CN101628205A - Nanofiltration membrane used for separating solvent from mixed oil and method - Google Patents
Nanofiltration membrane used for separating solvent from mixed oil and method Download PDFInfo
- Publication number
- CN101628205A CN101628205A CN200910090910A CN200910090910A CN101628205A CN 101628205 A CN101628205 A CN 101628205A CN 200910090910 A CN200910090910 A CN 200910090910A CN 200910090910 A CN200910090910 A CN 200910090910A CN 101628205 A CN101628205 A CN 101628205A
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- CN
- China
- Prior art keywords
- solvent
- membrane
- lithium chloride
- polyether sulfone
- propyl alcohol
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- 239000002904 solvent Substances 0.000 title claims abstract description 51
- 239000012528 membrane Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000001728 nano-filtration Methods 0.000 title abstract 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims abstract description 52
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims abstract description 47
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012046 mixed solvent Substances 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 238000003618 dip coating Methods 0.000 claims abstract description 8
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000005266 casting Methods 0.000 claims abstract description 6
- 238000001704 evaporation Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002131 composite material Substances 0.000 claims abstract description 5
- 238000011084 recovery Methods 0.000 claims abstract description 3
- STLFZKZBGXSIQJ-UHFFFAOYSA-N 1,1'-biphenyl;naphthalene Chemical group C1=CC=CC2=CC=CC=C21.C1=CC=CC=C1C1=CC=CC=C1 STLFZKZBGXSIQJ-UHFFFAOYSA-N 0.000 claims description 30
- 239000004695 Polyether sulfone Substances 0.000 claims description 30
- 229920006393 polyether sulfone Polymers 0.000 claims description 30
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical group CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 6
- 238000009833 condensation Methods 0.000 claims description 5
- 230000005494 condensation Effects 0.000 claims description 5
- 239000010779 crude oil Substances 0.000 claims description 4
- 239000003921 oil Substances 0.000 claims description 4
- 239000012467 final product Substances 0.000 claims description 3
- 208000035126 Facies Diseases 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- 239000013557 residual solvent Substances 0.000 claims description 2
- 238000004781 supercooling Methods 0.000 claims description 2
- 229920001187 thermosetting polymer Polymers 0.000 claims description 2
- 239000004519 grease Substances 0.000 abstract description 10
- 230000008020 evaporation Effects 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 abstract 4
- -1 poly(phthalazinone ether sulfone Chemical class 0.000 abstract 4
- 230000005540 biological transmission Effects 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 210000004379 membrane Anatomy 0.000 description 19
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 3
- 210000002469 basement membrane Anatomy 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 235000019198 oils Nutrition 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 241000500881 Lepisma Species 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 235000012343 cottonseed oil Nutrition 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229920001002 functional polymer Polymers 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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Abstract
The invention relates to a nanofiltration membrane used for separating solvent from mixed oil and a method, and the preparation method of the nanofiltration membrane comprises the steps of dissolving propanol, lithium chloride and poly(phthalazinone ether sulfone) in N-methyl pyrrolidinone, casting into a membrane after filtering solution, soaking the membrane in water, wherein, propanol: lithium chloride: poly(phthalazinone ether sulfone): N-methyl pyrrolidinone is equal to 1-18: 0.1-3: 10-25: 60-80 by parts by weight; dissolving propanol, lithium chloride and poly(phthalazinone ether sulfone) in mixed solvent of ethylene glycol monomethyl ether and acetone with the volume ratio of 1: 1, using the solution for dip-coating the membrane prepared by the step (1), and heating for forming a composite membrane, wherein, propanol: lithium chloride: poly(phthalazinone ether sulfone): mixed solvent is equal to 2-12: 0.1-2: 5-10: 80-95 by parts by weight. The solvent recovery rate of the method is greater than 65%, the residual amount of grease in the solvent is less than 1%, the removal rate of the transmission phase grease is greater than 99%, the solvent can be directly recycled, and the method can save energy by more than 60% in comparison with the direct evaporation process.
Description
Technical field
The present invention relates to a kind of method that is used for separating the solvent of miscella, be specifically related to a kind of method that adopts NF membrane effectively to separate the solvent in the miscella.
Background technology
The extraction of the grease in the oil plant (as soybean, cottonseed etc.) is adopted usually the method for hexane, No. 6 solvent naphtha equal solvent leachings both at home and abroad, the solvent extraction that contains grease is called as miscella mutually.Usually take evaporation to separate solvent and grease to the processing of miscella.It is about 20% to contain grease in the general miscella, produces 1 ton of grease and need evaporate about 5 tons of solvents, for condensing solvent steam needs auxiliary power equipment with the driving cooling water system, also can cause thermal pollution simultaneously.
