CN114058433A - Method for dechlorinating waste lubricating oil - Google Patents
Method for dechlorinating waste lubricating oil Download PDFInfo
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- CN114058433A CN114058433A CN202111481831.1A CN202111481831A CN114058433A CN 114058433 A CN114058433 A CN 114058433A CN 202111481831 A CN202111481831 A CN 202111481831A CN 114058433 A CN114058433 A CN 114058433A
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- lubricating oil
- dechlorinating
- waste lubricating
- dechlorination
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- 230000000382 dechlorinating effect Effects 0.000 title claims abstract description 75
- 239000010687 lubricating oil Substances 0.000 title claims abstract description 72
- 239000002699 waste material Substances 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000007864 aqueous solution Substances 0.000 claims abstract description 15
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 8
- XUJLWPFSUCHPQL-UHFFFAOYSA-N 11-methyldodecan-1-ol Chemical compound CC(C)CCCCCCCCCCO XUJLWPFSUCHPQL-UHFFFAOYSA-N 0.000 claims abstract description 7
- VEYPOAHLDFFNPD-UHFFFAOYSA-M benzyl-dodecyl-dimethylazanium;hydroxide Chemical compound [OH-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 VEYPOAHLDFFNPD-UHFFFAOYSA-M 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims abstract description 7
- 238000004064 recycling Methods 0.000 claims abstract description 6
- 238000006298 dechlorination reaction Methods 0.000 claims description 30
- 230000003068 static effect Effects 0.000 claims description 16
- 239000002808 molecular sieve Substances 0.000 claims description 7
- QOHMWDJIBGVPIF-UHFFFAOYSA-N n',n'-diethylpropane-1,3-diamine Chemical compound CCN(CC)CCCN QOHMWDJIBGVPIF-UHFFFAOYSA-N 0.000 claims description 7
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 230000014759 maintenance of location Effects 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 18
- 239000000460 chlorine Substances 0.000 abstract description 18
- 229910052801 chlorine Inorganic materials 0.000 abstract description 18
- 230000007797 corrosion Effects 0.000 abstract description 12
- 238000005260 corrosion Methods 0.000 abstract description 12
- 239000003054 catalyst Substances 0.000 abstract description 11
- 238000005984 hydrogenation reaction Methods 0.000 abstract description 11
- 239000003921 oil Substances 0.000 abstract description 6
- 231100000572 poisoning Toxicity 0.000 abstract description 3
- 230000000607 poisoning effect Effects 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 238000013329 compounding Methods 0.000 abstract 1
- 238000003756 stirring Methods 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 6
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 150000003071 polychlorinated biphenyls Chemical group 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 150000008280 chlorinated hydrocarbons Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000002480 mineral oil Substances 0.000 description 2
- 235000010446 mineral oil Nutrition 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- YJTKZCDBKVTVBY-UHFFFAOYSA-N 1,3-Diphenylbenzene Chemical group C1=CC=CC=C1C1=CC=CC(C=2C=CC=CC=2)=C1 YJTKZCDBKVTVBY-UHFFFAOYSA-N 0.000 description 1
- XGWLJUDRCACVMP-UHFFFAOYSA-N 2,2-diphenyl-1h-acenaphthylene Chemical class C1C(C=23)=CC=CC3=CC=CC=2C1(C=1C=CC=CC=1)C1=CC=CC=C1 XGWLJUDRCACVMP-UHFFFAOYSA-N 0.000 description 1
- XQFYGXFPKONEPY-UHFFFAOYSA-N 2,3-diphenylfuran Chemical compound O1C=CC(C=2C=CC=CC=2)=C1C1=CC=CC=C1 XQFYGXFPKONEPY-UHFFFAOYSA-N 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- OXAMBMYXAGPEHI-UHFFFAOYSA-N CN(C)CCCO.O Chemical compound CN(C)CCCO.O OXAMBMYXAGPEHI-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000002199 base oil Substances 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000009903 catalytic hydrogenation reaction Methods 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- VUNCWTMEJYMOOR-UHFFFAOYSA-N hexachlorocyclopentadiene Chemical compound ClC1=C(Cl)C(Cl)(Cl)C(Cl)=C1Cl VUNCWTMEJYMOOR-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000009972 noncorrosive effect Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
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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
- C10M175/0016—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
- C10M175/0008—Working-up used lubricants to recover useful products ; Cleaning with the use of adsorbentia
-
- 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)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention provides a method for dechlorinating waste lubricating oil, which comprises the steps of settling and filtering the waste lubricating oil, mixing the waste lubricating oil with an aqueous solution of a dechlorinating agent, heating the mixture, feeding the mixture into a dechlorinating tower, reacting at the temperature of 80-170 ℃, dehydrating an oil phase in the dechlorinating tower to obtain the dechlorinated waste lubricating oil, and returning a water phase to a dechlorinating agent tank for recycling, wherein the dechlorinating agent is prepared by compounding dodecyl dimethyl benzyl ammonium hydroxide, N.N-diethyl-1, 3-propylene diamine, isotridecyl alcohol polyoxyethylene polyoxypropylene ether and ethanol in proportion. The method for dechlorinating the waste lubricating oil provided by the invention has the advantages that the dechlorinating rate is more than 92%, the continuous operation is realized, the intermittent operation efficiency is higher compared with a reaction kettle, the operation is simple, and the problems of corrosion, pipeline blockage and catalyst poisoning caused by organic chlorine in the waste lubricating oil to a subsequent hydrogenation device can be effectively solved.
