CN110791317A - Waste lubricating oil hydrogenation regeneration pretreatment method - Google Patents
Waste lubricating oil hydrogenation regeneration pretreatment method Download PDFInfo
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- CN110791317A CN110791317A CN201910949462.0A CN201910949462A CN110791317A CN 110791317 A CN110791317 A CN 110791317A CN 201910949462 A CN201910949462 A CN 201910949462A CN 110791317 A CN110791317 A CN 110791317A
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- hydrogen
- lubricating oil
- waste lubricating
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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
- C10G67/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only
- C10G67/02—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only plural serial stages only
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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
- 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
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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
- 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
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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
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/10—Lubricating oil
Abstract
The invention discloses a waste lubricating oil hydrogenation regeneration pretreatment method, wherein the waste lubricating oil is firstly subjected to sedimentation in a sedimentation tank to remove most of water and large-particle mechanical impurities, and then is filtered by a filter to remove small-particle mechanical impurities, the obtained dehydrated and offline mechanical impurities and the waste lubricating oil can be completely or partially mixed with hydrogen and hydrogen supply fractions, the mixture enters a heating furnace for heating, and the material at the outlet of the heating furnace enters a hydrogen-hydrogen reactor for reaction; the reaction material coming out from the top of the hydrogen hydrogenation reactor is separated into hydrogen, light hydrocarbon, heavy oil at the bottom of the tower, hydrogen supply fraction and raw materials for subsequent hydrorefining by a hot high fraction, a cold low fraction, a flash tower and a reduced pressure fractionating tower. The method has the advantages that coking of the waste lubricating oil pretreatment heating furnace and damage of non-ideal components of the waste lubricating oil hydrogenation regeneration are prevented more thoroughly, the waste lubricating oil hydrorefining raw material is obtained, and the production period of the waste lubricating oil hydrogenation regeneration device is greatly prolonged.
Description
Technical Field
The invention belongs to the technical field of waste lubricating oil regeneration, and relates to a hydrogenation regeneration pretreatment method for waste lubricating oil.
Background
With the increase of mechanization degree, the increase of travel demand of people and other factors, the use amount of various lubricating oils is increasing. Because of the low consumption of the lubricating oil, a large amount of waste lubricating oil is generated, and resource recovery and environmental protection are the practical requirements for recycling the waste lubricating oil. The regeneration process of the waste lubricating oil begins in 1935, and is developed from sulfate clay to acid-free process, and the regeneration technology of the waste lubricating oil can be divided into repurification, re-refining and re-refining according to the modification mechanism and modification degree of the lubricating oil. The secondary purification refers to a method for removing impurities by physical methods such as sedimentation, filtration, water washing or centrifugal separation; there are two methods for re-refining: the method is a traditional acid washing-clay process, mainly comprises the steps of settling, distilling, acid washing, alkali washing, clay refining and the like, is harmful to the environment, and is an acid-free process comprising reduced pressure distillation, solvent extraction, chemical agent treatment and the like, so that the acid-free process is more environment-friendly, but the product quality is not high. Refining refers to the combination of purification and refining processes, and finally a hydrofining method is adopted to remove residual additives and aged byproducts to obtain a refined lubricating oil product with higher quality. Considering the product quality and the processing environmental protection requirement, the hydrogenation process is the mainstream technology for regenerating the waste lubricating oil, and the problems encountered by the prior waste lubricating oil hydrogenation regeneration technology are as follows: the heating furnace is easy to generate coke, the removal depth of the hydrogenation feeding impurities is not enough, the catalyst is easy to inactivate, the bed layer is easy to block, the production period of the device is short, and the operation cost is high.
Disclosure of Invention
The invention aims to provide a waste lubricating oil hydrogenation regeneration pretreatment method which has the beneficial effects of preventing a heating furnace for waste lubricating oil pretreatment from coking and deeply removing various impurities (particle impurities, condensation colloid, metal additives, organic ester, polyether, polyalcohol, chlorine-containing pollutants or chlorine-containing additives and the like) in the waste lubricating oil.
