CN111892279A - Method for measuring content of sludge oil in petrochemical industry - Google Patents
Method for measuring content of sludge oil in petrochemical industry Download PDFInfo
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- CN111892279A CN111892279A CN201910370581.0A CN201910370581A CN111892279A CN 111892279 A CN111892279 A CN 111892279A CN 201910370581 A CN201910370581 A CN 201910370581A CN 111892279 A CN111892279 A CN 111892279A
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- Prior art keywords
- sludge
- oil
- petrochemical industry
- weight
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- 239000010802 sludge Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 238000000605 extraction Methods 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- 239000003208 petroleum Substances 0.000 claims description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- 238000002390 rotary evaporation Methods 0.000 abstract description 12
- 239000000126 substance Substances 0.000 abstract description 9
- 238000005303 weighing Methods 0.000 abstract description 8
- 238000001035 drying Methods 0.000 abstract description 4
- 238000010992 reflux Methods 0.000 abstract description 4
- 239000002274 desiccant Substances 0.000 abstract description 3
- 238000004821 distillation Methods 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 2
- 238000005259 measurement Methods 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000011324 bead Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/14—Treatment of sludge; Devices therefor by de-watering, drying or thickening with addition of chemical agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/121—Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/32—Hydrocarbons, e.g. oil
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
- C02F2103/365—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds from petrochemical industry (e.g. refineries)
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention belongs to the field of industrial sludge treatment and disposal, and discloses a method for measuring the oil content of sludge in the petrochemical industry, which separates oil substances from the sludge by adopting a separation and weighing method, can accurately measure and calculate the oil content in the sludge, and comprises the following steps: (1) accurately weighing the weight W1 of the rotary evaporation flask; (2) accurately weighing the weight W2 of the round-bottom flask and the total weight W3 of the sludge to be tested and the round-bottom flask; (3) selecting a proper extraction solvent, and dissolving oil substances in the sludge in the extraction solvent; (4) a distillation reflux mode is selected to completely dissolve oil substances in the sludge in the extracted solvent; (5) separating out moisture and solids in the sludge by selecting a proper drying agent and a proper filtering mode; (6) separating the oil substance from the extraction solvent by selecting a proper separation mode; (7) accurately weighing the weight W4 of the rotary evaporation flask containing the separated oil substances; (8) and (4) calculating. The invention provides a feasible, rapid and accurate method for measuring the oil content of sludge in the petrochemical industry, which can meet the requirements of sludge treatment and disposal industries such as sludge dewatering, sludge drying and the like on oil content measurement data.
Description
Technical Field
The invention belongs to the field of industrial sludge treatment and disposal, and discloses a method for measuring the content of sludge oil in the petrochemical industry.
Background
Oily sludge belongs to hazardous waste, is a difficult point in the field of industrial sludge treatment and disposal, and before subsequent treatment and disposal, the determination of the oil content of the sludge is very important for selecting a proper treatment method. Therefore, in order to ensure the safe and stable operation of a downstream sludge treatment system, the scientific and efficient method for measuring the oil content is one of the key links for improving the sludge treatment efficiency and capacity, and the method for measuring the oil content of the sludge in the petrochemical industry is the most effective solution provided for the problem.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a feasible, rapid and accurate method for measuring the content of sludge oil in the petrochemical industry.
In order to solve the technical problems, the invention is realized by the following technical scheme:
(1) the weight of the rotary evaporation flask W1 was accurately weighed.
(2) The weight of the round-bottomed flask W2 and the total weight of the sludge to be tested and the round-bottomed flask W3 were accurately weighed.
(3) And (3) selecting a proper extraction solvent, and dissolving the oil substances in the sludge in the extraction solvent.
(4) And (3) selecting a distillation reflux mode to completely dissolve oil substances in the sludge into the extraction solvent.
(5) And (3) separating out moisture and solids in the sludge by selecting a proper drying agent and a proper filtering mode.
(6) And separating the oil substance from the extraction solvent by selecting a proper separation mode.
(7) The weight W4 of the rotary evaporation flask containing the separated oil substances was accurately weighed.
(8) Computing
Preferably, the extraction solvent is petroleum ether.
Preferably, the drying agent is anhydrous sodium sulfate.
Preferably, the separation mode is a rotary evaporator evaporation mode.
By adopting the technical scheme, the invention can provide a feasible, rapid and accurate method for measuring the content of the sludge oil in the petrochemical industry.
Drawings
FIG. 1 is a schematic view of a reflow apparatus used in the present invention;
reference numbers in the figures: 1-round bottom flask; 2-straight tube type condenser tube.
Detailed Description
The invention will be described in detail hereinafter with reference to the accompanying drawings, but the invention can be implemented in many different ways, which are defined and covered by the claims.
(1) Numbering and washing the rotary evaporation flasks (the volume is 100ml or 150ml), drying in an oven at 97-103 ℃ for 2h, taking out, cooling in a dryer for 30min, and weighing W1 g. The operation is repeated until the constant weight of the rotary evaporation flask is constant, and the weight difference of the two times of weighing is less than or equal to 0.005 g.
(2) The weight W2g of a dry round-bottomed flask (capacity 500ml) was accurately weighed, about 2.5g to 4g of sludge was added, and W3g was weighed.
(3) Adding 3-5 glass beads into a round bottom flask, and adding 100mL of petroleum ether at the temperature of 30-60 ℃. A straight pipe type condenser pipe 2 which is cleaned and dried is tightly connected to the round bottom flask 1, and the inner wall of the condenser pipe needs to be wiped dry by cotton in advance. When the condenser tube and the round-bottom flask are installed, the axes of the condenser tube and the round-bottom flask are overlapped. In order to avoid steam escaping, the gap of the plug should be coated with collodion. When the temperature of water entering the condensation pipe is greatly different from the room temperature, the upper end of the condensation pipe is plugged by cotton so as to prevent water vapor in the air from entering the condensation pipe to be condensed.
