CN109433016A - The preparation method of bionical water-oil separationg film - Google Patents
The preparation method of bionical water-oil separationg film Download PDFInfo
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- CN109433016A CN109433016A CN201811164099.3A CN201811164099A CN109433016A CN 109433016 A CN109433016 A CN 109433016A CN 201811164099 A CN201811164099 A CN 201811164099A CN 109433016 A CN109433016 A CN 109433016A
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- film
- mixture
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- reaction kettle
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000010408 film Substances 0.000 claims abstract description 44
- 239000000203 mixture Substances 0.000 claims abstract description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229920001661 Chitosan Polymers 0.000 claims abstract description 13
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052901 montmorillonite Inorganic materials 0.000 claims abstract description 12
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 11
- 238000001704 evaporation Methods 0.000 claims abstract description 10
- 230000008020 evaporation Effects 0.000 claims abstract description 10
- 229960002089 ferrous chloride Drugs 0.000 claims abstract description 10
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims abstract description 10
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 235000019441 ethanol Nutrition 0.000 claims abstract description 9
- 238000004321 preservation Methods 0.000 claims abstract description 9
- 239000010409 thin film Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims 1
- 238000004090 dissolution Methods 0.000 claims 1
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical compound FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 5
- 239000012528 membrane Substances 0.000 description 14
- 239000000463 material Substances 0.000 description 7
- 238000000926 separation method Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001471 micro-filtration Methods 0.000 description 2
- 238000001223 reverse osmosis Methods 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- 238000000108 ultra-filtration Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000002977 biomimetic material Substances 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001728 nano-filtration Methods 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 238000001612 separation test Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/08—Thickening liquid suspensions by filtration
- B01D17/085—Thickening liquid suspensions by filtration with membranes
Abstract
The invention discloses a kind of preparation methods of bionical water-oil separationg film, method includes the following steps: step 1, montmorillonite and chitosan are stirred, are added in ammonia spirit, obtain mixture one；Sodium hydroxide, solution of ferrous chloride and ethyl alcohol are mixed, obtain mixture two by step 2；Mixture one and mixture two are uniformly mixed by step 3, and reaction kettle is added, cooling in 250-280 DEG C of heat preservation 7-10h, spare；Calcium chloride solution is added in step 4, is heated to 60~120 DEG C, reacts 10~30min；Step 5, heating evaporation finally form thin film in container bottom；Step 6 pressurizes to film, forms the film with a thickness of 0.2-0.5mm.The present invention adheres to chitosan sufficiently on montmorillonite surface, and the seperation film separative efficiency being finally made is high.
Description
Technical field
The invention belongs to biomimetic material field more particularly to a kind of preparation methods of bionical water-oil separationg film.
Background technique
Seperation film is a kind of membranous type material that ability is penetrated with selectivity.It can usually divide by separating mechanism and the scope of application
For microfiltration membranes, ultrafiltration membrane, nanofiltration membrane, reverse osmosis membrane, osmotic evaporation film, amberplex etc..Seperation film refers to can be with specific shape
The separation two-phase or two-part interface of formula limitation and transmitting flowing material.The form of film can be solid, be also possible to liquid
State.The flowing material of envelope segmentation can be liquid, be also possible to gaseous.Seperation film is that one kind is special, has choosing
Selecting property penetrates the coating substances of function, it can make to flow intracorporal one or more of material permeances, and other substances are not through, thus
Play the role of being concentrated and isolating and purifying.From membrane technology come out since, microfiltration membranes, amberplex, reverse osmosis membrane, ultrafiltration membrane,
Gaseous jet simulation etc. is used widely in succession, since it can realize separation under conditions of maintaining primary objects system environment, and
It can efficiently be concentrated, enriched product, be effectively removed impurity, it is in addition easy to operate, it is compact-sized, low energy consumption, process simplification, nothing
Secondary pollution, and it is not required to addition chemical substance, just gradually becoming the basic unit operating process in food industry and medicine.