The technical scheme adopted by the invention is carried out according to the following steps:
(1) the waste lubricating oil is subjected to sedimentation in a sedimentation tank to remove most of water and large-particle mechanical impurities, and then is filtered by a filter to remove small-particle mechanical impurities, the obtained dehydrated offline mechanical impurity waste lubricating oil can be completely or partially mixed with hydrogen and hydrogen supply fractions, the mixture enters a heating furnace for heating, the heated mixture enters a hydrogen-hydrogen reactor for reaction, and the mixture can also be completely or partially mixed with a material from an outlet of the heating furnace and enters the hydrogen-hydrogen reactor for reaction;
(2) the reaction material coming out from the top of the hydrogen hydrogenation reactor is separated into hydrogen, light hydrocarbon, heavy oil at the bottom of the tower, hydrogen supply fraction and raw materials for subsequent hydrorefining by a hot high fraction, a cold low fraction, a flash tower and a reduced pressure fractionating tower.
Further, the operating conditions of the hydrogen hydrogenation reactor are that the reaction pressure is 5-15 MPa, the reaction temperature is 300-420 ℃, and the space velocity is 0.2-2.0 hr-1。
The high-pressure hydrogen comes from a subsequent hydrofining device, and a hydrogen source does not need to be independently provided for a hydrogen-in-situ reaction system; the feeding of the heating furnace can be a mixture of hydrogen and hydrogen supply fractions, or a mixture of hydrogen, hydrogen supply fractions and waste lubricating oil which is partially or totally dehydrated to remove mechanical impurities; the hydrogen supply fraction added into one furnace feed needs to be determined by laboratory test hydrogen supply capacity, and the hydrogen supply fraction can be all or partial fraction from the top of a flash tower, can be all or partial fraction from the side line of a reduced pressure fractionating tower minus the first line, and can be a mixture of the top fraction of the flash tower and the side line of the reduced pressure fractionating tower minus the first line. And combining all fractions or partial fractions of the side line minus one line of the vacuum fractionating tower, all materials of the side line minus two lines, all materials or partial materials at the top of the flash tower and all materials at the bottom of the cold low fraction, and using the combined materials as the feed of the regeneration device of the waste lubricating oil hydrogenation method.
Definition of hydrogen donor fraction: the petroleum fraction contains a certain amount of benzo (naphtho) naphthene parent structural components (such as tetrahydronaphthalene and 9,10 dihydroanthracene shown in the figure).
The component containing benzo (naphtho) naphthene parent structure can release hydrogen under certain conditions, can inhibit free radical decomposition reaction and macromolecular polycondensation reaction, and can be converted into the benzo (naphtho) naphthene parent structure component from the naphthalene (anthracene) parent structure component under the action of hydrogen, and the fraction containing the benzo (naphtho) naphthene parent structure component with high abundance is called as hydrogen supply fraction.
Drawings
FIG. 1 is a schematic process flow diagram for use in the process of the present invention.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention comprises the following steps:
(1) the method comprises the following steps of firstly settling the waste lubricating oil by a settling tank to remove most of water and large-particle mechanical impurities, filtering the waste lubricating oil by a filter to remove small-particle mechanical impurities, mixing all or part of the obtained dehydrated offline mechanical impurity waste lubricating oil with hydrogen and hydrogen supply fractions, heating the mixture in a heating furnace, allowing the material at the outlet of the heating furnace to enter a hydrogen-hydrogen reactor for reaction, and mixing all or part of the material at the outlet of the heating furnace with the material from the outlet of the heating furnace to enter the hydrogen-hydrogen reactor for reaction;
the operating conditions of the hydrogen hydrogenation reactor are that the reaction pressure is 5-15 MPa, the reaction temperature is 300-420 ℃, and the space velocity is 0.2-2.0 hr-1。
(2) The reaction material coming out from the top of the hydrogen hydrogenation reactor is separated into hydrogen, light hydrocarbon, heavy oil at the bottom of the tower, hydrogen supply fraction and raw materials for subsequent hydrorefining by a hot high fraction, a cold low fraction, a flash tower and a reduced pressure fractionating tower.
