CN110723874A - Solid-liquid separation method of rolling oil sludge - Google Patents
Solid-liquid separation method of rolling oil sludge Download PDFInfo
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- CN110723874A CN110723874A CN201910892711.7A CN201910892711A CN110723874A CN 110723874 A CN110723874 A CN 110723874A CN 201910892711 A CN201910892711 A CN 201910892711A CN 110723874 A CN110723874 A CN 110723874A
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- 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
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- 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
- C02F11/13—Treatment of sludge; Devices therefor by de-watering, drying or thickening by heating
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- 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
- C02F11/15—Treatment of sludge; Devices therefor by de-watering, drying or thickening by treatment with electric, magnetic or electromagnetic fields; by treatment with ultrasonic waves
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
- C10M175/0025—Working-up used lubricants to recover useful products ; Cleaning by thermal processes
- C10M175/0033—Working-up used lubricants to recover useful products ; Cleaning by thermal processes using distillation processes; devices therefor
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
- C10M175/005—Working-up used lubricants to recover useful products ; Cleaning using extraction processes; apparatus therefor
Abstract
A solid-liquid separation method of rolling oil sludge comprises the following steps: magnetic separation: under the action of a metal permanent magnetic strong magnetic field, magnetizing and aggregating micro metal powder in the oil sludge system, preliminarily separating micro metal iron powder from rolling oil, and discharging the rolling oil; extracting with a small molecular solvent: mixing the obtained oil-containing metal powder with a micromolecular solvent, fully stirring, precipitating, separating to obtain pure iron powder and a mixed solution, and drying and storing the recovered iron powder; low-temperature distillation separation: and distilling the mixed solution at low temperature, feeding the distilled micromolecule extract into an extract storage chamber in a gas state for condensation and liquefaction, recycling, and discharging and storing the separated rolling oil. The method has the advantages of simple and reasonable process, convenient operation and low energy consumption, can completely separate the rolling oil sludge, can obtain high-value metal powder and cooling rolling oil, and is suitable for recycling the oil sludge waste generated by a filtering system of a stainless steel rolling mill.
Description
Technical Field
The invention belongs to the technical field of recycling cold-rolled stainless steel solid waste, relates to a solid-liquid separation method, and particularly relates to a solid-liquid separation method of rolling oil sludge.
Background
In the stainless steel cold rolling process, rolling oil is filtered through a filter to produce a large amount of sludge, which generally precipitates over a long period of time and then forms high-concentration sludge-containing solid waste. Because the metal particles are highly dispersed in the rolling oil to form a stable suspension, the complete separation by a precipitation method is difficult to directly carry out, and because the diameter of the metal particles is 0.1-10 um, the rolling oil and the metal particles are difficult to separate by a filtration separation method, if the oil sludge is not subjected to solid-liquid separation, the filter is seriously blocked, and the normal work cannot be carried out.
The separation of the sludge can generally be carried out by direct "incineration" or by means of high-temperature heating or high-speed centrifugation, but it is not difficult, however, to have the following drawbacks: the high-temperature heating method consumes a large amount of heat energy, and the separated rolling oil is easy to deteriorate and is not suitable for reuse; the high-speed centrifugal separation consumes a large amount of electric energy, and has high energy consumption and high cost; direct burning is not available, thereby wasting precious resources and polluting the environment.
Therefore, a separation method with low energy consumption and convenient operation needs to be designed to meet the solid-liquid separation requirement of the oil sludge generated by the stainless steel mill filtration system.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a solid-liquid separation method of rolling oil sludge, which is simple and reasonable in process, convenient to operate and low in energy consumption, aiming at the technical current situation.
