CN102321255A - Ion type nano-composite hydrogel and preparation method thereof - Google Patents
Ion type nano-composite hydrogel and preparation method thereof Download PDFInfo
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Abstract
The invention provides an ion type nano-composite hydrogel and a preparation method thereof. The preparation method comprises the following steps of: dissolving acrylamide monomer, nano inorganic clay and gelatin in deionized water, stirring for 10 to 30 minutes in an inert atmosphere; adding auxiliary cross-linking agent and catalyst, stirring for 5 to 10 minutes in the inert atmosphere, and then adding an initiating agent; carrying out a free radical polymerization for 12 to 36 hours at a temperature of 0 to 30 DEG C; immersing reaction product in the deionized water at the temperature of 20 to 60 DEG C, changing deionized water at regular intervals of 5 to 8 hours, continuing for 48 to 72 hours to obtain the ion type nano-composite hydrogel. The preparation method has simple process and controllable condition; the prepared gel has excellent biocompatibility, mechanical property and optical property, and can be widely used in the field of tissue engineering.
Description
Technical field
The present invention relates to a kind of preparation method of hydrogel, be specifically related to a kind of preparation method of ionic Nanometer composite hydrogel.
Background technology
Hydrogel is a kind of macromolecular material of similar vital tissues; By in water, not dissolving but the macromolecule network and the water of swellable form; Have performances such as formability, water absorbability, film-forming properties, cohesiveness, thermal capacity be big, be widely used in bio-medical fields such as biological support, cell cultures, medicine controlled releasing, organizational project and wound, burn treatment and hemostasis.But the fragile mechanical property of hydrogel itself has restricted its further application.The birth of Nanometer composite hydrogel has then overcome the various shortcoming of traditional water gel, and breakthrough has been brought in this field of giving.Nanometer composite hydrogel be with inorganic nano-particle as the physical crosslinking agent, (room temperature, need not stir) forms through original position radical polymerization preparation under the condition of gentleness with monomer.Because Nanometer composite hydrogel distinctive organic (polymkeric substance)/inorganic (nanoclay) network structure makes it have excellent mechanical property and transparency, and good fast-response.
Lithium algae soil (laponite) is a kind of inorganic nano-particle of synthetic, and is synthetic through hydrothermal method in the presence of mineralizer by silicate, lithium salts and magnesium salts.Its structure and natural montmorillonite are similar; Be 2:1 layered silicate structure, promptly respectively have one on the octahedral both sides of magnesia with the silicon-oxy tetrahedron with Sauerstoffatom, wherein the magnesium atom of part divalence is replaced by the univalent lithium atom; Make ion surface have permanent negative charge, electric density is about 1.4e/nm
2Easily by aquation, homodisperse becomes discoid particle to lithium algae soil in the aqueous solution, and the diameter of discoid particle is 25 ~ 30nm, and thickness is about 1nm, and particle has good monodispersity.When aqueous solution pH was lower than 11, Mg-OH was protonated and make the particle edge have the positive charge of several to dozens of unit charge amounts.Lithium algae soil is divided into two types on gel (Gel) type and colloidal sol (Sol) type usually.Gel-type lithium algae soil rate of dispersion in water is slow and dispersion liquid gelation speed is fast, and colloidal sol type lithium algae soil disperses fast in water and dispersion liquid can keep stable in a very long time.That the present invention uses is laponite RDS, and this is a kind of colloidal sol type lithium algae soil, characteristics such as have good dispersivity, granularity is little, structure is clear and definite and controllability is good.Lithium algae soil has been played the part of the role an of a polyfunctional crosslinking agent in the forming process of Nanometer composite hydrogel, can improve mechanical property, optical property and the swelling capacity etc. of gel effectively.
