CN116144389A - Advanced refining method of waste mineral oil tower top oil composite solvent - Google Patents
Advanced refining method of waste mineral oil tower top oil composite solvent Download PDFInfo
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- 239000003921 oil Substances 0.000 title claims abstract description 105
- 239000002904 solvent Substances 0.000 title claims abstract description 101
- 238000000034 method Methods 0.000 title claims abstract description 45
- 239000002480 mineral oil Substances 0.000 title claims abstract description 33
- 235000010446 mineral oil Nutrition 0.000 title claims abstract description 32
- 239000002699 waste material Substances 0.000 title claims abstract description 28
- 238000007670 refining Methods 0.000 title claims abstract description 21
- 239000002131 composite material Substances 0.000 title claims abstract description 15
- 239000000295 fuel oil Substances 0.000 claims abstract description 46
- 230000018044 dehydration Effects 0.000 claims abstract description 28
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 230000008569 process Effects 0.000 claims abstract description 20
- 239000002253 acid Substances 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 11
- 238000001704 evaporation Methods 0.000 claims abstract description 8
- 230000008020 evaporation Effects 0.000 claims abstract description 8
- 238000004064 recycling Methods 0.000 claims abstract description 3
- 208000005156 Dehydration Diseases 0.000 claims abstract 10
- 230000008929 regeneration Effects 0.000 claims abstract 2
- 238000011069 regeneration method Methods 0.000 claims abstract 2
- 238000000605 extraction Methods 0.000 claims description 48
- 239000003795 chemical substances by application Substances 0.000 claims description 36
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 32
- 238000000638 solvent extraction Methods 0.000 claims description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000005520 cutting process Methods 0.000 claims description 20
- 239000012046 mixed solvent Substances 0.000 claims description 20
- 238000011084 recovery Methods 0.000 claims description 20
- 238000000926 separation method Methods 0.000 claims description 16
- 238000003860 storage Methods 0.000 claims description 12
- 238000009833 condensation Methods 0.000 claims description 11
- 230000005494 condensation Effects 0.000 claims description 11
- 230000003472 neutralizing effect Effects 0.000 claims description 10
- 238000004821 distillation Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000001556 precipitation Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical group CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 4
- 238000013329 compounding Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 238000005984 hydrogenation reaction Methods 0.000 abstract description 12
- 238000002360 preparation method Methods 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000003208 petroleum Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 239000010763 heavy fuel oil Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000346 nonvolatile oil Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000341 volatile oil Substances 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
- 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
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/006—Combinations of processes provided in groups C10G1/02 - C10G1/08
-
- 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
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/002—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal in combination with oil conversion- or refining processes
-
- 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
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/04—Diesel oil
-
- 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 invention discloses a method for deeply refining a waste mineral oil tower top oil composite solvent, which relates to the field of waste mineral oil regeneration, and comprises the following steps of: s1, a pretreatment step, namely firstly carrying out an acid-base neutralization process and a dehydration process, carrying out dehydration after the neutralization of the tower top oil raw material, firstly adding an acid value neutralizer into the tower top oil raw material, and recycling the neutralizer after separating and removing the neutralizer; then sending the neutralized tower top oil into a flash evaporation dehydration tower for heating dehydration treatment; the regenerated waste mineral oil tower top oil can be used as ship fuel oil or used as a raw material of a hydrogenation process, and reaches the national standard of six diesel after hydrogenation.
Description
Technical Field
The invention relates to the field of waste mineral oil, in particular to a method for deeply refining a composite solvent of waste mineral oil tower top oil.
Background
Mineral oil refers to a mixture of refined liquid hydrocarbons obtained from petroleum, which is obtained by atmospheric and vacuum fractionation, solvent extraction and dewaxing, hydrofining. Mineral oils include light, heavy fuel oils, lubricating oils, cooling oils, and other mineral hydrocarbons. Mineral oil can float on the surface of a water body to influence the exchange of air and water body interface oxygen; the oil dispersed in water, adsorbed to suspended particles, or present in an emulsified state in water is decomposed by microorganisms in water, and dissolved oxygen in water is consumed, thereby deteriorating water quality. The mineral oil is colorless semitransparent oily liquid, has no or almost no fluorescence, has no odor and no smell when cold, has slight petroleum smell when heated, is insoluble in water and ethanol, is soluble in volatile oil, is miscible in most of nonvolatile oil, is stable to light, heat, acid and the like, but can be slowly oxidized when being contacted with light and heat for a long time, and the waste mineral oil is extracted and refined from petroleum, coal and is the mineral oil which changes the original physical and chemical properties due to the action of external factors and cannot be continuously used in the processes of exploitation, processing and use.