The technical scheme adopted by the invention for solving the technical problems is as follows: a solid-liquid separation method of rolling oil sludge is characterized by comprising the following steps:
1) magnetic separation: under the action of a metal permanent magnetic strong magnetic field, magnetizing and aggregating micro metal powder suspended in an oil sludge system, preliminarily separating micro metal iron powder from rolling oil in the oil sludge, discharging the rolling oil, and pushing the residual oil-containing metal powder into a small molecule extraction chamber for treatment;
2) extracting with a small molecular solvent: mixing the obtained oil-containing metal powder with a micromolecular solvent, fully stirring, precipitating, separating to obtain pure iron powder and a mixed solution, and drying and storing the recovered iron powder;
3) low-temperature distillation separation: and distilling the mixed solution at low temperature, feeding the distilled micromolecule extract into an extract storage chamber in a gas state for condensation and liquefaction, recycling, and discharging and storing the separated rolling oil.
As an improvement, the magnetic separation of the step 1) is carried out in a magnetic separation device, and the magnetic separation device can adopt a non-contact type and an electrified automatic processing device.
Furthermore, the non-contact type is that an isolation medium is arranged between a magnetic material and the oil sludge, the magnetic material and the rolled oil sludge do not directly act, the isolation medium is made of a non-metal or metal material without the magnetic material, the magnetic material is made of a permanent magnet (steel) with a strong magnetic field, and the magnetic material has a magnetizing effect by penetrating through the isolation medium in a magnetic field range.
Further, the metal fine particles of the rolling sludge of the step 1) are classified into nonmagnetic 300-series stainless steel fine iron powder, ferromagnetic 400-series stainless steel fine iron powder and highly magnetic 200-series stainless steel fine iron powder according to the stainless steel component, and the sludge containing the 300-series stainless steel fine iron powder is subjected to a continuous strengthening magnetization treatment for 8 hours or more.
As an improvement, the micromolecular solvent extracted by the micromolecular solvent in the step 2) adopts an organic or inorganic micromolecular solvent, the micromolecular solvent has a chemical molecular weight of less than 100, is volatile, has a boiling point of 15-50 ℃ under standard atmospheric pressure, can also be prepared by mixing one or more solvents, and has an azeotropic point of not higher than 60 ℃.
Preferably, the micromolecular solvent is an organic micromolecular solvent, and the volume quantity V of the micromolecular solvent1With the volume V of the metal powder to be treated2The ratio of V to1:V2＝2～4。
Further, the low-temperature distillation separation in step 3) is to place the mixed solution obtained by extraction in step 2) in heating fu for low-temperature distillation, wherein the heating temperature is controlled to be less than or equal to 10 ℃ of the azeotropic point of the small molecular solvent, and when the temperature of the liquid in heating fu is higher than 10 ℃ of the azeotropic point of the small molecular solvent, the heating is stopped.
And finally, controlling the heating temperature to be 40-60 ℃, and stopping heating when the temperature of the liquid in the heating Fu is higher than 70 ℃.
Compared with the prior art, the invention has the advantages that: the method comprises the following steps of adopting three procedures of magnetic separation, micromolecular solvent extraction and low-temperature distillation separation, firstly magnetizing oil sludge by using a strong magnetic material, separating 80% of rolling oil and all stainless steel fine iron powder, mixing the rest 20% of rolling oil in the iron powder, further extracting the rolling oil by using micromolecular solvent in the modes of soaking, stirring, precipitating and the like, and further separating to obtain pure iron powder and an extraction mixed solution; and finally, distilling the extraction mixed solution at low temperature according to the principle that the boiling points of the rolling oil and the extraction liquid are different to obtain the extraction liquid and the pure rolling oil. The method has the advantages of simple and reasonable process, convenient operation and low energy consumption, can well separate the rolling oil sludge, can obtain high-value metal powder and cooling rolling oil, can recycle the rolling oil and the extraction liquid, and is suitable for recycling the oil sludge waste generated by a filtering system of a stainless steel rolling mill.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
