CN102585255A - Pectin/cellulose hydrogel material and preparation method thereof - Google Patents
Pectin/cellulose hydrogel material and preparation method thereof Download PDFInfo
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- CN102585255A CN102585255A CN2011100030408A CN201110003040A CN102585255A CN 102585255 A CN102585255 A CN 102585255A CN 2011100030408 A CN2011100030408 A CN 2011100030408A CN 201110003040 A CN201110003040 A CN 201110003040A CN 102585255 A CN102585255 A CN 102585255A
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Abstract
The invention relates to a preparation method for pectin/cellulose hydrogel material and a product thereof. The preparation method is characterized by comprising the following steps: respectively dissolving pectin and cellulose in an aqueous solution of NaOH/urea, mixing a combined NaOH/urea aqueous solution of pectin with a combined NaOH/urea aqueous solution of cellulose, carrying out uniform stirring so as to obtain a mixed solution, adding the cross-linking agent chloropropylene oxide, subjecting an obtained mixture to a chemical cross-linking reaction and allowing an obtained resultant to stand at a gelation temperature until pectin/cellulose hydrogel is formed, wherein, viscosity-average molecular weight of the cellulose is 30,000 to 100,000 Dalton. The pectin/cellulose hydrogel obtained in the invention has a water absorption rate of 20 to 120 g/g, has good hydroscopicity and mechanical strength and can be used in a wide variety of fields like agriculture, sanitation and biomedical materials.
Description
Technical field
The present invention relates to a kind of biodegradable natural polymer hydrogel material, particularly a kind of good biocompatibility pectin/cellulose materials and preparation method thereof belongs to natural macromolecular material and bio-medical material technical field.
Background technology
Oranges and tangerines are Chinese first fruit, and the waste residue staple after it is squeezed the juice is a pectin, are one group of polygalacturonic acids, are the main contributors of plant water keeping performance.Pectin is a kind of natural high moleculer eompound, has good gelationization and stable emulsifying effect, has been widely used in food, medicine, daily use chemicals and textile industry.Macromolecule hydrogel is a kind of hydrophilic swelling and the material that keeps large quantity of moisture, has been widely used in agricultural, medical material, filed of daily-use chemical industry.But because pectin is soluble in water, the gelatinous material poor mechanical property of system has limited its widespread use in bio-medical material, medicine controlled releasing and filed of daily-use chemical industry.Plant cellulose is a renewable resources the abundantest on the earth, in plant, plays the support structure effect, has the good mechanical performance.The pecto-cellulose mixing material promptly can keep the unique water retention property of pectin, can have the good mechanical performance again, for the biological safety developing material of natural degradable provides a new effective way.
The pectin gel of bibliographical information mainly is divided into formation on the spot or adds synthesized polymer material at present.Application number for the patent report of " 200710028603.2 " pectin/polyvinyl alcohol hydrogel material and preparation method thereof be used for the artificial nucleus prosthese because Z 150PH is harmful composition, its biocompatibility is poor, and human body is had hormesis.U.S. PCT patent " formation on the spot of pectin gel " adopts aloe pectin, under the effect of calcium ion, forms the material of gelation on the spot that can be used for carrying and continuing to discharge to animal body physiological agents on the spot, its poor mechanical property, and gel is crisp, cracky.
Summary of the invention
The objective of the invention is to overcome the defective of prior art, a kind of pectin/cellulose aquagel material is provided, this material good biocompatibility has biodegradability simultaneously, the material of higher physical strength.This pectin/cellulose aquagel material adds the absorption property of pectin ability strongthener, and Mierocrystalline cellulose provides the support structure effect, and material good mechanical performance is provided.Pectin derives from the big fruit oranges and tangerines of the first in the world cheap and easy to get waste residue, and the present invention also provides an effective way for the development and use of agricultural byproducts high added value.Preparing method of the present invention is simple, and raw materials cost is low, and whole technological process is pollution-free, and the products therefrom water cut is high, advantages of good adsorption effect, and good biocompatibility, biodegradable, and have excellent mechanical property.
For realizing above-mentioned purpose, the technical scheme that the present invention adopts is:
A kind of preparation method of pectin/cellulose aquagel, it comprises following step: in the aqueous solution of the NaOH/ urea that pectin, Mierocrystalline cellulose are dissolved in respectively; NaOH/ urea combination solution with pectin mixes with cellulosic NaOH/ urea combination solution then; Stir mixing solutions; Add the linking agent epoxy chloropropane again,, place under the gelling temp through chemical crosslink reaction; Until forming pectin/cellulose aquagel, used cellulosic viscosity-average molecular weight is 30,000～100,000 dalton.