The traditional preparation method of the waste mineral oil overhead oil has the defects that in the preparation process, the integral fuel oil component cannot reach the standard that the chromaticity is 1.0 chromaticity, the density is 0.83-0.85, the distillation range is 200-375 ℃, the closed flash point is more than 85 ℃, the waste mineral oil overhead oil cannot be used as ship fuel oil or as hydrogenation equipment raw material, the waste mineral oil overhead oil cannot be used as Guohu diesel oil after hydrogenation, in addition, in the preparation process, the integral process production cost is higher, the process procedure is relatively complex, the energy consumption is high and the like, and the preparation of the waste mineral oil overhead oil is inconvenient.
Accordingly, a method for deeply refining the waste mineral oil overhead complex solvent is provided by those skilled in the art to solve the problems set forth in the background art.
Disclosure of Invention
The invention aims to provide a method for deeply refining waste mineral oil overhead oil by using a composite solvent, which aims to solve the problems that in the traditional method for preparing waste mineral oil overhead oil provided in the background art, the integral fuel oil component cannot reach the standard that the chromaticity is 1.0, the density is 0.83-0.85, the distillation range is 200-375 ℃, the closed flash point is above 85 ℃, the method cannot be used as ship fuel oil or as hydrogenation equipment raw material, the method cannot be used as Guohuio diesel after hydrogenation, and the integral process production cost is higher, the process procedure is relatively complex and the energy consumption is high in the preparation process, and the like, so that the preparation of waste mineral oil overhead oil is inconvenient.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the method for deeply refining the waste mineral oil tower top oil composite solvent comprises the following steps of:
s1, a pretreatment step, namely firstly carrying out a neutralization process and a dehydration process, firstly adding a neutralization reagent into the tower top oil raw material, heating to 45 ℃, separating and removing the neutralization reagent after precipitating for 3 hours, and then sending the neutralized tower top oil into a flash evaporation dehydration tower for heating and dehydration;
s2, cutting components, namely cutting the components of the dehydrated oil product in a distillation tower, firstly cutting light components, sending the light components into a storage tank for storage, then cutting fuel oil components, sending the fuel oil components into an intermediate tank for solvent refining, and sending the rest components into the storage tank for heavy components;
s3, a double-solvent extraction step, namely, carrying out double-solvent extraction on cut fuel oil, wherein when the double-solvent extraction is carried out, the extraction solvent is N-methyl pyrrolidone, the extraction solvent is mixed with furfural in a ratio of 1:1 to prepare a mixed solvent, the mixed solvent is heated to 60-70 ℃ through a heat exchanger, then the fuel oil is heated to 60-70 ℃ through a heater, and then is injected into a mixer and an extraction tank for mutual solvent extraction, the ratio of the oil to the oil is 1:1 and 1:1.5, after 3-5-level countercurrent extraction, the extraction oil is reduced to 5-10 ℃ through the heat exchanger, the extraction oil is sent into a settling tower for precipitation solvent, the solvent content of the extraction oil is 4-8%, centrifugal separation is carried out in a centrifuge, the separation temperature is lower than 10 ℃, the centrifuge speed is higher than 10000 r/min, the centrifugal force is higher than 11500G, the solvent content of the extraction oil after centrifugal separation is 1-1.25%, the solvent content of the extraction oil is lower than 0.5% through organic film filtration, the extraction oil is sent into an extraction oil intermediate tank for waiting for the treatment of a stripping agent, and the separated red solvent is fully called as a solvent with a saturated solvent, and the solvent is completely recovered;
s4, reducing the acid value of the wet solvent, namely firstly, adding ethanolamine into the wet solvent when the acid value of the solvent is reduced, heating to 50 ℃ for mixing reaction for 2 hours, heating to 85 ℃ in a recovery tower for evaporation and recovery, wherein the condensation temperature during recovery is 1-5 ℃, mainly avoiding loss caused by incomplete condensation of the solvent, achieving colorless and clear mixed solvent for standby, and then sending the extract oil which cannot be evaporated into an extract oil tank;
s5, removing the agent from the extracted oil by a removing agent tower, wherein the removing agent temperature is 85 ℃, the recovery cooling temperature is lower than 5 ℃, the loss caused by non-condensation of the solvent is avoided, the temperature of the extracted oil is reduced to 5 ℃ after the removing agent of the extracted oil, the filtered fuel oil is sent into a finished product tank, the solvent content of the finished fuel oil is lower than one ten thousandth, and the removed mixed solvent is sent into a solvent extraction tank for mixed extraction.
