CN215327611U - Industry short-term test oil content equipment of oily sludge - Google Patents
Industry short-term test oil content equipment of oily sludge Download PDFInfo
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- CN215327611U CN215327611U CN202023254910.2U CN202023254910U CN215327611U CN 215327611 U CN215327611 U CN 215327611U CN 202023254910 U CN202023254910 U CN 202023254910U CN 215327611 U CN215327611 U CN 215327611U
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Abstract
The utility model relates to the technical field of oil content detection of sludge, in particular to equipment for industrially and rapidly detecting oil content of oily sludge. The device comprises a stirring device, a filtering device, an extraction liquid storage tank, an optical measuring device and a computer processing system, wherein the operations of the stirring device, the filtering device and the optical measuring device are controlled by the computer processing system, so that the error of manual operation is reduced, and the working efficiency of a laboratory technician during laboratory test is improved; and equipment is in the closed state during the detection, can effectively avoid solvent and oil to volatilize, and measuring result is more accurate, and the security is higher.
Description
Technical Field
The utility model relates to the technical field of sludge oil content detection, in particular to equipment for industrially and rapidly detecting oil content of oily sludge.
Background
The oil content is an important index in the process of disposing the oily sludge and is directly related to the adjustment of equipment model selection and operation conditions. The actual production and supervision processes of the oily sludge project need to regularly detect the oily sludge. However, the oily sludge is not uniformly distributed, and the detection period is generally long, so that the delay of the detection result brings adverse effects on the actual production.
The ultraviolet oil measurement method is a new method for measuring oil in water, which is newly released by the national ecological environment protection department in 2018, 10 and 10 months, and the national environmental protection standard of the people's republic of China: HJ970-2018 ultraviolet spectrophotometry (trial) for measuring water quality petroleum. The existing method for measuring oil in water has two standards, one is infrared spectrophotometry, the other is ultraviolet spectrophotometry, the infrared spectrophotometry is used for measuring oil in domestic sewage and industrial wastewater, and the ultraviolet spectrophotometry is used for measuring petroleum in surface water, underground water and seawater.
The measurement principle of the ultraviolet spectrophotometry is as follows: according to the principle of Lambert-beer's law of optical absorption, petroleum absorbs photometrically at the wavelength of 225nm of ultraviolet light, and the mass content of the petroleum is calculated by directly proportional relationship between the absorbance and the mass content of the petroleum.
At present, the national standard method for detecting the oily sludge needs more than 8 hours, most of the time is used for sample pretreatment (extraction and filtration), when an organic solvent is used for dissolving oil in the oily sludge, a horizontal oscillator is generally adopted for assisting the dissolution, then Soxhlet extraction filtration is adopted, and other treatment processes are added, so that the time is as long as 6-8 hours, and the method is difficult to adapt to the requirements of industrial production sites. During sample preparation, the organic solvent can volatilize to a certain extent, so that the detection precision and the physical health of people are influenced.
SUMMERY OF THE UTILITY MODEL
In order to overcome the defects of the prior art, the utility model aims to provide an industrial device for quickly detecting the oil content of oily sludge, which can quickly detect the oil content in the oily sludge.
The purpose of the utility model is realized by adopting the following technical scheme:
an industrial equipment for rapidly detecting the oil content of oily sludge comprises a stirring device, a filtering device, an extract liquor storage tank, an optical measuring device and a computer processing system; the stirring device is provided with an oily sludge inlet and an extractant inlet; the mixed liquid outlet of the stirring device is connected with the mixed liquid inlet of the filtering device; the stirring device and the filtering device are both provided with weight inductors; an extract liquid outlet of the filtering device is connected with an extract liquid inlet of the extract liquid storage tank; an extract liquid outlet of the extract liquid storage tank is connected with an extract liquid inlet of the optical measuring device; the stirring device, the filtering device, the extraction liquid storage tank and the optical measuring device are respectively in communication connection with the computer processing system.
Further, the stirring device is provided with a first branch pipe, a blow-off pipe and a second branch pipe; the first branch pipe is connected with a sewage discharge pipe through a first valve; the first branch pipe is connected with the second branch pipe through a second valve and a first power pump; the second branch pipe is connected with the filtering device; the blow-down pipe is connected with the extract liquor storage tank through a fourth valve; the first valve, the second valve, the fourth valve and the first power pump are respectively in communication connection with a computer processing system.
