CN117070247A - Demetallization pretreatment method for waste mineral oil - Google Patents
Demetallization pretreatment method for waste mineral oil Download PDFInfo
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- CN117070247A CN117070247A CN202311180648.7A CN202311180648A CN117070247A CN 117070247 A CN117070247 A CN 117070247A CN 202311180648 A CN202311180648 A CN 202311180648A CN 117070247 A CN117070247 A CN 117070247A
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- 239000002699 waste material Substances 0.000 title claims abstract description 91
- 239000002480 mineral oil Substances 0.000 title claims abstract description 72
- 235000010446 mineral oil Nutrition 0.000 title claims abstract description 72
- 238000002203 pretreatment Methods 0.000 title claims abstract description 15
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 66
- 238000000926 separation method Methods 0.000 claims abstract description 37
- 229910052751 metal Inorganic materials 0.000 claims abstract description 35
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 33
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 33
- 235000012501 ammonium carbonate Nutrition 0.000 claims abstract description 33
- 239000000243 solution Substances 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 27
- 150000003839 salts Chemical class 0.000 claims abstract description 23
- 239000000203 mixture Substances 0.000 claims abstract description 22
- BVCZEBOGSOYJJT-UHFFFAOYSA-N ammonium carbamate Chemical compound [NH4+].NC([O-])=O BVCZEBOGSOYJJT-UHFFFAOYSA-N 0.000 claims abstract description 19
- KXDHJXZQYSOELW-UHFFFAOYSA-N carbonic acid monoamide Natural products NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000004254 Ammonium phosphate Substances 0.000 claims abstract description 13
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims abstract description 13
- 235000019289 ammonium phosphates Nutrition 0.000 claims abstract description 13
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims abstract description 13
- 235000011130 ammonium sulphate Nutrition 0.000 claims abstract description 13
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000012153 distilled water Substances 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims description 40
- 238000004062 sedimentation Methods 0.000 claims description 29
- 150000001875 compounds Chemical class 0.000 claims description 24
- 239000012267 brine Substances 0.000 claims description 11
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 11
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 9
- 238000005054 agglomeration Methods 0.000 claims description 9
- 230000002776 aggregation Effects 0.000 claims description 9
- 229910052698 phosphorus Inorganic materials 0.000 claims description 9
- 239000011574 phosphorus Substances 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- 238000000605 extraction Methods 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 8
- 230000035484 reaction time Effects 0.000 claims description 8
- -1 compound salt Chemical class 0.000 abstract description 28
- 239000002184 metal Substances 0.000 abstract description 22
- 239000000126 substance Substances 0.000 abstract description 12
- 238000010438 heat treatment Methods 0.000 abstract description 6
- 239000007864 aqueous solution Substances 0.000 abstract description 4
- 239000002199 base oil Substances 0.000 abstract description 4
- 238000004939 coking Methods 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 230000008929 regeneration Effects 0.000 abstract description 2
- 238000011069 regeneration method Methods 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 abstract 1
- 239000012535 impurity Substances 0.000 description 22
- 230000000694 effects Effects 0.000 description 14
- 239000010705 motor oil Substances 0.000 description 12
- 239000003921 oil Substances 0.000 description 11
- 239000012266 salt solution Substances 0.000 description 9
- 239000010687 lubricating oil Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 239000000654 additive Substances 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000008394 flocculating agent Substances 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 239000011133 lead Substances 0.000 description 2
- HNNQYHFROJDYHQ-UHFFFAOYSA-N 3-(4-ethylcyclohexyl)propanoic acid 3-(3-ethylcyclopentyl)propanoic acid Chemical compound CCC1CCC(CCC(O)=O)C1.CCC1CCC(CCC(O)=O)CC1 HNNQYHFROJDYHQ-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000010812 mixed waste Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010913 used oil Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G53/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
- C10G53/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
- C10G53/04—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only including at least one extraction step
- C10G53/06—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only including at least one extraction step including only extraction steps, e.g. deasphalting by solvent treatment followed by extraction of aromatics
