CN111876197A - Pretreatment process for treating waste lubricating oil by chemical refining method - Google Patents
Pretreatment process for treating waste lubricating oil by chemical refining method Download PDFInfo
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- CN111876197A CN111876197A CN202010735013.9A CN202010735013A CN111876197A CN 111876197 A CN111876197 A CN 111876197A CN 202010735013 A CN202010735013 A CN 202010735013A CN 111876197 A CN111876197 A CN 111876197A
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- lubricating oil
- waste lubricating
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- reactor
- heat treatment
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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
- C10G53/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
- C10G53/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
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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
Abstract
The invention provides a pretreatment process for treating waste lubricating oil by a chemical refining method, which comprises the steps of chemical demetallization, heat treatment, thin film evaporation and post-heat treatment. The waste lubricating oil and diammonium hydrogen phosphate solution are mixed and then enter a three-stage serial chemical demetallization process, the dehydration and light oil removal are completed while chemical demetallization is performed, then the demetallized waste lubricating oil enters a heat treatment device, the waste lubricating oil after heat treatment enters a thin film evaporation device, a base oil fraction is distilled out, the obtained base oil fraction is subjected to low-temperature heat treatment once again to obtain the high-quality hydrogenation raw material, the sulfated ash content in the base oil fraction is reduced to 0.01%, and the removal rate of metal impurities can reach more than 99%.
Description
Technical Field
The invention belongs to the technical field of regenerated base oil of waste lubricating oil, and relates to a pretreatment process for treating waste lubricating oil by a chemical refining method.
Background
The lubricating oil additive is a mixture of several single agents which are mixed according to a certain proportion and a blending technology and can meet the requirements of a certain quality grade, and the performance and the service life of the lubricating oil are determined. These additives are usually of the metal salt type and contain heavy metals such as barium, calcium, lead, zinc and the like. Due to the existence of the heavy metals, no matter the traditional adsorption refining process is adopted, or the processes such as film evaporation, molecular distillation, solvent refining, hydrorefining and the like are adopted, so that the phenomena of furnace tube coking, heat exchanger blockage, serious coking of a fractionating tower plate, unclear interface during solvent refining, reactor blockage and catalyst coking inactivation during hydrogenation are easy to occur in the regeneration process of the waste lubricating oil, and the difficulty of regenerating the base oil by the waste lubricating oil is increased.
Therefore, the process technology for regenerating the base oil by using the waste lubricating oil widely adopted in China at present still has the problems of unstable process technology, short start-up period, high unit energy consumption, high operation cost, limited treatment capacity, serious secondary pollution, unstable quality of treated oil, low resource utilization degree and the like in the aspect of pretreatment process technology.
Disclosure of Invention
The invention aims to provide a pretreatment process for treating waste lubricating oil by a chemical refining method, which can effectively remove heavy metal organic matters in the waste lubricating oil, remove colloids, asphaltine and other undesirable components in the waste lubricating oil and provide high-quality raw materials for subsequent hydrorefining.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps of chemical demetallization, heat treatment, thin film evaporation and post heat treatment:
firstly, chemical demetallization: fully mixing the waste lubricating oil without any treatment with a diammonium hydrogen phosphate solution, then feeding the mixture into a first chemical demetallization reactor, reacting at the temperature of 85 ℃ and under normal pressure for 1.0 hour, and then feeding the mixture into a second chemical demetallization reactor; in a second chemical demetallization reactor, the materials react for 1.0h at the temperature of 130 ℃ and under normal pressure, and simultaneously, water and light oil are evaporated; heating the materials to 170 ℃, entering a third chemical demetallization reactor, reacting for 1.0h under normal pressure, and evaporating out residual moisture and light oil.
And (2) heat treatment: and heating the waste lubricating oil from the third chemical demetallization reactor to 320-380 ℃, and then reacting in a heat treatment reactor for 0.5-2.0 h, wherein the operating pressure of the reactor is 0.8 MPa.
