CN108034069A - A kind of phenylacetyl cellulose acetate ordered porous membrane material and preparation method thereof - Google Patents
A kind of phenylacetyl cellulose acetate ordered porous membrane material and preparation method thereof Download PDFInfo
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- CN108034069A CN108034069A CN201711438616.7A CN201711438616A CN108034069A CN 108034069 A CN108034069 A CN 108034069A CN 201711438616 A CN201711438616 A CN 201711438616A CN 108034069 A CN108034069 A CN 108034069A
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- phenylacetyl
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
- C08J9/286—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum the liquid phase being a solvent for the monomers but not for the resulting macromolecular composition, i.e. macroporous or macroreticular polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B3/00—Preparation of cellulose esters of organic acids
- C08B3/06—Cellulose acetate, e.g. mono-acetate, di-acetate or tri-acetate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B3/00—Preparation of cellulose esters of organic acids
- C08B3/22—Post-esterification treatments, including purification
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/05—Elimination by evaporation or heat degradation of a liquid phase
- C08J2201/0502—Elimination by evaporation or heat degradation of a liquid phase the liquid phase being organic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/10—Esters of organic acids
- C08J2301/12—Cellulose acetate
Abstract
The present invention relates to a kind of phenylacetyl cellulose acetate ordered porous membrane material and preparation method thereof.The material is phenylacetyl cellulose acetate, the material under high humidity conditions can high-efficient simple form ordered porous structural, there is the characteristic for easily forming ordered porous membrane.And; the phenylacetyl cellulose acetate ordered porous membrane material of the present invention has abundance, environmental-friendly, pollution-free; the features such as membrane material preparation method for material is simple, method for preparing porous film is easy, the perforated membrane degree of order is high, can meet the needs of different field application.
Description
Technical field
The present invention relates to a kind of cellulose derivative ordered porous membrane material and preparation method thereof.
Background technology
Thin polymer film with micro nano structure is in biomaterial, photoelectric material etc. all with critically important application
Value, so as to be widely studied and apply.In the past, different template sides can be used by preparing the film with micro nano structure
Method, such as the template such as Colloidal crystals, emulsion droplet, biological bacterium and filter membrane, but since its preparation process is complicated, template size
Fixed, template prepares the reasons such as difficulty, therefore hardly results in the film with adjustable dimension or single dispersing structure.In recent years,
Preparing under high humidity conditions for Widawski G.. Rawiso M. and Francois B. reports is thin with microstructure
The new method of film【Self-Organized Honeycomb Morphology of Star-Polymer Polystyrene
Films. Nature 369, 387~389(1994)】Gradually developed, and because it is simple controllable, be increasingly subject to people
Concern【Breath figures as a dynamic templating method for polymers and
nanomaterials. Advanced Materials 18, 973~989(2006)】.By this method, can utilize not
The perforated membrane of high-sequential is prepared with polymer【Formation of honeycomb-structured, porous
films via breath figures with different polymer architectures. Journal of
Polymer Science Part A: Polymer Chemistry 44, 2363~2375(2006)】。
Cellulose is nature natural polymer the abundantest, its most important application is exactly to be used as film material
Material, such as regenerated cellulose have been widely applied to film and many fields of porous material【Morphology and
permeability of cellulose/chitin blend membranes. Journal of Membrane Science
287, 19~28(2007)】.However, the cellulose base film of orderly pore structure is hardly resulted in using simple cellulosic structure,
Application of the cellulosic material in film applications is hindered significantly.By varying the structure of cellulose, be expected to for cellulose it is more in order
The preparation of pore membrane provides a kind of new way.However, the cellulosic material species for being used to prepare ordered porous membrane is few and structure compared with
Complexity, greatly limit application of such cellulosic material in different field.
The content of the invention
The purpose of the present invention is to provide a kind of phenylacetyl cellulose acetate ordered porous membrane material.
Another object of the present invention is to provide a kind of preparation side of phenylacetyl cellulose acetate ordered porous membrane material
Method.
It is still another object of the present invention to provide the letter that a kind of phenylacetyl cellulose acetate material prepares ordered porous membrane
Just method.