Up to the present; The water-soluble monomer that only contains amide group is (like N-NSC 11448 (NIPAm), N; N-DMAA (DMA), acrylic amide (AAm)) could prepare Nanometer composite hydrogel through the original position Raolical polymerizable with lithium algae soil with good mechanical properties and optical property; And the ubiquitous shortcoming of the Nanometer composite hydrogel of amides is that environment-responsive is poor, and unique what have environment-responsive is N-NSC 11448 (NIPAm) type Nanometer composite hydrogel.Tong; Z. etc. (Colloid and Polymer Science. 2007,285 479-484.) has prepared a kind of half interpenetrating network structure (IPN) Nanometer composite hydrogel with temperature and pH responsiveness with linear CMS (CMCS) and PNIPAm and lithium algae soil; But because CMCS is incompatible with PNIPAm; Make that prepared IPN Nanometer composite hydrogel transparency is low, and tensile strength is with respect to Haraguchi, (Macromolecules. 2002 for K. etc.; 35,10162-10171.) Nanometer composite hydrogel of initial preparation has reduced a lot.Recently, the monomer of ionic, (Macromolecules. 2009 like sodium acrylate; 42,3811-3817.) or sodium methacrylate (Polymer. 2009,50; 1933-1938.); Be introduced in the original position Raolical polymerizable of acrylic amide (AAm) and lithium algae soil, the N of trace, N'-methylene-bisacrylamide (BIS) is as auxiliary crosslinking agent; Can improve the stability of colloidal sol type lithium algae soil in system, prepared pH responsiveness ionic Nanometer composite hydrogel has mechanical property and transparency preferably.
The ionic Nanometer composite hydrogel is that the preparation of high-mechanical property and responsiveness aquagel provides a new direction.But, be that the hydrogel of matrix generally need improve its biocompatibility and can satisfy its application aspect the biological medicine material with the synthetic polymer.And traditional P AAm hydrogel has been widely used in protein separation; Super sorbent material and cell cultures etc.; Can find out that it has excellent biological compatibility, excellent conformality, lower hysteresis quality and the stretchiness of superelevation, this mainly is because the PAAm molecule has higher wetting ability and snappiness.Therefore; We plan the hydrolysate gelatin (gelatin) of natural polymer collagen is incorporated in the PAAm-laponite Nanometer composite hydrogel; Through AAm original position Raolical polymerizable in the mixing solutions of laponite and gelatin, prepare a kind of novel protein/polymer-based nano composite aquogel; Because gelatin is a kind of polyamphoteric electrolyte; Has definite iso-electric point (IEP); With gelatin as environmental response factor instead of propylene acid sodium or sodium methacrylate; Not only can give this ionic Nanometer composite hydrogel responsiveness, and can improve the biology performance of synthetic macromolecule based aquagel, more be applicable to bio-medical material.
So far, there are not patent and document that the research of PAAm/laponite/gelatin ionic Nanometer composite hydrogel is reported as yet.
Summary of the invention
The technical problem that quasi-solution of the present invention is determined is: design a kind of novel ionic Nanometer composite hydrogel, this gel had both had excellent biological compatibility and cellular affinity, had excellent mechanical property and high transparent again.This gel can be used for fields such as organizational project, cell cultures and wound auxiliary material.
The invention provides a kind of ionic Nanometer composite hydrogel, its preparation method is following:
(1) be dissolved in acrylic amide, nano inorganic clay and gelatin in the deionized water respectively; Wherein the mass percent concentration of acrylic amide is (5 ~ 10) %; The mass percent concentration of nano inorganic clay is (1 ~ 5) %; The mass percent concentration of gelatin is (1 ~ 5) %, in inert atmosphere, stirs then 10 ~ 30 minutes;
(2) add auxiliary crosslinking agent and catalyzer; After in inert atmosphere, stirring 5 ~ 10 minutes; Add initiator again and get mixing solutions; Wherein the add-on of auxiliary crosslinking agent is acrylic amide quality (0.1 ~ 0.5) %, and the add-on of catalyzer is (0.1 ~ 2) % of acrylic amide quality, and the add-on of initiator is (0.1 ~ 1) % of acrylic amide quality;
(3) above-mentioned mixing solutions was carried out Raolical polymerizable 12 ~ 36 hours under 0 ~ 30 ℃ temperature;
(4) reaction product is soaked in 20 ~ 60 ℃ the deionized water, whenever changes deionized water at a distance from 5 ~ 8 hours, lasting 48 ~ 72 hours, makes the ionic Nanometer composite hydrogel.
In above-mentioned technological case, said nano inorganic clay is synthetic clay laponite RDS, is a kind of trioctahedron polynite.
In above-mentioned technological case; The preparation method of said gelatin is following: to clean fresh healthy livestock animals skin or tendon is raw material, and through acetone degreasing, drying, be processed into fritter, the fritter of 10 weight parts is immersed in 1% sodium hydroxide solution of 100 ~ 150 weight parts 24 ~ 48 hours; Filter; With behind the deionized water wash raw material being placed 50 ℃ of following water-baths 4 ~ 8 hours, cross leaching filtrating, make the gelatin dry product through dialysis, freeze-drying again.
In above-mentioned technological case, said auxiliary crosslinking agent is a N,N methylene bis acrylamide.
