CN1539936A - Technique for regenerating waste lubricating oil - Google Patents

Technique for regenerating waste lubricating oil Download PDF

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Publication number
CN1539936A
CN1539936A CNA03127966XA CN03127966A CN1539936A CN 1539936 A CN1539936 A CN 1539936A CN A03127966X A CNA03127966X A CN A03127966XA CN 03127966 A CN03127966 A CN 03127966A CN 1539936 A CN1539936 A CN 1539936A
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China
Prior art keywords
lubricating oil
extraction
alkane solvents
tower
hydrofining
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CNA03127966XA
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Chinese (zh)
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CN100334189C (en
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娟 刘
刘娟
张璋
高万君
雷元柏
姜华
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荆门石油化工设计院
第一国际环保有限公司
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Publication of CN1539936A publication Critical patent/CN1539936A/en
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Publication of CN100334189C publication Critical patent/CN100334189C/en

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Abstract

A process for regenerating the used lubricating oil includes removing impurities, adding paraffin solvent, extracting at 30-130 deg.C under 3-16 MPa, settling at 80-150 deg.C under 3-16 MPa, and recovering solvent at 90-250 deg.C under d2-12 MPa to separate the paraffin solvent from regenerated lubricating oil.

Description

Process for regeneration of waste lubricating oil
Technical field: the present invention relates to the reclaiming process process that adopted in the waste lubricant oil regeneration in the petrochemical industry.
Background technology: at present, the waste lubricating oil amount of generation is quite big, accounts for 45% of lubricants capacity about 3,500,000 tons every year for China's oil production.This part waste lubricating oil generally acts as a fuel and burns or abandon, and causes environmental pollution, is used for regenerated waste lubricating oil amount and little.Domestic more existing waste lubricant oil regeneration factories also mostly are the factories of some small scales backward in technique now, and the reclaiming process that these factories adopted is sulfuric acid mostly--the carclazyte method, it comprises purification, pickling, clay-filtered and fractionating step, purifying step comprises sedimentation, filtration, coalescent, vacuum flashing, mainly is to remove water, part lightweight oil and mechanical impurity.The rerefined oil of this explained hereafter, of poor quality, secondary pollution is serious.
Technology contents: purpose of the present invention is exactly to fall behind at the process engineering for regenerating that is adopted in present China waste lubricant oil regeneration, the deficiency that secondary pollution is serious and a kind of process for regeneration of waste lubricating oil is provided, the rerefined oil of this explained hereafter, quality is good, and non-secondary pollution.Process for regeneration of waste lubricating oil comprises purification, pickling, clay-filtered and fractionating step, and its pickling and clay-filtered step are replaced by the alkane solvents extraction step; The alkane solvents extraction step is: with waste lubricating oil add alkane solvents in extraction tower 2 at temperature 30-130 ℃, extract under the condition of pressure 3-16Mpa, discard extract remainder, with extraction liquid in sedimentation tower 5 at temperature 80-150 ℃, carry out sedimentation under the condition of pressure 3-16Mpa, discard sediment, the extraction liquid after the sedimentation is sent in the alkane solvents recovery tower at temperature 90-250 ℃, separate under the condition of pressure 2-12Mpa, isolate alkane solvents and lubricating oil component.After the alkane solvents extraction step, also comprise the hydrofining step, the hydrofining step is: the lubricating oil after alkane solvents extraction add hydrogen and hydrogenation catalyst in hydrogenator 16 at temperature 280-370 ℃, carry out hydrofining under the condition of pressure 3-8Mpa, the lubricating oil after the hydrofining enters and isolates hydrogen and bright stock component in the high-pressure separator 17.The alkane solvents extraction step can replace with the hydrofining step.In the alkane solvents extraction step, also comprise the sediment that discards and extract remainder separating step again, the steps include: sediment and extract remainder are sent to evaporation in the extract remainder evaporator tower 3, the propane recovery utilization that evaporates, evaporation excess discharger.The hydrofining step also comprises the atmospheric stripping step, the steps include: to send into atmospheric stripping tower 20 through high-pressure separator 17 isolated lubricating oil components, and add nitrogen or water vapour carries out stripping, the waste gas that stripping goes out burns through incinerator, and the lubricating oil component behind the stripping is regenerated bright stock component; After separated hydrogen is sent into recycle hydrogen water cooler 18 cooling in high-pressure separator 17, after sending into branch flow container 19 again and removing liquid in the hydrogen, send in the hydrogenator 16 by circulating hydrogen compressor 21.Advantage of the present invention is the rerefined oil of producing, and quality is good, and non-secondary pollution.
