CN103055347A - Preparation method of cellulose gel material of onion structure - Google Patents
Preparation method of cellulose gel material of onion structure Download PDFInfo
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- CN103055347A CN103055347A CN2013100218789A CN201310021878A CN103055347A CN 103055347 A CN103055347 A CN 103055347A CN 2013100218789 A CN2013100218789 A CN 2013100218789A CN 201310021878 A CN201310021878 A CN 201310021878A CN 103055347 A CN103055347 A CN 103055347A
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Abstract
The invention discloses a preparation method of a cellulose gel material of an onion structure. The cellulose is dissolved in a low-temperature pre-cooled NaOH-urea aqueous solution to prepare a cellulose solution which is used for preparing a multi-layer cellulose gel material. The method comprises the following steps: soaking a pre-prepared agar template in a acetum solution with mass percentage of 2.5-10% for 1-10 minutes, then soaking in the cellulose solution with mass percentage of 0.5-5% for 1-10 minutes, thus obtaining a first layer of cellulose gel; then repeatedly soaking the agar in the acetum and cellulose solution to prepare the multi-layer cellulose gel material. The layer thickness of the cellulose gel material of the onion structure is controllable, the mice fiber-forming cell can be well adhered, proliferated and spread on the surface and wall of each layer of the multi-layer gel material; therefore, the material has wide application prospect in the biomedical field.
Description
Technical field
The present invention relates to a kind of preparation method of Bulbus Allii Cepae structural fibers element gel rubber material, belong to natural macromolecular material and Renewable resource field.
Background technology
The sandwich of Bulbus Allii Cepae shape is a kind of new type gel material, and it can be used as the biomaterial [Nature, 2008,452,76] in the fields such as drug release and organizational project.In recent years, utilize biomass to construct multi-level new material or biomimetic material has caused very large attention, and obtained greater advance.Tieing up plain is the abundantest renewable biomass resource, and inventor place laboratory has adopted the water at low temperature systems such as NaOH/ carbamide to realize the macromolecular quick dissolving of this intractable and proposed new dissolution mechanism [Macromolecules, 2008,41,9345].The cellulose solution that we have utilized dissolution in low temperature to obtain is developed a series of cellulose new materials, for example functional fiber hydrogel [Macromolecules, 2011,44,1642].Yet up to now, Bulbus Allii Cepae shape multi-layer fiber hydrogel does not have any report because of its preparation method relative complex.
Summary of the invention
The present invention wants the technical solution problem to provide a kind of straightforward procedure to prepare Bulbus Allii Cepae structure multi-layer fiber element gel rubber material.
The present invention is that to solve the problems of the technologies described above the thinking of taking be to be solidified layer by layer and assembled by the agar template to regulate cellulose solution that is loaded with acetic acid, regulates and control the thickness of gel layer by changing experiment condition.
Concrete technical scheme is:
(1) configuration quality concentration is that 0.5%-5% cellulose solution and mass fraction are the acetic acid of 2.5-10%;
(2) with bar-shaped or spherical agar as template, place acetum to soak, take out, put into again cellulose solution and soak, solidify rear taking-up;
(3) operation of repeating step (2) is until the number of plies that needs.
In the such scheme, it is 1-10 minute that the agar template places the acetum soak time, puts into cellulose solution again and soaks taking-up after 1-10 minute.
The size of described spherical agar template is that diameter is 2 millimeters-3.9 millimeters, and bar-shaped agar template diameter is 4.3mm.
Selected cellulose solution concentration is 0.5%-5%, cellulose concentration too hour, prepared multilayer gel material bed thickness is too little, its regular multiple structure and use inconvenient is hard to keep; On the other hand, cellulose solution concentration is too large, and viscosity is relatively excessive, is unfavorable for forming regular multilayer gel structure.