As a preferred embodiment of the present invention: in the pretreatment step, the neutralizing agent comprises sodium hydroxide solution and ethanolamine, the compounding ratio of the sodium hydroxide solution to the ethanolamine is 1:1, and the dehydration temperature of heating dehydration in the flash dehydration tower is 150 ℃.
As a preferred embodiment of the present invention: in the step of cutting the components, when the light components are cut, the temperature is constant temperature and normal temperature-220 ℃, the pressure is normal pressure, and when the fuel oil components are cut, the temperature is constant temperature and normal temperature 220-380 ℃, and the pressure is normal pressure.
As a preferred embodiment of the present invention: in the double-solvent extraction step, the pressure of a heat exchanger when the mixed solvent is heated to 60-70 ℃ by the heat exchanger is normal pressure, the pressure of the heat exchanger when the extracted oil is reduced to 5-10 ℃ by the heat exchanger is normal pressure, the pressure of a centrifuge is normal pressure when the separation temperature is less than 10 ℃, and the temperature of an extracted oil tank is lower than 10 ℃.
As a preferred embodiment of the present invention: in the step of reducing the acid value of the wet solvent, the content of ethanolamine added into the wet solvent is 0.5 per mill, the pressure in the process of mixing reaction for 2 hours is normal pressure, and the vacuum degree in the recovery tower is 1.333KPa.
As a preferred embodiment of the present invention: in the agent removing treatment step, the vacuum degree in the agent removing tower is 1.333KPa, and the filter consists of a filter screen made of pp material, so that trace particles are removed.
Compared with the prior art, the invention has the beneficial effects that:
the invention relates to a method for deeply refining waste mineral oil tower top oil composite solvent, which comprises the steps of double solvent extraction, acid value reduction and solvent removal treatment by wet solvent, so that high-quality finished fuel oil can be obtained, the solvent content of the finished fuel oil is lower than ten thousandth, the total fuel oil component can reach the standard that the chromaticity is 1.0 chromaticity, the density is 0.83-0.85, the distillation range is 200-375 ℃, the closed flash point is above 85 ℃, the method can be used as ship fuel oil or as raw material of hydrogenation equipment, and the method can be used as national six diesel after hydrogenation, and has the advantages of low production cost, simple process, low energy consumption, low investment and low operation cost in the preparation process.
Drawings
Other features, objects and advantages of the present invention will become more apparent upon reading of the detailed description of non-limiting embodiments, given with reference to the accompanying drawings in which:
FIG. 1 is a process flow diagram of the whole process of a method for deeply refining a complex solvent of a waste mineral oil overhead oil.
Detailed Description
In the embodiment of the invention, a method for deeply refining the waste mineral oil tower top oil composite solvent comprises the following steps:
s1, a pretreatment step, namely firstly, a neutralization step and a dehydration step are carried out, namely, a neutralizing agent is added into the tower top oil raw material, and is heated to 45 ℃, after 3 hours of precipitation, the neutralizing agent is separated and removed, the neutralizing agent is recycled, and then, the neutralized tower top oil is sent into a flash evaporation dehydration tower for heating dehydration;
s2, cutting components, namely cutting the components of the dehydrated oil product in a distillation tower, firstly cutting light components, sending the light components into a storage tank for storage, then cutting fuel oil components, sending the fuel oil components into an intermediate tank for solvent refining, and sending the rest components into the storage tank for heavy components;
s3, a double-solvent extraction step, namely, carrying out double-solvent extraction on cut fuel oil, wherein when the double-solvent extraction is carried out, the extraction solvent is N-methyl pyrrolidone, the extraction solvent is mixed with furfural in a ratio of 1:1 to prepare a mixed solvent, the mixed solvent is heated to 60-70 ℃ through a heat exchanger, then the fuel oil is heated to 60-70 ℃ through a heater, and then is injected into a mixer and an extraction tank for mutual solvent extraction, the ratio of the oil to the oil is 1:1 and 1:1.5, after 3-5-level countercurrent extraction, the extraction oil is reduced to 5-10 ℃ through the heat exchanger, the extraction oil is sent into a settling tower for precipitation solvent, the solvent content of the extraction oil is 4-8%, centrifugal separation is carried out in a centrifuge, the separation temperature is lower than 10 ℃, the centrifuge speed is higher than 10000 r/min, the centrifugal force is higher than 11500G, the solvent content of the extraction oil after centrifugal separation is 1-1.25%, the solvent content of the extraction oil is lower than 0.5% through organic film filtration, the extraction oil is sent into an extraction oil intermediate tank for waiting for the treatment of a stripping agent, and the separated red solvent is fully called as a solvent with a saturated solvent, and the solvent is completely recovered;
