CN117903835A - Solvent separation and recovery process of vinyl lubricating oil base oil - Google Patents
Solvent separation and recovery process of vinyl lubricating oil base oil Download PDFInfo
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- CN117903835A CN117903835A CN202211281777.0A CN202211281777A CN117903835A CN 117903835 A CN117903835 A CN 117903835A CN 202211281777 A CN202211281777 A CN 202211281777A CN 117903835 A CN117903835 A CN 117903835A
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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
- C10G7/00—Distillation of hydrocarbon oils
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Abstract
本发明公开了一种乙烯基润滑油基础油的溶剂分离回收工艺，包括以下步骤：步骤S1、反应液经脱溶单元得到有机溶剂蒸汽和粗油：步骤S2、有机溶剂蒸汽经溶剂精馏单元得到精馏后溶剂：步骤S3、含有溶剂蒸汽的尾气经尾气冷凝回收单元得到所述尾气冷凝液和尾气不凝气：步骤S4、所述尾气不凝气经尾气吸附单元。本发明主要解决现有技术存在反应产物分离效果差，产品品质低、无法达到工业规模的问题。
The invention discloses a solvent separation and recovery process for vinyl lubricating oil base oil, comprising the following steps: step S1, the reaction liquid is subjected to a desolventizing unit to obtain organic solvent vapor and crude oil; step S2, the organic solvent vapor is subjected to a solvent distillation unit to obtain a distilled solvent; step S3, the tail gas containing the solvent vapor is subjected to a tail gas condensation recovery unit to obtain the tail gas condensate and tail gas non-condensable gas; step S4, the tail gas non-condensable gas is subjected to a tail gas adsorption unit. The invention mainly solves the problems that the prior art has poor separation effect of reaction products, low product quality, and cannot reach industrial scale.
Description
Technical Field
The invention relates to the technical field of vinyl lubricating oil base oil, in particular to a solvent separation and recovery process of vinyl lubricating oil base oil.
Background
The base oils of industrial lubricants are obtained by petroleum cracking or alpha-olefin oligomerization. For example: the invention patent CN202010768868.1 discloses a system and a method for preparing high-grade lubricating oil mPAO, in particular to a method for preparing high-grade lubricating oil mPAO products by taking alpha-olefin as raw material. However, the current technology for selectively producing alpha-olefins above C6 is currently not mature, resulting in high prices.
In a new technical scheme provided by researchers in the field, high-performance base oil is directly prepared from low-cost olefins such as ethylene, propylene, butylene and the like, so that the preparation cost is greatly reduced. For example:
The invention patent CN201410555078.X discloses a novel polyolefin catalyst and a preparation technology thereof, in particular a catalytic system, which comprises a novel polyolefin: the iron, cobalt, nickel, palladium and platinum complexes can directly prepare oily hyperbranched polymers from simple olefins such as ethylene, propylene and butylene and polar olefins containing functional groups under the action of the catalyst through the regulation and control of the catalyst structure. However, the patent is directed only to producing a hydrogenated oily alkane mixture, and is not directed to a subsequent refining process and tail gas recovery process.
The invention patent CN201911032664.5 discloses a process method for directly synthesizing high-performance low-viscosity base oil by polymerization of low-carbon olefin, and discloses a process method for directly synthesizing high-performance low-viscosity base oil by polymerization of low-carbon olefin. The method comprises a plurality of procedures such as polymerization, hydrogenation, rectification and the like. The lubricant base oil with different basic physicochemical properties is prepared by adjusting the addition amount of different catalysts, the solvent amount and the change of reaction conditions. In addition, the invention patent CN201911032648.6 of the same applicant discloses a process method for directly synthesizing high-performance medium-viscosity base oil by polymerization of low-carbon olefin, and the invention patent CN201911032604.3 is a process method for directly synthesizing high-performance high-viscosity base oil by polymerization of low-carbon olefin.
However, the invention patents CN201911032664.5, CN201911032648.6, CN201911032604.3 are only methods for batch preparation of lubricating base oils on a laboratory scale, nor involve recovery of solvents and treatment of exhaust gases.
Disclosure of Invention
The invention provides a solvent separation and recovery process for vinyl lubricating oil base oil, which mainly solves the problems of poor separation effect of reaction products, low product quality and incapability of achieving industrial scale in the prior art.