Above-mentioned cellulose solution preparation method can adopt the known technology method, is not particularly limited.For example, described cellulose solution is obtained by 9wt%NaOH aqueous solution, LiOH/ carbamide, NaOH/ thiourea, NaOH/ aqueous solution of urea dissolving cellulos.
As a kind of preferred, cellulose solution is being chilled in advance by cellulose dissolution in-13 ℃ the NaOH/ aqueous solution of urea and is obtaining.
The present invention uses the agar template can be frozen into required form by aqueous agar solution under 5 ℃.
The agar template to regulate of gained cellulose solution through being loaded with acetic acid solidifies layer by layer and assembles, preparation multilayer tubular or spherical gel.By regulation and control cellulose solution and acetate concentration, agar template size and soak time are regulated and control the cellulose gel bondline thickness.
The inventive method adopts the cellulose paste dissolving is obtained cellulose solution, utilizes and is loaded with the agar of acetic acid as layer by layer gel and the assembling of template to regulate cellulose solution.In the process of this gelation, (acetate concentration is high in the agar template for acetic acid and cellulose concentration gradient inside and outside the agar template, and cellulose is high at agar template extracellular concentration) to induce, macromolecular chain carries out orderly arrangement by the exchange interaction of solvent, forms multilayered structure.By regulation and control cellulose solution and acetate concentration, agar template size and soak time are regulated and control the cellulose gel bondline thickness.We have prepared every layer of multi-layer fiber element gel that is about 20-450 μ m thickness.Because cellulose has excellent mechanical property, still can well keep its multiple structure after these multi-layer fiber hydrogel lyophilizing, in addition, cell culture experiments shows that every layer surface and layer wall can be cell adhesion, breeding and sprawling provides matrix, so this material can be used tissue stent material.
The obtained Bulbus Allii Cepae shape of the inventive method multi-layer fiber element gel rubber material has good biocompatibility, shape and bed thickness controllability, regular multiple structure and biodegradability.The inventive method technical process is simply pollution-free, is easy to industrialization.
Description of drawings
The left figure of Fig. 1 is the photo of embodiment 1 gained multi-layer fiber element gel, and right figure is multi-layer fiber element gel image scanning electromicroscopic photograph after the lyophilization.
The left figure of Fig. 2 is the photo of embodiment 2 gained multi-layer fibers element gel, and right figure is multi-layer fiber element gel image scanning electromicroscopic photograph after the lyophilization.
The left figure of Fig. 3 is the photo of embodiment 3 gained multi-layer fibers element gel, and right figure is multi-layer fiber element gel image scanning electromicroscopic photograph after the lyophilization.
The left figure of Fig. 4 is the photo of embodiment 4 gained multi-layer fibers element gel, and right figure is multi-layer fiber element gel image scanning electromicroscopic photograph after the lyophilization.
The left figure of Fig. 5 is embodiment 5 gained multi-layer fibers element gel photograph, and middle figure and right figure are stereoscan photograph behind the cultured cell.
The specific embodiment
Below will specify the present invention by specific embodiment, but these specific embodiments do not limit the present invention in any way protection domain.Raw material that the present embodiment is used is known compound, can buy in market.The thickness of multilayer gel is measured by microscope.
Embodiment 1
With 6-8wt%NaOH, it is freezing to-13 ° of C that 10-14wt% carbamide and water form dicyandiamide solution, dissolving cellulos obtains the 0.5wt% cellulose solution, it is to carry out solvent exchange 3min in 10% acetum that diameter 2mm agar ball is immersed in mass fraction, make the agar ball that is loaded with acetic acid, putting into cellulose solution 3min solidifies and makes the ground floor cellulose gel again, after agar ball with the ground floor cellulose gel is soaked in the same acetum displacement, again be soaked in and make second layer cellulose gel in the same cellulose solution, repeat process of setting and layer assembly, be immersed in that the time is 3min in the cellulose solution.Gained multi-layer fiber element gel rubber material bed thickness is 20 ± 6 μ m.