Description of drawings: accompanying drawing 1 is used the process flow sheet of alkane solvents extraction step for the present invention.
Accompanying drawing 2 is used the process flow sheet of hydrofining step for the present invention.
Embodiment: the required equipment of this technology comprises that extraction tower, sedimentation tower, recovery tower, hydrogenator and separator are general-purpose equipment in the existing petroleum chemicals course of processing.The patent that name is called " waste lubricant oil regeneration alkane solvents extraction tower ", " waste lubricant oil regeneration hydrogenator " and " laboratory purposes vacuum still " has been declared with " mat woven of fine bamboo strips one international environmental protection company limited " in Hong Kong by my unit in present patent application, be the equipment that is exclusively used in process for regeneration of waste lubricating oil laboratory usefulness or suitability for industrialized production.Alkane solvents can be used propane, butane, pentane or its mixture as solvent, and present embodiment adopts propane.Hydrogenation catalyst adopts metallic nickel, molybdenum, tungsten or cobalt.In the course of processing, at first waste lubricating oil is purified by sedimentation, filtration, coalescent and vacuum flashing step, mainly be to remove water, part lightweight oil and mechanical impurity.To purify the back waste lubricating oil then and pump into propane extraction tower 2 tops by extraction tower fresh feed pump 1, and pump into propane (ratio of propane and waste lubricating oil is 8: 1) by propane pump 10 in propane extraction tower bottom, 60 ℃ of temperature, extract under the condition of pressure 4.4Mpa.Because two-phase difference in specific gravity, the two is the counter-current flow mass transfer in tower, in the extract remainder at the bottom of the tower, only contain a spot of propane, being mainly imperfect compositions such as ash content, carbon residue sinks at the bottom of the tower, discard the extract remainder that sinks at the bottom of the tower or extract remainder is sent to evaporation in the extract remainder evaporator tower 3, the propane recovery utilization that evaporates or deliver to incinerator and burn, a small amount of excess discharger that the evaporation back is last.The extraction liquid that has dissolved lubricating oil comes out from cat head 2, after being heated to 80 ℃ in the extraction liquid well heater 4, deliver to again in the sedimentation tower 5 80 ℃ of temperature, carry out sedimentation under the condition of pressure 4.35Mpa, because temperature raises, propane solubleness descends, sediment is further separated out in a large number from the bottom, sediment is sent to evaporation in the extract remainder evaporator tower 3, and the propane that evaporates is delivered to incinerator and burned or recycle, evaporation excess discharger.。Extraction liquid after the sedimentation of sedimentation tower is drawn from the cat head of sedimentation tower 5, after recovery tower feed heater 6 is heated to 94-105 ℃, deliver to propane recovery tower 7-1 and propane recovery tower 7-2 more successively, at temperature 94-105 ℃, separate under the condition of pressure 4.3Mpa, after the propane that comes out from cat head is cooled to 40 ℃ by propane cooler 8, deliver to propane cycles jar 9 again, pump into propane extraction tower 2 bottoms by propane cycles pump 10 then.Isolated extraction liquid among the propane recovery tower 7-2 is delivered to extraction section tundish 12, be provided with heating coil in jar, can further heat and deviate from the extraction liquid dissolved small amounts of propane and deliver to incinerator and burn, that comes out from tundish 12 bottoms is the lubricating oil component of propane after refining, has so far finished the purification and the propane extraction step of waste lubricating oil.Institute's regenerated lubricating oil component is by after the separation column fractionation, and metal content and acid number in the rerefined oil obviously reduce, and has also deviate from polymeric additive and oxidative condensation product simultaneously.As the lubricating oil of need regeneration better quality, need the rerefined oil after the propane extraction is carried out hydrofinishing.Its hydrofining process is: will through the rerefined oil after the propane extraction by