s4, reducing the acid value of the wet solvent, namely firstly, adding ethanolamine into the wet solvent when the acid value of the solvent is reduced, heating to 50 ℃ for mixing reaction for 2 hours, heating to 85 ℃ in a recovery tower for evaporation and recovery, wherein the condensation temperature during recovery is 1-5 ℃, mainly avoiding loss caused by incomplete condensation of the solvent, achieving colorless and clear mixed solvent for standby, and then sending the extract oil which cannot be evaporated into an extract oil tank;
s5, removing the agent from the extracted oil by a removing agent tower, wherein the removing agent temperature is 85 ℃, the recovery cooling temperature is lower than 5 ℃, the loss caused by non-condensation of the solvent is avoided, the temperature of the extracted oil is reduced to 5 ℃ after the removing agent of the extracted oil, the filtered fuel oil is sent into a finished product tank, the solvent content of the finished product fuel oil is lower than one ten thousandth, and the removed mixed solvent is sent into a solvent extraction tank for mixed extraction.
The high-quality finished fuel oil can be obtained through the steps of double-solvent extraction, acid value reduction and solvent removal treatment by wet solvents, the solvent content of the finished fuel oil is lower than one ten thousandth, the total fuel oil component can reach the standard that the chromaticity is 1.0 chromaticity, the density is 0.83-0.85, the distillation range is 200-375 ℃, and the closed flash point is above 85 ℃.
In the pretreatment step, the neutralizing agent comprises sodium hydroxide solution and ethanolamine, the compounding ratio of the sodium hydroxide solution to the ethanolamine is 1:1, and the dehydration temperature of the flash dehydration tower for heating and dehydration is 150 ℃. In the step of cutting the components, when the light components are cut, the temperature is constant temperature and normal temperature-220 ℃, the pressure is normal pressure, and when the fuel oil components are cut, the temperature is constant temperature and normal temperature 220-380 ℃, and the pressure is normal pressure. In the double solvent extraction step, the pressure of a heat exchanger when the mixed solvent is heated to 60-70 ℃ by the heat exchanger is normal pressure, the pressure of the heat exchanger when the extracted oil is reduced to 5-10 ℃ by the heat exchanger is normal pressure, the pressure of a centrifuge is normal pressure when the separation temperature is less than 10 ℃, and the temperature of the extracted oil tank is lower than 10 ℃. In the step of reducing the acid value of the wet solvent, the content of ethanolamine added into the wet solvent is 0.5 per mill, the pressure in the process of mixing reaction for 2 hours is normal pressure, and the vacuum degree in the recovery tower is 1.333KPa. In the step of removing agent treatment, the vacuum degree in the agent removing tower is 1.333KPa, and the filter consists of a filter screen made of pp material, so that trace particles are prevented from being carried.
The catalyst can be used as ship fuel oil or as raw material of hydrogenation equipment, can be used as Guohuie diesel after hydrogenation, and has the advantages of low production cost, simple process, low energy consumption, small investment and low running cost in the preparation process.
The working principle of the invention is as follows: the method for deeply refining the waste mineral oil tower top oil composite solvent comprises the following steps:
s1, a pretreatment step, namely, firstly, carrying out a neutralization process and a dehydration process, adding a neutralization reagent into the tower top oil raw material, heating to 45 ℃, separating and removing the neutralization reagent after 3 hours of precipitation, recycling the neutralization reagent, and then, sending the neutralized tower top oil into a flash dehydration tower for heating and dehydration; in the pretreatment step, the neutralizing agent comprises sodium hydroxide solution and ethanolamine, the compounding ratio of the sodium hydroxide solution to the ethanolamine is 1:1, and the dehydration temperature of the flash dehydration tower for heating and dehydration is 150 ℃.
S2, cutting components, namely cutting the components of the dehydrated oil product in a distillation tower, firstly cutting light components, sending the light components into a storage tank for storage, then cutting fuel oil components, sending the fuel oil components into an intermediate tank for solvent refining, and sending the rest components into the storage tank for heavy components; in the step of cutting the components, when the light components are cut, the temperature is constant temperature and normal temperature-220 ℃, the pressure is normal pressure, and when the fuel oil components are cut, the temperature is constant temperature and normal temperature 220-380 ℃, and the pressure is normal pressure.