Embodiment 2
With 6-8wt%NaOH, it is freezing to-13 ° of C that 10-14wt% carbamide and water form dicyandiamide solution, dissolving cellulos obtains the 3wt% cellulose solution, it is to carry out solvent exchange 1min in 10% acetum that diameter 3.9mm agar ball is immersed in mass fraction, make the agar ball that is loaded with acetic acid, putting into cellulose solution solidifies 1min and makes the ground floor cellulose gel again, after agar ball with the ground floor cellulose gel is soaked in the same acetum displacement, again be soaked in and make second layer cellulose gel in the same cellulose solution, repeat process of setting and layer assembly, be immersed in that the time is 1min in the cellulose solution.Gained multi-layer fiber element gel rubber material bed thickness is 126 ± 25 μ m.
Embodiment 3
With 6-8wt%NaOH, it is freezing to-13 ° of C that 10-14wt% carbamide and water form dicyandiamide solution, dissolving cellulos obtains the 5wt% cellulose solution, it is to carry out solvent exchange 10min in 10% acetum that diameter 3.9mm agar ball is immersed in mass fraction, make the agar ball that is loaded with acetic acid, putting into cellulose solution 10min solidifies and makes the ground floor cellulose gel again, after agar ball with the ground floor cellulose gel is soaked in the same acetum displacement, again be soaked in and make second layer cellulose gel in the same cellulose solution, repeat process of setting and layer assembly, be immersed in that the time is 10min in the cellulose solution.Gained multi-layer fiber element gel rubber material bed thickness is 450 ± 35 μ m.
Embodiment 4
6-8wt%NaOH, 10-14wt% carbamide and water are formed dicyandiamide solution freezing to-13 ° of C, dissolving cellulos obtains the 3wt% cellulose solution, it is to carry out solvent exchange 3min in 2.5% acetum that diameter 3.9mm agar ball is immersed in mass fraction, make the agar ball that is loaded with acetic acid, putting into cellulose solution 3min solidifies and makes the ground floor cellulose gel again, after agar ball with the ground floor cellulose gel is soaked in the same acetum displacement, again be soaked in and make second layer cellulose gel in the same cellulose solution, repeat process of setting and layer assembly.Gained multi-layer fiber element gel rubber material bed thickness is 70 ± 5 μ m.
6-8wt%NaOH, 10-14wt% carbamide and water are formed dicyandiamide solution freezing to-13 ℃, dissolving cellulos obtains the 3wt% cellulose solution, it is to carry out solvent exchange 3min in 10% acetum that 4.3mm agar rod is immersed in mass fraction, make the agar rod that is loaded with acetic acid, putting into cellulose solution 3min solidifies and makes the ground floor cellulose gel again, after agar rod with the ground floor cellulose gel is soaked in the same acetum displacement, again be soaked in and make second layer cellulose gel in the same cellulose solution, repeat process of setting and layer assembly.After making the bar-shaped hydrogel of multilamellar, fall in the gel behind the alkali and salt with distill water dialysis, autoclaving, place 24 orifice plates to cultivate the mice fibroblast two days later, rinse postlyophilization well with the glutaraldehyde fixed cell and with phosphate buffer solution, by the scanning electric mirror observing cell upgrowth situation, cell can be on multiple-level surface and wall well adheres to, and breeds and sprawls.
Claims (6)
1. the preparation method of a Bulbus Allii Cepae structural fibers element gel rubber material is characterized in that, comprises the steps:
(1) configuration quality concentration is that 0.5%-5% cellulose solution and mass fraction are the acetic acid of 2.5-10%;
(2) with bar-shaped or spherical agar as template, place acetum to soak, take out, put into again cellulose solution and soak, solidify rear taking-up;
(3) operation of repeating step (2) is until the number of plies that needs.
2. preparation method according to claim 1 is characterized in that, it is 1-10 minute that the agar template places the acetum soak time, puts into cellulose solution again and soaks, and soaks after 1-10 minute and takes out.