As shown in fig. 1, a method for separating solid from liquid of rolling oil sludge is characterized by comprising the following steps:
1) magnetic separation: the magnetic separation is carried out in a magnetic separation device, under the action of a metal permanent magnetic strong magnetic field, high-concentration rolling oil sludge is magnetized and aggregated, micro metal powder suspended in an oil sludge system is magnetized and aggregated, micro metal iron powder in the oil sludge is primarily separated from rolling oil, the rolling oil is discharged, and the residual oil-containing metal powder is pushed into a small molecule extraction chamber for treatment;
the magnetic separation device can adopt a non-contact type and an electrified automatic processing device, the non-contact type is that an isolation medium is arranged between a magnetic material and oil sludge, the magnetic material and the rolling oil sludge do not directly act, but the rolling oil sludge is still in the magnetic field action range of the magnetic material, so that the acting force of the magnetic material on rolling oil can be ensured, metal fine iron powder can be well separated out and cannot be attached to the surface of a magnet to be difficult to peel off, the isolation medium adopts non-metal or metal materials without the magnetic material, such as metals of copper, aluminum and the like, and non-metal materials such as plastics and wood; but cannot adopt a metal material with magnetism; the magnetic material adopts a permanent magnet (steel) with a strong magnetic field, and the magnetic material has the function of passing through an isolation medium to carry out magnetization in the magnetic field range; the electrified automatic processing device has the characteristics of less manual intervention requirement, high intelligent degree, simple operation and the like;
the metal fine particles of the rolling sludge are classified into nonmagnetic 300-series stainless steel fine iron powder, ferromagnetic 400-series stainless steel fine iron powder and highly magnetic 200-series stainless steel fine iron powder, depending on the stainless steel component,
for the 400 series stainless steel oil sludge, the permanent magnet has strong attraction effect on micro iron powder in the oil sludge, when the oil sludge is in a magnetic field acting force range, all the micro iron powder in the oil sludge is quickly attracted to the near surface of the magnet and is tightly gathered together in a very short time, so that the micro metal iron powder in the oil sludge is separated from the rolling oil, the rolling oil is removed, and the residual oil-containing iron powder is pushed into a small-molecule extraction chamber for treatment;
for 200 series stainless steel oil sludge, the permanent magnet has certain magnetic force on micro iron powder in the oil sludge, when the oil sludge is in the magnetic field range of magnetic force lines of the magnet, the micro iron powder in the oil sludge is completely attracted to the near surface of the magnet and is tightly gathered together after a short period of time, so that the rolling oil and the micro metal iron powder in the oil sludge are separated from the rolling oil, the rolling oil is discharged, and the residual oil-containing iron powder is pushed into a small-molecule extraction chamber for treatment;
for 300 series stainless steel, the steel is a non-magnetic material and can not be magnetized in a magnetic field; however, as long as the fine metal powder sludge is subjected to forced magnetization treatment continuously for 8 to 24 hours under the action of a strong magnetic field, the fine iron powder in the 300-series stainless steel sludge can still be well magnetized, and finally the fine iron powder in the sludge can be gathered on the outer surface of a ferromagnetic material, so that the fine metal iron powder in the sludge can be separated from the rolling oil. In the processing step, about 80% of rolling oil in the oil sludge can be separated, and the rest about 20% of rolling oil is still mixed in the aggregated metal iron powder;
for various mixed stainless steel rolling oil sludge, the 300 series stainless steel oil sludge treatment process is carried out, and finally the rolling oil in the high-concentration oil sludge can be separated from the iron powder to obtain the high-purity rolling oil and the iron powder containing a small amount of rolling oil, the rolling oil can be directly recycled, and the oil-containing iron powder enters the next extraction process to be continuously separated to obtain pure iron powder and an oil-containing extraction liquid.