Description
Technical Field
The invention relates to a method for dechlorinating waste lubricating oil, belonging to the technical field of petrochemical industry.
Background
Chlorinated hydrocarbons are often present in the used lubricating oil, for example, chlorinated paraffin (with a chlorine content of 42-70%) is the most widely used chlorine-containing extreme pressure antiwear agent, and hexachlorocyclopentadiene is used as a raw material to synthesize a non-corrosive chlorine-containing extreme pressure agent. Other chlorinated hydrocarbons are mainly chlorinated aromatic hydrocarbons, which are commonly polychlorinated biphenyl (PCBs), diphenyl furan (PCDF), polychlorinated diphenyl acenaphthene (PCDD), polychlorinated terphenyl (PCT) and the like, wherein the polychlorinated biphenyl has high physical and chemical properties, is heat-resistant, acid-resistant, alkali-resistant, corrosion-resistant and oxidation-resistant, and has no corrosion to metals; high dielectric constant and excellent insulating property, so that it has been widely used as additive for heat carrier, insulating oil and lubricating oil, transformer and capacitor.
In the regeneration process of the waste lubricating oil, one of the indispensable links is to obtain high-quality base oil through hydrofining. Because the content and acid value of organic chlorine in the waste lubricating oil are high, hydrogen chloride and water are generated in the hydrogenation process, which brings great harm: 1. dew point corrosion and acid water scouring corrosion. When the temperature of the inner surface of the apparatus reaches the dew point temperature of water, H2O, HCl and H2S can generate acid with high concentration under the condition of liquid phase, and serious corrosion is caused to the device; 2. pipe blockage and fouling
And (6) corrosion. During the catalytic hydrogenation, HCl is generated from organic chloride, and NH may be generated from N-containing substances3Result in NH3Combined with HCl to form NH4Cl, causing pipe blockage and under-deposit corrosion; 3. the catalyst is poisoned. The hydrogenation catalyst generally comprises nickel and organic chlorineInorganic chlorine generated by the compound can cause sintering of nickel crystals and accelerate the aging of the catalyst.
How to remove organic chlorine in the waste lubricating oil with high efficiency and low cost to form a stable and high-efficiency waste lubricating oil pretreatment process system and ensure the stable operation of a subsequent hydrogenation process is a technical problem to be solved urgently. Patent CN112920842A provides a method for removing organochlorine from waste lubricating oil, which comprises adding the waste lubricating oil containing organochlorine into a reactor, adding a dechlorinating agent into the reactor, and using transition metal as promoter to effectively remove organochlorine from the waste lubricating oil at appropriate temperature and normal pressure. The method adopts a kettle type stirring reactor, after stirring and dechlorination, standing is needed to separate out solid components in a dechlorinating agent, and then an oil phase can enter a subsequent hydrofining working section, wherein the dechlorination process is intermittent and is not beneficial to a continuous large-scale lubricating oil hydrofining process. The patent CN110540876A provides a process for decolorizing and refining waste mineral oil and an operation method thereof, wherein the waste mineral oil is filtered, settled and dehydrated, organic acid and water-soluble additives in the oil product are removed by a water washing tank, oil-water separation is carried out, the oil phase is subjected to hydrofining under the action of a hydrogenation catalyst, the hydrodechlorination temperature condition is 200-450 ℃, and the hydrogen state of a hydrodechlorination reaction system is 0.9-8.5 MPa. The process adopts a hydrogenation mode to remove chlorine in the oil product to generate hydrogen chloride, and the problems of equipment corrosion, pipeline blockage, catalyst chlorine poisoning and the like can occur in the actual production, so that the continuous production is influenced.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a method for dechlorinating the waste lubricating oil, the dechlorinating rate of the method is more than 92 percent, the problems of equipment corrosion, pipeline blockage, catalyst chlorisis and the like can be effectively solved, and the method is favorable for the long-period operation of a waste lubricating oil hydrogenation device. The invention provides a dechlorination method of waste lubricating oil, which comprises the following steps:
