CN105315480A - Preparation method of single side oxidized cellulose film - Google Patents
Preparation method of single side oxidized cellulose film Download PDFInfo
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- CN105315480A CN105315480A CN201510861639.3A CN201510861639A CN105315480A CN 105315480 A CN105315480 A CN 105315480A CN 201510861639 A CN201510861639 A CN 201510861639A CN 105315480 A CN105315480 A CN 105315480A
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Abstract
The invention relates to a preparation method of a single side oxidized cellulose film. The preparation method is characterized by firstly preparing a porous cellulose film by adopting a phase transformation method, soaking the prepared cellulose film in a TEMPO/NaBr mixed solution with a certain pH (10-11), after carrying out treatment for 3-8 hours, immobilizing the cellulose film in molds in different thickness, preparing printing pulp with different NaClO contents to carry out printing treatment on one side of the cellulose film and carrying out washing treatment after reacting for a certain time, thus obtaining the single side oxidized cellulose film. The preparation method has the beneficial effects that the method is simple to operate, is mild in reaction conditions and high in reaction efficiency and is suitable for industrial production; obtainment of the single side oxidized cellulose functional film provides more possibility for functionalization application of the oxidized cellulose film; after being further processed, the single side oxidized cellulose film can be used in the fields of single side electric conduction, medical treatment, barrier films, and the like.
Description
Technical field
The invention belongs to a kind of preparing technical field of cellulosefilm, be specifically related to a kind of preparation method of one side SURGICEL film
Background technology
Cellulose membrane has a series of premium properties, and such as highly hydrophilic, excellent perviousness, stain resistance, resistance to good physical and chemical, high thermal resistance are good, high transparent and good physical and mechanical properties etc.; In addition raw material be easy to get, environmental protection and the feature such as renewable; Cellulose membrane is all applied widely in recent years in infiltration technology, Food processing, medical applications etc.
Hydroxyl on cellulose macromolecule chain and the vesicular structure of cellulose membrane make the added value of the shortcoming such as poor water resistance, resistance to chemical corrosion difference and further raising cellulose membrane improving cellulose membrane by the technology such as chemical modification and load become possibility.Due to the restriction of cellulose macromolecule polarity, when making the vesicular structure utilizing its film carry out the load of inorganic functional nanoparticle, often there is the problem of charge capacity and load firmness, for this reason, usually need to carry out pre-treatment to improve its surface polarity and the affinity to inorganic particulate to cellulose membrane, oxidation modification cellulose membrane is exactly a kind of method wherein commonly used.Cellulose oxidation mode is divided into selective oxidation and non-selective oxidation two kinds.Wherein, because the position of non-selective oxidation and the functional group of generation can not control to determine, so often carry out selective oxidation to it.So-called selective oxidation, namely with different oxygenant selective oxidation primary hydroxyls or secondary hydroxyl.The former obtains Monofunctional reagents, and the latter then obtains bifunctional material.
In recent years, the oxidation technology of cellulose membrane obtains very large progress, and oxidation efficiency is improved, and in oxidising process, Degradation is limited.But due to the selection of method for oxidation and oxidizing process, the oxidation of cellulose membrane is all often two-sided, cellulose membrane oxidative function film is restricted in the application in some field, when cellulose membrane adsorbing metal particles as two-sided oxidation makes conducting film, the single-sided conductive needed for some special occasions can not be met; For another example, when the wound dressings such as SURGICEL film adsorption antibacterial particle is used for medical field, the cellulose membrane of two-sided oxidation can cause unnecessary waste.The invention provides a kind of preparation method of one side SURGICEL film, technique is simple, and oxidation effectiveness is good, and the functionalized application that can be SURGICEL film provides more possibility.
Summary of the invention
The object of this invention is to provide a kind of preparation method of one side SURGICEL film, technique is simple, workable, can be used for suitability for industrialized production.The one side oxidation effectiveness of gained cellulose membrane is obvious, and the functionalized application for SURGICEL film provides more possibility, further after processing, can be used for the fields such as single-sided conductive, medical treatment and barrier film.
