CN108236846A - A kind of polymer compound film and preparation method thereof - Google Patents
A kind of polymer compound film and preparation method thereof Download PDFInfo
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- CN108236846A CN108236846A CN201611224678.3A CN201611224678A CN108236846A CN 108236846 A CN108236846 A CN 108236846A CN 201611224678 A CN201611224678 A CN 201611224678A CN 108236846 A CN108236846 A CN 108236846A
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- polymer compound
- compound film
- film
- casting solution
- cellulose acetate
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- 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
- 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
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
-
- 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
- B01D71/08—Polysaccharides
- B01D71/12—Cellulose derivatives
- B01D71/14—Esters of organic acids
- B01D71/16—Cellulose acetate
Abstract
The present invention relates to environmental monitorings and pollution control technology field, and in particular to a kind of polymer compound film belongs to technology field of membrane materials.The material of polymer compound film of the present invention includes cellulose acetate, acetone, dioxane and magnesium perchlorate, by mass percentage, cellulose acetate 15 25%, acetone 65 80%, dioxane 8 20% and magnesium perchlorate 1 3%.Addition adsorbent is not needed in the polymer compound film of the present invention, pass through the rational proportion of cellulose acetate, solvent and magnesium perchlorate, directly rely on the adsorption capacity of cellulose acetate in itself, improve the structural effectiveness of film, the bioaccumulation efficiency of film is improved, obtains effectively being enriched with the polymer compound film of toxic organic pollutant.
Description
Technical field
The present invention relates to environmental monitorings and pollution control technology field, and in particular to a kind of polymer compound film and its preparation
Method belongs to technology field of membrane materials.
Background technology
With natural or artificial synthesized macromolecule membrane, using outside energy or chemical potential difference as motive force, to bi-component or
The method that multi-component solute is detached with solvent, be classified, purified and is enriched with, is referred to as membrane separation process.Synthesis film can divide
For organic (polymer) film and inoranic membrane, most important one membrane material is organic matter, i.e. polymer or macromolecular.It is so far
Only, applied to most importantly cellulose esters mesentery in industry and laboratory, in addition synthetic polymeric membrane such as aliphatic and fragrance
The research of polyamide film, fragrance-heterocyclic polymer film, ionic film, polyvinyl and co-polymer membrane, PS membrane etc. is near
Also there is very big development over year.In recent years, with the introduction of technology and the acquirement of the successes achieved in research, the effective UF membrane of a batch
Device gradually has been widely used in fields such as water process, industrial separation, wastewater treatment, laboratory separation.
Can only pointedly therefrom select some emphasis since toxic pollutant is numerous in environmental monitoring
Pollutant is controlled.But the ratio that some toxic organic pollutants account for is less, but endanger it is but very big, have potential ecology and
Health threat, such as most carcinogenic substances belong to organic matter.
Traditional sample concentration pretreatment technology mainly generally uses water using active enrichment process, such as environmental monitoring department
Sample liquid/liquid extraction, XAD resin absorption, solid phase extraction, precipitation method etc..These methods are little for content in water body, have tired
Product property, the big lipophilicity toxic organic pollutant accumulation ability of risk of toxicity is poor, far can not meet low detection limits, high enrichment
The requirement of amount or there are a large amount of matrix interferences analysis measure the phenomenon that.
Invention content
The purpose of the present invention is be directed to the above-mentioned problems in the prior art, it is proposed that one kind can effectively be enriched with toxic
The polymer compound film of organic pollution.
The above-mentioned purpose of the present invention is achieved through the following technical solutions：A kind of polymer compound film, polymer compound film
Material includes cellulose acetate, acetone, dioxane and magnesium perchlorate, by mass percentage, cellulose acetate 15-25%,
Acetone 65-80%, dioxane 8-20% and magnesium perchlorate 1-3%.
Containing neutral esters as adsorbent in polymer compound film of the prior art, as glycerol trioleate or/
With phosphoglyceride, iron/aluminium compound, and addition adsorbent is not needed in the polymer compound film of the present invention, it is fine to pass through acetic acid
The rational proportion of dimension element, solvent and magnesium perchlorate directly by the adsorption capacity of cellulose acetate in itself, improves the structure effect of film
Energy improves the bioaccumulation efficiency of film, obtains effectively being enriched with the polymer compound film of toxic organic pollutant.It is and if multiple in the present invention
Cost can not only be increased by closing addition ester in film, can reduce the basic physicochemical property of film instead, and then reduce the structural effectiveness of film, drop
The bioaccumulation efficiency of low film.
Preferably, the polymer compound film material is by mass percentage, cellulose acetate 18%, acetone 70%,
Dioxane 10% and magnesium perchlorate 2%.