Assorted naphthalene biphenyl polyether sulfone (PPES) milipore filter is to be raw material with assorted naphthalene biphenyl polyether sulfone, N-methyl pyrrolidone (NMP) is a solvent, organic molecule propyl alcohol (PrOH) and inorganic molecules lithium chloride (LiCl) are as additive package, adopt the milipore filter (" preparation of low catching molecular PPES milipore filter " of phase inversion preparation, Gao Song etc., the functional polymer journal, the 21st the 3rd phase of volume, in September, 2008).In general, milipore filter is used to filter the above molecule of 1000 dalton.
Summary of the invention
Therefore, the method that the purpose of this invention is to provide the solvent in a kind of effective separation miscella of with low cost and environmental protection.
Be used to realize that the technical scheme of above-mentioned technical purpose is as follows:
A kind of NF membrane that is used for separating the solvent of miscella, the preparation method of this NF membrane may further comprise the steps:
(1) propyl alcohol, lithium chloride and assorted naphthalene biphenyl polyether sulfone are dissolved in the N-methyl pyrrolidone, solution is casting film after filtering, and film soaked in water, wherein count propyl alcohol: lithium chloride by weight: assorted naphthalene biphenyl polyether sulfone: N-methyl pyrrolidone=1～18: 0.1～3: 10～25: 60～80;
(2) propyl alcohol, lithium chloride and assorted naphthalene biphenyl polyether sulfone are dissolved in the mixed solvent that volume ratio is 1: 1 EGME and acetone, the film that makes with this solution dip-coating step (1), add the thermosetting composite membrane again, wherein count propyl alcohol: lithium chloride by weight: assorted naphthalene biphenyl polyether sulfone: mixed solvent=2～12: 0.1～2: 5～10: 80～95.
In a specific embodiments of the present invention, the preparation method of above-mentioned NF membrane may further comprise the steps:
(1) propyl alcohol, lithium chloride and assorted naphthalene biphenyl polyether sulfone are dissolved in the N-methyl pyrrolidone, solution removes bubble after filtering and leaves standstill, casting film; Soak in water film stopped evaporating solvent in air after, exchange of solvent gets final product fully, meter by weight wherein, propyl alcohol: lithium chloride: assorted naphthalene biphenyl polyether sulfone: N-methyl pyrrolidone=1～18: 0.1～3: 10～25: 60～80;
(2) propyl alcohol, lithium chloride and assorted naphthalene biphenyl polyether sulfone are dissolved in the mixed solvent that volume ratio is 1: 1 EGME and acetone, the film that makes with this solution dip-coating step (1), heat down at 100 ℃ again and formed composite membrane in 30 minutes, wherein count propyl alcohol: lithium chloride by weight: assorted naphthalene biphenyl polyether sulfone: mixed solvent=2～12: 0.1～2: 5～10: 80～95.
Above-mentioned NF membrane can be held back 200～1000 daltonian molecules.
The present invention also provides a kind of method of separating the solvent in the miscella, and this method may further comprise the steps:
(1) miscella is filtered through filter;
(2) filtrate is filtered by above-mentioned NF membrane, and the solvent of filtration is for recycling;
(3) unfiltered concentrated miscella is evaporated, the solvent that steams supplies to recycle after condensation.
In said method, solvent can be hexane and/or No. 6 solvent naphthas.
In a specific embodiments of said method, this method may further comprise the steps:
(1) miscella from infuser filters through mechanical filter, and filter residue is back to infuser;
(2) filtrate is filtered by the filter with above-mentioned NF membrane, and the solvent recovery of filtration supplies to recycle to solvent tank;
(3) unfiltered concentrated miscella enters the crude oil evaporimeter and evaporates, the organic vapor that evaporimeter steams is recovered to solvent tank after condensation, remaining material enters the stripping evaporimeter and removes residual solvent and obtain crude oil, steams thing through supercooling, water-oil separating, and organic facies enters solvent tank.
The present invention finds after deliberation, as basement membrane, carries out the assorted naphthalene biphenyl polyether sulfone NF membrane that the secondary dip-coating can obtain the penetrated preferably organic molecule with assorted naphthalene biphenyl polyether sulfone milipore filter, and this assorted naphthalene biphenyl polyether sulfone NF membrane has good solvent resistance.Therefore, at first adopted the micromolecular assorted naphthalene biphenyl polyether sulfone NF membrane of penetrated preferably organic matter that the solvent in the miscella is separated, its technological process as shown in Figure 1, solvent recovering rate is greater than 65%, oil residue in the solvent is less than 1%, see through phase grease clearance greater than 99%, solvent can directly recycle.Therefore, this method can be more energy-conservation more than 60% than direct evaporation technology, reduces cooling water amount and corresponding thermal pollution, reduces the free gas scale of construction.