reactor feed pump 13 with pump into raw material-generation oil heat exchanger 14 after circulating hydrogen mixes, after heat exchange, send into reactor feed well heater 15, send into after being heated to 300 ℃ in the hydrogenator 16, hydrogenation catalyst is housed in the reactor, 300 ℃ of temperature, carry out hydrofining reaction under the condition of pressure 4.0Mpa, in reactor, sulphur in the lubricating oil component, nitrogen, chlorine, oxygen, alkene etc. and hydrogen reaction, reacted reaction product is incoming stock-and generate to enter after oil heat exchanger 14 coolings and carry out gas-liquid separation in the high pressure separating tank 17, isolated lubricating oil component comes out to send into atmospheric stripping tower 20 from the bottom, feed nitrogen at the bottom of the tower and carry out stripping, the waste gas that stripping goes out enters incinerator and burns, and the lubricating oil component behind the stripping pumps through stripping column bottoms pump 22 and is the hydrolube component.After separated hydrogen is sent into recycle hydrogen water cooler 18 cooling in the high pressure separating tank 17, after sending into branch flow container 19 again and removing liquid in the hydrogen,, send in the hydrogenator 16 by circulating hydrogen compressor 21.Unifining process can make non-hydrocarbon compound hydrogenolysis such as sulphur in the waste lubricating oil component, nitrogen, oxygen effectively, make alkene, aromatic selective hydrogenation is saturated and can deviate from impurity such as metal and bituminous matter, have to handle wide, the advantages such as liquid yield is high, good product quality of raw material range.Regeneration bright stock component after this hydrofining has industrial application value after by the separation column fractionation, can be made into the lube product of the various trades mark after being in harmonious proportion.
The ultimate principle of the propane extracting and refining process in the process for regeneration of waste lubricating oil is:
Propane is the quite little alkane of relative molecular mass.It can not dissolve the high organic compound of relative molecular mass, but can dissolve the hydrocarbon of molecular mass in lube range and lighter hydrocarbon.So when propane mixes with waste lubricating oil, metal-salt that propane just can produce condensation product, colloid, bituminous matter, the organic acid corroding metal of additive in the waste lubricating oil and oxidation generation and other mechanical impurity are precipitated out, and are retained in the propane solution and will lubricate oil content.Propane boiled off just obtain the propane treated oil.
The ultimate principle of unifining process is:
1. be present in the oxygenatedchemicals in the waste oil
May there be various oxidation productss in the waste oil; Mainly be carboxylic-acid, carboxylic acid esters, aldehydes, ketone, alcohols, phenols, peralcohol class etc., also may contain remaining phenol type additive in the waste oil.Oxygenatedchemicals is the easiest hydrogenation, and generally very fast response generates corresponding hydrocarbon and water, also is accompanied by reactions such as taking off alkyl, isomerization, condensation, open loop simultaneously.
2. be present in the sulfocompound in the waste oil
It may be thiophene-based and hydrogenation thiophene-based that sulfocompound exists more, and a spot of sulfide, disulphide, also has thiophosphate from additive, olefine sulfide, phosphosulfurized olefin etc.The hydrogenation of sulfocompound is generally difficult than oxygenatedchemicals.Sulfide, disulphide is just reaction rapidly under the condition of mild hydrogenation, generates corresponding hydrocarbon and hydrogen sulfide; It is difficult that hydrogenation thiophene-based hydrogenation is wanted, and it wants earlier open loop, regeneration hydrocarbon and hydrogen sulfide.Thiophene-based is then more difficult, at first is ring filling, and open loop then is only then and generates hydrocarbon and hydrogen sulfide.
3, nitride in the waste oil
Nitride in the waste oil seldom, from base oil or additive.Classes of compounds has amine, pyridines, pyroles etc.Denitrogenation than dechlorination desulfurization because of difficult.Reaction generates corresponding hydrocarbon and ammonia.
4. the halogen compounds in the waste oil
Halogen compounds in the waste oil mainly is a chlorocarbon.Generate hydrogenchloride and corresponding hydrocarbon during the chlorocarbon hydrogenation, the complexity and the sulfocompound of hydrogenation are similar.
5, hydro carbons in the waste oil
Hydro carbons in the waste oil mainly is stable hydrocarbon and aromatic hydrocarbons, does not generally change under the hydroconversion condition of waste oil regeneration.Some lives through in the pyritous waste oil may contain alkene, and alkene is saturated by hydrogen institute when hydrogenation, generates corresponding stable hydrocarbon.