Still further, the stirring device comprises a blade stirrer.
Further, the filtering device comprises a filtering layer containing filtering media and a third branch pipe; the third branch pipe is connected with the extract liquid storage tank; the third branch pipe is provided with a third valve and a second power pump; and the third valve and the second power pump are respectively in communication connection with the computer processing system.
Furthermore, the filtering layer is divided into an upper layer and a lower layer, the upper layer is a microporous ceramic material filling layer, and the lower layer is an anhydrous sodium sulfate filling layer and/or a magnesium silicate filling layer.
Further, the filtering device is divided into an upper part and a lower part, and the shape of the lower part structure is conical.
Still further, the optical measuring device is an ultraviolet spectrophotometer.
Furthermore, the extract liquid storage tank is provided with a fourth branch pipe, the fourth branch pipe is connected with the optical measurement device, and the fourth branch pipe is provided with a fifth valve; and the fifth valve is in communication connection with the computer processing system.
The process for rapidly detecting the oil content of the oily sludge comprises the following steps:
1) mass m1Oil-containing sludge and mass m2Adding the extractant into a stirring device, mixing and stirring to obtain a mixed solution, and weighing the total mass M of the mixed solution by a weight sensor of the stirring device1And transmitting the data to a computer processing system;
2) conveying the mixed liquid obtained in the step 1) to a filtering device, filtering out filter residues and filtrate, and weighing the mass M of the filter residues by a weight sensor on the filtering device2And transmitting the data to a computer processing system;
3) conveying the filtrate obtained in the step 2) to an extraction liquid storage tank, injecting the filtrate into an optical measuring device through the extraction liquid storage tank, measuring the oil content N in the filtrate by the optical measuring device, and transmitting data to a computer processing system;
4) and the computer processing system calculates the oil content w in the oily sludge according to the measured data:
and displaying the measurement results on a computer processing system.
Further, in the step 1), the extracting agent is benzene or n-hexane, and the mass ratio of the oily sludge to the extracting agent is 1: 10-20. Because the oil in the oily sludge has certain absorption to the extractant, in order to reduce the measurement error, the extractant needs to be excessive, which is favorable for improving the accuracy of the measurement result.
Compared with the prior art, the utility model has the beneficial effects that:
the stirring device is used for fully mixing the sludge containing the mineral oil and the extracting agent; the filtering device is used for removing water and polar molecules of the mixed solution and separating filter residue and filtrate; the extraction liquid storage tank is used for storing the filtrate and transmitting the filtrate to the optical measurement device; the optical measuring device is used for measuring the mass content of the petroleum in the filtrate; and the computer processing system is used for calculating the petroleum content of the oily sludge. The operation of the stirring device, the filtering device and the optical measuring device is controlled by a computer processing system, so that the error of manual operation is reduced, and the working efficiency of a tester during testing is improved; and equipment is in the closed state during the detection, can effectively avoid solvent and oil to volatilize, and measuring result is more accurate, and the security is higher.
Drawings
FIG. 1 is a connection diagram of the apparatus of the present invention.
In the figure: 1. a stirring device; 101. a first valve; 102. a second valve; 1001. a first power pump; 103. a third valve; 1002. a second power pump; 104. a fourth valve; 105. a fifth valve; 11. a first branch pipe; 12. a second branch pipe; 13. thirdly, pipe distribution; 14. a fourth branch pipe; 15. a blow-off pipe; 201. a blade blender; 2. a filtration device; 202. a filter layer; 3. an extract liquid storage tank; 4. an optical measuring device; 5. a computer processing system.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and the detailed description, and it should be noted that any combination of the embodiments or technical features described below can be used to form a new embodiment without conflict.
As shown in figure 1, the equipment for industrially and rapidly detecting the oil content of the oily sludge comprises a stirring device 1, a filtering device 2, an extract liquid storage tank 3, an optical measuring device 4 and a computer processing system 5;
the stirring device 1 is provided with an oily sludge inlet and an extractant inlet; a blade stirrer 201 is arranged in the stirring device 1, a weight sensor is arranged at the bottom of the stirring device 1, and a first branch pipe 11 is connected to the bottom of the stirring device 1; the first branch pipe 11 is communicated with the sewage discharge pipe 15, and a first valve 101 is arranged between the first branch pipe 11 and the sewage discharge pipe 15; the first branch pipe 11 is simultaneously communicated with the second branch pipe 12, and a second valve 102 and a first power pump 1001 are arranged between the first branch pipe 11 and the second branch pipe 12; the stirring device 1 is communicated with the upper part of the filtering device 2 through a second branch pipe 12, and the second branch pipe 12 is used for conveying the mixed liquid of the oily sludge and the extracting agent of the stirring device 1 to the filtering device 2.