the waste lubricating oil is deposited and filtered, then stored in a waste lubricating oil tank 1, conveyed to the inlet of a static mixer 3 by a pump, the dechlorinating agent aqueous solution is stored in a dechlorinating agent tank 2 and conveyed to the inlet of the static mixer 3 by the pump, and the waste lubricating oil and the dechlorinating agent aqueous solution are dissolved in waterThe liquid is uniformly mixed in a static mixer 3, then the liquid enters a dechlorination tower 4 from the middle part of the reactor after being heated by a heater, the reaction temperature is 80-170 ℃, the retention time of the waste lubricating oil in the dechlorination tower 4 is 45-75min, and the proportion of the dechlorination agent to the waste lubricating oil is 100--1. The dechlorinated waste lubricating oil is extracted from the top of the dechlorinating tower 4 and enters the molecular sieve dehydrating tower 5 to be dehydrated to obtain the dechlorinated waste lubricating oil, the water phase of the dechlorinating tower 4 is extracted from the bottom of the tower and returned to the dechlorinating agent tank 2 for recycling, and part of the recycled dechlorinating agent aqueous solution can be discharged out of the dechlorinating agent tank 2 according to the dechlorinating effect in actual production and is supplemented with new dechlorinating agent aqueous solution.
The antichlor is prepared from the following raw materials in parts by mass: 8-15 parts of dodecyl dimethyl benzyl ammonium hydroxide, 30-65 parts of N, N-diethyl-1, 3-propane diamine, 5-20 parts of isotridecyl alcohol polyoxyethylene polyoxypropylene ether and 25-70 parts of ethanol. The dechlorinating agent is prepared according to the following steps: the raw materials weighed according to the proportion are added into a reaction container with a heating device, the temperature is controlled to be 55-90 ℃, the mixture is stirred for 1-3 hours, and the product is prepared after the mixture is fully stirred uniformly. The isotridecanol polyoxyethylene polyoxypropylene ether has a relative molecular weight of more than 10000, and the dodecyl dimethyl benzyl ammonium hydroxide has 12 carbon atoms and is prepared by adding beta-hydroxyethyl trimethylamine hydroxide and propylene oxide.
The invention has the advantages that:
(1) according to the dechlorination method provided by the invention, the dechlorination reaction is a continuous feeding production process, the production efficiency is high, the continuous operation can be realized, the operation is simpler, and the defects that the batch type dechlorination reaction process of a common kettle type reactor is low in production efficiency and is not beneficial to large-scale production are avoided. Compared with a kettle type reaction dechlorination process, the dechlorination process provided by the invention is more matched with the currently mainstream waste lubricating oil fixed bed continuous hydrogenation process, and can greatly improve the production efficiency of hydrofining of the waste lubricating oil.
(2) According to the dechlorination method provided by the invention, the dechlorination agent can be recycled, part of the recycled dechlorination agent aqueous solution is discharged out of the tank according to the dechlorination effect, and meanwhile, a new dechlorination agent aqueous solution is supplemented to ensure the dechlorination effect. The dechlorinating agent has the catalytic dechlorinating function of the rest components except that N, N-diethyl-1, 3-propane diamine and chlorine in the waste lubricating oil are continuously reacted and consumed, and basically no consumption is caused in the dechlorinating reaction. Under the condition of ensuring that sufficient N, N-diethyl-1, 3-propane diamine in the dechlorinating agent reacts with chlorine, the dechlorinating agent is recycled, so that the use amount of the dechlorinating agent can be greatly reduced, and the discharge amount of sewage can be greatly reduced because the dechlorinating agent is dissolved in water and is separated from the waste lubricating oil.
(3) The dechlorination method provided by the invention is provided with the molecular sieve dehydration tower, so that trace water in the lubricating oil can be effectively removed, on one hand, the phenomenon that the stable operation of the device is influenced due to the fact that the metal coalescence of active metal components is accelerated and the hydrogenation activity of the catalyst is reduced because the water content of the raw material is too high can be avoided; on the other hand, the condensation of water and HCl and H in the subsequent hydrogenation section can be effectively avoided2S can generate acid with high concentration under the condition of liquid phase, and serious corrosion is caused to the device.
