CN1188496C - Dewaxing solvent recovery process - Google Patents
Dewaxing solvent recovery process Download PDFInfo
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- CN1188496C CN1188496C CNB031134416A CN03113441A CN1188496C CN 1188496 C CN1188496 C CN 1188496C CN B031134416 A CNB031134416 A CN B031134416A CN 03113441 A CN03113441 A CN 03113441A CN 1188496 C CN1188496 C CN 1188496C
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- butanone
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Abstract
The present invention relates to a process for recovering lubrication oil dewaxing solvents, more specifically a process for recovering toluene-butanone solvents from water-containing dewaxing solvents which are stripped. The process comprises the steps that the water content of water-containing solvents is about 60% to 70% after single vaporization and oil removal; after heat is exchanged and temperature is raised, the water-containing solvents are pumped into a drying tower to separate out dried toluene and partial butanone solvents from the bottom of the drying tower; the water-containing solvents at the top of the drying tower is pumped into a water settling tank for settlement and delamination; toluene-butanone solvents at the upper layer of the water settling tank are dehydrated in a hydrophilic A-type inorganic molecular sieve membrane dehydration device and butanone is separated from water containing a small amount of butanone at the lower layer by an inorganic Silicalite hydrophobic molecular sieve membrane ketone-removing device; the separated water is recycled by a stripping tower or directly drained and dry solvents obtained by the separation of the two membrane devices are collected and recycled. The present invention uses a penetration vaporization technology to replace a traditional rectification technology and has the advantages of low energy consumption and simple operation technology and equipment.
Description
(technical field)
The present invention relates to a kind of technology of separating the purification solvent that from the dewaxing solvent of lubricating oil, reclaims, particularly from the water-containing solvent behind the lubricating oil dewaxing filtrate stripping, reclaim the technology of solvent.
(background technology)
In the petroleum industry, because lubricating oil component is close with wax component boiling point, the two is present in the same cut, and therefore dewaxing is a requisite operation in the lubricating oil processing process.Lubricating oil dewaxing need add insoluble or few molten butanone-toluene solvant to the oil dissolving and to wax, with the lubricating oil dissolved dilution in the cut, makes wax crystallization subsequently at low temperatures, refilters to separate and removes crystalline wax.Filtrate after the filtration needs butanone-toluene solvant Separation and Recovery is reused.Method commonly used is that the paraffin removal rear filtrate is come out solvent initial gross separation from lubricating oil by multistage flash evaporation, stripping, further purifies then.Because stripping process need feed a large amount of water vapour, therefore water is fully separated with solvent, be used further to dewaxing to reclaim dry solvent, isolated water is done stripping water or discharging.Usually require the recovered solvent water content less than 0.3wt%, butanone content is less than 0.02wt% in the water.
At present, the Separation and Recovery solvent adopts the single vaporization oil removing more from the water-containing solvent behind the dewaxed filtrate stripping, adopt a rectifying subsequently, isolate the dry solvent that toluene is the master at the bottom of tower, the cat head azeotrope is gone into after-fractionating tower through the sedimentation layering with the bottom water layer, separate water outlet, the top solvent layer is sent a rectifying tower back to and is separated, so repeatedly, makes water and separated from solvent at last.Owing to form azeotrope in the rectifying, so the required energy consumption of rectifying is big in this process, separation cycle is long, complicated operation, and solvent purity is difficult to reach requirement.
Summary of the invention)
The objective of the invention is to overcome existing rectificating method exists azeotrope to be difficult to isolating shortcoming, a kind of lubricating oil dewaxing solvent recovery process is provided, is guaranteeing to reduce the energy consumption in the water-containing solvent removal process under the qualified condition of water content, simplify the operation, improve the separation efficiency of water and solvent.
The inventive method comprises the steps:
Water-containing solvent behind the lubricating oil dewaxing filtrate stripping separated at the bottom of the tower through single vaporization remove oil content, cat head steams thing, and (moisture 60%～70wt%) heat exchange is gone into drying tower after heating up, and isolates toluene and part butanone dry solvent at the bottom of tower; The drying tower cat head is steamed thing pump into water slurry tank sedimentation layering, extract upper strata liquid, be heated to 60～120 ℃, it is sent into the molecular screen membrane dewatering unit, contained water is by film water vapour penetration, the side that sees through of film adopts vacuum take-off, and the water vapor cooling fluid that sees through dissolves device, reclaims to such an extent that seepage remaining liquid is dry butanone solvent; Extract the subnatant of slurry tank,, butanone solvent contained in the water is separated to deviate from and recovery by taking off the ketone step.
More than the said ketone step of taking off be: the subnatant of the slurry tank that extracts is heated to 30～60 ℃, send into the organic zeolite membrane deketo equipment, the side that sees through of film adopts vacuum take-off, butanone contained in the water gasifies by membrane permeation, isolate the gaseous state butanone, to reclaim after its cooling liquid, isolating seepage remaining liquid is water.
