CN111321031A - Purification method of waste lubricating oil - Google Patents
Purification method of waste lubricating oil Download PDFInfo
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- CN111321031A CN111321031A CN202010351727.XA CN202010351727A CN111321031A CN 111321031 A CN111321031 A CN 111321031A CN 202010351727 A CN202010351727 A CN 202010351727A CN 111321031 A CN111321031 A CN 111321031A
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- lubricating oil
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- 239000010687 lubricating oil Substances 0.000 title claims abstract description 88
- 239000002699 waste material Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000000746 purification Methods 0.000 title claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 66
- 239000012535 impurity Substances 0.000 claims abstract description 41
- 238000003756 stirring Methods 0.000 claims abstract description 34
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- 239000003921 oil Substances 0.000 claims abstract description 25
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 238000003825 pressing Methods 0.000 claims abstract description 9
- 238000001556 precipitation Methods 0.000 claims description 15
- 230000001376 precipitating effect Effects 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 9
- 239000002244 precipitate Substances 0.000 claims description 7
- 125000000129 anionic group Chemical group 0.000 claims description 6
- 125000002091 cationic group Chemical group 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 8
- 238000005189 flocculation Methods 0.000 abstract description 2
- 230000016615 flocculation Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000706 filtrate Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 230000003311 flocculating effect Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005491 wire drawing Methods 0.000 description 1
Images
Classifications
-
- 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
- C10M175/0016—Working-up used lubricants to recover useful products ; Cleaning with the use of chemical agents
-
- 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
-
- 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
- C10M175/0083—Lubricating greases
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Lubricants (AREA)
Abstract
The invention discloses a purification method of dirty and waste lubricating oil, in particular to a purification method capable of purifying high-viscosity lubricating oil containing various impurities, which comprises the following steps: adding concentrated sulfuric acid into the waste lubricating oil, stirring and heating to obtain a first mixture, standing for 7-15 days to obtain a second mixture, standing for layering after flocculation is formed, and filtering impurities to obtain a third mixture; and adding polyacrylamide into the third mixture, heating and stirring for 30 minutes, and performing filter pressing through a filter press when the temperature reaches about 80 ℃ to obtain pure lubricating oil. The technology of the invention is a novel purification treatment technology of waste and dirty lubricating oil, and is suitable for various lubricating oil production enterprises, in particular various oil consumption enterprises.
Description
Technical Field
The invention relates to the field of purification of dirty and waste lubricating oil, in particular to a lubricating oil purification method capable of flocculating and precipitating impurities.
Background
At present, in the related manufacturing industries of a large amount of used and consumed lubricating oil such as fasteners, hardware products, stainless steel and the like, the lubricating oil is scrapped and replaced due to the fact that a large amount of impurities such as coating agents, wire drawing powder, dust, metal chips and the like are mixed after the lubricating oil is used for a short time. Enterprises not only increase the purchase cost of new oil, but also have little treatment cost of waste lubricating oil and environmental protection pressure.
During the use process of the lubricating oil, particularly in the machine equipment using the oil in an open state, a specific process flow and the like, a large amount of various impurities can be easily mixed into the lubricating oil, part of the impurity particles are tiny and fine, and the lubricating oil is suspended in the oil liquid in a natural state and is mixed together without separation. The oil quality is deteriorated in a short time, and the oil can not be used and must be replaced.
In the prior art, the technology capable of better processing the lubricating oil with high impurity content is a distillation type process technology. But the huge complete equipment investment, site requirements and environmental protection requirements of the lubricating oil recycling system ensure that the lubricating oil recycling system is not adopted by general enterprises and is only suitable for petroleum smelting and large-scale waste lubricating oil recycling units.
The prior various technical methods for realizing solid-liquid separation and purifying oil products mainly comprise; naturally precipitating and filtering.
1. Natural precipitation technology: the cost is low, but the treatment process is long in time period, usually one year or more. It has no effect on lubricating oil with high viscosity.