Preferably, the polymer compound film material is by mass percentage, cellulose acetate 24%, acetone 65%,
Dioxane 8.8% and magnesium perchlorate 2.2%.
Preferably, the thickness of the polymer compound film is 45-70 μm, porosity 48-60%.If the thickness mistake of film
It is low or excessive, then it can not achieve enrichment toxic organic pollutant.
Preferably, the water content of the polymer compound film is 55-62%, elongation at break 8-12.8%, stretch
Intensity is 2.8-5.0kg.The mechanical effect of polymer compound film of the present invention is higher, and may be such that in practical application in the wild has not
The advantage of destructible.
The preparation method of the polymer compound film of the present invention, includes the following steps：
S1, casting solution is prepared：By the mass percent weighing of above-mentioned polymer compound film raw material, the material weighed up is mixed and is matched
Casting solution is made；
S2, casting solution is homogenized：By casting solution, isothermal vibration to film liquid is completely dissolved to obtain uniform casting film at 15-25 DEG C
Liquid；
S3, film：Uniform casting solution using L-S phase inversion methods is film-made, evaporates 25-40s at 18-28 DEG C；
S4, coagulating bath：The film liquid layer prepared in step S3 is immersed in temperature to impregnate 6- in 20-30 DEG C of weak aqua ammonia
15min, secure satisfactory grades sub- composite membrane.
The polymer compound film of the present invention has the application of enrichment toxic organic pollutant.
Polymer compound film of the present invention does not need to addition adsorbent, passes through the conjunction of cellulose acetate, solvent and magnesium perchlorate
Reason proportioning is on the one hand frame material using cellulose acetate family macromolecule directly by the adsorption capacity of cellulose acetate in itself
Material, while using the absorption property that high molecular material has in itself to Adsorption of Organic, the nanoscale aperture on film causes
The molecule of free solubilised state can enter, other are incorporated in cannot enter on particulate matter or Dissolved Organic Matter.The height of the present invention
Molecular compound film material has very strong adsorption capacity to organic pollution, is because organic pollution easily enters quilt in film
High molecular material is adsorbed.It, can be easily by the organic contamination of absorption using organic solvent such as n-hexane etc. by the similar principle that mixes
Object elutes, and after taking out film, can measure organic pollution concentration in organic solvent.According to the exhausted of recycling organic pollution
To the volume of content and raw water sample, the organic pollution concentration in raw water sample can obtain.
Compared with prior art, polymer compound film of the present invention is substantially increased by the proportioning of material to having in water body
The adsorption capacity of malicious organic pollution.
Description of the drawings
Fig. 1 is the electron-microscope scanning figure of polymer compound film of the present invention.
Fig. 2 is absorption dynamics curve of the polymer compound film of the present invention to six kinds of organo-chlorine pesticides.
Specific embodiment
The following is specific embodiments of the present invention, and technical scheme of the present invention is further described, but the present invention is simultaneously
It is not limited to these embodiments.
Embodiment 1
Prepare casting solution：By the mass percent weighing of polymer compound film raw material：Cellulose acetate 18%, acetone
The material weighed up is hybridly prepared into casting solution by the 70%th, dioxane 10% and magnesium perchlorate 2%；
Homogenize casting solution：By casting solution, isothermal vibration to film liquid is completely dissolved to obtain uniform casting solution at 24 DEG C；
Film：Uniform casting solution using L-S phase inversion methods is film-made, film liquid is poured on scraper plate and scrapes 45-70 μ m-thicks
Film liquid layer, evaporate 35s at 26 DEG C；
Coagulating bath：The related scraper plate of film liquid layer is immersed in temperature in 28 DEG C of weak aqua ammonias, to impregnate 8min together, it is washed to obtain
Polymer compound film of the present invention.After tested, the thickness of the polymer compound film is 45-70 μm, porosity 60%, and water content is
61%, elongation at break 12.5%, tensile strength 4.8kg.
Embodiment 2
Prepare casting solution：By the mass percent weighing of polymer compound film raw material：Cellulose acetate 24%, acetone
The material weighed up is hybridly prepared into casting solution by the 65%th, dioxane 8.8% and magnesium perchlorate 2.2%；
Homogenize casting solution：By casting solution, isothermal vibration to film liquid is completely dissolved to obtain uniform casting solution at 22 DEG C；
Film：Uniform casting solution using L-S phase inversion methods is film-made, film liquid is poured on scraper plate and scrapes 45-70 μ m-thicks
Film liquid layer, evaporate 35s at 22 DEG C；
Coagulating bath：The related scraper plate of film liquid layer is immersed in temperature in 22 DEG C of weak aqua ammonias, to impregnate 12min together, it is washed
Obtain polymer compound film of the present invention.After tested, the thickness of the polymer compound film is 45-70 μm, porosity 58%, water content
It is 62%, elongation at break 11.8%, tensile strength 5.0kg.