The fast development of process of industrialization while bringing convenience to people's lives, is also faced with the pollution such as waste water, exhaust gas
Caused environmental problem.One of effective technology as Environment control, membrane separation technique comes across early 20th century.In practical application
In, membrane separation technique faces lot of challenges, and fouling membrane and low separative efficiency are its key constraints.Further to have developed
Kind membrane separation technique, different separation membrane materials are developed in succession, wherein the graphite with excellent selectivity and stability
Alkene material is shown one's talent, and most potential non-traditional membrane material is become.Graphene is that carbon atom is constructed to be formed with hexa-atomic loop type
Two-dimension single layer crystal, have excellent mechanical performance and stability.Wherein, water-oil separationg film is also essential.
Summary of the invention
The present invention provides a kind of preparation method of bionical water-oil separationg film, separates to solve the deficiencies in the prior art
It is high-efficient.
In order to solve the above-mentioned technical problem, the invention adopts the following technical scheme:
The preparation method of bionical water-oil separationg film, comprising the following steps:
Step 1 stirs montmorillonite and chitosan, is added in ammonia spirit, obtains mixture one；
Sodium hydroxide, solution of ferrous chloride and ethyl alcohol are mixed, obtain mixture two by step 2；
Mixture one and mixture two are uniformly mixed by step 3, and reaction kettle is added, in 250-280 DEG C of heat preservation 7-10h,
It is cooling, it is spare；
Calcium chloride solution is added in step 4, is heated to 60~120 DEG C, reacts 10~30min；
Step 5, heating evaporation finally form thin film in container bottom；
Step 6 pressurizes to film, forms the film with a thickness of 0.2-0.5mm.
Preferably, reaction kettle is the hydrothermal reaction kettle containing polytetrafluoroethyllining lining.
Preferably, the chitosan is dissolved in the acetic acid solution that mass concentration is 2%.
Preferably, the mass concentration 70~80% of the solution of ferrous chloride.
Preferably, step 5 is heated to 130~140 DEG C.
The invention has the following advantages: the present invention adheres to chitosan sufficiently on montmorillonite surface, it is finally made
Seperation film separative efficiency is high.Wherein, the stability of film can be improved in the addition of calcium chloride solution, is convenient for subsequent pressurized treatments.
Specific embodiment
The present invention is further described in detail combined with specific embodiments below.
Embodiment 1
The preparation method of bionical water-oil separationg film, comprising the following steps:
Step 1 stirs montmorillonite and chitosan (being dissolved in the acetic acid solution that mass concentration is 2%),
It is added in ammonia spirit, obtains mixture one；
Sodium hydroxide, mass concentration are that 72% solution of ferrous chloride and ethyl alcohol mix, obtain mixture two by step 2；
Mixture one and mixture two are uniformly mixed by step 3, and reaction kettle is added, cooling in 270 DEG C of heat preservation 9h, standby
With；The reaction kettle is the hydrothermal reaction kettle containing polytetrafluoroethyllining lining
Calcium chloride solution is added in step 4, is heated to 100 DEG C, reacts 12min；
Step 5 is heated to 137 DEG C of evaporations, finally forms thin film in container bottom；
Step 6 pressurizes to film, forms the film with a thickness of 0.2-0.5mm.
Embodiment 2
The preparation method of bionical water-oil separationg film, comprising the following steps:
Step 1 stirs montmorillonite and chitosan (being dissolved in the acetic acid solution that mass concentration is 2%),
It is added in ammonia spirit, obtains mixture one；
Sodium hydroxide, mass concentration are that 70% solution of ferrous chloride and ethyl alcohol mix, obtain mixture two by step 2；
Mixture one and mixture two are uniformly mixed by step 3, and reaction kettle is added, cooling in 250 DEG C of heat preservation 7h, standby
With；The reaction kettle is the hydrothermal reaction kettle containing polytetrafluoroethyllining lining
Calcium chloride solution is added in step 4, is heated to 60 DEG C, reacts 10min；
Step 5 is heated to 140 DEG C of evaporations, finally forms thin film in container bottom；
Step 6 pressurizes to film, forms the film with a thickness of 0.2-0.5mm.