In above-mentioned technological case, said catalyzer is N, N, N ', N '-Tetramethyl Ethylene Diamine or sodium sulfite anhy 96.
In above-mentioned technological case, said initiator is Potassium Persulphate or ammonium persulphate.
In above-mentioned technological case, said ionic Nanometer composite hydrogel can be used for biological support, cell cultures, medicine controlled releasing, organizational project, wound and burn treatment.
Compared with present technology the present invention has many-sided positively effect and advantage, but concrete inductive generalization is following:
(1) select the good gelatin of biocompatibility as second component among the present invention; The nano inorganic clay is as the physical crosslinking agent; Adopt original position radical polymerization to prepare Nanometer composite hydrogel; Have excellent biocompatibility, higher transparency and favorable mechanical performance simultaneously, can be used for fields such as organizational project, cell cultures and wound dressing;
(2) preparation technology of the present invention is simple, is easy to control, need not specific installation, and normal temperature and pressure operation down is with low cost;
(3) the prepared Nanometer composite hydrogel of the present invention can be regulated its biocompatibility and mechanical property through changing reactant composition and nano inorganic clay consumption.
The present invention also has some otherwise advantages.
Embodiment
Provide three embodiment of the present invention below, the present invention is specifically described through embodiment.Be necessary to be pointed out that at this; Embodiment only is used for the present invention is further explained; Can not be interpreted as the restriction to protection domain of the present invention, the person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of the invention described above.
Embodiment 1
Get the laponite solution of 2ml mass percent concentration 5% and the gelatin solution of 2ml mass percent concentration 5% and in the 10ml centrifuge tube, mix formation homogeneous transparent solution, add the 0.25g acrylamide monomer, feed nitrogen, stirred 10 minutes.The N,N methylene bis acrylamide solution that adds 44 μ l mass percent concentrations 1.25% subsequently again, the N of 125 μ l mass percent concentrations 10%; N, N ', N '-Tetramethyl Ethylene Diamine solution; Mix continued and fed nitrogen 5 minutes, add the Ammonium Persulfate 98.5 solution of 110 μ l mass percent concentrations 0.4% again, then sealing rapidly; Place 20 ℃ of water-baths reaction after 24 hours, reactant takes out segment, is soaked in 50 ℃ of deionized waters 48 hours; Whenever changed deionized water one time, promptly obtain the Nanometer composite hydrogel of good springiness transparency high-biocompatibility at a distance from 8 hours.
Embodiment 2
Get the Laponite solution of 3ml mass percent concentration 5% and the gelatin solution of 1ml mass percent concentration 5% and in the 10ml centrifuge tube, mix formation homogeneous transparent solution, add the 0.25g acrylamide monomer, feed nitrogen, stirred 15 minutes.The N,N methylene bis acrylamide solution that adds 44 μ l mass percent concentrations 1.25% subsequently again, the N of 125 μ l mass percent concentrations 10%; N, N ', N '-Tetramethyl Ethylene Diamine solution; Mix continued and fed nitrogen 5 minutes, add the Ammonium Persulfate 98.5 solution of 110 μ l mass percent concentrations 0.4% again, then sealing rapidly; Place 20 ℃ of water-baths reaction after 24 hours, reactant takes out segment, is soaked in 40 ℃ of deionized waters 48 hours; Whenever changed deionized water one time, promptly obtain the Nanometer composite hydrogel of good springiness transparency high-biocompatibility at a distance from 8 hours.
Embodiment 3
Get the laponite solution of 1ml mass percent concentration 5% and the gelatin solution of 3ml mass percent concentration 5% and in the 10ml centrifuge tube, mix formation homogeneous transparent solution, add the 0.25g acrylamide monomer, feed nitrogen, stirred 10 minutes.The N,N methylene bis acrylamide solution that adds 44 μ l mass percent concentrations 1.25% subsequently again, the N of 125 μ l mass percent concentrations 10%; N, N ', N '-Tetramethyl Ethylene Diamine solution; Mix continued and fed nitrogen 5 minutes, add the Ammonium Persulfate 98.5 solution of 110 μ l mass percent concentrations 0.4% again, then sealing rapidly; Place 20 ℃ of water-baths reaction after 24 hours, reactant takes out segment, is soaked in 20 ℃ of ionized waters 48 hours; Whenever changed deionized water one time, promptly obtain the Nanometer composite hydrogel of good springiness transparency high-biocompatibility at a distance from 8 hours.