The filtering device 2 comprises a filtering layer 202, wherein the filtering layer 202 is divided into an upper layer and a lower layer, and microporous ceramic materials are filled in the upper layer and used for filtering solid particles; the lower layer is anhydrous sodium sulfate and magnesium silicate for absorbing water and other polar molecules in the filtrate; the bottom of the filtering device 2 is communicated with the upper part of the extraction liquid storage tank 3 through a third branch pipe 13, and the third branch pipe 13 is used for conveying the extraction liquid from the filtering device 2 to the extraction liquid storage tank 3; a third valve 103 and a second power pump 1002 are arranged on the third branch pipe 13; the bottom of the filter device 2 is provided with a weight sensor. The filtering device 2 is divided into an upper part and a lower part, and the outline of the lower structure is conical.
The side bottom of the extraction liquid storage tank 3 injects extraction liquid into the optical measurement device 4 through a fourth branch pipe 14, and a fifth valve 105 is arranged on the fourth branch pipe 14; the bottom of the extract liquid storage tank 3 is communicated with a drain pipe 15, and a fourth valve 104 is arranged between the extract liquid storage tank and the drain pipe; the bottom of the extraction liquid storage tank 3 is provided with a weight sensor.
The optical measuring device 4 is an ultraviolet spectrophotometer, and converts an optical signal of ultraviolet rays passing through the sample into an electric signal and transmits the electric signal to the computer processing system 5. The computer processing system 5 controls the opening and closing and time states of each valve and each power pump; processing the signals transmitted by each weight sensor; controlling the stirring state of the blade stirrer 201; displaying the detection result of the sample; .
The process for rapidly detecting the oil content of the oily sludge comprises the following steps:
1) the first valve 101 and the second valve 102 are closed, and a certain mass of oily sludge m is added1And an extractant m2Adding into a blade stirrer 201, stirring to obtain a mixed solution, controlling the stirring speed and time by a computer processing system 5, and measuring the total mass M of the mixed solution of the oily sludge and the extractant by a weight sensing device arranged at the bottom of the stirring device 11；
2) Opening a second valve 102 and a first power pump 1001, conveying the mixed liquor extracted from the stirring device 1 to a filtering device 2 through a second branch pipe 12, filtering solid particles, moisture and polar molecules in the mixed liquor by the filtering device 2, opening a third valve 103 and a second power pump 1002 during filtering, and conveying the extraction liquor into an extraction liquor storage tank 3 through a third branch pipe 13;
3) the bottom of the filtering device 2 is provided with a weight inductor, and the mass of the filter residue is weighed to be M2The filter residue mainly comprises solid particles and water in the oily sludge; when mass M of filter residue2When the change is not changed, the extract liquid is completely filtered; after the filtration is finished, closing the fourth valve 104 and the fifth valve 105, and recovering an extraction liquid from the extraction liquid storage tank 3, wherein the main components of the extraction liquid are an extracting agent and petroleum;
4) opening a fifth valve 105, injecting the extraction liquid into the optical measuring device 4 through a fourth branch pipe 14, and measuring the content N of the petroleum in the extraction liquid through the optical measuring device 4;
5) the M obtained above1、M2And N are transmitted to the computer processing system 5, and the oil content w of the oily sludge is calculated by the following formula:
the computer processing system 5 calculates and displays the results.
The opening and closing of each valve and the power pump in the steps are controlled by a computer processing system 5.