Thin film evaporation: and (3) after heat exchange, the heat-treated waste lubricating oil enters a wiped film evaporator, and under the operating conditions that the pressure is 100-140 Pa and the temperature is 300-340 ℃, colloid, asphaltene, metal organic additives, metal salts and the like in the waste lubricating oil are left in the distillation residues and separated from the base oil.
Fourthly, performing post-heat treatment: and exchanging heat of the distilled base oil fraction by a heat exchanger to 140-180 ℃, then feeding the base oil fraction into a post-heat treatment reactor, performing low-temperature heat treatment for 24-72 hours, and filtering by adopting a 10-micron automatic back-flushing filter, and then feeding the base oil fraction into a subsequent hydrofining device.
The invention has the advantages that:
the concentration of the diammonium phosphate aqueous solution is allowed to change in a large range, so that the waste lubricating oil can enter a chemical demetallization process without dehydration and impurity removal, and the process flow is simplified.
The additive and heat-sensitive substances in the waste lubricating oil can be effectively destroyed by chemical demetallization and heat treatment, and the removal rate of metals in the waste lubricating oil can reach more than 99 percent.
The wiped film evaporator has the advantages of low evaporation temperature, high mass transfer efficiency, short retention time and large evaporation capacity, cracking is reduced, and the recovery rate of the base oil is improved.
The post-heat treatment can further destroy residual additives or decomposition products thereof and substances generating heat precipitation so as to avoid reactor blockage and catalyst coking and deactivation during hydrogenation.
Drawings
FIG. 1 is a block diagram of a process flow of the present invention.
In the figure, 1 is a raw material tank, 2 is a first chemical demetallization reactor, 3 is a second chemical demetallization reactor, 4 is a third chemical demetallization reactor, 5 is a heat treatment reactor, 6 is a wiped film evaporator, and 7 is a post heat treatment reactor.
Detailed Description
The invention discloses a pretreatment process for treating waste lubricating oil by a chemical refining method, and the process flow of the invention is clearly and completely described by combining the attached drawings of the invention.
Example 1
As shown in fig. 1, the waste lubricating oil in the raw material tank 1 is fully mixed with a diammonium hydrogen phosphate solution, enters a first chemical demetallization reactor 2, reacts at 85 ℃ and normal pressure for 1.0 hour, and then enters a second chemical demetallization reactor 3 through heat exchange; the materials react for 1.0h at the temperature of 130 ℃ and under normal pressure, and simultaneously, moisture and light oil are evaporated from the chemical demetallization second reactor 3; then the materials are heated to 170 ℃ and enter a third chemical demetallization reactor 4 to react for 1.0 hour under normal pressure, and residual moisture and light oil are evaporated; heating the waste lubricating oil discharged from the third chemical demetallization reactor 4 to 380 ℃, and then entering the heat treatment reactor 5 for reaction for 0.5 h; the heat-treated waste lubricating oil enters a wiped film evaporator 6 after heat exchange, and colloid, asphaltene, metal organic additives, metal salts and the like in the waste lubricating oil are left in distillation residues and separated from the base oil under the operating conditions of the pressure of 100Pa and the temperature of 300 ℃. And exchanging heat of the distilled base oil fraction by a heat exchanger to 160 ℃, then feeding the base oil fraction into a post-heat treatment reactor 7, performing low-temperature heat treatment for 48 hours, and filtering to obtain the base oil fraction which can be fed into a subsequent hydrofining device.