A solvent separation and recovery process of vinyl lubricating oil base oil comprises the following steps:
Step S1, obtaining organic solvent steam and crude oil from the reaction liquid through a desolventizing unit:
The reaction liquid and/or tail gas condensate enters a climbing film evaporator for heating, and then enters a steam separation tank for separation to obtain organic solvent steam and crude oil;
step S2, the organic solvent vapor is subjected to solvent rectification to obtain a rectified solvent:
the organic solvent steam enters a rectifying tower to be rectified, tower bottom liquid is cooled by a rectifying tower bottom cooler and then is pumped to a rectified solvent storage tank by a rectifying tower bottom liquid pump;
Step S3, obtaining the tail gas condensate and the tail gas noncondensable gas by a tail gas condensation recovery unit from the tail gas containing solvent vapor:
the tail gas containing solvent vapor is condensed by a first-stage tail gas condenser and a second-stage tail gas condenser in sequence, and the condensed tail gas condensate is respectively collected in a first condensate receiving tank and a second condensate receiving tank;
step S4, enabling the tail gas noncondensable gas to pass through a tail gas adsorption unit:
The tail gas noncondensable gas enters a tail gas adsorption tower, and a very small amount of solvent which is not condensed is adsorbed, so that the tail gas noncondensable gas reaches the emission standard and is discharged to the atmosphere.
Preferably, in step S1, a part of the crude oil enters a climbing film evaporator through an evaporator circulating pump to be mixed with the reaction liquid, circulated, evaporated and desolventized, and the other part enters a stripping tower, wherein nitrogen is introduced into the tower bottom of the stripping tower, the top of the stripping tower is vacuumized, the trace organic solvent in the crude oil is deeply removed, and the top gas of the stripping tower is cooled by a cooler and then reaches a trace organic solvent storage tank.
Preferably, in step S2, the operation temperature of the rectifying tower is between-10 and 120 ℃, and the pressure is between ATM and 0.35MpaG.
Preferably, in step S2, the top gas of the rectifying tower flows back to the rectifying tower after passing through a rectifying tower top cooler and a top liquid storage tank.
Preferably, in step S2, the organic solvent vapor is fed from the bottom of the rectifying column.
Preferably, the non-condensable gas at the top of the rectifying tower directly enters the tail gas incineration system.
Preferably, in the step S2, the tower bottom liquid of the rectifying tower is cooled to 10-40 ℃ through a tower bottom cooler of the rectifying tower.
Preferably, in step S3, the tail gas containing solvent vapor includes one or more of main catalyst preparation tail gas, cocatalyst preparation tail gas, dichloromethane temporary storage tail gas, polymerization reaction tail gas, quenching unit tail gas and stripping tail gas.
Preferably, in step S3, the cooling liquid of the primary tail gas condenser is a cooling liquid of-30 ℃.
Preferably, in step S3, the coolant of the secondary tail gas condenser is a circulating working fluid from the TCU cryorefrigeration system.
Preferably, in the step S3, the operation temperature of the primary tail gas condenser is-20-30 ℃, the operation temperature of the secondary tail gas condenser is-90-20 ℃, and the operation pressure is-0.05-0.1 MpaG.
Compared with the prior art, the invention has the following technical effects:
(1) The invention provides a solvent separation and recovery method of vinyl lubricating oil base oil, which greatly improves the solvent recovery rate, solves the problem that harmful substances such as dioxin and phosgene are generated after the traditional halogen-containing materials are directly combusted, and realizes the continuous separation and recovery of halogen-containing organic solvents in the vinyl lubricating oil base oil.
(2) The process provided by the invention is a continuous industrialized separation and recovery process, and can realize stable and convenient production operation on an industrial scale.
(3) The invention adopts a combination system of molecular distillation, rectification and cold energy coupling, condensation and adsorption separation aiming at the solvent property and product property of the vinyl lubricating oil base oil, and realizes high recovery rate of the solvent through adjustment of various parameters.
(4) The invention can realize stable production operation under the industrial production scale of 1000-100000 tons/year.
Drawings
FIG. 1 is a flow chart of a method for separating and recovering solvent of a vinyl lubricant base oil according to the present invention;
The reference symbols in the drawings indicate the description:
10-desolventizing unit, 11-liter membrane evaporator, 12-steam separating tank, 13-evaporator circulating pump, 14-stripping tower, 15-cooler, 16-trace organic solvent storage tank,
20-Solvent rectification unit, 21-rectification tower, 22-rectification tower bottom cooler, 23-rectification tower bottom liquid pump, 24-rectification solvent storage tank, 25-rectification tower top cooler, 26-tower top liquid storage tank,
30-Tail gas condensation recovery unit, 31-first-stage tail gas condenser, 32-second-stage tail gas condenser, 33-first condensate receiving tank, 34-second condensate receiving tank, 35-TCU low-temperature refrigeration system,
40-Tail gas adsorption unit, 41-tail gas adsorption tower.