The method for dechlorinating the waste lubricating oil provided by the invention has the advantages that the dechlorinating rate is more than 92%, the continuous operation can be realized, the intermittent operation efficiency is higher compared with a reaction kettle, the operation is simple, and the problems of corrosion, pipeline blockage and catalyst poisoning caused by organic chlorine in the waste lubricating oil to a subsequent hydrogenation device can be effectively solved.
Drawings
FIG. 1 is a schematic process flow diagram of a method for dechlorinating waste lubricating oil according to the present invention, wherein: 1 is a waste lubricating oil tank, 2 is a dechlorinating agent tank, 3 is a static mixer, 4 is a dechlorinating tower, and 5 is a molecular sieve dehydration tower.
Detailed Description
The characteristics of the catalyst, the preparation method and the catalytic performance of the catalyst of the present invention will be described in detail with reference to the following specific examples, but the present invention is not limited to these examples and does not limit the scope of the present invention.
Example 1:
waste lubricating oil containing 1157ppm of chlorine is settled and filtered, then is stored in a waste lubricating oil tank 1 and is conveyed to the inlet of a static mixer 3 through a pump, and dechlorinating agent aqueous solution is stored in a dechlorinating agent tank2, the waste lubricating oil is conveyed to the inlet of a static mixer 3 through a pump, the waste lubricating oil and the dechlorinating agent aqueous solution are uniformly mixed in the static mixer 3, then the mixture is heated by a heater and enters a dechlorinating tower 4 from the middle part of the reactor, the reaction temperature is 80 ℃, the residence time of the waste lubricating oil in the dechlorinating tower 4 is 45-75min, and the ratio of the dechlorinating agent to the waste lubricating oil is 100 mu g.g-1. The dechlorinated waste lubricating oil is extracted from the top of the dechlorinating tower 4 and enters the molecular sieve dehydrating tower 5 to be dehydrated to obtain the dechlorinated waste lubricating oil, and the water phase of the dechlorinating tower 4 is extracted from the bottom of the tower and returned to the dechlorinating agent tank 2 for recycling. The antichlor is prepared by adding 15 parts by weight of dodecyl dimethyl benzyl ammonium hydroxide, 30 parts by weight of N, N-diethyl-1, 3-propane diamine, 20 parts by weight of isotridecyl alcohol polyoxyethylene polyoxypropylene ether and 50 parts by weight of ethanol into a reaction vessel with a heating device, controlling the temperature to be 55 ℃, stirring for 1 hour, and fully and uniformly stirring. The detection and analysis of the embodiment show that the chlorine removal rate of the waste lubricating oil reaches 94.6 percent.
Example 2:
waste lubricating oil containing 865ppm of chlorine is settled and filtered, then is stored in a waste lubricating oil tank 1, and is conveyed to an inlet of a static mixer 3 through a pump, a dechlorinating agent aqueous solution is stored in a dechlorinating agent tank 2 and is conveyed to the inlet of the static mixer 3 through the pump, the waste lubricating oil and the dechlorinating agent aqueous solution are uniformly mixed in the static mixer 3, then the mixture is heated by a heater and enters a dechlorinating tower 4 from the middle part of the reactor, the reaction temperature is 170 ℃, the residence time of the waste lubricating oil in the dechlorinating tower 4 is 60min, and the proportion of the dechlorinating agent to the waste lubricating oil is 1000 mu g.g-1. The dechlorinated waste lubricating oil is extracted from the top of the dechlorinating tower 4 and enters the molecular sieve dehydrating tower 5 to be dehydrated to obtain the dechlorinated waste lubricating oil, and the water phase of the dechlorinating tower 4 is extracted from the bottom of the tower and returned to the dechlorinating agent tank 2 for recycling. The antichlor is prepared by adding 12 parts by weight of dodecyl dimethyl benzyl ammonium hydroxide, 45 parts by weight of N, N-diethyl-1, 3-propane diamine, 12 parts by weight of isotridecyl alcohol polyoxyethylene polyoxypropylene ether and 25 parts by weight of ethanol into a reaction vessel with a heating device, controlling the temperature to be 70 ℃, stirring for 2 hours, and fully and uniformly stirring. The detection and analysis of the embodiment show that the chlorine removal rate of the waste lubricating oil reaches 93.2%。
Example 3:
settling and filtering waste lubricating oil containing 1542ppm of chlorine, storing in a waste lubricating oil tank 1, pumping to an inlet of a static mixer 3, storing a dechlorinating agent aqueous solution in a dechlorinating agent tank 2, pumping to an inlet of the static mixer 3, uniformly mixing the waste lubricating oil and the dechlorinating agent aqueous solution in the static mixer 3, heating by a heater, feeding into a dechlorinating tower 4 from the middle part of the reactor, reacting at 130 ℃, keeping the waste lubricating oil in the dechlorinating tower 4 for 45min, and controlling the ratio of the dechlorinating agent to the waste lubricating oil to be 500 mu g.g-1. The dechlorinated waste lubricating oil is extracted from the top of the dechlorinating tower 4 and enters the molecular sieve dehydrating tower 5 to be dehydrated to obtain the dechlorinated waste lubricating oil, and the water phase of the dechlorinating tower 4 is extracted from the bottom of the tower and returned to the dechlorinating agent tank 2 for recycling. The antichlor is prepared by adding 8 parts by weight of dodecyl dimethyl benzyl ammonium hydroxide, 65 parts by weight of N, N-diethyl-1, 3-propane diamine, 5 parts by weight of isotridecyl alcohol polyoxyethylene polyoxypropylene ether and 70 parts by weight of ethanol into a reaction vessel with a heating device, controlling the temperature to be 90 ℃, stirring for 3 hours, and fully and uniformly stirring. The detection and analysis of the embodiment show that the chlorine removal rate of the waste lubricating oil reaches 94.1%.
