CN108816055A - A kind of preparation method of biodegradable water-oil separating perforated membrane - Google Patents
A kind of preparation method of biodegradable water-oil separating perforated membrane Download PDFInfo
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- CN108816055A CN108816055A CN201810724501.2A CN201810724501A CN108816055A CN 108816055 A CN108816055 A CN 108816055A CN 201810724501 A CN201810724501 A CN 201810724501A CN 108816055 A CN108816055 A CN 108816055A
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- polylactic acid
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- film
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- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000012528 membrane Substances 0.000 title claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 38
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 36
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910002012 Aerosil® Inorganic materials 0.000 claims abstract description 21
- 229920006381 polylactic acid film Polymers 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000006185 dispersion Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 239000004626 polylactic acid Substances 0.000 claims abstract description 11
- 229920000747 poly(lactic acid) Polymers 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 238000005266 casting Methods 0.000 claims abstract description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000004090 dissolution Methods 0.000 claims abstract description 4
- 239000011521 glass Substances 0.000 claims abstract description 4
- 230000006698 induction Effects 0.000 claims abstract description 3
- 238000005191 phase separation Methods 0.000 claims abstract description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 20
- 235000019441 ethanol Nutrition 0.000 claims description 17
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- 229910052681 coesite Inorganic materials 0.000 claims description 10
- 229910052906 cristobalite Inorganic materials 0.000 claims description 10
- 235000006408 oxalic acid Nutrition 0.000 claims description 10
- 229910052682 stishovite Inorganic materials 0.000 claims description 10
- 229910052905 tridymite Inorganic materials 0.000 claims description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
- 229960004756 ethanol Drugs 0.000 claims description 7
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 230000003075 superhydrophobic effect Effects 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 239000000908 ammonium hydroxide Substances 0.000 claims description 4
- 238000001879 gelation Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000007711 solidification Methods 0.000 claims description 3
- 230000008023 solidification Effects 0.000 claims description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 244000025254 Cannabis sativa Species 0.000 claims 1
- 241000790917 Dioxys <bee> Species 0.000 claims 1
- 229910003978 SiClx Inorganic materials 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 238000007654 immersion Methods 0.000 claims 1
- 238000000352 supercritical drying Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000010409 thin film Substances 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 13
- 239000010408 film Substances 0.000 description 12
- 238000000926 separation method Methods 0.000 description 10
- 235000019198 oils Nutrition 0.000 description 9
- 239000004094 surface-active agent Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000010586 diagram Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 235000019476 oil-water mixture Nutrition 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 1
- GHQPBDDZGPAVJP-UHFFFAOYSA-N azanium;methanol;hydroxide Chemical compound N.O.OC GHQPBDDZGPAVJP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 229920001600 hydrophobic polymer Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000002120 nanofilm Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000007762 w/o emulsion Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
-
- 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
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
-
- 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
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/48—Polyesters
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/38—Hydrophobic membranes
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Silicon Compounds (AREA)
- Biological Depolymerization Polymers (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention provides a kind of preparation method of biodegradable water-oil separating perforated membrane, using ethyl orthosilicate and methanol solution as raw material, silica dioxide gel is prepared using sol-gal process, after then carrying out hydrophobically modified to it, supercritical drying obtains aerosil.This aeroge is added in ethanol solution, aerosil/alcohol dispersion liquid is made, for use;Polylactic acid film is prepared using non-solvent induction phase separation method later, in a solvent by the dissolution of pretreated polylactic acid, constant temperature stirs to get casting solution, casting solution is poured on to clean glass plate surface, after certain thickness scraper knifing, preforming polylactic acid film is immersed in the alcohol dispersion liquid containing aerosil, aerosil@polylactic acid film is obtained after curing and drying.This thin film preparation process is simple, has excellent water-oil separating performance, and biodegradable after use, has broad application prospects.
Description
Technical field
The invention belongs to polymeric material fields, and in particular to it is a kind of low cost, can be prepared on a large scale super-hydrophobic-super oleophylic
The preparation method of polymer porous film.This perforated membrane can be used for separating the separation of the oil hydrosol of addition surfactant.