Detailed Description
The invention relates to a process for separating and recovering halogen-containing organic solvents in a process for preparing vinyl lubricating oil base oil, which solves the technical problems that: 1. the method solves the problem of industrial continuous recovery of the halogen-containing organic solvent, and solves the problem of direct combustion of tail gas of the halogen-containing organic solvent to produce harmful substances such as dioxin, phosgene and the like in the prior art.
In view of the above problems, the present invention provides a solvent separation and recovery process for vinyl lubricant base oil, as shown in fig. 1, specifically, the process comprises the following steps:
Step S1: the reaction solution is subjected to a desolventizing unit 10 to obtain organic solvent vapor and crude oil.
Specifically, the reaction liquid from the reaction kettle and/or the tail gas condensate from the tail gas condensation recovery unit 30 enter the climbing film evaporator 11 for heating, then enter the steam separation tank 12, and are separated to obtain the organic solvent steam and the crude oil.
In one embodiment, the crude oil is pumped to the climbing film evaporator 11 through the evaporator circulating pump 13, and is mixed with the reaction liquid and the tail gas condensate for circulation, evaporation and desolventizing.
In another embodiment, the crude oil enters a stripping tower 14, wherein nitrogen is introduced into the tower bottom of the stripping tower 14, the tower top of the stripping tower 14 is vacuumized, trace organic solvent in the crude oil is deeply removed, and the tower top gas of the stripping tower 14 is cooled by a cooler 15 and then reaches a trace organic solvent storage tank 16.
In a preferred embodiment, part of crude oil is pumped to the climbing film evaporator 11 through the evaporator circulating pump 13 to be mixed with the reaction liquid and the tail gas condensate for circulation evaporation and desolventizing; and the other part of the crude oil enters a stripping tower 14, nitrogen is introduced into the tower bottom of the stripping tower 14, the tower top of the stripping tower 14 is vacuumized, trace organic solvent in the crude oil is deeply removed, and the tower top gas of the stripping tower 14 is cooled by a cooler 15 and then reaches a trace organic solvent storage tank 16.
Step S2: the organic solvent vapor is subjected to solvent rectification by a solvent rectification unit 20 to obtain a rectified solvent;
Specifically, the organic solvent vapor enters the rectifying tower 21 from the bottom of the rectifying tower 21 for rectification, and the tower bottom liquid is cooled by a rectifying tower bottom cooler 22 and then pumped to a rectified solvent storage tank 24 by a rectifying tower bottom liquid pump 23; the top gas of the rectifying tower 21 flows back to the rectifying tower 21 after passing through a rectifying tower top cooler 25 and a tower top liquid storage tank 26, and the non-condensable gas at the top of the rectifying tower 21 directly enters a tail gas incineration system.
In a preferred embodiment, the rectification column 21 is operated at a temperature of-10 to 120℃and a pressure of ATM to 0.35MpaG.
In a preferred embodiment, in step S2, the bottom liquid of the rectifying tower 21 is cooled to 10-40 ℃ by a bottom cooler of the rectifying tower; further, cooling to 20 ℃.
Step S3: the tail gas containing solvent vapor is subjected to a tail gas condensation recovery unit 30 to obtain the tail gas condensate and the tail gas noncondensable gas.
Specifically, the tail gas containing solvent vapor is condensed by a first-stage tail gas condenser 31 and a second-stage tail gas condenser 32 in sequence, and the condensed tail gas condensate is respectively collected in a first condensate receiving tank 33 and a second condensate receiving tank 34; specifically, the tail gas containing solvent vapor comprises one or more of main catalyst preparation tail gas, cocatalyst preparation tail gas, dichloromethane temporary storage tail gas, polymerization reaction tail gas, quenching unit tail gas and stripping tail gas.
In one embodiment, in step S3, the cooling fluid of the primary tail gas condenser 31 is a cooling fluid at-30 ℃.
In a preferred embodiment, in step S3, the coolant of the secondary tail gas condenser 32 is recycled working fluid from the TCU cryorefrigeration system 35.
Step S4: the tail gas noncondensable gas passes through a tail gas adsorption unit 40;
The tail gas noncondensable gas enters the tail gas adsorption tower 41, and a very small amount of solvent which is not condensed is adsorbed, so that the tail gas noncondensable gas reaches the emission standard and is discharged to the atmosphere.