The reaction material from the top of the hydrogen-hydrogenation reactor is subjected to hot high-temperature separation, cold high-temperature separation and cold low-temperature separation to obtain hydrogen and light hydrocarbon components, and the hot high-temperature separation, cold high-temperature separation and cold low-temperature separation are mature processes for separating the hydrogen and the light hydrocarbon components by a high-pressure hydrogenation process.
The material from the bottom of the hot high fraction enters a flash tower, light fraction is flashed from the top of the flash tower, all or part of the light fraction can be used as hydrogen supply fraction, or part or all of the light fraction can be combined with other materials to be used as a raw material for subsequent hydrofining, and the material from the bottom of the flash tower enters a vacuum fractionating tower.
The top of the vacuum fractionating tower is connected with a vacuum-pumping system, and a part or all of the reduced line distilled from the side line of the vacuum fractionating tower can be used as a hydrogen supply fraction, and can also be combined with other fractions to be used as a raw material for subsequent hydrofining; the second-line-reduced fraction distilled from the side line of the vacuum fractionating tower is combined with other fractions to be used as a raw material for subsequent hydrofining; and (4) heavy oil discharging device at the bottom of the reduced pressure fractionating tower.
And (4) enabling the bottom material of the cold high fraction to enter a cold low fraction, and combining the bottom material of the cold low fraction with other materials to be used as a raw material for subsequent hydrofining. FIG. 1 is a process flow of the process of the present invention.
The specific data of the embodiment of the invention are shown in the following tables 1 and 2. The items in the table include the main process conditions of the hydrogen-hydrogenation pretreatment, the feed yield of the hydrogen-hydrogenation pretreated product used for hydrofining, and the main harmful impurities of the waste lubricating oil hydroregeneration refining device. The implementation case results show that the effect of removing the main harmful impurities of hydrofining is good after the waste lubricating oil is pretreated by hydrogen-hydrogen, the impurities which pollute the hydrofining catalyst and block a bed layer are basically removed, and the long-period operation of a hydrogenation device can be ensured.
Table 1 implementation of hydrogen-supplying pretreatment process for waste lubricant oil and experimental case two
Table 2 implementation of pretreatment process for hydrogenation of waste lubricant oil in presence of hydrogen and experimental case four
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not intended to limit the present invention in any way, and all simple modifications, equivalent variations and modifications made to the above embodiments according to the technical spirit of the present invention are within the scope of the present invention.
Claims (6)
1. A spent lubricating oil hydrogenation regeneration pretreatment method is characterized in that:
(1) the waste lubricating oil is firstly subjected to sedimentation in a sedimentation tank to remove most of water and large-particle mechanical impurities, and then is filtered by a filter to remove small-particle mechanical impurities, so that the obtained dehydrated offline mechanical impurity waste lubricating oil is mixed with hydrogen and hydrogen supply fractions, enters a heating furnace for heating and then enters a hydrogen-hydrogen supply reactor for reaction, or is mixed with the hydrogen and the hydrogen supply fractions from the outlet of the heating furnace and enters the hydrogen-hydrogen supply reactor for reaction;
(2) the reaction material coming out from the top of the hydrogen hydrogenation reactor is separated into hydrogen, light hydrocarbon, heavy oil at the bottom of the tower, hydrogen supply fraction and raw materials for subsequent hydrorefining by a hot high fraction, a cold low fraction, a flash tower and a reduced pressure fractionating tower.
2. The spent lubricating oil hydroregeneration pretreatment method according to claim 1, characterized in that: the process is a pre-pretreatment part of the waste lubricating oil hydrogenation regeneration process, and hydrogen is derived from a waste lubricating oil hydrogenation regeneration device, so that the hydrogen does not need to be separately provided for the waste lubricating oil hydrogenation regeneration pretreatment device.