Claims (7)
1. ionic Nanometer composite hydrogel is characterized in that the preparation method may further comprise the steps:
(1) be dissolved in acrylic amide, nano inorganic clay and gelatin in the deionized water respectively; Wherein the mass percent concentration of acrylic amide is (5 ~ 10) %; The mass percent concentration of nano inorganic clay is (1 ~ 5) %; The mass percent concentration of gelatin is (1 ~ 5) %, in inert atmosphere, stirs then 10 ~ 30 minutes;
(2) add auxiliary crosslinking agent and catalyzer; After in inert atmosphere, stirring 5 ~ 10 minutes; Add initiator again and get mixing solutions; Wherein the add-on of auxiliary crosslinking agent is acrylic amide quality (0.1 ~ 0.5) %, and the add-on of catalyzer is (0.1 ~ 2) % of acrylic amide quality, and the add-on of initiator is (0.1 ~ 1) % of acrylic amide quality;
(3) above-mentioned mixing solutions was carried out Raolical polymerizable 12 ~ 36 hours under 0 ~ 30 ℃ temperature;
(4) reaction product is soaked in 20 ~ 60 ℃ the deionized water, whenever changes deionized water at a distance from 5 ~ 8 hours, lasting 48 ~ 72 hours, makes the ionic Nanometer composite hydrogel.
2. ionic Nanometer composite hydrogel according to claim 1 is characterized in that said nano inorganic clay is synthesis of clay laponite RDS, is a kind of trioctahedron polynite.
3. ionic Nanometer composite hydrogel according to claim 1; The preparation method who it is characterized in that said gelatin is following: to clean fresh healthy livestock animals skin or tendon is raw material, and through acetone degreasing, drying, be processed into fritter, the fritter of 10 weight parts is immersed in 1% sodium hydroxide solution of 100 ~ 150 weight parts 24 ~ 48 hours; Filter; With behind the deionized water wash raw material being placed 50 ℃ of following water-baths 4 ~ 8 hours, cross leaching filtrating, make the gelatin dry product through dialysis, freeze-drying again.
4. ionic Nanometer composite hydrogel according to claim 1 is characterized in that said auxiliary crosslinking agent is a N,N methylene bis acrylamide.
5. ionic Nanometer composite hydrogel according to claim 1 is characterized in that said catalyzer is N, N, N ', N '-Tetramethyl Ethylene Diamine or sodium sulfite anhy 96.
6. ionic Nanometer composite hydrogel according to claim 1 is characterized in that said initiator is Potassium Persulphate or ammonium persulphate.
7. ionic Nanometer composite hydrogel according to claim 1 is characterized in that said ionic Nanometer composite hydrogel can be used for biological support, cell cultures, medicine controlled releasing, organizational project, wound and burn treatment.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103013138A (en) * | 2012-12-11 | 2013-04-03 | 四川大学 | Gelatin-based nano-composite material and preparation method thereof |
| CN104356319A (en) * | 2014-11-03 | 2015-02-18 | 四川大学 | Porous biological material using modified gelatin as crosslinking agent and preparation method of porous biological material |
| CN104448161A (en) * | 2014-12-05 | 2015-03-25 | 四川大学 | Organic composite hydrogel cross-linked by modified gelatin nano-microsphere and preparation method of organic composite hydrogel |
| US20160144068A1 (en) * | 2013-06-19 | 2016-05-26 | The Brigham And Women's Hospital, Inc. | Nanocomposite Hydrogels |
| CN106496656A (en) * | 2016-12-02 | 2017-03-15 | 国家海洋局第三海洋研究所 | A kind of agar/clay composite material of high intensity and preparation method thereof |
| CN107057255A (en) * | 2016-12-02 | 2017-08-18 | 国家海洋局第三海洋研究所 | A kind of gelatin/clay composite material of high intensity and preparation method thereof |
| CN107663377A (en) * | 2017-08-24 | 2018-02-06 | 浙江大学 | It is a kind of that there is temperature sensitive and the mixing hydrogel and its 3D printing method of light sensitive characteristic |
| CN109331216A (en) * | 2018-11-28 | 2019-02-15 | 福建师范大学 | A kind of quick-acting haemostatic powder hydrogel and preparation method thereof |