Specifically; Preparation process in the technical scheme of the present invention is: with pectin under room temperature; Add mass percent concentration and be 6～10% NaOH, mass percent concentration and be in the aqueous solution of NaOH/ urea of 4～12% urea; Stir until making pectolysis, obtain mass percent concentration and be the NaOH/ urea combination solution of 1～6% pectin.
The amount of the linking agent epoxy chloropropane that adds in the above-mentioned steps and the ratio of mixing solutions are 0.5～1.5ml/10g.
Gelling temp is 30～60 ℃ in the above-mentioned steps.The Gel Treatment time is 2～12h.
Utilize the three-dimensional net structure of hydrogel to carry out cell cultures, the result shows that cell can well stick and rise in value in hydrogel.Therefore Mierocrystalline cellulose/pectin the hydrogel material of the present invention's preparation is a kind of good timbering material.
Description of drawings
Fig. 1: for the present invention prepares the hydrogel material outward appearance that pectin/Mierocrystalline cellulose forms.
Fig. 2: be that hydrogel material pattern of the present invention and cell compatibility detect.Wherein: Fig. 2 A is a gelatinous material tangent plane pattern, and Fig. 2 B is that cell is in hydrogel material surface growth situation.
Embodiment
Through specific embodiment technical scheme of the present invention is further specified below, its purpose is to help better to understand content of the present invention, but the protection domain that these specific embodiments do not limit the present invention in any way.
Embodiment 1
3 gram pectin are scattered in 97 grams contain in the mixed aqueous solution of 6wt%NaOH and 4wt% urea, under room temperature (22-25 ℃), stir until pectolysis.With 3 gram Mierocrystalline cellulose (viscosity-average molecular weight M
η=9.2 * 10
4) be scattered in 97 grams and contain in the mixed aqueous solution of 6wt%NaOH and 4wt% urea, precooling is to-10 ℃, and the stirring of thawing after 20 hours obtains transparent cellulose solution.Get 10g pectin solution and 30g cellulose solution and mix, obtain pectin and cellulose mixed solution, wherein pectin element and cellulosic weight ratio are 1: 3, and pectin and Mierocrystalline cellulose close and account for 3% of pectin and cellulose mixed solution.The epoxy chloropropane of 4ml is added drop-wise in the 40g mixing solutions, is warming up to 60 ℃, obtain pectin and cellulosic weight ratio after 2 hours and be 1: 3 composite aquogel.Through test, the gel compressive strength is 44.3KPa, and equilibrium swelling is than being 26g/g.
Embodiment 2
3 gram pectin are scattered in 97 grams contain in the mixed aqueous solution of 8wt%NaOH and 9wt% urea, at room temperature (with embodiment 1) stirs until pectolysis.With 3 gram Mierocrystalline cellulose (viscosity-average molecular weight M
η=9.2 * 10
4) be scattered in 97 grams and contain in the mixed aqueous solution of 6wt%NaOH and 4wt% urea, precooling is to-16 ℃, and the stirring of thawing after 16 hours obtains transparent cellulose solution.Get 20g pectin solution and 20g cellulose solution and mix, obtain pectin and cellulose mixed solution; Wherein pectin and cellulosic weight ratio are 1: 1, and pectin and Mierocrystalline cellulose close and account for pectin and cellulose mixed solution 3%.The epoxy chloropropane of 4ml is added drop-wise in the 40g mixing solutions, is warming up to 40 ℃, obtain pectin and cellulosic weight ratio after 6 hours and be 1: 1 composite aquogel.Its compressive strength is 32.9KPa, and equilibrium swelling is than being 32.4g/g.
Embodiment 3
3 gram pectin are scattered in 97 grams contain in the mixed aqueous solution of 10wt%NaOH and 12wt% urea, at room temperature stir until pectolysis.With 3 gram Mierocrystalline cellulose (viscosity-average molecular weight M
η=9.2 * 10
4) be scattered in 97 grams and contain in the mixed aqueous solution of 6wt%NaOH and 4wt% urea, precooling is to-20 ℃, and the stirring of thawing after 8 hours obtains transparent cellulose solution.Get 30g pectin solution and 10g cellulose solution and mix, obtain pectin and cellulose mixed solution; Wherein pectin and cellulosic weight ratio are 3: 1, and pectin and Mierocrystalline cellulose close and account for 3% of pectin and cellulose mixed solution.The epoxy chloropropane of 4ml is added drop-wise in the 40g mixing solutions, is warming up to 30 ℃, obtain pectin and cellulosic weight ratio after 12 hours and be 3: 1 compound water congealing glue material.Its compressive strength is 3.2KPa, and equilibrium swelling is than being 117.8g/g.