3. The spent lubricating oil hydroregeneration pretreatment method according to claim 1, characterized in that: the operating conditions of the hydrogen hydrogenation reactor are that the reaction pressure is 5-15 MPa, the reaction temperature is 300-420 ℃, and the space velocity is 0.2-2.0 hr-1。
4. The spent lubricating oil hydroregeneration pretreatment method according to claim 1, characterized in that: the feed to the heating furnace can be a mixture of hydrogen and a hydrogen supply fraction, and can also be a mixture of hydrogen, a hydrogen supply fraction and waste lubricating oil which is completely or partially dehydrated and subjected to mechanical impurity removal.
5. The spent lubricating oil hydroregeneration pretreatment method according to claim 1, characterized in that: the hydrogen supply fraction is determined by laboratory test hydrogen supply capacity, and is derived from all fractions or partial fractions at the top of the flash tower, or all fractions or partial fractions at the first line of the reduced pressure fractionating tower side line distillation, or a mixture of the top fractions of the flash tower and the first line of the reduced pressure fractionating tower side line distillation.
6. The spent lubricating oil hydroregeneration pretreatment method according to claim 1, characterized in that: and the side line of the reduced pressure fractionating tower distills all or part of the first-line-reduced fraction, all materials of the second-line-reduced fraction, all or part of materials at the top of the flash tower and the materials at the bottom of the cold low fraction, and the combined materials are used as the feed of the regeneration device of the waste lubricating oil hydrogenation method.
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Citations (7)
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| CN101041789A (en) * | 2007-04-30 | 2007-09-26 | 京福马(北京)石油化工高新技术有限公司 | Waste lubricating oil hydrogenation reproducing method |
| CN107267198A (en) * | 2017-08-11 | 2017-10-20 | 南京康鑫成生物科技有限公司 | A kind of method that waste lubricating oil liquid-phase hydrogenatin prepares lube base oil |
| CN107325839A (en) * | 2017-07-12 | 2017-11-07 | 宁波中循环保科技有限公司 | Method for regenerating waste lubricating oil |
| CN107892990A (en) * | 2017-11-14 | 2018-04-10 | 新疆聚力环保科技有限公司 | A kind of method of waste mineral oil perhydro type regeneration production top-grade lubricating oil base oil |
| CN108130129A (en) * | 2018-02-13 | 2018-06-08 | 新疆聚力环保科技有限公司 | Waste mineral oil two-stage hydrogenation handles regeneration technology and method for preparing catalyst |
| CN108251156A (en) * | 2018-01-31 | 2018-07-06 | 新疆聚力环保科技有限公司 | A kind of method of full fraction waste mineral oil two-stage hydrogenation processing regeneration technology |
| CN110041963A (en) * | 2019-04-22 | 2019-07-23 | 中国科学院青岛生物能源与过程研究所 | A kind of technique of waste mineral oil homogeneous hydrogenation pretreatment and dechlorination |
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2019
- 2019-10-08 CN CN201910949462.0A patent/CN110791317B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101041789A (en) * | 2007-04-30 | 2007-09-26 | 京福马(北京)石油化工高新技术有限公司 | Waste lubricating oil hydrogenation reproducing method |
| CN107325839A (en) * | 2017-07-12 | 2017-11-07 | 宁波中循环保科技有限公司 | Method for regenerating waste lubricating oil |
| CN107267198A (en) * | 2017-08-11 | 2017-10-20 | 南京康鑫成生物科技有限公司 | A kind of method that waste lubricating oil liquid-phase hydrogenatin prepares lube base oil |
| CN107892990A (en) * | 2017-11-14 | 2018-04-10 | 新疆聚力环保科技有限公司 | A kind of method of waste mineral oil perhydro type regeneration production top-grade lubricating oil base oil |
| CN108251156A (en) * | 2018-01-31 | 2018-07-06 | 新疆聚力环保科技有限公司 | A kind of method of full fraction waste mineral oil two-stage hydrogenation processing regeneration technology |
| CN108130129A (en) * | 2018-02-13 | 2018-06-08 | 新疆聚力环保科技有限公司 | Waste mineral oil two-stage hydrogenation handles regeneration technology and method for preparing catalyst |
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