Example 1
The equipment for industrially and rapidly detecting the oil content of the oily sludge is applied to the measurement of the oily sludge in a certain waste incineration plant in Guangzhou, and the specific operation is as follows:
1) the first valve 101 and the second valve 102 are closed, and m is11.40g oil-containing sludge and m2Adding 15.00g of n-hexane into a blade stirrer 201, stirring to obtain a mixed solution, controlling the stirring speed of the blade stirrer 201 to be 3000rpm/s and the stirring time to be 10min by a computer processing system 5, and measuring the total mass M of the mixed solution of the oily sludge and the extractant by a weight sensing device arranged at the bottom of the stirring device 11＝16.40g；
2) Opening a second valve 102 and a first power pump 1001, conveying the mixed liquor extracted from the stirring device 1 to a filtering device 2 through a second branch pipe 12, filtering solid particles, moisture and polar molecules in the mixed liquor by the filtering device 2, opening a third valve 103 and a second power pump 1002 during filtering, and conveying the extraction liquor into an extraction liquor storage tank 3 through a third branch pipe 13;
3) the bottom of the filtering device 2 is provided with a weight inductor which is called that the mass of filter residue is M21.00g, wherein the filter residue mainly comprises solid particles and water in the oily sludge; when mass M of filter residue2When the value is not changed within 1 minute, the extraction liquid is completely filtered; after the filtration is finished, closing the fourth valve 104 and the fifth valve 105, and recovering an extraction liquid from the extraction liquid storage tank 3, wherein the main components of the extraction liquid are normal hexane and petroleum;
4) opening a fifth valve 105, injecting the extract into the optical measuring device 4 through a fourth branch pipe 14, and measuring the mass content N of the petroleum in the extract by using the optical measuring device 4 (an ultraviolet spectrophotometer) to be 1.20%;
5) the M obtained above1、M2And N are transmitted to the computer processing system 5, and the oil content w of the oily sludge is calculated by the following formula:
6) After the oil content detection is finished, opening a fourth valve 104 and a first valve 101 to completely discharge waste liquid in the industrial equipment for quickly detecting the oil content of the oily sludge;
the whole detection process time does not exceed 30 minutes.
In the measuring process, the operation of each device and the calculation of data are completed by the computer processing system 5 through program control, and an experimenter only needs to add an extracting agent and oily sludge into the stirring device 1, wherein the time for displaying the results from the step 1) to the step 5) is 28 min.
Comparative example 1
Comparative example 1 the oil content of the oily sludge was measured by conventional soxhlet extraction-ultraviolet absorption photometry, comprising the following steps:
1. preparation of solutions
(1) Standard oil: extracting an oil product from an oily sludge sample by using 30-60 ℃ petroleum ether subjected to dearomatization and redistillation, dehydrating by using anhydrous sodium sulfate, filtering, and putting the filtrate in a constant temperature box at 65 +/-5 ℃ to completely remove residual petroleum ether to obtain a standard oil product.
(2) Standard oil stock solution: 0.100g of a standard oil product is accurately weighed, dissolved in petroleum ether, transferred into a 100mL volumetric flask, diluted to the marked line and stored in a refrigerator, the solution containing 1100mg of oil per mL.
(3) Standard oil use solution: the stock oil was diluted 10-fold with petroleum ether, which contained 0.10mg of oil per ml, just prior to use.
(4) Preparing (60-90 ℃ fraction) dearomatized petroleum ether: silica gel with 60-100 meshes of coarse pores and 70-120 meshes of neutral chromatographic alumina (activated for 4 hours at 150-160 ℃) are filled into a glass column with the inner diameter of 25mm and the height of 750mm before being completely cooled by a column chromatography method. The lower layer of silica gel was 600mm high and covered with 50mm thick alumina, and commercial petroleum ether (60-90 ℃ fraction) was passed through the column to remove aromatics. Collecting petroleum ether in a narrow-mouth bottle, measuring the treated petroleum ether with water as reference at 225nm on an ultraviolet spectrophotometer to ensure that the light transmittance is not less than 80%.
2. Drawing of standard curve
To 750 mL volumetric flasks were added 0, 2.00, 4.00, 8.00, 12.00, 20.00 and 25.00mL of standard oil use solutions, respectively, and diluted to the mark with petroleum ether (60-90 ℃ C.). Absorbance was measured at 254nm on an ultraviolet spectrophotometer using a 1cm quartz cuvette with dearomatized petroleum ether as a reference.
3. Determination of oil-containing sludge sample
(1) 20g of oily sludge sample dehydrated at 105 ℃ in advance is wrapped by filter paper, the wrapped sample is placed into a Soxhlet extractor, petroleum ether with the volume of 1/2-1/3 is added into a round-bottom flask, and the mixture is refluxed and condensed for 6 hours.