The said ketone step of taking off can also be: with sending into rectifying tower after the slurry tank subnatant heating of extracting, through azeotropic distillation, get the solvent butanone at the bottom of the tower; Cat head steams water vapor and sends into after condensation in the water slurry tank.
Wetting ability A type organic zeolite membrane is adopted in said molecular screen membrane dehydration.
Said inorganic molecule sieve takes off ketone and adopts Silicalite hydrophobicity organic zeolite membrane.
The side that sees through out of the film of molecular screen membrane deketo equipment and molecular screen membrane dewatering unit keeps vacuum tightness 1-10 mmhg.
The separating obtained water of above-mentioned each film device returns in the stripping tower of FEOL as the stripping water.
Each installs separating obtained dry solvent and merges and be collected into solvent tank and utilize.
The present invention will permeate the recovery technology that gasification technology, water vapour penetration technology are respectively applied for water-containing solvent, adopt different mineral membranes according to the different water cut solvent that produces in the sepn process, adopt Silicalite hydrophobicity organic zeolite membrane to deviate from butanone for the big lower floor's solvent of water-content; Adopt the dehydration of wetting ability A type organic zeolite membrane for the less upper strata solvent of water content.Adopted advanced infiltration gasification (PV) and water vapour penetration (VP) technology to substitute traditional azeotropic distillation technology among the present invention.Silicalite hydrophobicity organic zeolite membrane adopts the infiltration gasification technology, utilize molecular screen membrane selective adsorption performance, butanone in the mixed solution is adsorbed to face, the side that sees through at film keeps vacuum, utilize the effect of the vapor partial pressure difference of film both sides butanone, be attracted to butanone on the face and see through film and vaporization and separate.Wetting ability A type organic zeolite membrane adopts the water vapour penetration technology, and the water vapour penetration technology is compared with the infiltration gasification technology, by than High Operating Temperature, makes water vapor arrive face, with the form of saturated vapor through film and separated, treatment capacity is bigger.More than can realize by the heat exchanging temperature controlling.The present invention is recyclable to obtain the dry solvent that water content is lower than 0.3wt%, is recovered to solvent tank after this part solvent cooling and utilizes.
Solvent recovery process of the present invention can reduce the use of auxiliary facility, technological process and operation are all simplified greatly, the separation efficiency height, energy consumption is low, compare with traditional rectification process, approximately can save the energy consumption of 1/2-1/3,, reduce the cost of novel process to a great extent owing to the reduction greatly of energy consumption.
(description of drawings)
Fig. 1 be depositing in water fall separate with membrane sepn dewater, membrane sepn takes off the solvent recuperation schema that ketone technology combines.
Fig. 2 be depositing in water fall separate with membrane sepn dewater, rectifying takes off the solvent recuperation schema that ketone technology combines.
Each label is expressed as follows among the figure: 1-filtrate evaporator tower, and the 2-interchanger, the 3-drying tower, the 4-pump, 5-water slurry tank, the 6-interchanger, the 7-pump, the 8-interchanger, the 9-film takes off the butanone device, 10-film dewatering unit, 11-rectifying tower, 12, the 13-vacuum pump.
(embodiment)
Embodiment 1
Referring to Fig. 1, in this example, membrane separation unit 9 and 10 is vitrified pipes that outer wall scribbles organic zeolite membrane.Wherein film dewatering unit 9 adopts the dehydration of A type hydrophilic inorganic molecular screen membrane; Film takes off butanone device 10 and adopts Silicalite hydrophobicity organic zeolite membrane to deviate from butanone.
Technical process is as follows: through the evaporation in early stage, dewaxed filtrate (being aqueous toluene-butanone solvent) after stripping is handled, enter into single vaporization tower 1, after 2 heat exchange of overhead vapours process interchanger, enter into drying tower 3, at the bottom of tower, obtain toluene-butanone combination drying solvent based on toluene, it is moisture butanone and small amount of toluene that cat head steams thing, be pumped into standing demix in the water slurry tank 5 with pump 4, upper strata liquid is the butanone of moisture 3%-4%, 6 heat exchange are warming up to 105 ℃ through interchanger, be pumped into and carry out water vapour penetration in the molecular screen membrane dewatering unit 10, the side that sees through of film is aspirated with vacuum pump 12, keeps vacuum tightness 7 mmhg, and obtaining seepage remaining liquid (promptly seeing through liquid) is qualified dry solvent butanone, it is water more than 95% that film sees through liquid, returns stripping tower and makes the stripping water.The subnatant of water slurry tank 5 is the water that contains solvent (being mainly butanone) 10%.Use pump 7 that subnatant is pumped into interchanger 8, heat exchange is warming up to 60 ℃, entering molecular screen membrane takes off in the butanone device 9, film sees through side and takes out very to 1 mmhg with vacuum pump 13, seepage remaining liquid is a water, pumps into stripping tower or directly discharging, sees through side and obtains dry butanone solvent, water content reclaims stand-by through entering solvent tank after the condensation below 1% with film dewatering unit 10 effusive dry solvents in the lump.