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G17/00—Refining of hydrocarbon oils in the absence of hydrogen, with acids, acid-forming compounds or acid-containing liquids, e.g. acid sludge
- C10G17/09—Refining of hydrocarbon oils in the absence of hydrogen, with acids, acid-forming compounds or acid-containing liquids, e.g. acid sludge with acid salts
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G21/00—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents
- C10G21/06—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents characterised by the solvent used
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1003—Waste materials
- C10G2300/1007—Used oils
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/205—Metal content
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes
Abstract
The application discloses a demetallization pretreatment method of waste mineral oil, which is characterized in that ammonium sulfate, ammonium bicarbonate, ammonium carbamate, ammonium carbonate and ammonium phosphate are compounded into compound salt, and the compound salt is mixed with distilled water to prepare compound salt water solution with the mass concentration of 10-15%; adding the prepared aqueous solution into the waste mineral oil according to the addition amount of 5-12% of the mass of the waste mineral oil, and fully stirring for 30-60min at the temperature of 40-50 ℃ to obtain a mixed material; heating the mixture to 50-70 ℃, preserving heat and reacting for 8-24 hours, settling, and conveying the settled mixture to solid-liquid separation. The method can effectively remove the metal salts in the waste mineral oil by reaction, so that the total content of metal elements in the waste mineral oil is reduced from 3300PPm to below 370PPm, the ash index is reduced from 0.7% to below 0.05%, the problem of heating and coking in the regeneration process of the waste mineral oil can be effectively avoided, and meanwhile, the technical indexes such as oxidation stability, light stability, acid value and the like of the regenerated base oil are greatly improved due to the fact that the metal salt substances in the waste mineral oil are greatly reduced.
Description
Technical Field
The application belongs to the technical field of waste oil treatment, and particularly relates to a demetallization pretreatment method for waste mineral oil.
Background
At present, the known pretreatment technology of the vehicular mixed waste mineral oil comprises heating sedimentation, mechanical filtration, flocculation sedimentation and the like, the heating sedimentation technology mainly utilizes steam to heat and reduce viscosity of the waste lubricating oil, hydrocarbon substances and impurities in the waste lubricating oil realize natural sedimentation separation due to different densities, the hydrocarbon substances are at the upper part, the impurities are at the lower part, but the sedimentation separation period is longer due to smaller density differences, the efficiency is lower, and oxidized polar organic matters in the oil cannot be separated; the mechanical filtration mainly utilizes the microporous structure of the filter element material to screen and filter particulate impurities in the lubricating oil, but the mechanical filtration only can filter the mechanical impurities in the oil, but has no filtration effect on organic naphthenic acid, alkaline nitrogen, combined water, metallic salts and other fluid impurities generated by oxidation of the lubricating oil in the use process, has low filtration precision, and still has serious coking tendency in the high-temperature heating process; the flocculating settling is mainly to add flocculating agent into the waste lubricating oil, make impurity in the waste lubricating oil flocculate and be called the large-particle substance or flocculate, separate from the waste lubricating oil after settling, but will introduce the impurity ion additionally in flocculating agent that is added, will produce the more serious corrosion phenomenon to the later stage and distill the course of working, and the separation process is not thorough, contain a large amount of oleaginous in the sediment, it is low to regenerate the base oil yield.
Disclosure of Invention
In order to solve the problems in the prior art, the application provides a demetallization pretreatment method for waste mineral oil, which further optimizes the prior art.
A demetallization pretreatment method for waste mineral oil comprises the following steps:
(1) Ammonium sulfate, ammonium bicarbonate, ammonium carbamate, ammonium carbonate and ammonium phosphate are compounded into compound salt, and the compound salt solution is prepared by mixing the compound salt with distilled water;
(2) Mixing and extracting: adding the compound salt water solution into the waste mineral oil, and mixing and extracting to obtain a mixed material; the compound salt water solution and the waste mineral oil are fully and uniformly mixed, and the water mainly hydrolyzes the additives and the salt components in the waste mineral oil and dissolves the additives and the salt components in the water, so that the extraction and separation of the additives and the salt substances are realized.