In a preferred embodiment, the cooling medium of the secondary tail gas condenser can be prepared from low-temperature ethylene, liquid nitrogen, liquid ammonia and the like existing in a factory, so that the vaporization of the low-temperature medium is realized while the solvent is recovered, and the cold coupling is completed.
The present invention will be described in detail and in detail by way of the following examples, which are not intended to limit the scope of the invention, for better understanding of the invention.
Example 1
Step S1, the reaction liquid passes through a desolventizing unit 10 to obtain organic solvent steam and crude oil:
Quantitatively feeding the reaction liquid (the mass fraction CH 2Cl2 wt%, the LPE-44.3wt%, the LPE-4013wt% and the other light hydrocarbons 0.7%) into a climbing film evaporator 11 to heat to 100 ℃, then feeding the reaction liquid into a steam separation tank 12, and feeding the separated organic solvent steam into a solvent rectifying unit 20; and (3) continuously feeding a part of crude oil after preliminary desolventizing into a climbing film evaporator 11 through an evaporator circulating pump 13 to be mixed with reaction liquid, circularly evaporating for desolventizing, feeding the other part of crude oil into a stripping tower 14, introducing nitrogen into a tower kettle, vacuumizing the tower top, deeply removing trace methylene dichloride solvent in the oil, and cooling the tower top gas of the stripping tower 14 through a cooler 15 to reach a trace organic solvent storage tank 16.
Step S2, the organic solvent steam is subjected to solvent rectification by a solvent rectification unit 20 to obtain a rectified solvent:
Methylene dichloride steam (CH 2Cl2 98.7.7wt%; other light hydrocarbons 1.3wt%) from the desolventizing process 10 directly enters a rectifying tower 21 for rectification, tower bottom feeding is adopted, tower top non-condensable gas directly enters a tail gas incineration system, tower bottom liquid is cooled to 25 ℃ through a rectifying tower bottom cooler 22 and then pumped to a rectified methylene dichloride storage tank 24 through a rectifying tower bottom liquid pump 23, the operation temperature of the process system is-10-120 ℃, and the pressure is ATM-0.35MpaG;
Step S3: the tail gas containing solvent vapor is subjected to a tail gas condensation recovery unit 30 to obtain tail gas condensate and tail gas noncondensable gas;
The tail gas containing dichloromethane vapor (including main catalyst preparation tail gas, cocatalyst preparation tail gas, dichloromethane temporary storage tail gas, polymerization tail gas, quenching unit tail gas and stripping tail gas, and one or more of supplementing dichloromethane tail gas) is combined and sequentially enters a primary tail gas condenser 31 and a secondary tail gas condenser 32, the condensed dichloromethane is respectively collected in a first condensate receiving tank 33 and a second condensate receiving tank 34, and the tail gas condensate and the reaction liquid are converged and enter a climbing film evaporator 11. Wherein the cooling liquid of the first-stage tail gas condenser 31 is cooling liquid at-30 ℃; the coolant from the secondary tail gas condenser 32 is the circulating working fluid from the TCU cryorefrigeration system 35. The operation temperature of the primary tail gas condenser is-20 to 30 ℃, the operation temperature of the secondary tail gas condenser is-90 to-20 ℃, and the pressure is-0.05 to 0.1MpaG.
Step S4: the tail gas noncondensable gas passes through a tail gas adsorption unit 40;
the tail gas containing solvent vapor is condensed by the first-stage tail gas condenser 31 and the second-stage tail gas condenser 32 in sequence, the generated tail gas noncondensable gas enters the tail gas adsorption tower 41, and the little uncondensed methylene dichloride reaches the emission standard after being adsorbed and is discharged to the atmosphere.
The above description of the specific embodiments of the present invention has been given by way of example only, and the present invention is not limited to the above described specific embodiments. Any equivalent modifications and substitutions for the present invention will occur to those skilled in the art, and are also within the scope of the present invention. Accordingly, equivalent changes and modifications are intended to be included within the scope of the present invention without departing from the spirit and scope thereof.