Claims (5)
1. The method for dechlorinating the waste lubricating oil is characterized by comprising the following steps of:
the waste lubricating oil is deposited and filtered, then is stored in a waste lubricating oil tank, and is conveyed to an inlet of a static mixer through a pump, a dechlorinating agent aqueous solution is stored in a dechlorinating agent tank and is conveyed to the inlet of the static mixer through the pump, the waste lubricating oil and the dechlorinating agent aqueous solution are uniformly mixed in the static mixer, then is heated by a heater and enters a dechlorinating tower from the middle part of a reactor, the reaction temperature is 80-170 ℃, the dechlorinated waste lubricating oil is extracted from the top of the dechlorinating tower and then enters a molecular sieve dehydrating tower, dechlorinated waste lubricating oil is obtained after dehydration, and a water phase of the dechlorinating tower is extracted from the bottom of the tower and is returned to the dechlorinating agent tank for recycling;
the dechlorinating agent is prepared from the following raw materials in parts by weight: 8-15 parts of dodecyl dimethyl benzyl ammonium hydroxide, 30-65 parts of N, N-diethyl-1, 3-propane diamine, 5-20 parts of isotridecyl alcohol polyoxyethylene polyoxypropylene ether and 25-70 parts of ethanol.
2. Dechlorination process according to claim 1, characterized in that: the dechlorination agent water solution is stored in a dechlorination agent tank, part of the dechlorination agent water solution which is recycled can be discharged out of the tank according to the dechlorination effect, and new dechlorination agent water solution is supplemented.
3. Dechlorination process according to claim 1, characterized in that: the retention time of the waste lubricating oil in the dechlorination tower is 45-75min, and the ratio of the dechlorination agent to the waste lubricating oil is 100--1。
4. Dechlorination process according to claim 1, characterized in that: the dechlorinating agent is prepared according to the following steps: the raw materials weighed according to the proportion are added into a reaction container with a heating device, the temperature is controlled to be 55-90 ℃, the mixture is stirred for 1-3 hours, and the product is prepared after the mixture is fully stirred uniformly.
5. Dechlorination process according to claim 1, characterized in that: the dechlorination rate of the waste lubricating oil dechlorinated by the method is more than 92 percent.
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| CN202111481831.1A CN114058433B (en) | 2021-12-07 | 2021-12-07 | Method for dechlorinating waste lubricating oil |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5132006A (en) * | 1989-02-02 | 1992-07-21 | Huels Aktiengesellschaft | Liquid dehalogenating agents |
| JPH1192771A (en) * | 1997-09-19 | 1999-04-06 | Ebara Corp | Reproduction of waste oil |
| CN108587766A (en) * | 2018-06-06 | 2018-09-28 | 武汉科林精细化工有限公司 | A kind of free of contamination waste lubricating oil cyclic regeneration pretreating process |
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Denomination of invention: A dechlorination method for waste lubricating oil Granted publication date: 20221118 Pledgee: Industrial and Commercial Bank of China Limited Hubei pilot Free Trade Zone Wuhan Branch Pledgor: HUBEI RUNCHI ENVIRONMENTAL PROTECTION TECHNOLOGY CO.,LTD. Registration number: Y2024980011406 |