(3) The reaction: reacting the mixed materials; CO generated by the hydrolysis of the compound salt in the aqueous solution by the reaction 3 -2 、OH - The plasma fully reacts with additives and salt substances dissolved in water to lead the iron, copper, lead and magnesium in the waste mineral oil,Calcium, zinc, silicon, phosphorus or other ash elements are subjected to coupling reaction and converted into salt precipitates;
(4) Agglomeration sedimentation: settling after the step (3) is finished; the ammonium carbamate in the solution causes macromolecular organic matters such as colloid asphaltene and the like generated after salt precipitates and a dispersion system generated in the mixed materials are destroyed to agglomerate and settle.
(5) Solid-liquid separation: the settled mixed materials are conveyed into a centrifuge or a membrane separation device to realize continuous solid-liquid separation, thereby realizing the effective removal and separation of metal elements and phosphorus, silicon or other nonmetallic ash elements in the waste mineral oil.
Preferably, in the step (1), the salt in the brine solution is a composition of ammonium sulfate and ammonium bicarbonate in a mass ratio of (1-3): 1-3, or a composition of ammonium bicarbonate and ammonium carbamate in a mass ratio of (1-3): 1-3, or a composition of ammonium bicarbonate and ammonium carbonate in a mass ratio of (1-3): 1-3, or a composition of ammonium carbamate and ammonium carbonate in a mass ratio of (1-3): 1-3, or a composition of ammonium carbonate and ammonium phosphate in a mass ratio of (1-3): 1-3.
Further preferably, in step (1), the mass concentration of the brine solution is 10% -15%.
Further preferably, in the step (1), the salt is a composition of ammonium sulfate and ammonium bicarbonate in a mass ratio of 1:1, or a composition of ammonium bicarbonate and ammonium carbamate in a mass ratio of 1:1, or a composition of ammonium bicarbonate and ammonium carbonate in a mass ratio of 1:1, or a composition of ammonium carbamate and ammonium carbonate in a mass ratio of 1:1, or a composition of ammonium carbonate and ammonium phosphate in a mass ratio of 1:1.
Preferably, in the step (2), the compound saline solution is added into the waste mineral oil according to the addition amount of 5-12% of the mass of the waste mineral oil, and the mixing extraction temperature is 40-50 ℃ for 30-60min.
Preferably, in step (3), the reaction temperature is 50-70℃and the reaction time is 8-24 hours.
Preferably, in step (4), the settling time is 4-12 hours.
The application has the following beneficial effects:
1. the method can effectively remove the metal salts in the waste mineral oil by reaction, so that the total content of the metal elements in the waste mineral oil is reduced from 3300PPm to below 370PPm, the ash index is reduced from 0.7% to below 0.05%, the problem of heating and coking in the regeneration process of the waste mineral oil can be effectively avoided, and meanwhile, the technical indexes such as oxidation stability, light stability, acid value and the like of the regenerated base oil are greatly improved due to the greatly reduced metal salt substances in the waste mineral oil, the metal element removal rate of the waste mineral oil can reach more than 80-90%, the coking tendency in the processing process of the waste mineral oil is greatly delayed, and the product quality of the regenerated base oil can be remarkably improved.
2. The compound salt with double functions of reaction sedimentation and agglomeration flocculation is prepared by orderly compounding amine salts such as ammonium sulfate, ammonium bicarbonate, ammonium carbamate, ammonium carbonate, ammonium phosphate and the like, and the removal rate of metal elements in the waste mineral oil can reach more than 80 percent.
3. The addition amount of the extractant solution needs to reach 5-12%, the extractant solution cannot fully react with the additive salts in the waste oil when the extractant solution is too low, and the reactant precipitate can generate hydrogen peroxide substances dissolved in water when the extractant solution is too high, so that the metal removal effect is affected.