Embodiment 3
Prepare casting solution：By the mass percent weighing of polymer compound film raw material：Cellulose acetate 15-25%, acetone
The material weighed up is hybridly prepared into casting solution by 65-80%, dioxane 8-20% and magnesium perchlorate 1-3%；
Homogenize casting solution：By casting solution, isothermal vibration to film liquid is completely dissolved to obtain uniform casting solution at 20 DEG C；
Film：Uniform casting solution using L-S phase inversion methods is film-made, film liquid is poured on scraper plate and scrapes 45-70 μ m-thicks
Film liquid layer, evaporate 30s at 20 DEG C；
Coagulating bath：The related scraper plate of film liquid layer is immersed in temperature in 25 DEG C of weak aqua ammonias, to impregnate 6min together, it is washed to obtain
Polymer compound film of the present invention.After tested, the thickness of the polymer compound film is 45-70 μm, porosity 59%, and water content is
61%, elongation at break 12.8%, tensile strength 4.4kg.
Embodiment 4
Prepare casting solution：By the mass percent weighing of polymer compound film raw material：Cellulose acetate 15-25%, acetone
The material weighed up is hybridly prepared into casting solution by 65-80%, dioxane 8-20% and magnesium perchlorate 1-3%；
Homogenize casting solution：By casting solution, isothermal vibration to film liquid is completely dissolved to obtain uniform casting solution at 18 DEG C；
Film：Uniform casting solution using L-S phase inversion methods is film-made, film liquid is poured on scraper plate and scrapes 45-70 μ m-thicks
Film liquid layer, evaporate 25s at 28 DEG C；
Coagulating bath：The related scraper plate of film liquid layer is immersed in temperature in 20 DEG C of weak aqua ammonias, to impregnate 15min together, it is washed
Obtain polymer compound film of the present invention.After tested, the thickness of the polymer compound film is 45-70 μm, porosity 52%, water content
It is 56%, elongation at break 11.5%, tensile strength 3.5kg.
Embodiment 5
Prepare casting solution：By the mass percent weighing of polymer compound film raw material：Cellulose acetate 15-25%, acetone
The material weighed up is hybridly prepared into casting solution by 65-80%, dioxane 8-20% and magnesium perchlorate 1-3%；
Homogenize casting solution：By casting solution, isothermal vibration to film liquid is completely dissolved to obtain uniform casting solution at 25 DEG C；
Film：Uniform casting solution using L-S phase inversion methods is film-made, film liquid is poured on scraper plate and scrapes 45-70 μ m-thicks
Film liquid layer, evaporate 40s at 18 DEG C；
Coagulating bath：The related scraper plate of film liquid layer is immersed in temperature in 30 DEG C of weak aqua ammonias, to impregnate 6min together, it is washed to obtain
Polymer compound film of the present invention.After tested, the thickness of the polymer compound film is 45-70 μm, porosity 54%, and water content is
57%, elongation at break 11.2%, tensile strength 3.8kg.
Application Example
Polymer compound film in embodiment 1-5 is used to be enriched with to the application of toxic organic pollutant.
Performance test
1st, polymer compound film obtained in embodiment 1 is subjected to electron-microscope scanning, as shown in Figure 1.It can be obtained from Fig. 1, this
The compactness of invention polymer compound film is good, uniform surface.
2nd, a concentration of 500ng/L of indoor simulation organo-chlorine pesticide is tested, constant temperature extracting experiment is carried out on shaking table, is stood sudden and violent
Dew 2,4,6,8,10h, takes out polymer compound film of the invention in 3 embodiments 1, and all enrichment experiments take every 1h to replace
The mode of solution.Polymer compound film is dialysed for 24 hours through n-hexane, and analyzing organo-chlorine pesticide in n-hexane with GC-ECD contains
Amount, the results are shown in Figure 2.
The capillary chromatographic column using two kinds of opposed polarities is tested, analysis condition is as follows：Carrier gas：High pure nitrogen；Detector (μ
ECD) make-up gas：High pure nitrogen, make-up gas flow 30mL/min.Chromatographic column：SPB-1701 capillary chromatographic columns (30m ×
0.25mm×0.25m).Post case uses temperature programming：Begin 60 DEG C of temperature, keeps 2min；Then the heating of the first rank is with 20 DEG C/min liters
To 160 DEG C；Second-order heating rises to 260 DEG C, then keep 5min with 4 DEG C/min.Corresponding injector temperature：200℃；Injection port is adopted
With constant current mode, flow velocity 0.9mL/min, linear velocity 27cm/s, Splitless injecting-Sample 1L.Corresponding detector temperature：280℃.
