CN105131209A - Preparation method for nano-composite hydrogel - Google Patents
Preparation method for nano-composite hydrogel Download PDFInfo
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- CN105131209A CN105131209A CN201510635312.4A CN201510635312A CN105131209A CN 105131209 A CN105131209 A CN 105131209A CN 201510635312 A CN201510635312 A CN 201510635312A CN 105131209 A CN105131209 A CN 105131209A
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Abstract
The invention relates to a preparation method for nano-composite hydrogel. Added oxidized graphene has the similar lamellar structure as laponite, and meanwhile the surface of the oxidized graphene has the abundant hydroxyl and carboxyl functional groups, so that an esterification reaction can take place between the oxidized graphene and RAFT with carboxyl; precise polymers are grafted on the surface of the oxidized graphene through RAFT polymerization; the oxidized graphene serves as the crosslinking point, therefore, the strength and mechanical property of the hydrogel can be improved, and meanwhile the defect that ionic monomers cannot be used in a laponite system can be overcome; through RAFT polymerization, homopolymers or segmented copolymers are adopted as the polymers grafted on the oxidized graphene, the molecular weight of the polymers is controllable, the molecular weight distribution index is narrower (PDI=1.10-1.38), and the mole grafting rate is higher. The method is simple, and the raw material selection range is wide.
Description
Technical field
The present invention relates to the preparation field of hydrogel, specifically a kind of preparation method of Nanometer composite hydrogel.
Background technology
Hydrogel be by hydrophilic polymer form can be swelling and keep large quantity of moisture and do not dissolved to obtain cross-linked network in water.In water, swellable is to certain volume for they, and water-break deswelling is under certain condition that a class set water suction, water conservation, controlled release are in the functional high molecule material of one.Macromolecule hydrogel material, due to the constitutional features of its uniqueness and physicochemical property, has a wide range of applications in fields such as the chemical mechanical devices of flexibility, selective filter, biological medicine, organizational projects.But the mechanical property of traditional chemical cross-linked hydrogel is poor, limit its range of application to a certain extent.At present, in raising hydrogel intensity, newly developed mainly contains topological framework hydrogel, nanostructure hydrogel, double-network hydrogel.Wherein Nanometer composite hydrogel has preparation method simply, the advantage of favorable repeatability.But now widely used nanoparticle is lithium algae soil mainly, but when lithium algae soil is nano material, selected organic monomer must be the monomer of non-ionic type, and the hydrogel intensity of preparation need to improve.At present adopt RAFT to be aggregated in the report of the graphene oxide sheet interlayer intercalation polymeric that can conduct electricity about nano-hydrogel considerably less, less see the report adopting RAFT polymerization to carry out synthesis of nano composite aquogel.
Summary of the invention
Mechanical property for above-mentioned traditional chemical cross-linked hydrogel hydrogel intensity that is poor, preparation need the problem improved, and the invention provides a kind of preparation method of Nanometer composite hydrogel.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A preparation method for Nanometer composite hydrogel, comprises the following steps:
(1) preparation of surface of graphene oxide grafting RAFT reagent
Graphene oxide is dissolved in organic solvent, after abundant stirring, the ultrasonic graphene sheet layer that makes fully is separated, add dry RAFT reagent afterwards, stirred at ambient temperature 10 ~ 20min, then add dewatering agent and catalyzer, stirred at ambient temperature 15 ~ 24h, after having reacted, revolve and steam except desolventizing, wash away excessive RAFT reagent with methylene dichloride, remaining part is graphene oxide grafts, drying for standby under vacuum condition;
(2) the mini-emulsion polymerization reaction of surface of graphene oxide graft homopolymer
Get step (1) gained graphene oxide grafts to be added to the water, abundant ultrasonic disperse, then adds initiator wherein successively, monomer, n-hexadecane, abundant ultrasonic disperse, add emulsifying agent again, stir 1 ~ 1.5h, abundant ultrasonic disperse, logical nitrogen 10 ~ 15min, is warming up to 70 ~ 80 DEG C and starts reaction, continues logical nitrogen, after 2h, again add initiator and monomer, be warming up to 80 ~ 85 DEG C, insulation reaction 2h, cool to room temperature, can obtain Nanometer composite hydrogel;
Organic solvent in described step (1) is DMF, dimethyl sulfoxide (DMSO) or tetrahydrofuran (THF);
Dewatering agent in described step (1) is N, N '-dicyclohexylcarbodiimide, N, N'-diisopropylcarbodiimide or 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride;
Catalyzer in described step (1) is DMAP or 1-hydroxy benzo triazole;
In described step (2), initiator is Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile), azo-bis-iso-dimethyl, azo-bis-isobutyrate hydrochloride, azo two isobutyl imidazoline hydrochloride or 4,4 '-azo two (4-cyanopentanoic acid);
Monomer in described step (2) is one in acrylamide, vinylformic acid, 4-vinylpridine, NIPA or its arbitrary combination;
In described step (1), the consumption of each component is as follows, the quality of graphene oxide: account for 0.2 ~ 10% of system total mass, the quality of RAFT reagent: account for 0.5 ~ 20% of system total mass, the quality of dewatering agent: account for 0.5 ~ 20% of system total mass, the quality of catalyzer: account for 0.1 ~ 5% of system total mass;
In described step (2), the consumption of each component is as follows, graphene oxide grafts 10 ~ 20mg, water 10 ~ 50mL, initiator 0.1 ~ 0.2mg, monomer 3 ~ 6g, n-hexadecane 0.1 ~ 0.2g, emulsifying agent 0.05 ~ 0.1g;
Emulsifying agent in described step (2) is Sodium dodecylbenzene sulfonate.