2) Extracting with a small molecular solvent: mixing the obtained oil-containing metal powder with a micromolecular solvent, fully stirring, precipitating, separating to obtain pure iron powder and a mixed solution, and drying and storing the recovered iron powder;
wherein the extraction liquid micromolecule solvent adopts organic or inorganic micromolecule solvent, the chemical molecular weight of the extraction liquid micromolecule solvent is less than 100, the extraction liquid micromolecule solvent is volatile, the boiling point is 15-50 ℃ under the standard atmospheric pressure, the extraction liquid micromolecule solvent also can be prepared by mixing one or more solvents, and the azeotropic point is not higher than 60 ℃;
the oil-containing metal powder is extracted by adopting the micromolecular solvent because the metal powder has a strong surface area, the rolling oil is organic and is a macromolecular solvent, the micromolecular organic liquid is easy to coat the micro metal powder, and the rolling oil is easy to dilute, so that the micro metal powder is released from the macromolecular rolling oil, the micro metal powder is aggregated into clusters due to the adsorption force of surface molecules between metals, and the micromolecular solvent is difficult to exist between metal powder clusters, so that the micro metal powder is easy to separate. The small molecular organic solvent is easy to be mixed and dissolved with the rolling oil, but the boiling point of the rolling oil is far higher than that of the small molecular solvent, so that good conditions are created for subsequent continuous separation. If the inorganic solvent is used for washing the oil-containing metal powder, the inorganic solution is a polar molecule, so that the micro metal powder is easily adsorbed, and the aim of high separation can be fulfilled;
preferably, the small molecular solvent is organic small molecular solvent such as acetone, butanone and the like, and the volume amount V of the small molecular solvent1With the volume V of the metal powder to be treated2The ratio of V to1:V22-4. Generally, 3 times of the solvent is used to obtain good extraction effect, the solvent amount is too large, the subsequent energy consumption is high, the solvent amount is too small, the extraction is insufficient, and the extraction effect is possibly not ideal.
3) Low-temperature distillation separation: the low-temperature distillation is used for further recovering the rolling oil and the micromolecular extraction liquid, so that the recycling is realized, the environmental pollution is reduced, and the aim of changing waste into valuable is fulfilled.
The specific process is as follows: and (2) placing the mixed solution in heating-Fu to carry out low-temperature distillation, controlling the heating temperature to be 40-60 ℃, stopping heating when the temperature of the liquid in the heating-Fu is higher than 70 ℃, allowing the distilled micromolecule extract to enter an extract storage chamber in a gaseous state to be condensed and liquefied so as to be recycled, discharging and storing the separated rolling oil, and continuously participating in the rolling mill process oil after the separated rolling oil is qualified.
Because the heating temperature is low, the low-temperature waste heat can be easily obtained in the actual production process of the stainless steel, so that the energy is saved in the actual application.
The working principle is as follows: the stainless steel oil sludge is finally separated through three steps of magnetic separation, micromolecular solvent extraction and low-temperature distillation. The rolling oil sludge is firstly separated in a magnetic separator to obtain a clarified rolling oil product and oily iron powder, the rolling oil with a small amount of oil in the iron powder needs to be stirred, mixed, washed, precipitated and drained in an extraction chamber of the next procedure to obtain a metal fine iron powder product and an extraction mixed solution, the mixed extraction liquid is drained into a low-temperature distillation chamber, the mixed extraction liquid is heated at the low temperature of 40-60 ℃, and the extraction liquid and the residual rolling oil are obtained through evaporation. Thus, a complete sludge treatment process is formed, fine iron powder in the sludge is separated from the rolling oil finally, and the extract is recovered. The rolling oil sludge is completely separated, the rolling oil and the extraction liquid can be recycled, and the pure stainless steel fine iron powder is a valuable product and can be directly sold.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the technical principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A solid-liquid separation method of rolling oil sludge is characterized by comprising the following steps:
1) magnetic separation: under the action of a metal permanent magnetic strong magnetic field, magnetizing and aggregating micro metal powder suspended in an oil sludge system, preliminarily separating micro metal iron powder from rolling oil in the oil sludge, discharging the rolling oil, and pushing the residual oil-containing metal powder into a small molecule extraction chamber for treatment;
2) extracting with a small molecular solvent: mixing the obtained oil-containing metal powder with a micromolecular solvent, fully stirring, precipitating, separating to obtain pure iron powder and a mixed solution, and drying and storing the recovered iron powder;
3) low-temperature distillation separation: and distilling the mixed solution at low temperature, feeding the distilled micromolecule extract into an extract storage chamber in a gas state for condensation and liquefaction, recycling, and discharging and storing the separated rolling oil.