Claims (10)
1. The solvent separation and recovery process of the vinyl lubricating oil base oil is characterized by comprising the following steps of:
Step S1, obtaining organic solvent steam and crude oil from the reaction liquid through a desolventizing unit:
The reaction liquid and/or tail gas condensate enters a climbing film evaporator for heating, and then enters a steam separation tank for separation to obtain organic solvent steam and crude oil;
step S2, the organic solvent vapor is subjected to solvent rectification to obtain a rectified solvent:
the organic solvent steam enters a rectifying tower to be rectified, tower bottom liquid is cooled by a rectifying tower bottom cooler and then is pumped to a rectified solvent storage tank by a rectifying tower bottom liquid pump;
Step S3, obtaining the tail gas condensate and the tail gas noncondensable gas by a tail gas condensation recovery unit from the tail gas containing solvent vapor:
the tail gas containing solvent vapor is condensed by a first-stage tail gas condenser and a second-stage tail gas condenser in sequence, and the condensed tail gas condensate is respectively collected in a first condensate receiving tank and a second condensate receiving tank;
step S4, enabling the tail gas noncondensable gas to pass through a tail gas adsorption unit:
The tail gas noncondensable gas enters a tail gas adsorption tower, and a very small amount of solvent which is not condensed is adsorbed, so that the tail gas noncondensable gas reaches the emission standard and is discharged to the atmosphere.
2. The process for separating and recovering solvent from vinyl lubricant base oil according to claim 1, wherein in step S1, a part of crude oil enters a climbing film evaporator through an evaporator circulating pump to be mixed, circulated, evaporated and desolventized with the reaction liquid, and the other part enters a stripping tower, wherein nitrogen is introduced into a tower bottom of the stripping tower, the top of the stripping tower is vacuumized, trace organic solvent in the crude oil is deeply removed, and the top gas of the stripping tower is cooled by a cooler and then reaches a trace organic solvent storage tank.
3. The process for separating and recovering a solvent from a base oil of a vinyl lubricant according to claim 1, wherein in step S2, the rectifying column is operated at a temperature of-10 to 120 ℃ and a pressure of ATM to 0.35 mpa.
4. The process for separating and recovering a solvent from a base oil of a vinyl lube oil according to claim 1 wherein in step S2, the top gas of the rectifying column is returned to the rectifying column through a rectifying column top cooler and a top liquid tank.
5. The process for solvent separation and recovery of a vinyl lube base oil according to claim 1 wherein in step S2, the organic solvent vapor is fed from the bottom of the rectifying column.
6. The process for solvent separation and recovery of a vinyl lube base oil according to claim 1 wherein the non-condensable gas at the top of the rectifying tower directly enters the tail gas incineration system.
7. The process for separating and recovering a solvent from a base oil of a vinyl lubricant according to claim 1, wherein in step S2, the bottom liquid of the rectifying column is cooled to 10 to 40 ℃ by a bottom cooler of the rectifying column.
8. The process for separating and recovering solvent from a base oil of a vinyl lubricant according to claim 1, wherein in step S3, the tail gas containing solvent vapor comprises one or more of main catalyst preparation tail gas, cocatalyst preparation tail gas, dichloromethane temporary storage tail gas, polymerization reaction tail gas, quenching unit tail gas and stripping tail gas.
9. The process for solvent separation and recovery of a vinyl lube base oil according to claim 1 wherein in step S3, the cooling liquid of the primary tail gas condenser is a cooling liquid of-30 ℃.
10. The process for solvent separation and recovery of a vinyl lube base oil according to claim 1 wherein in step S3 the cooling liquid of the secondary tail gas condenser is a circulating working liquid from a TCU cryogenic refrigeration system.
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| CN202211281777.0A CN117903835A (en) | 2022-10-19 | 2022-10-19 | Solvent separation and recovery process of vinyl lubricating oil base oil |
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| CN106132533A (en) * | 2014-01-06 | 2016-11-16 | 大林产业株式会社 | ethylene and alpha-olefin polymerization device and preparation method |
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| CN108218658A (en) * | 2018-03-20 | 2018-06-29 | 浙江省天正设计工程有限公司 | A kind of integrated acetylene recycle device and recovery process |
| CN111228837A (en) * | 2020-03-17 | 2020-06-05 | 上海森松制药设备工程有限公司 | Waste solvent recovery system and method |
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2022
- 2022-10-19 CN CN202211281777.0A patent/CN117903835A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106132533A (en) * | 2014-01-06 | 2016-11-16 | 大林产业株式会社 | ethylene and alpha-olefin polymerization device and preparation method |
| CN106833736A (en) * | 2017-03-29 | 2017-06-13 | 山东铂铠环保科技有限公司 | A kind of method of waste oil regeneration base oil |
| CN108218658A (en) * | 2018-03-20 | 2018-06-29 | 浙江省天正设计工程有限公司 | A kind of integrated acetylene recycle device and recovery process |
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