| CN110183581A (en) * | 2019-04-19 | 2019-08-30 | 武汉理工大学 | Preparation method based on the dual network structuring polymer hydrogel being physical crosslinking entirely |
| CN110935406A (en) * | 2019-11-29 | 2020-03-31 | 中国石油大学(华东) | High-strength polysaccharide-nano-laponite composite microsphere and preparation method thereof |
| CN112661918A (en) * | 2020-12-04 | 2021-04-16 | 汕头大学 | temperature-pH dual-response hydrogel and preparation method and application thereof |
| US11083780B2 (en) | 2015-07-20 | 2021-08-10 | The Brigham And Women's Hospital, Inc. | Shear-thinning compositions as an intravascular embolic agent |
| CN113550066A (en) * | 2021-06-02 | 2021-10-26 | 杭州恒邦实业有限公司 | Polymer fiber composite decorative paper and production method thereof |
| CN115572394A (en) * | 2022-10-11 | 2023-01-06 | 佛山职业技术学院 | Hydrogel with high mechanical strength and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103013138B (en) * | 2012-12-11 | 2014-10-15 | 四川大学 | Gelatin-based nano-composite material and preparation method thereof |
| CN103013138A (en) * | 2012-12-11 | 2013-04-03 | 四川大学 | Gelatin-based nano-composite material and preparation method thereof |
| US10034958B2 (en) * | 2013-06-19 | 2018-07-31 | The Brigham And Women's Hospital, Inc. | Nanocomposite hydrogels |
| US20160144068A1 (en) * | 2013-06-19 | 2016-05-26 | The Brigham And Women's Hospital, Inc. | Nanocomposite Hydrogels |
| CN104356319A (en) * | 2014-11-03 | 2015-02-18 | 四川大学 | Porous biological material using modified gelatin as crosslinking agent and preparation method of porous biological material |
| CN104448161A (en) * | 2014-12-05 | 2015-03-25 | 四川大学 | Organic composite hydrogel cross-linked by modified gelatin nano-microsphere and preparation method of organic composite hydrogel |
| CN104448161B (en) * | 2014-12-05 | 2017-02-22 | 四川大学 | Organic composite hydrogel cross-linked by modified gelatin nano-microsphere and preparation method of organic composite hydrogel |
| US11083780B2 (en) | 2015-07-20 | 2021-08-10 | The Brigham And Women's Hospital, Inc. | Shear-thinning compositions as an intravascular embolic agent |
| US11426450B2 (en) | 2015-07-20 | 2022-08-30 | The Brigham And Women's Hospital, Inc. | Shear-thinning compositions as an intravascular embolic agent |
| CN106496656A (en) * | 2016-12-02 | 2017-03-15 | 国家海洋局第三海洋研究所 | A kind of agar/clay composite material of high intensity and preparation method thereof |
| CN107057255A (en) * | 2016-12-02 | 2017-08-18 | 国家海洋局第三海洋研究所 | A kind of gelatin/clay composite material of high intensity and preparation method thereof |
| CN107057255B (en) * | 2016-12-02 | 2020-01-31 | 国家海洋局第三海洋研究所 | high-strength gelatin/clay composite material and its preparing process |
| CN107663377A (en) * | 2017-08-24 | 2018-02-06 | 浙江大学 | It is a kind of that there is temperature sensitive and the mixing hydrogel and its 3D printing method of light sensitive characteristic |
| CN109331216A (en) * | 2018-11-28 | 2019-02-15 | 福建师范大学 | A kind of quick-acting haemostatic powder hydrogel and preparation method thereof |
| CN109331216B (en) * | 2018-11-28 | 2021-03-30 | 福建师范大学 | Quick hemostatic hydrogel and preparation method thereof |
| CN110183581A (en) * | 2019-04-19 | 2019-08-30 | 武汉理工大学 | Preparation method based on the dual network structuring polymer hydrogel being physical crosslinking entirely |
| CN110935406A (en) * | 2019-11-29 | 2020-03-31 | 中国石油大学(华东) | High-strength polysaccharide-nano-laponite composite microsphere and preparation method thereof |
| CN112661918A (en) * | 2020-12-04 | 2021-04-16 | 汕头大学 | temperature-pH dual-response hydrogel and preparation method and application thereof |
| CN113550066A (en) * | 2021-06-02 | 2021-10-26 | 杭州恒邦实业有限公司 | Polymer fiber composite decorative paper and production method thereof |
| CN115572394A (en) * | 2022-10-11 | 2023-01-06 | 佛山职业技术学院 | Hydrogel with high mechanical strength and preparation method thereof |
| CN115572394B (en) * | 2022-10-11 | 2024-04-23 | 佛山职业技术学院 | Hydrogel with high mechanical strength and preparation method thereof |
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Application publication date: 20120118 |