Embodiment 2
See Fig. 2, through the evaporation in early stage, dewaxed filtrate (being aqueous toluene-butanone solvent) after stripping is handled, enter into single vaporization tower 1, after 2 heat exchange of overhead vapours process interchanger, enter into drying tower 3, at the bottom of tower, obtain toluene-butanone combination drying solvent based on toluene, it is moisture butanone and small amount of toluene that cat head steams thing, be pumped into standing demix in the water slurry tank 5 with pump 4, upper strata liquid is the butanone of moisture 3%-4%, 6 heat exchange are warming up to 105 ℃ through interchanger, are pumped into and carry out water vapour penetration in the molecular screen membrane dewatering unit 10, and the side that sees through of film is aspirated with vacuum pump 12, keep vacuum tightness 7 mmhg, obtaining seepage remaining liquid (promptly not seeing through liquid) is qualified dry solvent butanone, and it is water more than 95% that film sees through liquid, returns stripping tower and makes the stripping water.The subnatant of water slurry tank is the water that contains 10% solvent (being mainly butanone), is sent to rectifying tower 11 by pump 7 after interchanger 8 heats up, and through azeotropic distillation, gets the solvent butanone at the bottom of the tower, is recovered into solvent tank; Cat head steams water vapor and returns water slurry tank 5 and separate.
Claims (6)
1. dewaxing solvent reclaims technology, lubricating oil dewaxing filtrate separated at the bottom of the tower by single vaporization through the water-containing solvent behind the stripping remove oil content, cat head steams goes into drying tower after the thing heat exchange heats up, at the bottom of tower, isolate toluene and part butanone dry solvent, it is characterized in that the drying tower cat head steams thing and pumps into water slurry tank sedimentation layering, extract upper strata liquid, be heated to 60～120 ℃, it is sent into the molecular screen membrane dewatering unit, contained water is by film water vapour penetration, and the side that sees through of film adopts vacuum take-off, keeps vacuum tightness 1-10 mmhg, the water vapor cooling fluid that sees through dissolves device, reclaims to such an extent that seepage remaining liquid is dry butanone solvent; Extract the subnatant of slurry tank,, butanone solvent contained in the water is separated to deviate from and recovery by taking off the ketone step.
2. the dewaxing solvent according to claim 1 reclaims technology, it is characterized in that the said ketone step of taking off is: the subnatant of the slurry tank that extracts is heated to 30～60 ℃, send into the organic zeolite membrane deketo equipment, the side that sees through of film adopts vacuum take-off, keep vacuum tightness 1-10 mmhg, butanone contained in the water is isolated the gaseous state butanone by film water vapour penetration, to reclaim after its cooling liquid, isolating seepage remaining liquid is water.
3. the dewaxing solvent according to claim 1 reclaims technology, it is characterized in that the said ketone step of taking off is: with sending into rectifying tower after the slurry tank subnatant heating of extracting, through azeotropic distillation, get the solvent butanone at the bottom of the tower, be recovered into solvent tank; Cat head steams water vapor and is recovered to the water slurry tank.
4. reclaim technology according to the dewaxing solvent of claim 1, it is characterized in that said molecular screen membrane dehydration adopts wetting ability A type organic zeolite membrane.
5. the dewaxing solvent according to claim 2 reclaims technology, it is characterized in that said inorganic molecule sieve takes off ketone and adopts Silicalite hydrophobicity organic zeolite membrane.
6. the dewaxing solvent according to claim 1 or 2 or 3 or 4 or 5 reclaims technology, it is characterized in that each is installed separating obtained water sends back in the stripping tower of FEOL as the stripping water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031134416A CN1188496C (en) | 2003-05-13 | 2003-05-13 | Dewaxing solvent recovery process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031134416A CN1188496C (en) | 2003-05-13 | 2003-05-13 | Dewaxing solvent recovery process |
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| Publication Number | Publication Date |
|---|---|
| CN1451718A CN1451718A (en) | 2003-10-29 |
| CN1188496C true CN1188496C (en) | 2005-02-09 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB031134416A Expired - Fee Related CN1188496C (en) | 2003-05-13 | 2003-05-13 | Dewaxing solvent recovery process |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106349140B (en) * | 2016-10-26 | 2018-03-06 | 湖南聚仁化工新材料科技有限公司 | A kind of method for preparing anhydrous peroxide organic carboxyl acid solution |
| CN107400049A (en) * | 2017-08-03 | 2017-11-28 | 广东新华粤石化股份有限公司 | The separation method of non-solvent component in a kind of ketone benzene binary solvent |
| CN109569421A (en) * | 2018-12-19 | 2019-04-05 | 西安近代化学研究所 | A kind of composite explosives aqueous suspension cladding granulating solvent recovery process |
| CN113214061A (en) * | 2021-05-27 | 2021-08-06 | 新中天环保股份有限公司 | Process for recovering butanone from waste solvent in adhesive industry |
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- 2003-05-13 CN CNB031134416A patent/CN1188496C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN1451718A (en) | 2003-10-29 |
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