2. The filtration technology: the lubricating oil with high impurity content and high viscosity can not be treated.
The technologies have respective advantages and disadvantages, the effect and the benefit of purifying oil products are not ideal, and a large amount of high-viscosity dirty and waste lubricating oil generated by oil enterprises always has no good purification treatment equipment and process technology, cannot be recycled and reused, and can only be used as waste treatment.
Therefore, the traditional purification method of the dirty and waste lubricating oil cannot purify the lubricating oil containing various impurities and high viscosity well.
Disclosure of Invention
Aiming at the technical problems, the invention designs and develops a method for purifying the dirty and waste lubricating oil, which can purify the high-viscosity dirty and waste lubricating oil.
The technical scheme provided by the invention is as follows:
a purification method of waste lubricating oil comprises the following steps:
adding a precipitation flocculant to the waste lubricating oil to obtain a first mixture;
after the first mixture is stirred for 20-30 minutes, continuously stirring and heating the first mixture to 70-90 ℃, keeping the temperature and continuously stirring for 60-100 minutes to obtain a second mixture;
cooling the second mixture, standing, precipitating impurities, and filtering to remove filter residues to obtain a third mixture;
and adding polyacrylamide into the third mixture, heating to 70-80 ℃ under the stirring condition, then carrying out filter pressing, and separating precipitates to obtain pure lubricating oil.
Preferably, the mass ratio of the precipitation flocculant to the dirty and waste lubricating oil is 2-5%.
Preferably, the precipitation flocculant is concentrated sulfuric acid.
Preferably, the concentration of the concentrated sulfuric acid is 75% -98%.
Preferably, in the step of adding the precipitation flocculant to the dirty and used lubricating oil, the precipitation flocculant is added to the dirty and used lubricating oil under stirring.
Preferably, in the step of cooling the second mixture, standing, precipitating impurities, filtering to remove filter residues to obtain a third mixture, the standing time is 7-15 days.
Preferably, the polyacrylamide is added into the third mixture, and the third mixture is heated to 70-80 ℃ under the stirring condition, wherein the heating speed is 2-4 ℃/min during the heating operation of 70-80 ℃.
Preferably, the mass ratio of the polyacrylamide to the third mixture is 0.0005% to 0.0015%.
Preferably, when the lubricating oil is 150# to 220# forming oil, cationic polyacrylamide is added.
Preferably, the lubricating oil is 46# to 120# cold-heading lubricating oil or heat-treated dirty lubricating oil, and anionic polyacrylamide is added.
According to the method for purifying the waste lubricating oil, the flocculating settling agent is added into the waste lubricating oil, and various impurities in the waste lubricating oil can be settled by heating, stirring and other technical modes, so that oil and impurities are separated, and the purer lubricating oil can be obtained after the settled impurities are removed. And then through adding polyacrylamide, through heating stirring reaction, can wrap up relatively fine impurity in the oil and form great graininess or flocculent impurity, be convenient for filter. Therefore, pure lubricating oil can be obtained after filter pressing through the synergistic effect of the precipitation flocculant and the polyacrylamide on the waste lubricating oil. The content of impurities in the purified lubricating oil is between 10 and 100 grams per ton, and the diameter of the impurities is less than 2 to 5 UM.
Drawings
FIG. 1 shows the steps of a method for purifying waste lubricating oil provided by the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, belong to the scope of the present invention.
Referring to fig. 1, the present invention provides a method for purifying waste lubricating oil, comprising the following steps:
and S001, adding a precipitation flocculant into the waste lubricating oil, and uniformly stirring to obtain a first mixture.
And S002, heating the first mixture to 70-90 ℃ while stirring, keeping the temperature, and continuously stirring for 60-100 minutes to obtain a second mixture.
And S003, cooling, standing the second mixture, precipitating impurities, and filtering to obtain a third mixture.