(2) And (3) dissolving the residual substances by using dearomatized petroleum ether, transferring the residual substances into a 100mL volumetric flask for constant volume, and measuring the absorbance of the oily sludge sample under the same condition with the standard sample.
(3) The oil content was checked on a standard curve and calculated.
Comparative example 1 the same batch of oily sludge as in example 1 was measured, the calculated oil content in comparative example 1 was 13.47%, and the total time consumed in the measurement procedure in comparative example 1 was 10h16 min.
In summary, the measurement time of example 1 is much shorter than that of comparative example 1, and the measurement process can be effectively shortened. The whole process of comparative example 1 requires manual operation, the error rate is higher than that of the present invention, and in the measurement process, experimenters need to contact with toxic solvents, which may cause damage to the health of the experimenters. And since the measurement process of comparative example 1 is performed in an open environment, the outside may cause contamination and easily cause volatilization of oil, thereby causing deviation of the measurement result.
The equipment for industrially and rapidly detecting the oil content of the oily sludge is suitable for detecting the oil content of the oily sludge on site, the equipment is in a closed state in the operation process, no external pollution is introduced, and an experimenter does not need to contact a toxic solvent.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (8)
1. An industrial equipment for rapidly detecting the oil content of oily sludge is characterized by comprising a stirring device, a filtering device, an extract liquor storage tank, an optical measuring device and a computer processing system;
the stirring device is provided with an oily sludge inlet and an extractant inlet; the mixed liquid outlet of the stirring device is connected with the mixed liquid inlet of the filtering device; the stirring device and the filtering device are both provided with weight inductors; an extract liquid outlet of the filtering device is connected with an extract liquid inlet of the extract liquid storage tank; an extract liquid outlet of the extract liquid storage tank is connected with an extract liquid inlet of the optical measuring device; the stirring device, the filtering device, the extraction liquid storage tank and the optical measuring device are respectively in communication connection with the computer processing system.
2. The industrial equipment for rapidly detecting the oil content of the oily sludge according to claim 1, wherein the stirring device is provided with a first branch pipe, a sewage discharge pipe and a second branch pipe; the first branch pipe is connected with a sewage discharge pipe through a first valve; the first branch pipe is connected with the second branch pipe through a second valve and a first power pump; the second branch pipe is connected with the filtering device; the blow-down pipe is connected with the extract liquor storage tank through a fourth valve; the first valve, the second valve, the fourth valve and the first power pump are respectively in communication connection with the computer processing system.
3. The industrial equipment for rapidly detecting the oil content of the oily sludge according to claim 1, wherein the stirring device is a blade stirrer.
4. The industrial equipment for rapidly detecting the oil content of the oily sludge according to claim 1, wherein the filtering device comprises a filtering layer containing a filtering medium and a third branch pipe; the third branch pipe is connected with the extract liquid storage tank; the third branch pipe is provided with a third valve and a second power pump; and the third valve and the second power pump are respectively in communication connection with the computer processing system.
5. The industrial equipment for rapidly detecting the oil content of oily sludge according to claim 4, wherein the filtering layer is divided into an upper layer and a lower layer, the upper layer is a microporous ceramic material filling layer, and the lower layer is an anhydrous sodium sulfate filling layer and/or a magnesium silicate filling layer.
6. The industrial equipment for rapidly detecting the oil content of oily sludge according to claim 1, wherein the filtering means is divided into an upper part and a lower part, and the shape of the lower part is tapered.
7. The industrial equipment for rapidly detecting the oil content of the oily sludge according to claim 1, wherein the optical measuring device is an ultraviolet spectrophotometer.
8. The industrial equipment for rapidly detecting the oil content of the oily sludge according to claim 1, wherein the extract liquid storage tank is provided with a fourth branch pipe, the fourth branch pipe is connected with the optical measuring device, and the fourth branch pipe is provided with a fifth valve; and the fifth valve is in communication connection with the computer processing system.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112777885A (en) * | 2020-12-29 | 2021-05-11 | 广州维港环保科技有限公司 | Equipment and process for industrially and rapidly detecting oil content of oily sludge |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112777885A (en) * | 2020-12-29 | 2021-05-11 | 广州维港环保科技有限公司 | Equipment and process for industrially and rapidly detecting oil content of oily sludge |
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