Example 2
As shown in fig. 1, the waste lubricating oil in the raw material tank 1 is fully mixed with a diammonium hydrogen phosphate solution, enters a first chemical demetallization reactor 2, reacts at 85 ℃ and normal pressure for 1.0 hour, and then enters a second chemical demetallization reactor 3 through heat exchange; the materials react for 1.0h at the temperature of 130 ℃ and under normal pressure, and simultaneously, moisture and light oil are evaporated from the chemical demetallization second reactor 3; then the materials are heated to 170 ℃ and enter a third chemical demetallization reactor 4 to react for 1.0 hour under normal pressure, and residual moisture and light oil are evaporated; heating the waste lubricating oil discharged from the third chemical demetallization reactor 4 to 345 ℃, and then reacting in a heat treatment reactor 5 for 1.5 h; the heat-treated waste lubricating oil enters a wiped film evaporator 6 after heat exchange, and colloid, asphaltene, metal organic additives, metal salts and the like in the waste lubricating oil are left in distillation residues and separated from base oil under the operating conditions that the pressure is 140Pa and the temperature is 340 ℃. And exchanging heat of the distilled base oil fraction by a heat exchanger to 140 ℃, then feeding the base oil fraction into a post-heat treatment reactor 7, performing low-temperature heat treatment for 72 hours, and filtering the base oil fraction to obtain the subsequent hydrorefining device.
Example 3
As shown in fig. 1, the waste lubricating oil in the raw material tank 1 is fully mixed with a diammonium hydrogen phosphate solution, enters a first chemical demetallization reactor 2, reacts at 85 ℃ and normal pressure for 1.0 hour, and then enters a second chemical demetallization reactor 3 through heat exchange; the materials react for 1.0h at the temperature of 130 ℃ and under normal pressure, and simultaneously, moisture and light oil are evaporated from the chemical demetallization second reactor 3; then the materials are heated to 170 ℃ and enter a third chemical demetallization reactor 4 to react for 1.0 hour under normal pressure, and residual moisture and light oil are evaporated; heating the waste lubricating oil discharged from the third chemical demetallization reactor 4 to 320 ℃, and then entering the heat treatment reactor 5 for reaction for 2.0 hours; the heat-treated waste lubricating oil enters a wiped film evaporator 6 after heat exchange, and colloid, asphaltene, metal organic additives, metal salts and the like in the waste lubricating oil are left in distillation residues and separated from the base oil under the operating conditions that the pressure is 120Pa and the temperature is 320 ℃. And exchanging heat of the distilled base oil fraction by a heat exchanger to 180 ℃, then feeding the base oil fraction into a post-heat treatment reactor 7, performing low-temperature heat treatment for 24 hours, and filtering the base oil fraction to obtain the base oil fraction which can be fed into a subsequent hydrofining device.
Table 1 shows the properties of the used lubricating oil feedstock and its demetallized oil
Claims (7)
1. A pretreatment process for treating waste lubricating oil by a chemical refining method is characterized by comprising the steps of chemical demetallization, heat treatment, thin film evaporation and post-heat treatment, and specifically comprises the following steps:
mixing waste lubricating oil which is not subjected to any treatment with a diammonium hydrogen phosphate solution, sequentially feeding the mixed waste lubricating oil and diammonium hydrogen phosphate solution into three-stage chemical demetallization reactors connected in series, reacting for a period of time at different temperatures and pressures, and condensing and separating water and light oil evaporated from a second reactor and a third reactor for chemical demetallization;
and secondly, heating the waste lubricating oil discharged from the third chemical demetallization reactor, then feeding the heated waste lubricating oil into a heat treatment reactor, treating the waste lubricating oil for a period of time, feeding the waste lubricating oil into a thin film evaporator, cooling the distilled base oil fraction, then feeding the base oil fraction into a post heat treatment reactor, treating the base oil fraction at a certain temperature for a period of time, and filtering the base oil fraction to obtain the high-quality hydrogenation raw material.
2. The pretreatment process for treating waste lubricating oil by a chemical refining method according to claim 1, characterized in that the operation conditions of the three-stage tandem chemical demetallization reactor in the step are as follows: mixing the waste lubricating oil with a diammonium hydrogen phosphate solution, then feeding the mixture into a first chemical demetallization reactor, reacting at the temperature of 85 ℃ and under normal pressure for 1.0h, and then feeding the mixture into a second chemical demetallization reactor; in a second chemical demetallization reactor, the materials react for 1.0h at the temperature of 130 ℃ and under normal pressure, and simultaneously, water and light oil are evaporated; heating the materials to 170 ℃, entering a third chemical demetallization reactor, reacting for 1.0h under normal pressure, and evaporating out residual moisture and light oil.