4. The mixing temperature is 40-50 ℃, the excessive temperature can decompose the extractant solution, the generation of reaction precipitates is affected, the excessive temperature can affect the mixing effect, the extractant component can not be fully contacted with the metal additive in the lubricating oil, and the metal removal effect is affected;
5. the reaction sedimentation temperature is 50-70 ℃, the generation of reaction sedimentation is affected by the decomposition of the extractant solution due to the overhigh temperature, and the reaction sedimentation period is greatly prolonged due to the overlow temperature;
6. the reaction sedimentation time is 4-12 hours, so that the metal elements in the waste mineral oil can be fully reacted and settled.
The specific embodiment is as follows:
the application will be further illustrated with reference to specific examples. The scope of the application as claimed is not limited to the examples.
Example 1
A demetallization pretreatment method for waste mineral oil comprises the following steps:
(1) Ammonium sulfate, ammonium bicarbonate, ammonium carbamate, ammonium carbonate and ammonium phosphate are compounded into compound salt, and the compound salt solution is prepared by mixing the compound salt with distilled water;
(2) Mixing and extracting: adding the compound salt water solution into the waste mineral oil, and mixing and extracting to obtain a mixed material;
(3) The reaction: reacting the mixed materials;
(4) Agglomeration sedimentation: settling after the step (3) is finished;
(5) Solid-liquid separation: the settled mixed materials are conveyed into a centrifuge or a membrane separation device to realize continuous solid-liquid separation, thereby realizing the effective removal and separation of metal elements and phosphorus, silicon or other nonmetallic ash elements in the waste mineral oil.
Preferably, in the step (1), the mass ratio of the ammonium sulfate, the ammonium bicarbonate, the ammonium carbamate, the ammonium carbonate and the ammonium phosphate is as follows: group a ammonium sulfate: ammonium bicarbonate = 1:1, group B ammonium bicarbonate: ammonium carbamate = 1:1, group C ammonium bicarbonate: ammonium carbonate = 1:1, group D ammonium carbamate: ammonium carbonate = 1:1, group E ammonium carbonate: ammonium phosphate=1:1, and the compound brine solution with the mass concentration of 12% is prepared in sequence.
Preferably, in the step (2), the compound brine solution is added into the waste mineral oil according to the addition amount of 7% of the mass of the waste mineral oil, and the mixed extraction temperature is 45 ℃ for 40min.
Preferably, in step (3), the reaction temperature is 60℃and the reaction time is 20 hours.
Preferably, in the method, in step (4), the sedimentation time is 10 hours.
The test results of the experimental oil products are shown in the following table 1:
TABLE 1
According to the test data in table 1, it can be determined that the selected ammonium sulfate, ammonium bicarbonate, ammonium carbamate, ammonium carbonate, ammonium phosphate and other salt substances have certain removal effects on the removal of metal impurities in the waste engine oil, wherein the compound salt of ammonium bicarbonate and ammonium carbonate has better removal effects on metal elements in the waste engine oil.
Example 2
A demetallization pretreatment method for waste mineral oil comprises the following steps:
(1) Ammonium sulfate, ammonium bicarbonate, ammonium carbamate, ammonium carbonate and ammonium phosphate are compounded into compound salt, and the compound salt solution is prepared by mixing the compound salt with distilled water;
(2) Mixing and extracting: adding the compound salt water solution into the waste mineral oil, and mixing and extracting to obtain a mixed material;
(3) The reaction: reacting the mixed materials;
(4) Agglomeration sedimentation: settling after the step (3) is finished;
(5) Solid-liquid separation: the settled mixed materials are conveyed into a centrifuge or a membrane separation device to realize continuous solid-liquid separation, thereby realizing the effective removal and separation of metal elements and phosphorus, silicon or other nonmetallic ash elements in the waste mineral oil.
The effect of removing metal impurities in the waste engine oil is researched by changing the blending proportion of ammonium bicarbonate and ammonium carbonate, and the optimal blending proportion is determined.
