. The device for improving the detection accuracy of oily sludge water and oil content according to claim 1 is characterized in that: The upper end of the sample rack (3) is provided with an adjustment rack hook (5a), and the upper end of the adjustment rack hook (5a) is overlapped with an annular rack (5), the annular rack (5) is a double-layer ring, and the upper ring of the annular rack (5) is fixedly connected with a threaded barrel (5b), the threaded barrel (5b) is a hollow barrel and is provided with an external thread on the outside, and the top of the threaded barrel (5b) is provided with a threaded barrel screw cap (5c), and the threaded barrel screw cap (5c) is provided with a through hole for two lower liquid channels (12) to pass through, and the outer wall of the threaded barrel screw cap (5c) is provided with a thread and is threadedly connected with the inner thread (18) of the fixed sleeve, and the outer diameter of the threaded barrel screw cap (5c) is the same as the outer diameter of the bottle mouth (1b), and a sample net (4) is suspended at the lower part of the sample rack (3).

3. The device for improving the detection accuracy of oily sludge water and oil content according to claim 2 is characterized in that: The outlet of the circulating condenser (15) is connected to the liquid inlet hose of the left condenser tube (14), the liquid outlet of the left condenser tube (14) is connected to the liquid inlet hose of the right condenser tube (14), and the liquid outlet of the right condenser tube (14) is connected to the inlet hose of the circulating condenser (15).

4. The device for improving the detection accuracy of oily sludge water and oil content according to claim 3 is characterized in that: The detection and analysis module includes a volumetric flask and an analysis device. The analysis device can be an infrared photometer, an ultraviolet photometer or a chromatograph.

5. The device for improving the detection accuracy of oily sludge water and oil content according to claim 4 is characterized in that: The detection and analysis module also includes an anhydrous sodium sulfate filling column, which needs to be dried at 550°C.

6. The device for improving the detection accuracy of oily sludge water and oil content according to claim 5 is characterized in that: The U-shaped tube (6) is provided with a scale, the bottle mouth (1b) is provided with an internal thread, and the internal thread of the bottle mouth (1b) is threadedly connected to the sample rack (3).

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