3. The pretreatment process for treating waste lubricating oil by a chemical refining method according to claim 1, characterized in that moisture and light oil evaporated by the second and third reactors for chemical demetallization in the step of the pretreatment are introduced into a same condenser to be condensed and then enter a gas-liquid separator for separation, the exhaust gas is sent to a boiler for combustion, and the light oil is used as fuel.
4. The pretreatment process for treating the waste lubricating oil by the chemical refining method according to claim 1, characterized in that the operation conditions of the thermal treatment reactor in the second step are as follows: the reaction pressure is 0.8MPa, the reaction temperature is 320-380 ℃, and the reaction time is 0.5-2.0 h.
5. The pretreatment process for treating the waste lubricating oil by the chemical refining method according to claim 1, characterized in that the thin film evaporator is a wiped film evaporator, and the operation conditions are as follows: the pressure is 100-140 Pa and the temperature is 300-340 ℃.
6. The pretreatment process for treating the waste lubricating oil by the chemical refining method according to claim 1, characterized in that the steps are as follows: the temperature is 140-180 ℃, and the reaction time is 24-72 h.
7. The pretreatment process for treating the waste lubricating oil by the chemical refining method according to claim 1, characterized in that the filtering in the step II is a 10-micron automatic backwashing filter.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113969209A (en) * | 2021-11-08 | 2022-01-25 | 湖北润驰环保科技有限公司 | Process for removing impurities and improving quality of waste lubricating oil through full-fraction hydrogen pretreatment |
Citations (6)
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|---|---|---|---|---|
| US4360420A (en) * | 1980-10-28 | 1982-11-23 | Delta Central Refining, Inc. | Distillation and solvent extraction process for rerefining used lubricating oil |
| CN1871330A (en) * | 2003-09-23 | 2006-11-29 | 西耐尔工程集团有限公司 | Used oil regeneration method involving stripping and distillation |
| CN101173202A (en) * | 2006-11-01 | 2008-05-07 | 中国石油化工股份有限公司 | Waste lubricant oil recovery utilization method |
| CN102260584A (en) * | 2011-06-24 | 2011-11-30 | 上海宝钢废旧油处理有限公司 | Industrial waste lubricating oil regeneration process |
| CN109679760A (en) * | 2018-12-11 | 2019-04-26 | 中国石油大学(华东) | A kind of pretreated demetalization-centrifugation-extraction combined technical method of waste lubricating oil |
| CN109868180A (en) * | 2019-04-23 | 2019-06-11 | 湖北润驰环保科技有限公司 | A kind of pretreating process of the waste lubricating oil cyclic regeneration of environmental protection |
-
2020
- 2020-07-28 CN CN202010735013.9A patent/CN111876197A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4360420A (en) * | 1980-10-28 | 1982-11-23 | Delta Central Refining, Inc. | Distillation and solvent extraction process for rerefining used lubricating oil |
| CN1871330A (en) * | 2003-09-23 | 2006-11-29 | 西耐尔工程集团有限公司 | Used oil regeneration method involving stripping and distillation |
| CN101173202A (en) * | 2006-11-01 | 2008-05-07 | 中国石油化工股份有限公司 | Waste lubricant oil recovery utilization method |
| CN102260584A (en) * | 2011-06-24 | 2011-11-30 | 上海宝钢废旧油处理有限公司 | Industrial waste lubricating oil regeneration process |
| CN109679760A (en) * | 2018-12-11 | 2019-04-26 | 中国石油大学(华东) | A kind of pretreated demetalization-centrifugation-extraction combined technical method of waste lubricating oil |
| CN109868180A (en) * | 2019-04-23 | 2019-06-11 | 湖北润驰环保科技有限公司 | A kind of pretreating process of the waste lubricating oil cyclic regeneration of environmental protection |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113969209A (en) * | 2021-11-08 | 2022-01-25 | 湖北润驰环保科技有限公司 | Process for removing impurities and improving quality of waste lubricating oil through full-fraction hydrogen pretreatment |
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