Preferably, in the step (1), the blending ratio of the ammonium bicarbonate and the ammonium carbonate is as follows: group A3:1, group B2:1, group C1:1, group D1:2, and group E1:3 are sequentially prepared into a compound saline solution with the mass concentration of 12%.
Preferably, in the step (2), the compound brine solution is added into the waste mineral oil according to the addition amount of 7% of the mass of the waste mineral oil, and the mixed extraction temperature is 45 ℃ for 40min.
Preferably, in step (3), the reaction temperature is 60℃and the reaction time is 20 hours.
Preferably, in the method, in step (4), the sedimentation time is 10 hours.
The test results of the experimental oil products are shown in the following table 2:
TABLE 2
According to the test data in Table 2, when the blending ratio of ammonium bicarbonate to ammonium carbonate is 1:1, the obtained compound brine solution has the best effect of removing metal impurities in the waste engine oil.
Example 3
A demetallization pretreatment method for waste mineral oil comprises the following steps:
(1) Mixing salt and distilled water to prepare a compound salt water solution;
(2) Mixing and extracting: adding the compound salt water solution into the waste mineral oil, and mixing and extracting to obtain a mixed material;
(3) The reaction: reacting the mixed materials;
(4) Agglomeration sedimentation: settling after the step (3) is finished;
(5) Solid-liquid separation: the settled mixed materials are conveyed into a centrifuge or a membrane separation device to realize continuous solid-liquid separation, thereby realizing the effective removal and separation of metal elements and phosphorus, silicon or other nonmetallic ash elements in the waste mineral oil.
And (3) researching the removal effect of the compound salt solution in the step (2) on the metal impurities in the used oil by changing the addition amount of the compound salt solution, and determining the optimal addition amount.
Preferably, in the step (1), the ammonium bicarbonate and the ammonium carbonate are mixed according to a mixing ratio of 1:1 to prepare the compound saline solution with the mass concentration of 12 percent.
Preferably, in the step (2), the addition amount of the compound brine solution according to the mass of the waste mineral oil is as follows: group A5%, group B7%, group C9%, group D11%, and group E13%, respectively, adding into waste mineral oil, and mixing at 45deg.C for 40min.
Preferably, in step (3), the reaction temperature is 60℃and the reaction time is 20 hours.
Preferably, in the method, in step (4), the sedimentation time is 10 hours.
The test results of the experimental oil products are shown in the following table 3:
TABLE 3 Table 3
According to the test data table 3, the blending ratio of ammonium bicarbonate and ammonium carbonate is 1:1, the metal impurity removal rate in the waste engine oil is improved along with the increase of the addition amount of the compound salt solution, and when the addition amount reaches 9% of the mass of the waste engine oil, the metal impurity removal efficiency in the waste engine oil is not improved any more, so that the ideal waste engine oil demetallization pretreatment effect can be achieved when the addition amount is 9%.
Example 4
A demetallization pretreatment method for waste mineral oil comprises the following steps:
(1) Mixing salt and distilled water to prepare a compound salt water solution;
(2) Mixing and extracting: adding the compound salt water solution into the waste mineral oil, and mixing and extracting to obtain a mixed material;
(3) The reaction: reacting the mixed materials;
(4) Agglomeration sedimentation: settling after the step (3) is finished;
(5) Solid-liquid separation: the settled mixed materials are conveyed into a centrifuge or a membrane separation device to realize continuous solid-liquid separation, thereby realizing the effective removal and separation of metal elements and phosphorus, silicon or other nonmetallic ash elements in the waste mineral oil.
And (3) researching the removal effect of the reaction temperature on the metal impurities in the waste engine oil by changing the reaction temperature in the step (3), and determining the optimal reaction temperature.
Preferably, in the step (1), the ammonium bicarbonate and the ammonium carbonate are mixed according to a mixing ratio of 1:1 to prepare the compound saline solution with the mass concentration of 12 percent.