2. The solid-liquid separation method according to claim 1, characterized in that: the magnetic separation of the step 1) is carried out in a magnetic separation device, and the magnetic separation device can adopt a non-contact type and an electrified automatic processing device.
3. The solid-liquid separation method according to claim 2, characterized in that: the non-contact type is characterized in that an isolation medium is arranged between a magnetic material and the oil sludge, the magnetic material and the rolled oil sludge do not directly act, the isolation medium is made of a non-metal or metal material without the magnetic material, the magnetic material is made of a permanent magnet (steel) with a strong magnetic field, and the magnetic material has a magnetizing effect of penetrating through the isolation medium in a magnetic field range.
4. The solid-liquid separation method according to claim 1, characterized in that: the metal fine particles of the rolling sludge of the step 1) are classified into nonmagnetic 300-series stainless steel fine iron powder, ferromagnetic 400-series stainless steel fine iron powder and stronger magnetic 200-series stainless steel fine iron powder according to the stainless steel components, and the sludge containing the 300-series stainless steel fine iron powder needs to be subjected to a continuous strengthening magnetization treatment for more than 8 hours.
5. The solid-liquid separation method according to claim 1, characterized in that: the micromolecular solvent extracted by the micromolecular solvent in the step 2) adopts an organic or inorganic micromolecular solvent, the chemical molecular weight of the micromolecular solvent is less than 100, the micromolecular solvent is volatile, the boiling point of the micromolecular solvent is 15-50 ℃ under the standard atmospheric pressure, the micromolecular solvent can also be prepared by mixing one or more solvents, and the azeotropic point of the micromolecular solvent is not higher than 60 ℃.
6. The solid-liquid separation method according to claim 5, characterized in that: the micromolecular solvent adopts an organic micromolecular solvent, and the volume quantity V of the micromolecular solvent1With the volume V of the metal powder to be treated2The ratio of V to1:V2＝2～4。
7. The solid-liquid separation method according to claim 1, characterized in that: the low-temperature distillation separation in the step 3) is to place the mixed solution obtained by extraction in the step 2) in heating-up-fu for low-temperature distillation, wherein the heating temperature is controlled to be less than or equal to 10 ℃ of the azeotropic temperature of the small molecular solvent, and when the temperature of the liquid in the heating-up-fu is higher than 10 ℃ of the azeotropic temperature of the small molecular solvent, the heating is stopped.
8. The solid-liquid separation method according to claim 7, characterized in that: the heating temperature is controlled to be 40-60 ℃, and when the temperature of the liquid in the heating Fu is higher than 70 ℃, the heating is stopped.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003181494A (en) * | 2001-12-19 | 2003-07-02 | Jfe Steel Kk | Method for separating iron particle from fat and oil in sludge |
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- 2019-09-20 CN CN201910892711.7A patent/CN110723874A/en active Pending
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| JP2003181494A (en) * | 2001-12-19 | 2003-07-02 | Jfe Steel Kk | Method for separating iron particle from fat and oil in sludge |
| CN104096410A (en) * | 2013-04-09 | 2014-10-15 | 何荣志 | Magnetic automatic filter for fluid |
| CN104946893A (en) * | 2015-06-09 | 2015-09-30 | 武汉钢铁(集团)公司 | Method of extracting superfine iron from cold rolling greasy filth |
| CN108659945A (en) * | 2017-03-30 | 2018-10-16 | 宝山钢铁股份有限公司 | A kind of Magnetic filter formula impurity treatment method of cold mill complex emulsion |
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