Background technique
Currently, most based superhydrophobic thin films (such as polyvinylidene difluoride film, polypropylene film) are with higher on the market
Oil-water selectivity and brilliance separating effect the features such as, but the hydrophobic polymer film of most water-oil separating is
High molecular material, it is long etc. to be difficult to the time degraded or degraded in the natural environment, and the reusable property of film compared with
Difference is easy to generate secondary pollution etc. after usage, and the processing of waste polymer film is difficult, further increases processing oil
The cost of aqueous mixtures.Therefore, more and more researchers begin to focus on can natural degradation material research and development, develop one kind
Biodegradable high molecular film material has become the important mode that material generates secondary pollution that solves.
In recent decades, the performance excellent due to poly-lactic acid material, such as excellent physical and mechanical property, it is preferable to extend
Degree and tensile strength, it is easily processed into type the advantages that, be always considered as most promising environment-friendly materials, and material itself
With certain hydrophobicity (being 79 ° to the contact angle of water in air under room temperature), also it is expected to develop into special wellability
Biodegradable separation material.There is stabilization however, still lacking general and easy method at present and carrying out large scale preparation
Surface wettability, high mechanical stability, can practical application efficient polylactic acid separation material.And aerosil due to
Its highly porous three-dimensional structure, numerous micro/nano level gaps and show unique property, micro nano structure can will be empty
Gas captures and shows super-hydrophobic feature.But since the intensity of network of silica is low, application receives great limit
System.Therefore one kind is biodegradable and can be had broad application prospects with the water-oil separating film that iterative cycles utilize.
Summary of the invention
The invention proposes a kind of low cost, super-hydrophobic-super lipophilic polymer of biodegradable that can be prepared on a large scale are more
The method of pore membrane.Main preparation step is as follows:
(1) aerosil/alcohol dispersion liquid preparation:Aerosil is prepared using sol-gal process,
Ethyl orthosilicate is dissolved in methanol first, stirs a period of time after oxalic acid solution is added.Then, it is added and contains a certain amount of ammonium hydroxide
Methanol solution, and the solution is futher stirred, finally, by solution gel at a constant temperature.SiO2After gelation, take a certain amount of
Dehydrated alcohol be added in gel, and replace at a constant temperature, remove oxalic acid and unreacted chemical substance etc., be added later suitable
Ethyl alcohol/n-hexane mixed solution containing trim,ethylchlorosilane of amount is to SiO2Hydrophobically modified is carried out, ethanol washing processing is repeated
Four times to ensure to completely remove oxalic acid and other chemical residues etc..After washing, gel is subjected to supercritical drying, is crushed simultaneously
Appropriate dehydrated alcohol is added, it is uniform by stirring and ultrasonic disperse, SiO is made2Aeroge/alcohol dispersion liquid.
(2) preparation of aerosil@polylactic acid film:It is thin using non-solvent induction phase separation method preparation polylactic acid
Film, in a solvent by the dissolution of pretreated polylactic acid, constant temperature stir to get casting solution, stand under certain temperature and remove bubble.
Casting solution is poured on to clean glass plate surface, after certain thickness scraper knifing, preforming polylactic acid film is immersed
In alcohol dispersion liquid containing aerosil, solidification obtains polylactic acid super-hydrophobic film, is finally dried in vacuo.
Preferred ethyl orthosilicate in step (1) in the present invention, methanol, oxalic acid solution (10mmol/L) volume ratio be 1:
2:0.5;The volume ratio of ammonium hydroxide (20%) and methanol is 1:6;Gelling temp is 25-50 DEG C, gel time 0.5-2h, time swap
6-10h;Gel is crushed to later and is added appropriate dehydrated alcohol, content, which can uniformly be made, by stirring and ultrasonic disperse is
Aerosil/alcohol dispersion liquid of 0.1%-5%.