Claims (5)

1, process for regeneration of waste lubricating oil comprises purification, pickling, clay-filtered and fractionating step, it is characterized in that its pickling and clay-filtered step are replaced by the alkane solvents extraction step; The alkane solvents extraction step is: with waste lubricating oil add alkane solvents in extraction tower (2) at temperature 30-130 ℃, extract under the condition of pressure 3-16Mpa, discard extract remainder, with extraction liquid in sedimentation tower (5) at temperature 80-150 ℃, carry out sedimentation under the condition of pressure 3-16Mpa, discard sediment, extraction liquid after the sedimentation is sent in the alkane solvents recovery tower at temperature 90-250 ℃, separate under the condition of pressure 2-12Mpa, isolate alkane solvents and lubricating oil component.
2, process for regeneration of waste lubricating oil according to claim 1, it is characterized in that after the alkane solvents extraction step, also comprising the hydrofining step, the hydrofining step is: the lubricating oil after alkane solvents extraction add hydrogen and hydrogenation catalyst in hydrogenator (16) at temperature 280-370 ℃, carry out hydrofining under the condition of pressure 3-8Mpa, the lubricating oil after the hydrofining enters and isolates hydrogen and bright stock component in the high-pressure separator (17).
3, process for regeneration of waste lubricating oil according to claim 1 is characterized in that the alkane solvents extraction step can replace with the hydrofining step.
4, process for regeneration of waste lubricating oil according to claim 1, it is characterized in that in the alkane solvents extraction step, also comprising the sediment that discards and extract remainder separating step again, the steps include: sediment and extract remainder are sent to evaporation in the extract remainder evaporator tower (3), the propane recovery utilization that evaporates, evaporation excess discharger.
5, process for regeneration of waste lubricating oil according to claim 2, it is characterized in that the hydrofining step also comprises the atmospheric stripping step, the steps include: to send into atmospheric stripping tower (20) through the isolated lubricating oil component of high-pressure separator (17), and add nitrogen or water vapour carries out stripping, the waste gas that stripping goes out burns through incinerator, and the lubricating oil component behind the stripping is regenerated bright stock component; After separated hydrogen is sent into recycle hydrogen water cooler (18) cooling in high-pressure separator (17), after sending into branch flow container (19) again and removing liquid in the hydrogen, send in the hydrogenator (16) by circulating hydrogen compressor (21).
CNB03127966XA 2003-04-26 2003-04-26 Technique for regenerating waste lubricating oil CN100334189C (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101735882A (en) * 2009-12-10 2010-06-16 武汉科技学院 Method for regenerating base oil by waste internal-combustion engine oil
CN101173202B (en) * 2006-11-01 2010-09-15 中国石油化工股份有限公司 Waste lubricant oil recovery utilization method
CN102658009A (en) * 2012-05-12 2012-09-12 辽宁留德润滑油有限公司 On-line hydrogen sulfide removing and recycling device of waste lubricating oil regeneration distillation tail gas
CN102732369A (en) * 2011-04-06 2012-10-17 新疆奎屯新西亚石油化工有限公司 Regeneration process for waste lubricating oil
CN101861373B (en) * 2008-08-08 2014-09-10 清油有限公司 Process and system for re-refining used lubeoils
CN104531328A (en) * 2015-01-08 2015-04-22 劳淑仪 Hydrogenating and regenerating technology for complete hydrogenation type used lubricating oil
CN107216908A (en) * 2017-07-23 2017-09-29 张家彬 A kind of used oil extraction tower pitch discharge technique
CN107287018A (en) * 2017-08-06 2017-10-24 张家彬 A kind of process for regeneration of waste lubricating oil
CN107699332A (en) * 2017-08-16 2018-02-16 张家彬 A kind of waste lubricating oil extraction tower pitch discharge method
CN108003914A (en) * 2017-11-30 2018-05-08 广东电网有限责任公司电力科学研究院 A kind of purification method of the benzyldithio toluene of insulating oil

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4073720A (en) * 1976-10-22 1978-02-14 The United States Of America As Represented By The United States Department Of Energy Method for reclaiming waste lubricating oils
US5935417A (en) * 1996-12-17 1999-08-10 Exxon Research And Engineering Co. Hydroconversion process for making lubricating oil basestocks
CN1107109C (en) * 2000-10-26 2003-04-30 中国石油化工股份有限公司 Process for recovering waste oil

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101173202B (en) * 2006-11-01 2010-09-15 中国石油化工股份有限公司 Waste lubricant oil recovery utilization method
CN101861373B (en) * 2008-08-08 2014-09-10 清油有限公司 Process and system for re-refining used lubeoils
CN101735882A (en) * 2009-12-10 2010-06-16 武汉科技学院 Method for regenerating base oil by waste internal-combustion engine oil
CN101735882B (en) * 2009-12-10 2013-01-23 武汉科技学院 Method for regenerating base oil by waste internal-combustion engine oil
CN102732369A (en) * 2011-04-06 2012-10-17 新疆奎屯新西亚石油化工有限公司 Regeneration process for waste lubricating oil
CN102658009A (en) * 2012-05-12 2012-09-12 辽宁留德润滑油有限公司 On-line hydrogen sulfide removing and recycling device of waste lubricating oil regeneration distillation tail gas
CN104531328A (en) * 2015-01-08 2015-04-22 劳淑仪 Hydrogenating and regenerating technology for complete hydrogenation type used lubricating oil
CN107216908A (en) * 2017-07-23 2017-09-29 张家彬 A kind of used oil extraction tower pitch discharge technique
CN107287018A (en) * 2017-08-06 2017-10-24 张家彬 A kind of process for regeneration of waste lubricating oil
CN107699332A (en) * 2017-08-16 2018-02-16 张家彬 A kind of waste lubricating oil extraction tower pitch discharge method
CN108003914A (en) * 2017-11-30 2018-05-08 广东电网有限责任公司电力科学研究院 A kind of purification method of the benzyldithio toluene of insulating oil
CN108003914B (en) * 2017-11-30 2020-05-01 广东电网有限责任公司电力科学研究院 Method for purifying dibenzyl disulfide of insulating oil

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