For reaching above-mentioned technical purpose, a kind of preparation method of cellulosefilm of monoplanar surface oxidation, is characterized in that, specifically comprise the following steps:
(1) cellulosefilm is prepared: adopt phase transition method to prepare porous cellulose film;
(2) buffered soln configuration: 3-5g boric acid is dissolved in the water of certain volume, dilutes with certain density alkaline solution, makes pH value of solution be 10-11;
(3) dipping of cellulose membrane: the buffered soln getting 0.2-5g Sodium Bromide and the configuration in above-mentioned (2) of 0.03-0.6gTEMPO agent dissolves, after magnetic agitation mixes, cellulose membrane is immersed in the solution configured after 3-8h, for subsequent use after dry 20min at 80 DEG C
(4) printing slurry configuration:, get the buffered soln prepared in 20-80ml above-mentioned (2), add sodium alginate 3-6g, in water-bath during ebuillition of heated, slowly add 4-16ml chlorine bleach liquor, mixture stir, homogeneous rear for subsequent use.
(5) preparation of one side SURGICEL: the cellulosefilm obtained in above-mentioned (3) is fixed in the mould of different thickness, the method of printing is adopted to process cellulosefilm one side, after reaction 0.5-2h, cellulose membrane deionized water rinses rear drying at room temperature repeatedly, prepares the cellulosefilm of one side oxidation.
The porous cellulose film of described step (1) is the one in regenerated cellulose film, nano-cellulose film and bacteria cellulose film.
Alkaline solution in described step (2) is the one in sodium hydroxide, potassium hydroxide and lithium hydroxide.
The invention has the beneficial effects as follows:
(1) the present invention adopts the method for printing technology, can effectively regulate and control oxidation area, prepares the cellulosefilm of one side oxidation.
(2) the method is simple to operate, not only reaction conditions is gentle, in preparation process, clorox consumption is few, reaction efficiency is high, and can oxidation products be made to have certain intensity while the more original physicochemical characteristics of maintenance regenerated cellulose film, and then meet the application of material in some field.
(3) for the functionalized application of SURGICEL film provides more possibility, further after processing, can be used for the fields such as single-sided conductive, medical treatment and barrier film.
Accompanying drawing explanation
Fig. 1 is Fourier infrared spectrum (FTIR) figure on cellulose membrane one side oxidation rear film two sides in embodiment 1
Embodiment
Below in conjunction with embodiment, the present invention is described in detail
Embodiment 1
(1) cellulosefilm is prepared: be dispersed in by linters in basic solution, gained cellulose suspension puts cryogenic freezing, 24h takes out later, high speed machine stirs, centrifugal, the cellulose solution obtained by this simple method is pushing lamellar on a glass, then immerses concentrated sulfuric acid solution and solidifies regeneration and obtain transparency cellulose film, and cellulose membrane is repeatedly for subsequent use after deionized water washing.
(2) buffered soln configuration: 3.3-3.6g boric acid is dissolved in the water of 800ml, dilutes with the sodium hydroxide solution of 0.1mol/L, makes pH value of solution be 10-11
(3) dipping of cellulose membrane: the buffered soln getting 2g Sodium Bromide and the configuration in above-mentioned (2) of 0.3gTEMPO agent dissolves, after magnetic agitation mixes, cellulose membrane is immersed in the solution configured after 5h, for subsequent use after dry 20min at 80 DEG C
(4) printing slurry configuration:, get the buffered soln prepared in 40ml above-mentioned (2), add sodium alginate 4.5g, in water-bath during ebuillition of heated, slowly add 4ml chlorine bleach liquor, mixture stir, homogeneous rear for subsequent use.
(5) preparation of one side SURGICEL: it is in the mould of 3mm that the cellulosefilm obtained in above-mentioned (3) is fixed on thickness, the method of printing is adopted to process cellulosefilm one side, after reaction 1h, cellulose membrane deionized water rinses rear drying at room temperature repeatedly, prepares the cellulosefilm of one side oxidation.
The mensuration of the carboxyl-content of the cellulose membrane of the one side oxidation that embodiment 1 obtains adopts acid base titration.The carboxyl-content of the cellulose membrane that the one side that embodiment 1 obtains after measured is oxidized is 0.012mmol/L.
Embodiment 2
(1) prepare cellulosefilm: under room temperature, will bacteria cellulose dip treating 90min in 100mL ethylenediamine solution of over dry be dried to, and then use a large amount of distilled water and methanol wash, 80 DEG C of vacuum dryings.In 250mL tri-mouthfuls of round-bottomed flasks, add 100mLDMAc, 8g, through the LiCl of 150 DEG C of vacuum dryings, then stirs, and heats there-necked flask with oil bath pan.After LiCl dissolves completely, then add the bacteria cellulose after quadrol dip treating, heated and stirred 3h, be cooled to room temperature and leave standstill until it dissolves completely.Above-mentioned bacterial cellulose solution is striking film forming on constant temp. heating sheet glass, immerses 25 DEG C of precipitation bath, then naturally dries.
