CN101628205B - 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
- CN101628205B CN101628205B CN2009100909102A CN200910090910A CN101628205B CN 101628205 B CN101628205 B CN 101628205B CN 2009100909102 A CN2009100909102 A CN 2009100909102A CN 200910090910 A CN200910090910 A CN 200910090910A CN 101628205 B CN101628205 B CN 101628205B
- Authority
- CN
- China
- Prior art keywords
- solvent
- lithium chloride
- membrane
- polyether sulfone
- propyl alcohol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
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 (like 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, and organic molecule propyl alcohol (PrOH) and inorganic molecules lithium chloride (LiCl) adopt the milipore filter (" preparation of low catching molecular PPES milipore filter " of phase inversion preparation as additive package; 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 following:
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 being dissolved in volume ratio is in 1: 1 the mixed solvent of 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; In water, soak film stopped evaporating solvent in air after, solvent exchange 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 being dissolved in volume ratio is in 1: 1 the mixed solvent of 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) filtrating is filtered through above-mentioned NF membrane, and the solvent of filtration supplies to recycle;
(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) filtrating is filtered through the filter with above-mentioned NF membrane, and the solvent recovery of filtration supplies to recycle to solvent tank;
(3) unfiltered concentrated miscella entering crude oil evaporimeter evaporates; The organic vapor that evaporimeter steams is recovered to solvent tank after condensation; Remaining material entering stripping evaporimeter removes residual solvent and obtains crude oil, steams thing through supercooling, water-oil separating, and organic facies gets into 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 is as shown in Figure 1, and solvent recovering rate is greater than 65%, and the 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, specify embodiment of the present invention in conjunction with accompanying drawing, 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 has been merely and has illustrated the present invention, rather than in order to limit scope of the present 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 following: vacuum drying PPES and additive are dissolved in NMP in proportion, filtration, deaeration, leave standstill.Casting solution is cast on the glass plate, process 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 solvent exchange 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 down at 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, filtrating is under 1MPa, 25 ℃, and with the filtration of PPES NF membrane, 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, filtrating is under 1MPa, 25 ℃, and with the filtration of PPES NF membrane, 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 (4)
1. method of separating the solvent in the miscella, this method may further comprise the steps:
(1) miscella is filtered through filter;
(2) filtrating is filtered through NF membrane, and the solvent of filtration supplies to recycle;
(3) unfiltered concentrated miscella is evaporated, the solvent that steams supplies to recycle after condensation;
Wherein said NF membrane is held back 200～1000 daltonian molecules, and 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 being dissolved in volume ratio is in 1: 1 the mixed solvent of 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. method 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; In water, soak film stopped evaporating solvent in air after, solvent exchange 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 being dissolved in volume ratio is in 1: 1 the mixed solvent of 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. method according to claim 1 is characterized in that, said solvent is hexane and/or No. 6 solvent naphthas.