The cellulose derivative material for being used to prepare ordered porous membrane of the present invention is phenylacetyl cellulose acetate, it is tied
Structure formula is：
Wherein：
R1For CH3CO；
R2For CH3CO、C6H5CH2CO or H；
In R1And R2Three substituents in, preferable CH3CO、C6H5CH2The substitution value of tri- kinds of different substituents of CO and H is：
CH3The substitution value of CO is greater than or equal to 2, C6H5CH2Substitution value of the substitution value of CO equal to or more than 0.1, H is less than or equal to
0.4。
The preparation method of the phenylacetyl cellulose acetate material for being used to prepare ordered porous membrane of the present invention includes following
Step：
Under 25 ~ 50 degrees Celsius, cellulose acetate is fully dissolved in tetrahydrofuran, pyridine, triethylamine acid binding agent are added, in ice
Tetrahydrofuran solution under water-bath with phenylacetyl halogen reacts, and the molar ratio of hydroxyl and phenylacetyl halogen wherein on cellulose acetate is
1:0.5~1:10；Under ice-water bath reaction 4 ~ 24 it is small when after, in room temperature the reaction was continued 48 ~ 72 it is small when, then add water terminate reaction,
Reaction mixture precipitation, filtering, drying, obtain phenylacetyl cellulose acetate.
The preparation method that ordered porous membrane is prepared using phenylacetyl cellulose acetate ordered porous membrane material of the present invention
Comprise the following steps：
Weigh a certain amount of phenylacetyl cellulose acetate to be dissolved in volatile organic solvent, be made into 0.1~100 g/l
Solution；It is in the environment of 30 ~ 95%, temperature is 0 ~ 50 degree Celsius in relative humidity, phenylacetyl cellulose acetate solution is dripped
It is added in planar substrates, spontaneously dries film forming, obtain the perforated membrane with ordered porous structural.
The phenylacetyl cellulose acetate ordered porous membrane material of the present invention has abundance, environmental-friendly, pollution-free,
The features such as membrane material preparation method for material is simple, method for preparing porous film is easy, the perforated membrane degree of order is high, can meet different field application
Needs.
Brief description of the drawings
When Fig. 1 embodiment of the present invention 1 is used to prepare perforated membrane, its pore structure has high-sequential.
When Fig. 2 embodiment of the present invention 2 is used to prepare perforated membrane, its pore structure has high-sequential.
Embodiment
Embodiment 1：
（1）The preparation of phenylacetyl cellulose acetate
A. 1.0 grams of cellulose acetates are weighed, are added in 18.0 milliliters of tetrahydrofurans, at room temperature stirring and dissolving.
B. after dissolving, 0.4 milliliter of pyridine is added into mixed liquor, is uniformly mixed.
C. tetrahydrofuran solution 2.0 milliliter of the configuration containing 0.2 milliliter of phenyllacetyl chloride, is slowly dropped under ice-water bath and holds
In cellulose acetate/tetrahydrofuran solution of continuous stirring.Drop finishes, continue under ice-water bath stirring 6 it is small when, then continue at room temperature
Stir 48 it is small when.
D. reaction mixture is added to 100 milliliters of water and terminates reaction, obtains precipitated product.
E. precipitated product reuses tetrahydrofuran dissolving, aqueous precipitation, and dissolving repeatedly precipitates three times, is finally placed in 50
It is dry in degree Celsius vacuum drying chamber, obtain phenylacetyl cellulose acetate.
（2）The preparation of phenylacetyl cellulose acetate ordered porous membrane
A. 100 milligrams of phenylacetyl cellulose acetates are weighed, are added in 10 milliliters of dichloromethane, fully dissolving, be made into 10 grams/
The dichloromethane solution risen.
B. in the environment of relative humidity is 70%, temperature is 22 degrees Celsius, the solution obtained in 25 microlitres of step a is measured,
It is added dropwise on the sheet glass cleaned up, spontaneously dries film forming, obtain the poroid film with ordered porous structural.
Embodiment 2：
（1）The preparation process of phenylacetyl cellulose acetate is the same as embodiment 1
A. 2.0 grams of cellulose acetates are weighed, are added in 35.0 milliliters of tetrahydrofurans, at room temperature stirring and dissolving.
B. after dissolving, 1.0 milliliters of pyridine is added into mixed liquor, is uniformly mixed.
C. tetrahydrofuran solution 4.0 milliliter of the configuration containing 1.5 milliliters of phenyllacetyl chlorides, is slowly dropped under ice-water bath and holds
In cellulose acetate/tetrahydrofuran solution of continuous stirring.Drop finish, continue under ice-water bath stirring 12 it is small when, then at room temperature after
When continuous stirring 72 is small.
D. reaction mixture is added to 150 milliliters of water and terminates reaction, obtains precipitated product.
E. precipitated product reuses tetrahydrofuran dissolving, aqueous precipitation, and dissolving repeatedly precipitates three times, is finally placed in 50
It is dry in degree Celsius vacuum drying chamber, obtain phenylacetyl cellulose acetate.