S3, a double-solvent extraction step, namely, carrying out double-solvent extraction on cut fuel oil, wherein when the double-solvent extraction is carried out, the extraction solvent is N-methyl pyrrolidone, the extraction solvent is mixed with furfural in a ratio of 1:1 to prepare a mixed solvent, the mixed solvent is heated to 60-70 ℃ through a heat exchanger, then the fuel oil is heated to 60-70 ℃ through a heater, and then is injected into a mixer and an extraction tank for mutual solvent extraction, the ratio of the oil to the oil is 1:1 and 1:1.5, after 3-5-level countercurrent extraction, the extraction oil is reduced to 5-10 ℃ through the heat exchanger, the extraction oil is sent into a settling tower for precipitation solvent, the solvent content of the extraction oil is 4-8%, centrifugal separation is carried out in a centrifuge, the separation temperature is lower than 10 ℃, the centrifuge speed is higher than 10000 r/min, the centrifugal force is higher than 11500G, the solvent content of the extraction oil after centrifugal separation is 1-1.25%, the solvent content of the extraction oil is lower than 0.5% through organic film filtration, the extraction oil is sent into an extraction oil intermediate tank for waiting for the treatment of a stripping agent, and the separated red solvent is fully called as a solvent with a saturated solvent, and the solvent is completely recovered; in the double solvent extraction step, the pressure of a heat exchanger when the mixed solvent is heated to 60-70 ℃ by the heat exchanger is normal pressure, the pressure of the heat exchanger when the extracted oil is reduced to 5-10 ℃ by the heat exchanger is normal pressure, the pressure of a centrifuge is normal pressure when the separation temperature is less than 10 ℃, and the temperature of the extracted oil tank is lower than 10 ℃.
S4, reducing the acid value of the wet solvent, namely firstly, adding ethanolamine into the wet solvent when the acid value of the solvent is reduced, heating to 50 ℃ for mixing reaction for 2 hours, heating to 85 ℃ in a recovery tower for evaporation and recovery, wherein the condensation temperature during recovery is 1-5 ℃, mainly avoiding loss caused by incomplete condensation of the solvent, achieving colorless and clear mixed solvent for standby, and then sending the extract oil which cannot be evaporated into an extract oil tank; in the step of reducing the acid value of the wet solvent, the content of ethanolamine added into the wet solvent is 0.5 per mill, the pressure in the process of mixing reaction for 2 hours is normal pressure, and the vacuum degree in the recovery tower is 1.333KPa.
S5, removing the agent from the extracted oil by a removing agent tower, wherein the removing agent temperature is 85 ℃, the recovery cooling temperature is lower than 5 ℃, the loss caused by non-condensation of the solvent is avoided, the temperature of the extracted oil is reduced to 5 ℃ after the removing agent of the extracted oil, the filtered fuel oil is sent into a finished product tank, the solvent content of the finished product fuel oil is lower than one ten thousandth, and the removed mixed solvent is sent into a solvent extraction tank for mixed extraction. In the step of removing agent treatment, the vacuum degree in the agent removing tower is 1.333KPa, and the filter consists of a filter screen made of pp material, so that trace particles are prevented from being carried.
The acid value and the catalyst removing treatment step are reduced through a double solvent extraction procedure, then the wet solvent is used for obtaining high-quality finished fuel oil, the solvent content of the finished fuel oil is lower than one ten thousandth, the total fuel oil component can reach the standard that the chromaticity is 1.0 chromaticity, the density is 0.83-0.85, the distillation range is 200-375 ℃, the closed flash point is more than 85 ℃, the finished fuel oil can be used as ship fuel oil, can also be used as raw material of hydrogenation equipment, can be used as national six diesel after hydrogenation, and has the advantages of low production cost, simple process, low energy consumption, small investment and low running cost in the preparation process.