Embodiment 3
The preparation method of bionical water-oil separationg film, comprising the following steps:
Step 1 stirs montmorillonite and chitosan (being dissolved in the acetic acid solution that mass concentration is 2%),
It is added in ammonia spirit, obtains mixture one；
Sodium hydroxide, mass concentration are that 80% solution of ferrous chloride and ethyl alcohol mix, obtain mixture two by step 2；
Mixture one and mixture two are uniformly mixed by step 3, and reaction kettle is added, cooling in 280 DEG C of heat preservation 10h, standby
With；The reaction kettle is the hydrothermal reaction kettle containing polytetrafluoroethyllining lining
Calcium chloride solution is added in step 4, is heated to 120 DEG C, reacts 30min；
Step 5 is heated to 130 DEG C of evaporations, finally forms thin film in container bottom；
Step 6 pressurizes to film, forms the film with a thickness of 0.2-0.5mm.
Embodiment 4
The preparation method of bionical water-oil separationg film, comprising the following steps:
Step 1 stirs montmorillonite and chitosan (being dissolved in the acetic acid solution that mass concentration is 2%),
It is added in ammonia spirit, obtains mixture one；
Sodium hydroxide, mass concentration are that 78% solution of ferrous chloride and ethyl alcohol mix, obtain mixture two by step 2；
Mixture one and mixture two are uniformly mixed by step 3, and reaction kettle is added, cooling in 270 DEG C of heat preservation 8h, standby
With；The reaction kettle is the hydrothermal reaction kettle containing polytetrafluoroethyllining lining
Calcium chloride solution is added in step 4, is heated to 110 DEG C, reacts 20min；
Step 5 is heated to 132 DEG C of evaporations, finally forms thin film in container bottom；
Step 6 pressurizes to film, forms the film with a thickness of 0.2-0.5mm.
Reference examples 1
The difference from embodiment 1 is that: non-shell adding glycan.
The preparation method of bionical water-oil separationg film, comprising the following steps:
Montmorillonite is added in ammonia spirit, obtains mixture one by step 1；
Sodium hydroxide, mass concentration are that 72% solution of ferrous chloride and ethyl alcohol mix, obtain mixture two by step 2；
Mixture one and mixture two are uniformly mixed by step 3, and reaction kettle is added, cooling in 270 DEG C of heat preservation 9h, standby
With；The reaction kettle is the hydrothermal reaction kettle containing polytetrafluoroethyllining lining
Calcium chloride solution is added in step 4, is heated to 100 DEG C, reacts 12min；
Step 5 is heated to 137 DEG C of evaporations, finally forms thin film in container bottom；
Step 6 pressurizes to film, forms the film with a thickness of 0.2-0.5mm.
Reference examples 2
The difference from example 2 is that: not plus calcium chloride solution.
The preparation method of bionical water-oil separationg film, comprising the following steps:
Step 1 stirs montmorillonite and chitosan (being dissolved in the acetic acid solution that mass concentration is 2%),
It is added in ammonia spirit, obtains mixture one；
Sodium hydroxide, mass concentration are that 70% solution of ferrous chloride and ethyl alcohol mix, obtain mixture two by step 2；
Mixture one and mixture two are uniformly mixed by step 3, and reaction kettle is added, cooling in 250 DEG C of heat preservation 7h, standby
With；The reaction kettle is the hydrothermal reaction kettle containing polytetrafluoroethyllining lining
Step 4 is heated to 140 DEG C of evaporations, finally forms thin film in container bottom；
Step 5 pressurizes to film, forms the film with a thickness of 0.2-0.5mm.
Performance test: being fixed to oily-water seperating equipment for the present invention, carries out oil-water separation test (oil is hexamethylene):
| Water-oil separating rate % | |
| Embodiment 1 | 99.8 |
| Embodiment 2 | 99.3 |
| Embodiment 3 | 99.7 |
| Embodiment 4 | 99.6 |
| Reference examples 1 | 81.2 |
As can be seen from the table, chitosan of the invention sufficiently adheres on montmorillonite surface, and separative efficiency is high.Calcium chloride is molten
The stability of film can be improved in liquid, is convenient for subsequent pressurized treatments.
The above, preferable specific embodiment only of the invention, the scope of protection of the present invention is not limited to this, any ripe
Know those skilled in the art within the technical scope of the present disclosure, the letter for the technical solution that can be become apparent to
Altered or equivalence replacement are fallen within the protection scope of the present invention.