Claims (7)
1. the preparation method of a pectin/cellulose aquagel is characterized in that comprising following step: in the aqueous solution of the NaOH/ urea that pectin, Mierocrystalline cellulose are dissolved in respectively; NaOH/ urea combination solution with pectin mixes with cellulosic NaOH/ urea combination solution then; Stir mixing solutions; Add the linking agent epoxy chloropropane again,, place under the gelling temp through chemical crosslink reaction; Until forming pectin/cellulose aquagel, used cellulosic viscosity-average molecular weight is 30,000～100,000 dalton.
2. the preparation method of pectin/cellulose aquagel according to claim 1; It is characterized in that: with pectin under room temperature; Add mass percent concentration and be 6～10% NaOH, mass percent concentration and be in the aqueous solution of NaOH/ urea of 4～12% urea; Stir until making pectolysis, obtain mass percent concentration and be the NaOH/ urea combination solution of 1～6% pectin.
3. the preparation method of pectin/cellulose aquagel according to claim 1, it is characterized in that: the amount of the linking agent epoxy chloropropane of adding and the ratio of mixing solutions are 0.5～1.5ml/10g.
4. the preparation method of pectin/cellulose aquagel according to claim 1, it is characterized in that: gelling temp is 30～60 ℃.
5. according to the preparation method of the described pectin/cellulose aquagel of claim 1, it is characterized in that: the Gel Treatment time is 2～12h.
6. the preparation method of pectin/cellulose aquagel according to claim 1, it is characterized in that: the Gel Treatment time is 6h.
7. pectin/cellulose aquagel the material of each said method preparation of claim 1-6.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103599566A (en) * | 2013-10-21 | 2014-02-26 | 中山大学 | Tissue engineering natural gel stent material and preparation method and application thereof |
| CN104327307A (en) * | 2014-10-29 | 2015-02-04 | 广州纤维产品检测研究院 | Method for preparing biodegradable cellulose hydrogel |
| CN106478963A (en) * | 2016-10-11 | 2017-03-08 | 中国农业科学院油料作物研究所 | Flaxseed gum/cellulose composite aquogel and preparation method thereof |
| WO2021019577A1 (en) * | 2019-07-31 | 2021-02-04 | Gurjar Narayan Lal | Eco-friendly water retention natural polymer and method thereof |
| CN112724422A (en) * | 2020-12-29 | 2021-04-30 | 兰州大学 | Bacteriostatic wheat straw cellulose composite hydrogel and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070009580A1 (en) * | 2004-06-30 | 2007-01-11 | Dicosmo Frank | Non-adhesive hydrogels |
| CN101164676A (en) * | 2007-08-22 | 2008-04-23 | 武汉大学 | Method for preparing cellulose gel film |
-
2011
- 2011-01-06 CN CN2011100030408A patent/CN102585255A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070009580A1 (en) * | 2004-06-30 | 2007-01-11 | Dicosmo Frank | Non-adhesive hydrogels |
| CN101164676A (en) * | 2007-08-22 | 2008-04-23 | 武汉大学 | Method for preparing cellulose gel film |
Non-Patent Citations (2)
| Title |
|---|
| 《Macromolecular Booscience》 20070531 Jinping Zhou et al. "Hydrogels Prepared from Unsubstituted Cellulose in NaOH/Urea Aqueous Solution" 第7卷, 第6期 * |
| JINPING ZHOU ET AL.: ""Hydrogels Prepared from Unsubstituted Cellulose in NaOH/Urea Aqueous Solution"", 《MACROMOLECULAR BOOSCIENCE》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103599566A (en) * | 2013-10-21 | 2014-02-26 | 中山大学 | Tissue engineering natural gel stent material and preparation method and application thereof |
| CN103599566B (en) * | 2013-10-21 | 2015-05-20 | 中山大学 | Tissue engineering natural gel stent material and preparation method and application thereof |
| CN104327307A (en) * | 2014-10-29 | 2015-02-04 | 广州纤维产品检测研究院 | Method for preparing biodegradable cellulose hydrogel |
| CN106478963A (en) * | 2016-10-11 | 2017-03-08 | 中国农业科学院油料作物研究所 | Flaxseed gum/cellulose composite aquogel and preparation method thereof |
| WO2021019577A1 (en) * | 2019-07-31 | 2021-02-04 | Gurjar Narayan Lal | Eco-friendly water retention natural polymer and method thereof |
| CN114269885A (en) * | 2019-07-31 | 2022-04-01 | Ef聚合物株式会社 | Environment-friendly water-retaining natural polymer and method thereof |
| CN112724422A (en) * | 2020-12-29 | 2021-04-30 | 兰州大学 | Bacteriostatic wheat straw cellulose composite hydrogel and preparation method and application thereof |
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Application publication date: 20120718 |