Preferably, in the step (2), the compound brine solution is added into the waste mineral oil according to the adding amount of 9% of the mass of the waste mineral oil, and the mixing extraction temperature is 45 ℃ for 40min.
Preferably, in step (3), the reaction temperatures are respectively: group A50 ℃, group B55 ℃, group C60 ℃, group D65 ℃, group E70 ℃, and reaction time 20 hours.
Preferably, in the method, in step (4), the sedimentation time is 10 hours.
The test results of the experimental oil products are shown in the following table 4:
according to the test data table 4, the blending ratio of ammonium bicarbonate and ammonium carbonate is 1:1, the addition amount of the compound salt solution is 9%, the removal rate of metal impurities in the waste engine oil is improved firstly and then the waste is reduced along with the increase of the reaction temperature, and the possible reasons are that when the reaction temperature is improved, part of solid salt substances generated by the reaction are decomposed, and the reaction products are dissolved into the oil again, so that the removal rate of the impurities is influenced, and the optimal reaction temperature is 55 ℃.
Example 5
A demetallization pretreatment method for waste mineral oil comprises the following steps:
(1) Mixing salt and distilled water to prepare a compound salt water solution;
(2) Mixing and extracting: adding the compound salt water solution into the waste mineral oil, and mixing and extracting to obtain a mixed material;
(3) The reaction: reacting the mixed materials;
(4) Agglomeration sedimentation: settling after the step (3) is finished;
(5) Solid-liquid separation: the settled mixed materials are conveyed into a centrifuge or a membrane separation device to realize continuous solid-liquid separation, thereby realizing the effective removal and separation of metal elements and phosphorus, silicon or other nonmetallic ash elements in the waste mineral oil.
And (3) researching the removal effect of the sedimentation time on the metal impurities in the waste engine oil by changing the sedimentation time in the step (4), and determining the optimal sedimentation time.
Preferably, in the step (1), the ammonium bicarbonate and the ammonium carbonate are mixed according to a mixing ratio of 1:1 to prepare the compound saline solution with the mass concentration of 12 percent.
Preferably, in the step (2), the compound brine solution is added into the waste mineral oil according to the adding amount of 9% of the mass of the waste mineral oil, and the mixing extraction temperature is 45 ℃ for 40min.
Preferably, in step (3), the reaction temperature is 55℃and the reaction time is 20 hours.
Preferably, in the method, in step (4), the sedimentation time is respectively: group a for 4 hours, group B for 6 hours, group C for 8 hours, group D for 10 hours, and group E for 12 hours.
The test results of the experimental oil products are shown in the following table 5:
TABLE 5
According to the test data table 5, under the conditions of the proportion of the compound salt solution, the addition amount and the reaction temperature, the removal rate of the metal impurities in the waste engine oil is improved along with the extension of the sedimentation time, and when the removal rate reaches a certain degree, the removal efficiency basically tends to be stable, and the optimal sedimentation time is determined to be 10 hours according to the production requirement.
Example 5
A demetallization pretreatment method for waste mineral oil comprises the following steps:
(1) The mixing ratio of ammonium bicarbonate and ammonium carbonate is 1:1;
(2) Mixing and extracting: adding a compound saline solution with a certain concentration into waste mineral oil, and mixing and extracting to obtain a mixed material;
(3) The reaction: reacting the mixed materials;
(4) Agglomeration sedimentation: settling after the step (3) is finished;
(5) Solid-liquid separation: the settled mixed materials are conveyed into a centrifuge or a membrane separation device to realize continuous solid-liquid separation, thereby realizing the effective removal and separation of metal elements and phosphorus, silicon or other nonmetallic ash elements in the waste mineral oil.
Preferably, in the step (2), the compound salt is sequentially prepared according to the concentration of the aqueous solution of 100% of group A, 5% of group B, 10% of group C, 15% of group D and 20% of group E (100% concentration is that distilled water is not added, the compound salt is directly added into the waste mineral oil), the prepared compound salt solution is added into the waste mineral oil according to the adding amount of 9% of the mass of the waste mineral oil, and the mixed extraction temperature is 45 ℃ for 40min.