(2) buffered soln configuration: 3.3-3.6g boric acid is dissolved in the water of 800ml, dilutes with the sodium hydroxide solution of 0.1mol/L, makes pH value of solution be 10-11.
(3) dipping of cellulose membrane: the buffered soln getting 2g Sodium Bromide and the configuration in above-mentioned (2) of 0.3gTEMPO agent dissolves, after magnetic agitation mixes, cellulose membrane is immersed in the solution configured after 4h, for subsequent use after dry 20min at 80 DEG C
(4) printing slurry configuration:, get the buffered soln prepared in 20ml above-mentioned (2), add sodium alginate 4.5g, in water-bath during ebuillition of heated, slowly add 4ml chlorine bleach liquor, mixture stir, homogeneous rear for subsequent use.
(5) preparation of one side SURGICEL: it is in the mould of 2mm that the cellulosefilm obtained in above-mentioned (3) is fixed on thickness, the method of printing is adopted to process cellulosefilm one side, after reaction 0.5h, cellulose membrane deionized water rinses rear drying at room temperature repeatedly, prepares the cellulosefilm of one side oxidation.
The mensuration of the carboxyl-content of the cellulose membrane of the one side oxidation that embodiment 2 obtains adopts acid base titration.After measured, the carboxyl-content of the cellulose membrane that the one side that embodiment 2 obtains is oxidized is 0.022mmol/L.
Embodiment 3
(1) prepare cellulosefilm: the nano-cellulose suspension obtained through acidolysis is diluted to 0,5wt%, the ultrasonic power process 10min of 300W when ice bath, to guarantee that nano-cellulose is dispersed in water.Then change membrane filter appts with the glass being covered with organic filter film and filter above-mentioned diluent, and use vacuum pump vacuum filtration.Be formed uniformly after nano-cellulose film until nano-cellulose and together take out together with organic filter film, after covering a slice organic filter film, at room temperature dry 2 ~ 3 days, then in the vacuum drying oven moving on to 60 DEG C dry 2 ~ 3 days.Open after drying and can obtain transparent nano-cellulose film.
(2) buffered soln configuration: 3.3-3.6g boric acid is dissolved in the water of 800ml, dilutes with the potassium hydroxide solution of 0.1mol/L, makes pH value of solution be 10-11.
(3) dipping of cellulose membrane: the buffered soln getting 2g Sodium Bromide and the configuration in above-mentioned (2) of 0.3gTEMPO agent dissolves, after magnetic agitation mixes, cellulose membrane is immersed in the solution configured after 8h, for subsequent use after dry 20min at 80 DEG C
(4) printing slurry configuration:, get the buffered soln prepared in 50ml above-mentioned (2), add sodium alginate 5g, in water-bath during ebuillition of heated, slowly add 9ml chlorine bleach liquor, mixture stir, homogeneous rear for subsequent use.
(5) preparation of one side SURGICEL: it is in the mould of 3mm that the cellulosefilm obtained in above-mentioned (3) is fixed on thickness, the method of printing is adopted to process cellulosefilm one side, after reaction 1.5h, cellulose membrane deionized water rinses rear drying at room temperature repeatedly, prepares the cellulosefilm of one side oxidation.
The mensuration of the carboxyl-content of the cellulose membrane of the one side oxidation that embodiment 3 obtains adopts acid base titration.After measured, the carboxyl-content of the cellulose membrane that the one side that embodiment 3 obtains is oxidized is 0.014mmol/L.
Embodiment 4
(1) cellulosefilm is prepared: be dispersed in basic solution by 5g linters, gained cellulose suspension puts cryogenic freezing, 12-24h takes out later, high speed machine stirs, centrifugal, the cellulose solution obtained by this simple method is pushing lamellar on a glass, then immerses concentrated sulfuric acid solution and solidifies regeneration and obtain transparency cellulose film, and cellulose membrane is repeatedly for subsequent use after deionized water washing.
(2) buffered soln configuration: 3.3-3.6g boric acid is dissolved in the water of 800ml, dilutes with the lithium hydroxide solution of 0.1mol/L, makes pH value of solution be 10-11.
(3) dipping of cellulose membrane: the buffered soln getting 2g Sodium Bromide and the configuration in above-mentioned (2) of 0.3gTEMPO agent dissolves, after magnetic agitation mixes, cellulose membrane is immersed in the solution configured after 8h, for subsequent use after dry 20min at 80 DEG C
(4) printing slurry configuration:, get the buffered soln prepared in 50ml above-mentioned (2), add 4g sodium alginate, in water-bath during ebuillition of heated, slowly add 5ml chlorine bleach liquor, mixture stir, homogeneous rear for subsequent use.