(4) And heating the round-bottom flask by using an electric heating sleeve, and controlling the reflux speed to enable 2-4 drops of liquid to drop per second from the inclined opening of the condensation pipe. The reflux time was kept at 1.5 h.
(5) After the distillation was completed, the flask was allowed to cool, and the apparatus was disassembled.
(6) Anhydrous sodium sulfate (analytically pure, oven dried at 600 ℃ for 3h) was placed in a sand-core funnel at a height of about 2/3, and the distillate from the round-bottomed flask was filtered through the sand-core funnel into a rotary-steamed flask that had been constant weight. The round bottom flask, sand core funnel was washed three times with a small amount of petroleum ether and the washings were combined into a rotary evaporation flask.
(7) The rotary evaporation flask is stably placed in a water bath at 77-83 ℃, and petroleum ether is evaporated by using a rotary evaporator.
(8) Taking the rotary evaporation flask out of the water bath, putting the rotary evaporation flask in a constant temperature box with the temperature of 69-71 ℃ for drying for 2h, cooling the rotary evaporation flask in a drier for 30min, weighing the W4g to 0.0001g, putting the rotary evaporation flask in the constant temperature box for 15min, cooling and weighing. Repeating the operation until the weight is constant, wherein the weight difference of two times is not more than 0.0005g, and taking the minimum value calculation result.
(9) And (3) calculating: the oil content X is (W4-W1)/(W3-W2) × 100%.
(10) Testing twice in parallel, taking the arithmetic mean of the two results as the test result
The invention provides a feasible, rapid and accurate method for measuring the oil content of sludge in the petrochemical industry, which can meet the requirements of sludge treatment and disposal industries such as sludge dewatering, sludge drying and the like on oil content measurement data.
The above description is only for the preferred embodiment of the present invention and is not intended to limit the scope of the present invention, and all equivalent flow transformations made by using the contents of the specification and drawings, or applied directly or indirectly to other related technical fields, are included in the scope of the present invention.
Claims (3)
1. A method for measuring the content of sludge oil in the petrochemical industry is characterized by comprising the following steps: in the step (3), petroleum ether is used as a separation extraction solvent.
2. The method for measuring the content of sludge oil in the petrochemical industry according to claim 1, wherein the method comprises the following steps: anhydrous sodium sulfate was used as the dry filter medium in step (5).
3. The method for measuring the content of sludge oil in the petrochemical industry according to claim 1, wherein the method comprises the following steps: and (6) separating the petroleum ether by using a rotary evaporator.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910370581.0A CN111892279A (en) | 2019-05-06 | 2019-05-06 | Method for measuring content of sludge oil in petrochemical industry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910370581.0A CN111892279A (en) | 2019-05-06 | 2019-05-06 | Method for measuring content of sludge oil in petrochemical industry |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111892279A true CN111892279A (en) | 2020-11-06 |
Family
ID=73169377
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910370581.0A Pending CN111892279A (en) | 2019-05-06 | 2019-05-06 | Method for measuring content of sludge oil in petrochemical industry |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111892279A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102778409A (en) * | 2012-06-05 | 2012-11-14 | 中国石油大学(北京) | Device and method used for measuring content of oil and/ or liquid water in sample |
| CN104597215A (en) * | 2015-02-10 | 2015-05-06 | 浙江海洋学院 | Method for directly measuring components in oil sludge |
| CN104697884A (en) * | 2015-02-10 | 2015-06-10 | 浙江海洋学院 | Method for determining aged oil sludge components based on two-time reflux and one-time determination of sample tube weight |
| CN105645704A (en) * | 2015-12-29 | 2016-06-08 | 安徽理工大学 | Method for treating, extracting and purifying organic chloride pesticide in sediment of coal mining subsidence area |
| US20160376169A1 (en) * | 2013-11-27 | 2016-12-29 | Orege | Method of deodorizing sludge and device for performing said method |
| CN107098554A (en) * | 2017-06-01 | 2017-08-29 | 武汉巨正环保科技有限公司 | A kind of processing method of oil field sludge recycling |
| CN107884303A (en) * | 2017-11-24 | 2018-04-06 | 东隆环保科技有限公司 | A kind of greasy filth oil content measuring method |
-
2019
- 2019-05-06 CN CN201910370581.0A patent/CN111892279A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102778409A (en) * | 2012-06-05 | 2012-11-14 | 中国石油大学(北京) | Device and method used for measuring content of oil and/ or liquid water in sample |
| US20160376169A1 (en) * | 2013-11-27 | 2016-12-29 | Orege | Method of deodorizing sludge and device for performing said method |
| CN104597215A (en) * | 2015-02-10 | 2015-05-06 | 浙江海洋学院 | Method for directly measuring components in oil sludge |
| CN104697884A (en) * | 2015-02-10 | 2015-06-10 | 浙江海洋学院 | Method for determining aged oil sludge components based on two-time reflux and one-time determination of sample tube weight |
| CN105645704A (en) * | 2015-12-29 | 2016-06-08 | 安徽理工大学 | Method for treating, extracting and purifying organic chloride pesticide in sediment of coal mining subsidence area |
| CN107098554A (en) * | 2017-06-01 | 2017-08-29 | 武汉巨正环保科技有限公司 | A kind of processing method of oil field sludge recycling |
| CN107884303A (en) * | 2017-11-24 | 2018-04-06 | 东隆环保科技有限公司 | A kind of greasy filth oil content measuring method |
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Application publication date: 20201106 |