As can be seen from Figure 2, polymer compound film of the invention has very such as organo-chlorine pesticide of toxic organic pollutant in water body
Strong adsorption capacity, it is every to endrin (endrin), drinox (aldrin), β-six six six, γ-six six six and Heptachlor epoxide
Gram film distinguishes adsorbable 164.7ng, 101.5ng, 94.3ng, 71.3ng, 116.1ng per hour.
Specific embodiment described herein is only an example for the spirit of the invention.Technology belonging to the present invention is led
The technical staff in domain can do various modifications or supplement to described specific embodiment or substitute in a similar way, but simultaneously
The spirit or beyond the scope of the appended claims of the present invention is not deviated by.
It is skilled to this field although having been made a detailed description to the present invention and being cited some specific embodiments
For technical staff, as long as it is obvious that can make various changes or correct without departing from the spirit and scope of the present invention.
Claims (7)
1. a kind of polymer compound film, which is characterized in that the material of polymer compound film includes cellulose acetate, acetone, dioxy
Six rings and magnesium perchlorate, by mass percentage, cellulose acetate 15-25%, acetone 65-80%, dioxane 8-20% and
Magnesium perchlorate 1-3%.
2. polymer compound film according to claim 1, which is characterized in that the polymer compound film material presses quality hundred
Divide than meter, cellulose acetate 18%, acetone 70%, dioxane 10% and magnesium perchlorate 2%.
3. polymer compound film according to claim 1, which is characterized in that the polymer compound film material presses quality hundred
Divide than meter, cellulose acetate 24%, acetone 65%, dioxane 8.8% and magnesium perchlorate 2.2%.
4. according to the polymer compound film described in claims 1 or 2 or 3, which is characterized in that the thickness of the polymer compound film
It is 45-70 μm, porosity 48-60%.
5. according to the polymer compound film described in claims 1 or 2 or 3, which is characterized in that the polymer compound film it is aqueous
It measures as 55-62%, elongation at break 8-12.8%, tensile strength 2.8-5.0kg.
6. a kind of preparation method of polymer compound film as described in claim 1, which is characterized in that the method is included such as
Lower step：
S1, casting solution is prepared：By the mass percent weighing of above-mentioned polymer compound film raw material, the material weighed up is hybridly prepared into
Casting solution；
S2, casting solution is homogenized：By casting solution, isothermal vibration to film liquid is completely dissolved to obtain uniform casting solution at 15-25 DEG C；
S3, film：Uniform casting solution using L-S phase inversion methods is film-made, evaporates 25-40s at 18-28 DEG C；
S4, coagulating bath：The film liquid layer prepared in step S3 is immersed in temperature to impregnate 6-15min in 20-30 DEG C of weak aqua ammonia, is obtained
Polymer compound film.
7. polymer compound film as described in claim 1 has the application of enrichment toxic organic pollutant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611224678.3A CN108236846A (en) | 2016-12-27 | 2016-12-27 | A kind of polymer compound film and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611224678.3A CN108236846A (en) | 2016-12-27 | 2016-12-27 | A kind of polymer compound film and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN108236846A true CN108236846A (en) | 2018-07-03 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201611224678.3A Pending CN108236846A (en) | 2016-12-27 | 2016-12-27 | A kind of polymer compound film and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109265833A (en) * | 2018-09-29 | 2019-01-25 | 桐城市强峰包装有限公司 | It is a kind of for being injected intravenously the composite membrane outer cover of plastic containers insert port |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1395983A (en) * | 2002-08-26 | 2003-02-12 | 中国科学院生态环境研究中心 | Preparing process and application of composite biolipid/cellulose acetate membrane |
| CN1640531A (en) * | 2004-01-13 | 2005-07-20 | 中国科学院生态环境研究中心 | Acetyl cellulose/Fe-Al oxide composite membrane, and its preparing method and use |
| US9192894B2 (en) * | 2012-06-11 | 2015-11-24 | Enerage Inc. | Electrochemical separation membrane and the manufacturing method thereof |
-
2016
- 2016-12-27 CN CN201611224678.3A patent/CN108236846A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1395983A (en) * | 2002-08-26 | 2003-02-12 | 中国科学院生态环境研究中心 | Preparing process and application of composite biolipid/cellulose acetate membrane |
| CN1640531A (en) * | 2004-01-13 | 2005-07-20 | 中国科学院生态环境研究中心 | Acetyl cellulose/Fe-Al oxide composite membrane, and its preparing method and use |
| US9192894B2 (en) * | 2012-06-11 | 2015-11-24 | Enerage Inc. | Electrochemical separation membrane and the manufacturing method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 代瑞华等: "醋酸纤维素吸附剂的制备及其性能表征", 《环境科学》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109265833A (en) * | 2018-09-29 | 2019-01-25 | 桐城市强峰包装有限公司 | It is a kind of for being injected intravenously the composite membrane outer cover of plastic containers insert port |
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