And S004, adding polyacrylamide into the third mixture, heating to 70-80 ℃ under the stirring condition, then carrying out filter pressing, and separating precipitates to obtain pure lubricating oil.
During the use of lubricating oil, there are great amount of impurities of different sizes, including mechanical impurity, water, oxygen-containing compound, metal salt, etc. the present invention purifies similar lubricating oil and makes it possible to reuse it in industrial application. Adding a flocculating agent into the waste lubricating oil for precipitation, fully stirring and mixing, heating to completely react, cooling, standing and filtering, and removing part of impurities with larger particles to obtain a third mixture. Adding polyacrylamide into the third mixture, fully stirring and heating to ensure that the third mixture completely reacts and can wrap relatively fine impurities in the oil to form larger granular or flocculent impurities, and thus, pure lubricating oil can be obtained after filter pressing through the synergistic effect of the precipitated flocculant and the polyacrylamide on the waste lubricating oil.
In the invention, the mass ratio of the precipitation flocculant to the dirty and waste lubricating oil is preferably 2-5%.
In the invention, the precipitated flocculant is added into the waste lubricating oil while stirring.
In one embodiment, after the addition of the precipitated flocculant is completed, the mixture is stirred for 20 to 30 minutes, and the precipitated flocculant and the dirty and used lubricating oil are stirred uniformly.
The flocculating and precipitating agent of the invention can lead the dispersed particles in the dirty and used lubricating oil to form visible precipitable and filterable substances.
In the present invention, the precipitation flocculant is preferably concentrated sulfuric acid.
The concentrated sulfuric acid in the invention can chemically react with most impurities in the waste lubricating oil to effectively form flocculate.
In the present invention, the concentration of the concentrated sulfuric acid is preferably 75% to 98%, and more preferably 98%.
The source of the 98% concentrated sulfuric acid is not particularly limited in the present invention, and a commercially available product of the above concentrated sulfuric acid known to those skilled in the art may be used. The invention adopts concentrated sulfuric acid with specific concentration, which not only can ensure the precipitation flocculation effect of larger particle impurities, but also can ensure the control of the water content in the finished oil.
In S003, the time for standing is preferably 7 to 15 days.
The standing in the invention is natural sedimentation, the operation is simple, and the impurity removal effect is good.
In S004, the mixture is preferably heated to 70 to 80 degrees, more preferably to 80 degrees, under stirring conditions, and the heating rate is preferably 2 to 4 ℃/min, more preferably 2.6 ℃/min.
The method of S004 can be operated by adopting novel oil stain solid-liquid separation equipment disclosed in the patent application No. ZL 201520896514.
In the invention, the flocculant and the waste lubricating oil are fully reacted by stirring and heating
The mass ratio of polyacrylamide to the third mixture in the present invention is preferably 0.0005% to 0.0015%.
The polyacrylamide of the invention ensures that small particle impurities in the waste lubricating oil after the first precipitation continue to flocculate and precipitate.
In the present invention, when the waste lubricating oil is 150# to 220# molding oil, cationic polyacrylamide is preferably added.
The 150# to 220# forming oil can be specifically forming oil with viscosity between 150# and 220 #.
The cationic polyacrylamide can better react with the forming oil.
In the present invention, when the dirty and used lubricating oil is 46# to 120# cold heading lubricating oil or heat treatment dirty lubricating oil, anionic polyacrylamide is preferably added.
The cold heading lubricating oil of 46# to 120# may specifically be cold heading oil with a viscosity between 46# and 120 #.
The anionic polyacrylamide can better react with the cold heading oil.
The following is a detailed description of the embodiments.
Example 1
Adding concentrated sulfuric acid with the concentration of 98% into the dirty and waste lubricating oil to obtain a first mixture, wherein the mass ratio of the concentrated sulfuric acid with the concentration of 98% to the dirty and waste lubricating oil is 2: 100.
after the first mixture was stirred for 20 minutes, the first mixture was heated to 70 ℃ while continuing stirring, and the temperature was maintained and stirring was continued for 100 minutes to obtain a second mixture.