Claims (5)
1. the preparation method of bionical water-oil separationg film, which comprises the following steps:
Step 1 stirs montmorillonite and chitosan, is added in ammonia spirit, obtains mixture one；
Sodium hydroxide, solution of ferrous chloride and ethyl alcohol are mixed, obtain mixture two by step 2；
Mixture one and mixture two are uniformly mixed by step 3, and reaction kettle is added, cooling in 250-280 DEG C of heat preservation 7-10h,
It is spare；
Calcium chloride solution is added in step 4, is heated to 60~120 DEG C, reacts 10~30min；
Step 5, heating evaporation finally form thin film in container bottom；
Step 6 pressurizes to film, forms the film with a thickness of 0.2-0.5mm.
2. the preparation method of bionical water-oil separationg film according to claim 1, which is characterized in that reaction kettle is to contain poly- four
The hydrothermal reaction kettle of vinyl fluoride liner.
3. the preparation method of bionical water-oil separationg film according to claim 1, which is characterized in that the chitosan dissolution
In the acetic acid solution that mass concentration is 2%.
4. the preparation method of bionical water-oil separationg film according to claim 1, which is characterized in that the frerrous chloride is molten
The mass concentration 70~80% of liquid.
5. the preparation method of bionical water-oil separationg film according to claim 1, which is characterized in that step 5 is heated to 130
~140 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811164099.3A CN109433016A (en) | 2018-10-04 | 2018-10-04 | The preparation method of bionical water-oil separationg film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811164099.3A CN109433016A (en) | 2018-10-04 | 2018-10-04 | The preparation method of bionical water-oil separationg film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109433016A true CN109433016A (en) | 2019-03-08 |
Family
ID=65545705
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811164099.3A Withdrawn CN109433016A (en) | 2018-10-04 | 2018-10-04 | The preparation method of bionical water-oil separationg film |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1916052A (en) * | 2006-08-18 | 2007-02-21 | 天津理工大学 | Method for preparing interpolymer bionic membrane material of poly-asparagine and chitosan |
| US20130052116A1 (en) * | 2009-04-24 | 2013-02-28 | Nathaniel A. Barney | Chitosan films with reduced shrinkage and laminates made therefrom |
| CN103342826A (en) * | 2013-07-10 | 2013-10-09 | 南京林业大学 | Preparation method of chitin nano-fiber/montmorillonite composite membrane material |
| CN103923329A (en) * | 2014-04-25 | 2014-07-16 | 北京航空航天大学 | Super-strength transparent imitated shell composite thin film and preparation method thereof |
| CN105038055A (en) * | 2015-08-06 | 2015-11-11 | 中国人民解放军军械工程学院 | Method for preparing graded carbon fiber-graphene based shell layered bionic electromagnetic shielding film |
| CN105924687A (en) * | 2016-06-07 | 2016-09-07 | 西南科技大学 | Preparation method of anti-radiation biomimetic membrane |
-
2018
- 2018-10-04 CN CN201811164099.3A patent/CN109433016A/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1916052A (en) * | 2006-08-18 | 2007-02-21 | 天津理工大学 | Method for preparing interpolymer bionic membrane material of poly-asparagine and chitosan |
| US20130052116A1 (en) * | 2009-04-24 | 2013-02-28 | Nathaniel A. Barney | Chitosan films with reduced shrinkage and laminates made therefrom |
| CN103342826A (en) * | 2013-07-10 | 2013-10-09 | 南京林业大学 | Preparation method of chitin nano-fiber/montmorillonite composite membrane material |
| CN103923329A (en) * | 2014-04-25 | 2014-07-16 | 北京航空航天大学 | Super-strength transparent imitated shell composite thin film and preparation method thereof |
| CN105038055A (en) * | 2015-08-06 | 2015-11-11 | 中国人民解放军军械工程学院 | Method for preparing graded carbon fiber-graphene based shell layered bionic electromagnetic shielding film |
| CN105924687A (en) * | 2016-06-07 | 2016-09-07 | 西南科技大学 | Preparation method of anti-radiation biomimetic membrane |
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Application publication date: 20190308 |
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