Description of drawings
Below, describe embodiment of the present invention in conjunction with the accompanying drawings in detail, wherein:
Fig. 1 is the process chart of the method for the solvent in the separation miscella of the present invention.
The specific embodiment
Below in conjunction with the specific embodiment the present invention is further described in detail, the embodiment that provides is only in order to illustrate the present invention, rather than in order to limit the scope of the invention.
The preparation of embodiment 1 assorted naphthalene biphenyl polyether sulfone NF membrane
With assorted naphthalene biphenyl polyether sulfone is raw material, and N-methyl pyrrolidone (NMP) is a solvent, and organic molecule propyl alcohol (PrOH) and inorganic molecules lithium chloride (LiCl) adopt the milipore filter of phase inversion preparation as additive package.Wherein, count propyl alcohol: lithium chloride by weight: assorted naphthalene biphenyl polyether sulfone: N-methyl pyrrolidone=9: 1: 17: 70.
The preparation method is as follows: vacuum drying PPES and additive are dissolved in NMP in proportion, filtration, deaeration, leave standstill.Casting solution is cast on the glass plate, make film with glass slicker, stop evaporation 15 seconds in the air, change in the condensation water-bath, the dipping film forming is soaked more than 24 hours through water purification, gets final product after exchange of solvent is complete.As basement membrane, carry out the secondary dip-coating with made film.Lotion is a raw material with assorted naphthalene biphenyl polyether sulfone, and the mixed solvent of EGME and acetone (volume ratio is 1: 1) is a solvent, and organic molecule propyl alcohol (PrOH) and inorganic molecules lithium chloride (LiCl) are as additive package.Wherein, count propyl alcohol: lithium chloride by weight: assorted naphthalene biphenyl polyether sulfone: mixed solvent=7: 0.9: 7.5: 85.The film of dip-coating obtains assorted naphthalene biphenyl polyether sulfone NF membrane through heat treatment in 30 minutes under 100 ℃.
Embodiment 2 assorted naphthalene biphenyl polyether sulfone NF membrane are separated the solvent in the miscella
Get the miscella that the 20kg hexane leaches, through 400 purpose strainer filterings, filtrate is filtered with the PPES NF membrane under 1MPa, 25 ℃, and flux is 21 l/m
2Hour, transit dose is 67% of an inlet amount, is 0.87% through the fat content mutually, the grease clearance is 99.3%.
Embodiment 3 assorted naphthalene biphenyl polyether sulfone NF membrane are separated the solvent in the miscella
Get the miscella that No. 6 solvent naphthas of 20kg leach, through 400 purpose strainer filterings, filtrate is filtered with the PPES NF membrane under 1MPa, 25 ℃, and flux is 20l/m
2Hour, transit dose is 65% of an inlet amount, is 0.89% through the fat content mutually, the grease clearance is 99.1%.
Claims (6)
1. NF membrane that is used for separating the solvent of miscella, the preparation method of this NF membrane may further comprise the steps:
(1) propyl alcohol, lithium chloride and assorted naphthalene biphenyl polyether sulfone are dissolved in the N-methyl pyrrolidone, solution is casting film after filtering, and film soaked in water, wherein count propyl alcohol: lithium chloride by weight: assorted naphthalene biphenyl polyether sulfone: N-methyl pyrrolidone=1～18: 0.1～3: 10～25: 60～80;
(2) propyl alcohol, lithium chloride and assorted naphthalene biphenyl polyether sulfone are dissolved in the mixed solvent that volume ratio is 1: 1 EGME and acetone, the film that makes with this solution dip-coating step (1), add the thermosetting composite membrane again, wherein count propyl alcohol: lithium chloride by weight: assorted naphthalene biphenyl polyether sulfone: mixed solvent=2～12: 0.1～2: 5～10: 80～95.