And cooling the second mixture, standing for 7 days, precipitating impurities, filtering to remove filter residues to obtain a filtrate, and obtaining the filtrate, namely the third mixture.
Adding polyacrylamide to the third mixture, wherein the mass ratio of the polyacrylamide to the third mixture is 0.0005: 100, heating to 70 ℃ under the stirring condition, then carrying out filter pressing, and separating precipitates to obtain pure lubricating oil.
One ton of treated pure lubricating oil is kept stand for 6 months, impurities precipitated at the bottom are filtered, quality detection is carried out on the impurities, and the test result shows that the content of the obtained impurities is not higher than 0.01 percent, and the diameter of the impurities is less than 2-5 mu M.
Example 2
Adding concentrated sulfuric acid with the concentration of 98% into the waste molding oil to obtain a first mixture, wherein the mass ratio of the concentrated sulfuric acid with the concentration of 98% to the waste lubricating oil is 5: 100.
and after stirring the first mixture for 30 minutes, continuously stirring while heating the first mixture to 80 ℃, keeping the temperature, and continuously stirring for 100 minutes to obtain a second mixture.
And cooling the second mixture, standing for 15 days, precipitating impurities, filtering to remove filter residues to obtain a filtrate, and obtaining the filtrate, namely the third mixture.
Adding a cationic polyacrylamide to the third mixture, wherein the mass ratio of the cationic polyacrylamide to the third mixture is 0.001: 100, heating to 80 ℃ under the stirring condition, then carrying out filter pressing, and separating precipitates to obtain pure lubricating oil.
The test method is the same as that of the example 1, and the test result shows that the content of the obtained impurities is not higher than 0.01 percent, and the diameters of the impurities are less than 2-5 mu M.
Example 3
Adding concentrated sulfuric acid with the concentration of 98% into the cold heading oil to obtain a first mixture, wherein the mass ratio of the concentrated sulfuric acid with the concentration of 98% to the dirty and waste lubricating oil is 3: 100.
and after stirring the first mixture for 25 minutes, continuously stirring and heating the first mixture to 90 ℃, keeping the temperature and continuously stirring for 100 minutes to obtain a second mixture.
And cooling the second mixture, standing for 15 days, precipitating impurities, filtering to remove filter residues to obtain a filtrate, and obtaining the filtrate, namely the third mixture.
Adding an anionic polyacrylamide to the third mixture, wherein the mass ratio of the anionic polyacrylamide to the third mixture is 0.0015: 100, heating to 80 ℃ under stirring, then carrying out filter pressing, and separating precipitates. Obtaining pure lubricating oil. .
The test method is the same as that of the example 1, and the test result shows that the content of the obtained impurities is not higher than 0.01 percent, and the diameters of the impurities are less than 2-5 mu M.
The above description of the embodiments is only for the purpose of assisting understanding of the method of the present invention and the core idea thereof, and it should be noted that those skilled in the art can make several improvements and modifications to the present invention without departing from the principle of the present invention, and these improvements and modifications also fall into the protection scope of the claims of the present invention.
Claims (10)
1. A purification method of waste lubricating oil is characterized by comprising the following steps:
adding a precipitation flocculant into the waste lubricating oil, and uniformly mixing to obtain a first mixture;
heating the first mixture to 70-90 ℃ while stirring, keeping the temperature, and continuously stirring for 60-100 minutes to obtain a second mixture;
cooling the second mixture, standing, precipitating impurities, and filtering to remove filter residues to obtain a third mixture;
and adding polyacrylamide into the third mixture, heating to 70-80 ℃ under the stirring condition, then carrying out filter pressing, and separating precipitates to obtain pure lubricating oil.
2. The method for purifying dirty and used lubricating oil according to claim 1, wherein the mass ratio of the precipitation flocculant to the dirty and used lubricating oil is 2-5: 100.