The solvent for preferably dissolving polylactic acid in the present invention in step (2) is N-Methyl pyrrolidone, content 0.5%-
4%, the temperature of constant temperature stirring is 80-100 DEG C, mixing time 10-12h, later the standing 6h removal bubble at 80 DEG C, after knifing
It is dried in vacuo for 24 hours at 40 DEG C.Compared with the material with unique wellability reported before, film prepared by the present invention has
Following beneficial effect:
(1) super-hydrophobic-super oleophylic Biodegradable film of the present invention has wider application range, such as oil water mixture
Separation, the separation without the stable oil hydrosol of surfactant and surfactant;
(2) there is economic convenient preparation process;
(3) present invention has selected the polylactic acid with biodegradable characteristics as raw material, more biological environmental production, and
Being finished biodegradable can not will form white garbage.
Detailed description of the invention
Fig. 1 is the scanning electron microscope diagram piece of aerosil@polylactic acid film in embodiment 1;
Fig. 2 is the scanning electron microscope diagram piece of aerosil@polylactic acid film in embodiment 2;
Fig. 3 is the scanning electron microscope diagram piece of aerosil@polylactic acid film in embodiment 3;
Fig. 4 is the oil-water separation figure of aerosil@polylactic acid film in embodiment 2;
Fig. 5 is the microscope photo in embodiment 2 after the water-oil separating of aerosil@polylactic acid film in water.
Specific embodiment
Technical solution of the present invention is described in detail below by specific embodiment, but the scope of the present invention
It is not restricted by the embodiments.
Embodiment 1-3
(1)SiO2The preparation of aeroge/alcohol dispersion liquid
1ml ethyl orthosilicate is dissolved in 2ml methanol, and is slowly added to 0.5ml oxalic acid solution into the mixture, and stir
Mix 30min.Then, the methanol solution 5ml for containing 0.6ml ammonium hydroxide (20%) will be added, and the solution is futher stirred
15min forms gel after solution is placed 1h at 25 DEG C.After gelation, 20ml dehydrated alcohol is added in gel, and
At 25 DEG C replace 6h remove oxalic acid and unreacted chemical substance etc., later be added 5ml containing 5% trim,ethylchlorosilane ethyl alcohol/
The mixed solution of n-hexane repeats ethanol washing and handles four times to ensure to completely remove oxalic acid and other chemical residues etc..
After washing, SiO2 aeroge is obtained by supercritical drying, appropriate dehydrated alcohol is added in gained SiO2 aeroge, passes through stirring
It is uniform with ultrasonic disperse, it is respectively prepared 0.1%, 0.5%, 1% SiO2Aeroge/alcohol dispersion liquid.
(2) preparation of aerosil@polylactic acid film
The pretreated polylactic acid of 1g is dissolved in 100gNMP solvent, continued mechanical stirring 12h is obtained at 85 DEG C
Even casting solution, 80 DEG C of standing 8h remove bubble, casting solution are poured on to clean glass plate surface, is scraped with 200 μ m-thick scrapers
After film, preforming polylactic acid film is immersed respectively contain 0.1%, 0.5% at once, the ethyl alcohol of 1% aerosil
In dispersion liquid, solidification obtains aerosil@polylactic acid film, is dried in vacuo at 40 DEG C and obtains finished product for 24 hours.Then it is surveyed
Surface texture and contact angle, and its mechanical property is tested, specific data are shown in Table 1.
For the oil and water separation capability for testing super-hydrophobic film, the present invention is prepared for having nanoscale and micro- containing surfactant
The water-in-oil emulsion of meter level drop size.For common oil water mixture (such as oil slick), common super hydrophobic material
Realize the separation of oil with water.And for oil hydrosol (especially adding the oil hydrosol of surfactant), common is super thin
Limitation of the water material due to itself aperture, it is difficult to realize the separation of oil hydrosol.The present invention is with thin with embodiment 2- polylactic acid
Film and 0.5%SiO2Water-oil separating experiment is carried out for the film obtained after airsetting alcohol dispersion liquid is compound, as shown in figure 4, point
From the white emulsion form of oil water mixture preceding plus that surfactant is stable, and collected filtrate becomes colorless after separating
Bright liquid does not observe that Fig. 5 is shown in the presence of micro/nano level drop from microscope, realizes the grease cream containing surfactant
The separation of liquid.