（2）The preparation process of phenylacetyl cellulose acetate ordered porous membrane is the same as embodiment 1
A. 130 milligrams of phenylacetyl cellulose acetates are weighed, are added in 10 milliliters of dichloromethane, fully dissolving, be made into 13 grams/
The dichloromethane solution risen.
B. in the environment of relative humidity is 88%, temperature is 20 degrees Celsius, the solution obtained in 25 microlitres of step a is measured,
It is added dropwise on the sheet glass cleaned up, spontaneously dries film forming, obtain the poroid film with ordered porous structural.
The phenylacetyl cellulose acetate that will be obtained, the wiring solution-forming in easy volatile solvent, in certain relative humidity bar
Solution is dripped under part and is formed a film in sheet glass, during by optical microphotograph sem observation membrane superficial tissue（As shown in Figure 1, Figure 2）, it was demonstrated that its tool
There is the characteristic for easily forming orderly porous membrane structure well, it is simple and convenient that it prepares the process of ordered porous membrane, available for template
With the highly ordered porous materials of the needs such as cell culture growth.
Claims (3)
1. a kind of phenylacetyl cellulose acetate ordered porous membrane material, it is characterized in that, the material is phenylacetyl acetic acid fibre
Dimension element, its structural formula are：
Explanation:Explanation:Explanation:Explanation:Explanation:Explanation:Explanation:Explanation:Explanation:Explanation:Explanation:Explanation:Explanation:Explanation:Explanation:Explanation:Explanation:Explanation: E:A kind of cellulose esterification derivative ordered porous membrane materials of a kind of cellulose esterification derivative ordered porous membrane material Ji Qizhibeifangfa of scientific research Xiang Guan Zhuan Lis patents 6- and preparation method thereof-submit 100001 9254dest_path_image001.jpg of Ban 7cd322ac-dd25-4784-82fd-67436febdf3b
Wherein：
R1For CH3CO；
R2For CH3CO、C6H5CH2CO or H；
In R1And R2Three substituents in, preferable CH3CO、C6H5CH2The substitution value of tri- kinds of different substituents of CO and H is：
CH3The substitution value of CO is greater than or equal to 2, C6H5CH2Substitution value of the substitution value of CO equal to or more than 0.1, H is less than or equal to
0.4。
2. phenylacetyl cellulose acetate ordered porous membrane material according to claim 1, it is characterized in that, the system of the material
Preparation Method comprises the following steps：
Under 25 ~ 50 degrees Celsius, cellulose acetate is dissolved in tetrahydrofuran, pyridine, triethylamine acid binding agent are added, in ice-water bath
Lower and phenylacetyl halogen tetrahydrofuran solution reacts, and the molar ratio of the hydroxyl wherein on cellulose acetate and phenylacetyl halogen is 1:
0.5~1:10；Under ice-water bath reaction 4 ~ 24 it is small when after, in room temperature the reaction was continued 48 ~ 72 it is small when, then add water terminate reaction, instead
Liquid precipitate, filtering, drying should be mixed, obtains phenylacetyl cellulose acetate.
3. phenylacetyl cellulose acetate ordered porous membrane material according to claim 1, it is characterized in that, utilize the material
The method for preparing ordered porous membrane comprises the following steps：
Weigh a certain amount of phenylacetyl cellulose acetate to be dissolved in volatile organic solvent, be made into 0.1~100 g/l
Solution；It is in the environment of 30 ~ 95%, temperature is 0 ~ 50 degree Celsius in relative humidity, phenylacetyl cellulose acetate solution is dripped
It is added in planar substrates, spontaneously dries film forming, obtain the perforated membrane with ordered porous structural.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111218016A (en) * | 2019-07-11 | 2020-06-02 | 湖南工业大学 | High-hydrophobicity cellulose-based derivative ordered porous membrane material and preparation method thereof |
| CN113197344A (en) * | 2021-05-13 | 2021-08-03 | 云南中烟工业有限责任公司 | Composite acetate fiber, preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105801921A (en) * | 2014-12-31 | 2016-07-27 | 湖南工业大学 | Cellulose esterification derivative ordered porous membrane material and preparation method thereof |
-
2017
- 2017-12-27 CN CN201711438616.7A patent/CN108034069A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105801921A (en) * | 2014-12-31 | 2016-07-27 | 湖南工业大学 | Cellulose esterification derivative ordered porous membrane material and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111218016A (en) * | 2019-07-11 | 2020-06-02 | 湖南工业大学 | High-hydrophobicity cellulose-based derivative ordered porous membrane material and preparation method thereof |
| CN113197344A (en) * | 2021-05-13 | 2021-08-03 | 云南中烟工业有限责任公司 | Composite acetate fiber, preparation method and application thereof |
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Application publication date: 20180515 |