3. preparation method according to claim 1 is characterized in that, the size of described spherical agar template is that diameter is 2 millimeters-3.9 millimeters, and bar-shaped agar template diameter is 4.3mm.
4. preparation method according to claim 1 and 2 is characterized in that, described cellulose solution is obtained by 9wt%NaOH aqueous solution, LiOH/ carbamide, NaOH/ thiourea, NaOH/ aqueous solution of urea dissolving cellulos.
5. preparation method according to claim 4 is characterized in that, described cellulose solution is being chilled in advance by cellulose dissolution in-13 ℃ the NaOH/ aqueous solution of urea and is obtaining.
6. preparation method according to claim 1 and 2 is characterized in that, described agar template by aqueous agar solution at 5 ℃ of lower solidification formings.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105199113A (en) * | 2015-09-16 | 2015-12-30 | 盐城工学院 | Preparation method of alternate layered chitosan/alginic acid composite water gel material |
| CN107320780A (en) * | 2017-06-27 | 2017-11-07 | 上普博源（北京）生物科技有限公司 | A kind of multilayer aquagel of hollow tubular structure and preparation method and application |
| CN111518284A (en) * | 2020-05-06 | 2020-08-11 | 盐城工学院 | Preparation method of chitin multilayer hydrogel material |
| CN112143002A (en) * | 2020-09-02 | 2020-12-29 | 五邑大学 | Preparation method of multi-dimensional oriented cellulose hydrogel |
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| CN1318582A (en) * | 2000-04-17 | 2001-10-24 | 武汉大学 | Cellulose film preparing method |
| WO2006092540A1 (en) * | 2005-03-04 | 2006-09-08 | Universite Claude Bernard Lyon I | Multiple-membrane polysaccharide capsules and in particular of chitosan and method for preparing same |
| US20120040463A1 (en) * | 2007-09-07 | 2012-02-16 | Centre National De La Recherche Scientifique | Hollow, notably multi-membrane fibers, method for preparation thereof by spinning and device for applying said method |
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Patent Citations (4)
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| CN1318582A (en) * | 2000-04-17 | 2001-10-24 | 武汉大学 | Cellulose film preparing method |
| WO2006092540A1 (en) * | 2005-03-04 | 2006-09-08 | Universite Claude Bernard Lyon I | Multiple-membrane polysaccharide capsules and in particular of chitosan and method for preparing same |
| US20120040463A1 (en) * | 2007-09-07 | 2012-02-16 | Centre National De La Recherche Scientifique | Hollow, notably multi-membrane fibers, method for preparation thereof by spinning and device for applying said method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105199113A (en) * | 2015-09-16 | 2015-12-30 | 盐城工学院 | Preparation method of alternate layered chitosan/alginic acid composite water gel material |
| CN105199113B (en) * | 2015-09-16 | 2017-10-17 | 盐城工学院 | A kind of preparation method of alternately stratiform chitosan/alginic acid compound hydrogel material |
| CN107320780A (en) * | 2017-06-27 | 2017-11-07 | 上普博源（北京）生物科技有限公司 | A kind of multilayer aquagel of hollow tubular structure and preparation method and application |
| CN107320780B (en) * | 2017-06-27 | 2020-04-28 | 上普博源（北京）生物科技有限公司 | Multilayer hydrogel with hollow tube structure and preparation method and application thereof |
| CN111518284A (en) * | 2020-05-06 | 2020-08-11 | 盐城工学院 | Preparation method of chitin multilayer hydrogel material |
| CN111518284B (en) * | 2020-05-06 | 2022-10-18 | 盐城工学院 | Preparation method of chitin multilayer hydrogel material |
| CN112143002A (en) * | 2020-09-02 | 2020-12-29 | 五邑大学 | Preparation method of multi-dimensional oriented cellulose hydrogel |
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