3. The method of purifying spent lubricating oil according to claim 2, wherein the precipitating flocculant is concentrated sulfuric acid.
4. The method for purifying the waste lubricating oil according to claim 3, wherein the concentrated sulfuric acid has a concentration of 75% to 98%.
5. The method of claim 1, wherein the step of adding the precipitating flocculant to the dirty and used lubricating oil is performed by adding the precipitating flocculant to the dirty and used lubricating oil under stirring.
6. The method for purifying the dirty and used lubricating oil according to claim 1, wherein in the step of cooling the second mixture, standing the mixture for 7 to 15 days to precipitate impurities, and filtering the mixture to remove filter residues to obtain a third mixture, the time for standing is 7 to 15 days.
7. The method according to claim 1, wherein the step of adding polyacrylamide to the third mixture and heating the mixture to 70-80 ℃ with stirring is performed at a heating rate of 2-4 ℃/min in an operation of heating the mixture to 70-80 ℃.
8. The method of purifying the used lubricating oil according to claim 1, wherein the mass ratio of the polyacrylamide to the third mixture is 0.0005 to 0.0015: 100.
9. the method of claim 1, wherein cationic polyacrylamide is added when the dirty/used lubricating oil is a forming oil.
10. The method for purifying the used lubricating oil according to claim 1, wherein when the used lubricating oil is cold heading oil, anionic polyacrylamide is added.
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Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1574081A (en) * | 1977-05-09 | 1980-09-03 | Huels Chemische Werke Ag | Process for purifying exhaust oil |
CN1616615A (en) * | 2004-09-29 | 2005-05-18 | 上海宝钢废旧油处理站 | Parifying and regenerating process for high and medium viscosity waste oils |
CN102504934A (en) * | 2011-11-21 | 2012-06-20 | 洛阳昊海工贸有限公司 | Technology for regenerating waste internal combustion engine oil |
CN104531210A (en) * | 2015-01-04 | 2015-04-22 | 河南师范大学 | Decoloration and deodorization technology for waste plastic cracking crude oil |
CN104745285A (en) * | 2015-04-16 | 2015-07-01 | 中科院广州能源所盱眙凹土研发中心 | Regeneration method for waste lubrication oil |
JP2016053125A (en) * | 2014-09-04 | 2016-04-14 | 全国オイルリサイクル協同組合 | Waste oil regeneration method |
CN108017202A (en) * | 2017-12-12 | 2018-05-11 | 西北大学 | A kind for the treatment of for reuse technique of copper drawing fluid waste liquid |
-
2020
- 2020-04-28 CN CN202010351727.XA patent/CN111321031A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1574081A (en) * | 1977-05-09 | 1980-09-03 | Huels Chemische Werke Ag | Process for purifying exhaust oil |
CN1616615A (en) * | 2004-09-29 | 2005-05-18 | 上海宝钢废旧油处理站 | Parifying and regenerating process for high and medium viscosity waste oils |
CN102504934A (en) * | 2011-11-21 | 2012-06-20 | 洛阳昊海工贸有限公司 | Technology for regenerating waste internal combustion engine oil |
JP2016053125A (en) * | 2014-09-04 | 2016-04-14 | 全国オイルリサイクル協同組合 | Waste oil regeneration method |
CN104531210A (en) * | 2015-01-04 | 2015-04-22 | 河南师范大学 | Decoloration and deodorization technology for waste plastic cracking crude oil |
CN104745285A (en) * | 2015-04-16 | 2015-07-01 | 中科院广州能源所盱眙凹土研发中心 | Regeneration method for waste lubrication oil |
CN108017202A (en) * | 2017-12-12 | 2018-05-11 | 西北大学 | A kind for the treatment of for reuse technique of copper drawing fluid waste liquid |
Non-Patent Citations (1)
Title |
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陆希峰, 天津科学技术出版社 * |
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