Preferably, in step (3), the reaction temperature is 55℃and the reaction time is 20 hours.
Preferably, in the method, in step (4), the sedimentation time is 10 hours, respectively.
The test results of the experimental oil products are shown in the following table 6:
TABLE 6
According to the test data table 6, the compound salt is directly added into the waste mineral oil for reaction treatment, so that the metal impurities are hardly removed, the compound salt needs to be prepared into an aqueous solution, and the salt substances in the waste mineral oil are firstly extracted by using water, so that the salt substances are transferred to a water phase and then react with compound salt solutes in the water, thereby achieving the purpose of removing the metal impurities. And the metal impurity removing effect is improved and then reduced along with the increase of the concentration of the compound saline solution, and the metal impurity removing effect is optimal when the concentration of the water solution is 12% -15%.
The above embodiments are merely preferred embodiments of the present application, and should not be construed as limiting the present application, and the embodiments and features of the embodiments of the present application may be arbitrarily combined with each other without collision. The protection scope of the present application is defined by the claims, and the protection scope includes equivalent alternatives to the technical features of the claims. I.e., equivalent replacement modifications within the scope of this application are also within the scope of the application.
Claims (7)
1. The demetallization pretreatment method of the waste mineral oil is characterized by comprising the following steps:
(1) Mixing ammonium sulfate, ammonium bicarbonate, ammonium carbamate, ammonium carbonate or ammonium phosphate or a combination thereof with distilled water to prepare a saline solution;
(2) Mixing and extracting: adding the saline solution into the waste mineral oil, mixing and extracting to obtain a mixed material;
(3) The reaction: reacting the mixed materials;
(4) Agglomeration sedimentation: settling after the step (3) is finished;
(5) Solid-liquid separation: the settled mixed materials are conveyed into a centrifuge or a membrane separation device to realize continuous solid-liquid separation, thereby realizing the effective removal and separation of metal elements and phosphorus, silicon or other nonmetallic ash elements in the waste mineral oil.
2. The demetallization pretreatment method of waste mineral oil according to claim 1, wherein in the step (1), the salt is a composition of ammonium sulfate and ammonium bicarbonate in a mass ratio of (1-3): 1-3, or a composition of ammonium bicarbonate and ammonium carbamate in a mass ratio of (1-3): 1-3, or a composition of ammonium bicarbonate and ammonium carbonate in a mass ratio of (1-3): 1-3, or a composition of ammonium carbamate and ammonium carbonate in a mass ratio of (1-3): 1-3, or a composition of ammonium carbonate and ammonium phosphate in a mass ratio of (1-3): 1-3).
3. The process for demetallization pretreatment of waste mineral oil according to claim 2, wherein in step (1), the mass concentration of the brine solution is 10% to 15%.
4. The demetallization pretreatment method of waste mineral oil according to claim 2, wherein in the step (1), the salt is a composition of ammonium sulfate and ammonium bicarbonate in a mass ratio of 1:1, or a composition of ammonium bicarbonate and ammonium carbamate in a mass ratio of 1:1, or a composition of ammonium bicarbonate and ammonium carbonate in a mass ratio of 1:1, or a composition of ammonium carbamate and ammonium carbonate in a mass ratio of 1:1, or a composition of ammonium carbonate and ammonium phosphate in a mass ratio of 1:1.
5. The method for demetallizing and pre-treating waste mineral oil according to claim 1, wherein in the step (2), the compound brine solution is added into the waste mineral oil according to the addition amount of 5% -12% of the mass of the waste mineral oil, and the mixing extraction temperature is 40-50 ℃ for 30-60min.
6. The method for demetallization pretreatment of waste mineral oil according to claim 1, wherein in the step (3), the reaction temperature is 50 to 70 ℃ and the reaction time is 8 to 24 hours.
7. The method for demetallization pretreatment of waste mineral oil according to claim 1, wherein in the step (4), the settling time is 4 to 12 hours.
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