The foregoing description is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical solution of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (6)
1. The method for deeply refining the waste mineral oil tower top oil composite solvent is characterized by comprising the following steps of:
s1, a pretreatment step, namely firstly carrying out oil neutralization and dehydration treatment on overhead oil generated in the regeneration process of waste mineral oil in sequence, firstly adding a neutralizing agent with an acid value of 1 permillage into the overhead oil raw material, heating to 45 ℃, precipitating for 3 hours, separating and removing the neutralizing agent, recycling the neutralizing agent, and then sending the neutralized overhead oil into a flash evaporation dehydration tower for heating and dehydration treatment;
s2, cutting components, namely cutting the components of the dehydrated oil product in a distillation tower, firstly cutting light components, sending the light components into a storage tank for storage, then cutting fuel oil components, sending the fuel oil components into an intermediate tank for solvent refining, and sending the rest components into the storage tank for heavy components;
s3, a double-solvent extraction step, namely, carrying out double-solvent extraction on cut fuel oil, wherein when the double-solvent extraction is carried out, the extraction solvent is N-methyl pyrrolidone, the extraction solvent is mixed with furfural in a ratio of 1:1 to prepare a mixed solvent, the mixed solvent is heated to 60-70 ℃ through a heat exchanger, then the fuel oil is heated to 60-70 ℃ through a heater, and then is injected into a mixer and an extraction tank for mutual solvent extraction, the ratio of the oil to the oil is 1:1 and 1:1.5, after 3-5-level countercurrent extraction, the extraction oil is reduced to 5-10 ℃ through the heat exchanger, the extraction oil is sent into a settling tower for precipitation solvent, the solvent content of the extraction oil is 4-8%, centrifugal separation is carried out in a centrifuge, the separation temperature is lower than 10 ℃, the centrifuge speed is higher than 10000 r/min, the centrifugal force is higher than 11500G, the solvent content of the extraction oil after centrifugal separation is 1-1.25%, the solvent content of the extraction oil is lower than 0.5% through organic film filtration, the extraction oil is sent into an extraction oil intermediate tank for waiting for the treatment of a stripping agent, and the separated red solvent is fully called as a solvent with a saturated solvent, and the solvent is completely recovered;
s4, reducing the acid value of the wet solvent, namely firstly, adding ethanolamine into the wet solvent when the acid value of the solvent is reduced, heating to 50 ℃ for mixing reaction for 2 hours, heating to 85 ℃ in a recovery tower for evaporation and recovery, wherein the condensation temperature during recovery is 1-5 ℃, mainly avoiding loss caused by incomplete condensation of the solvent, achieving colorless and clear mixed solvent for standby, and then sending the extract oil which cannot be evaporated into an extract oil tank;
s5, removing the agent from the extracted oil by a stripping tower, wherein the stripping temperature is 85 ℃, the recovery cooling temperature is lower than 5 ℃, the loss caused by incapability of condensing the solvent is avoided, the temperature of the extracted oil is reduced to 5 ℃ after the stripping agent is removed, the filtered fuel oil is sent into a finished product tank, the solvent content of the finished fuel oil is lower than one ten thousandth, and the separated mixed solvent is sent into a solvent extraction tank for mixed extraction.
2. The method for deeply refining the waste mineral oil tower top oil composite solvent according to claim 1, wherein in the pretreatment step, the neutralizing agent comprises sodium hydroxide solution and ethanolamine, the compounding ratio of the sodium hydroxide solution to the ethanolamine is 1:1, and the dehydration temperature of heating dehydration in the flash dehydration tower is 150 ℃.
3. The method for deeply refining the waste mineral oil tower top oil composite solvent according to claim 1, wherein in the step of cutting the components, the temperature is constant temperature normal temperature-220 ℃ and the pressure is normal pressure when the light components are cut, and the temperature is constant temperature normal temperature 220-380 ℃ and the pressure is normal pressure when the fuel oil components are cut.
4. The method for deeply refining the waste mineral oil overhead oil composite solvent according to claim 1, wherein in the step of double solvent extraction, the pressure of the heat exchanger when the mixed solvent is heated to 60-70 ℃ by the heat exchanger is normal pressure, the pressure of the heat exchanger when the extracted oil is reduced to 5-10 ℃ by the heat exchanger is normal pressure, the pressure of the centrifuge is normal pressure when the separation temperature is less than 10 ℃, and the temperature of the extracted oil tank is less than 10 ℃.
5. The method for deeply refining the waste mineral oil overhead oil composite solvent according to claim 1, wherein in the step of reducing the acid value of the wet solvent, the content of ethanolamine added into the wet solvent is 0.5 per mill, the pressure during the mixing reaction for 2 hours is normal pressure, and the vacuum degree in the recovery tower is 1.333KPa.
6. The method for deeply refining the waste mineral oil tower top oil composite solvent according to claim 1, wherein in the removing agent treatment step, the vacuum degree in the removing agent tower is 1.333KPa, and the filter consists of a filter screen made of pp material and filters carried trace particles.
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