Table 1
Project | Embodiment 1 | Embodiment 2 | Embodiment 3 |
SiO2Aeroge mass fraction/% | 0.1% | 0.5% | 1% |
Contact angle/° | 148 | 156 | 157 |
Tensile strength/MPa | 12.0 | 11.5 | 10.8 |
Elongation at break/% | 5.5 | 4.5 | 3.8 |
Claims (3)
1. a kind of preparation method of biodegradable water-oil separating perforated membrane, which is characterized in that preparation method is as follows:(1) dioxy
The preparation of SiClx aeroge/alcohol dispersion liquid:Aerosil is prepared using sol-gal process, first by ethyl orthosilicate
It is dissolved in methanol, stirs a period of time after oxalic acid solution is added;Then the methanol solution for containing a certain amount of ammonium hydroxide is added, and should
Solution futher stirs, by solution gel at a constant temperature;SiO2After gelation, a certain amount of dehydrated alcohol is taken to be added to gel
In, and replace at a constant temperature, remove oxalic acid and unreacted chemical substance etc., is added later suitable containing trim,ethylchlorosilane
Ethyl alcohol/n-hexane mixed solution is to SiO2Hydrophobically modified is carried out, ethanol washing is repeated and handles four times to ensure to completely remove grass
Gel, after washing, is crushed and is added appropriate dehydrated alcohol by acid and other chemical residues, equal by stirring and ultrasonic disperse
It is even, SiO is made2Aeroge/alcohol dispersion liquid;
(2) preparation of aerosil@polylactic acid film:Polylactic acid film is prepared using non-solvent induction phase separation method,
In a solvent by the dissolution of pretreated polylactic acid, constant temperature stirs to get casting solution, stands under certain temperature and removes bubble, will cast
Film liquid is poured on clean glass plate surface, and after certain thickness scraper knifing, the immersion of preforming polylactic acid film is contained
In the alcohol dispersion liquid of aerosil, solidification obtains polylactic acid super-hydrophobic film, is finally dried in vacuo.
2. a kind of preparation method of biodegradable water-oil separating perforated membrane according to claim 1, which is characterized in that
Ethyl orthosilicate in step (1), methanol, oxalic acid solution (10mmol/L) volume ratio be 1:2:0.5;Ammonium hydroxide (20%) and methanol
Volume ratio be 1:6;Gelling temp is 25-50 DEG C, gel time 0.5-2h, time swap 6-10h.
3. a kind of preparation method of biodegradable water-oil separating perforated membrane according to claim 1, which is characterized in that
The solvent of dissolution polylactic acid is N-Methyl pyrrolidone in step (2), and content 0.5%-4%, the temperature of constant temperature stirring is 80-
100 DEG C, mixing time 10-12h, 6h is stood at 80 DEG C later and removes bubble, is dried in vacuo for 24 hours at 40 DEG C after knifing.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114410090A (en) * | 2022-01-25 | 2022-04-29 | 高国惠 | Preparation method of packaging film |
CN114425269A (en) * | 2022-01-26 | 2022-05-03 | 武汉纺织大学 | Efficient oil-water separation composite foam based on surface engineering and preparation method thereof |
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CN114410090A (en) * | 2022-01-25 | 2022-04-29 | 高国惠 | Preparation method of packaging film |
CN114410090B (en) * | 2022-01-25 | 2023-08-15 | 佛山市顺德区建德包装实业有限公司 | Preparation method of packaging film |
CN114425269A (en) * | 2022-01-26 | 2022-05-03 | 武汉纺织大学 | Efficient oil-water separation composite foam based on surface engineering and preparation method thereof |
CN114425269B (en) * | 2022-01-26 | 2023-12-22 | 武汉纺织大学 | High-efficiency oil-water separation composite foam based on surface engineering and preparation method thereof |
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