(5) preparation of one side SURGICEL: it is in the mould of 3mm that the cellulosefilm obtained in above-mentioned (3) is fixed on thickness, the method of printing is adopted to process cellulosefilm one side, after reaction 2h, cellulose membrane deionized water rinses rear drying at room temperature repeatedly, prepares the cellulosefilm of one side oxidation.
The mensuration of the carboxyl-content of the cellulose membrane of the one side oxidation that embodiment 4 obtains adopts acid base titration.After measured, the carboxyl-content of the cellulose membrane that the one side that embodiment 4 obtains is oxidized is 0.024mmol/L.
Claims (4)
1. the preparation method of an one side SURGICEL film, it is characterized in that, phase transition method is adopted to prepare porous cellulose film, being immersed in by the cellulose membrane prepared in TEMPO/NaBr mixing solutions, is 10-11 with alkaline solution dilution pH, after process 3-8h, cellulose membrane is fixed in the mould of different thickness, the printing slurry of preparation different N aClO content carries out printing treatment to its one side, through washing process after reaction for some time, obtains one side SURGICEL film.
2. the preparation method of a kind of one side SURGICEL film according to claim 1, is characterized in that described cellulose membrane is the one in regenerated cellulose film, nano-cellulose film and bacteria cellulose film.
3. the preparation method of a kind of one side SURGICEL film according to claim 1, is characterized in that described alkaline solution is the one in sodium hydroxide, potassium hydroxide and lithium hydroxide.
4. a preparation method for one side SURGICEL film as claimed in claim 1, comprising:
(1) cellulosefilm is prepared: adopt phase transition method to prepare porous cellulose film;
(2) buffered soln configuration: 3-5g boric acid is dissolved in the water of certain volume, dilutes with certain density alkaline solution, makes pH value of solution be 10-11;
(3) dipping of cellulose membrane: the buffered soln getting 0.2-5g Sodium Bromide and the configuration in above-mentioned (2) of 0.03-0.6gTEMPO agent dissolves, after magnetic agitation mixes, cellulose membrane is immersed in the solution configured after 3-8h, for subsequent use after dry 20min at 80 DEG C
(4) printing slurry configuration:, get the buffered soln prepared in 20-80ml above-mentioned (2), add sodium alginate 3-6g, in water-bath during ebuillition of heated, slowly add 4-16ml chlorine bleach liquor, mixture stir, homogeneous rear for subsequent use.
(5) preparation of one side SURGICEL: the cellulosefilm obtained in above-mentioned (3) is fixed in the mould of different thickness, the method of printing is adopted to process cellulosefilm one side, after reaction 0.5-2h, cellulose membrane deionized water rinses rear drying at room temperature repeatedly, prepares the cellulosefilm of one side oxidation.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106220904A (en) * | 2016-08-22 | 2016-12-14 | 王利萍 | A kind of preparation method of NCC modified sodium alginate degradable composite membrane |
| CN106732440A (en) * | 2016-11-16 | 2017-05-31 | 江南大学 | A kind of preparation method of multifunctional porous cellophane adsorbent |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103333356A (en) * | 2013-06-27 | 2013-10-02 | 无锡贝迪生物工程有限公司 | Method for preparing collagen modified regenerated cellulose composite material |
| CN103951757A (en) * | 2014-04-03 | 2014-07-30 | 石家庄亿生堂医用品有限公司 | Medical absorbable oxycellulose material and preparation method thereof |
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2015
- 2015-11-27 CN CN201510861639.3A patent/CN105315480A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103333356A (en) * | 2013-06-27 | 2013-10-02 | 无锡贝迪生物工程有限公司 | Method for preparing collagen modified regenerated cellulose composite material |
| CN103951757A (en) * | 2014-04-03 | 2014-07-30 | 石家庄亿生堂医用品有限公司 | Medical absorbable oxycellulose material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| CHRISTA FITZBINDER等: ""Onesided surface modification of cellulose fabric by printing a modified TEMPO mediated oxidant"", 《CARBOHYDRATE POLYMERS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106220904A (en) * | 2016-08-22 | 2016-12-14 | 王利萍 | A kind of preparation method of NCC modified sodium alginate degradable composite membrane |
| CN106732440A (en) * | 2016-11-16 | 2017-05-31 | 江南大学 | A kind of preparation method of multifunctional porous cellophane adsorbent |
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Application publication date: 20160210 |