4. according to each described method in the claim 1 to 3, 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) filtrating is filtered through the filter with said NF membrane, and the solvent recovery of filtration supplies to recycle to solvent tank;
(3) unfiltered concentrated miscella entering crude oil evaporimeter evaporates; The organic vapor that evaporimeter steams is recovered to solvent tank after condensation; Remaining material entering stripping evaporimeter removes residual solvent and obtains crude oil, steams thing through supercooling, water-oil separating, and organic facies gets into 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 |
Applications Claiming Priority (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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101628205A CN101628205A (en) | 2010-01-20 |
| CN101628205B true CN101628205B (en) | 2012-04-04 |
Family
ID=41573585
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100909102A Expired - Fee Related CN101628205B (en) | 2009-08-14 | 2009-08-14 | Nanofiltration membrane used for separating solvent from mixed oil and method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101628205B (en) |
Families Citing this family (4)
| 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 |
| 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 |
| CN103285734B (en) * | 2013-06-25 | 2015-07-15 | 深圳市森科妍科技有限公司 | A treatment process and a system for waste organic solvents based on nano filter membranes |
| 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 |
Citations (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 |
| CN101628206A (en) * | 2009-08-14 | 2010-01-20 | 房诗宏 | Nanofiltration membrane for removing gossypol in cottonseeds and method |
-
2009
- 2009-08-14 CN CN2009100909102A patent/CN101628205B/en not_active Expired - Fee Related
Patent Citations (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 |
| CN101628206A (en) * | 2009-08-14 | 2010-01-20 | 房诗宏 | Nanofiltration membrane for removing gossypol in cottonseeds and method |
Non-Patent Citations (2)
| Title |
|---|
| 王珺.磺化杂萘联苯聚醚砜复合纳滤膜的研究.《中国优秀硕士学位论文》.2007,第4章. * |
| 高嵩.低截留分子量PPES超滤膜的制备.《功能高分子学报》.2008,第21卷(第3期),318-320页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101628205A (en) | 2010-01-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101628205B (en) | Nanofiltration membrane used for separating solvent from mixed oil and method | |
| CN205740622U (en) | A kind of percolate coagulating sedimentation, evaporation joint processing system | |
| CN102352054B (en) | Recovery process of solvent in polyphenylene sulfide resin production process | |
| CN1133833A (en) | Method and apparatus for recovering carboxylic acids from aqueous solutions | |
| CN109134339B (en) | Method for recovering solvent for para-aramid fiber production | |
| CN105218317B (en) | The method and device that ethanol is reclaimed in a kind of hexanitrobibenzyl production | |
| CN101544429B (en) | Extraction-hyperfiltration-reverse osmosis combined method for treating PTA refined wastewater | |
| CN101224933B (en) | Treatment method for zero discharge of ionic liquid water solution | |
| CN100593520C (en) | Polyimide copolymer infiltration vaporization separation film for treating phenols-containing waste water and preparing method thereof | |
| CN103709022A (en) | Process and device for recovering butanone by pervaporation method | |
| CN111662746A (en) | Method for synchronously demetallizing, desalting and dehydrating coal tar | |
| CN101921204B (en) | Method for recycling DMAC (Dimethyl Acetylamide) from waste spandex stock solution | |
| CN101628206B (en) | Nanofiltration membrane for removing gossypol in cottonseeds and method | |
| CN206467171U (en) | Reclaim, purify the device of N methyl pyrrolidones | |
| CN104003566B (en) | The recovery method of many components waste liquid in high-performance aramid fiber fibrid production process | |
| CN105602695A (en) | Waste lubricating oil regeneration treatment method | |
| CN206359484U (en) | A kind of used oil refines fuel oil refining system | |
| CN113788738A (en) | Comprehensive treatment method of alcohol, water and oil mixed solution | |
| CN203648245U (en) | Novel agglomerate separation oil filter | |
| CN113480412A (en) | Method for recovering phenol in alkylphenol production wastewater | |
| CN108774149B (en) | Solvent recycling method and device in PVDF separation membrane production | |
| CN202744415U (en) | Landfill leachate treatment device | |
| CN221014549U (en) | Recycling system of amide chloride aqueous solution | |
| CN112391186A (en) | Method for separating phenolic compounds from coal tar | |
| CN104961187A (en) | Method for treating wastewater with organic solvents |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| ASS | Succession or assignment of patent right |
Free format text: FORMER OWNER: LIU JINCAI Owner name: DEZHOU ZHONGDIAN BIO-TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: FANG SHIHONG Effective date: 20101222 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 100083 5-1204, FURUN JIAYUAN, NO.6, XUEYUAN ROAD, HAIDIAN DISTRICT, BEIJING TO: 253200 S. SIDE OF YANCHI STREET, XIAJIN COUNTY, DEZHOU CITY, SHANDONG PROVINCE |
|
| TA01 | Transfer of patent application right |
Effective date of registration: 20101222 Address after: 253200 Shandong city of Dezhou province Xiajin County yanchishan Street South Applicant after: Dezhou Zhongdian Biotechnology Co., Ltd. Address before: 100083 Beijing city Haidian District No. 6 Xueyuan Road Furun homes 5-1204 Applicant before: Fang Shihong Co-applicant before: Liu Jincai |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120404 Termination date: 20190814 |