2. NF membrane according to claim 1 is characterized in that, the preparation method of this NF membrane may further comprise the steps:
(1) propyl alcohol, lithium chloride and assorted naphthalene biphenyl polyether sulfone are dissolved in the N-methyl pyrrolidone, solution removes bubble after filtering and leaves standstill, casting film; Soak in water film stopped evaporating solvent in air after, exchange of solvent gets final product fully, meter by weight wherein, propyl alcohol: lithium chloride: assorted naphthalene biphenyl polyether sulfone: N-methyl pyrrolidone=1～18: 0.1～3: 10～25: 60～80;
(2) propyl alcohol, lithium chloride and assorted naphthalene biphenyl polyether sulfone are dissolved in the mixed solvent that volume ratio is 1: 1 EGME and acetone, the film that makes with this solution dip-coating step (1), heat down at 100 ℃ again and formed composite membrane in 30 minutes, wherein count propyl alcohol: lithium chloride by weight: assorted naphthalene biphenyl polyether sulfone: mixed solvent=2～12: 0.1～2: 5～10: 80～95.
3. NF membrane according to claim 1 and 2 is characterized in that, described NF membrane is held back 200～1000 daltonian molecules.
4. method of separating the solvent in the miscella, this method may further comprise the steps:
(1) miscella is filtered through filter;
(2) filtrate is by filtering according to each described NF membrane in the claim 1 to 3, and the solvent of filtration is for recycling;
(3) unfiltered concentrated miscella is evaporated, the solvent that steams supplies to recycle after condensation.
5. method according to claim 4 is characterized in that, described solvent is hexane and/or No. 6 solvent naphthas.
6. according to claim 4 or 5 described methods, it is characterized in that, said method comprising the steps of:
(1) miscella from infuser filters through mechanical filter, and filter residue is back to infuser;
(2) filtrate is filtered by the filter that has according to each described NF membrane in the claim 1 to 3, and the solvent recovery of filtration supplies to recycle to solvent tank;
(3) unfiltered concentrated miscella enters the crude oil evaporimeter and evaporates, the organic vapor that evaporimeter steams is recovered to solvent tank after condensation, remaining material enters the stripping evaporimeter and removes residual solvent and obtain crude oil, steams thing through supercooling, water-oil separating, and organic facies enters solvent tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100909102A CN101628205B (en) | 2009-08-14 | 2009-08-14 | Nanofiltration membrane used for separating solvent from mixed oil and method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009100909102A CN101628205B (en) | 2009-08-14 | 2009-08-14 | Nanofiltration membrane used for separating solvent from mixed oil and method |
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| CN101628205A true CN101628205A (en) | 2010-01-20 |
| CN101628205B CN101628205B (en) | 2012-04-04 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102190611A (en) * | 2011-04-01 | 2011-09-21 | 四川天华股份有限公司 | Method for purifying N-methyl pyrrolidone and gamma-butyrolactone |
| CN101628206B (en) * | 2009-08-14 | 2012-04-04 | 德州中钿生物科技有限公司 | Nanofiltration membrane for removing gossypol in cottonseeds and method |
| WO2014206224A1 (en) * | 2013-06-25 | 2014-12-31 | 深圳市森科妍科技有限公司 | Waste organic solvent treatment process and system based on nano filtration membrane |
| CN108774582A (en) * | 2018-06-12 | 2018-11-09 | 合肥丰洁生物科技有限公司 | A kind of film condensing device for plant oil extract |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1088970A (en) * | 1992-12-30 | 1994-07-06 | 朱新民 | Leach mixing oil vacuum evaporation method and device |
| CN101628206B (en) * | 2009-08-14 | 2012-04-04 | 德州中钿生物科技有限公司 | Nanofiltration membrane for removing gossypol in cottonseeds and method |
-
2009
- 2009-08-14 CN CN2009100909102A patent/CN101628205B/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101628206B (en) * | 2009-08-14 | 2012-04-04 | 德州中钿生物科技有限公司 | Nanofiltration membrane for removing gossypol in cottonseeds and method |
| CN102190611A (en) * | 2011-04-01 | 2011-09-21 | 四川天华股份有限公司 | Method for purifying N-methyl pyrrolidone and gamma-butyrolactone |
| CN102190611B (en) * | 2011-04-01 | 2012-11-14 | 四川天华股份有限公司 | Method for purifying N-methyl pyrrolidone and gamma-butyrolactone |
| WO2014206224A1 (en) * | 2013-06-25 | 2014-12-31 | 深圳市森科妍科技有限公司 | Waste organic solvent treatment process and system based on nano filtration membrane |
| CN108774582A (en) * | 2018-06-12 | 2018-11-09 | 合肥丰洁生物科技有限公司 | A kind of film condensing device for plant oil extract |
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| Publication number | Publication date |
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| CN101628205B (en) | 2012-04-04 |
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