Beneficial effect of the present invention:
The preparation method of Nanometer composite hydrogel provided by the invention, the graphene oxide added have with lithium algae great soil group like laminated structure, the surface of simultaneous oxidation Graphene has abundant hydroxyl and carboxyl functional group, esterification can be there is with the RAFT with carboxyl, polymkeric substance accurate in surface of graphene oxide grafting is aggregated in again by RAFT, because graphene oxide serves as cross-linking set, intensity and the mechanical property of hydrogel can be improved, the shortcoming that lithium algae soil body system can not use ionic comonomer can be overcome simultaneously; Be polymerized by RAFT, the polymkeric substance of grafting on graphene oxide is homopolymer or segmented copolymer, and its molecular weight is controlled, molecular weight distributing index narrower (PDI=1.10-1.38), and mole percentage of grafting is higher; The method is simple, and material choice scope is large.
Embodiment
Below in conjunction with embodiment, the present invention is further elaborated.
A preparation method for Nanometer composite hydrogel, comprises the following steps:
(1) preparation of surface of graphene oxide grafting RAFT reagent
Graphene oxide is dissolved in organic solvent, after abundant stirring, the ultrasonic graphene sheet layer that makes fully is separated, add dry RAFT reagent afterwards, stirred at ambient temperature 10 ~ 20min, then add dewatering agent and catalyzer, stirred at ambient temperature 15 ~ 24h, after having reacted, revolve and steam except desolventizing, wash away excessive RAFT reagent with methylene dichloride, remaining part is graphene oxide grafts, drying for standby under vacuum condition;
(2) the mini-emulsion polymerization reaction of surface of graphene oxide graft homopolymer
Get step (1) gained graphene oxide grafts to be added to the water, abundant ultrasonic disperse, then adds initiator wherein successively, monomer, n-hexadecane, abundant ultrasonic disperse, add emulsifying agent again, stir 1 ~ 1.5h, abundant ultrasonic disperse, logical nitrogen 10 ~ 15min, is warming up to 70 ~ 80 DEG C and starts reaction, continues logical nitrogen, after 2h, again add initiator and monomer, be warming up to 80 ~ 85 DEG C, insulation reaction 2h, cool to room temperature, can obtain Nanometer composite hydrogel.
Graphene oxide in described step (1), adopts conventional hummers method preparation and is revised.Provide the method below to contribute to understanding technical scheme of the present invention: in beaker, add 98% vitriol oil 20 ~ 30ml, 13g graphite and 0.5 ~ 2g SODIUMNITRATE, 0 ~ 4 DEG C is cooled in ice bath, slowly add 2 ~ 5g potassium permanganate under agitation condition, in process, make reacting liquid temperature below 20 DEG C; Then by beaker as in 35 DEG C of waters bath with thermostatic control, continue stirring 0.5 ~ 1h; Slowly add water under agitation, make reacting liquid temperature reach 95 ~ 100 DEG C, continue stirring 15 ~ 60min; Add aqueous hydrogen peroxide solution after finally being diluted by reaction solution with water, washing, filtration, then be washed till neutrality can obtain graphene oxide through dialysis, deionized water.
Embodiment 1
In the DMF that 150mL is refining, add 0.2g graphene oxide, be transferred to after fully stirring and whipping appts, reflux and N are housed
2in the there-necked flask of entrance, there-necked flask is inserted in ultrasonic device and carry out ultrasonic 20min, graphene sheet layer is fully separated, add pre-dry RAFT reagent 0.4g, after stirring 20min, add 0.5gN, N '-dicyclohexylcarbodiimide and 0.2g4-Dimethylamino pyridine, stirred at ambient temperature 24h, after having reacted, revolve and steam except desolventizing, wash away excessive RAFT reagent with methylene dichloride, through vacuum-drying, graphene oxide grafts can be obtained, getting gained grafts 20mg joins in the deionized water of 50mL, abundant ultrasonic disperse, then azo-bis-isobutyrate hydrochloride 0.07mg is added successively wherein, refining acrylamide 0.75g, n-hexadecane 0.1g, abundant ultrasonic disperse, add Sodium dodecylbenzene sulfonate 0.1g again, stir 1.5h, abundant ultrasonic disperse, logical nitrogen 15min, be warming up to 75 DEG C and start reaction, after continuing logical nitrogen 2h, add acrylamide 3g again, NIPA 1.5g, azo-bis-isobutyrate hydrochloride 0.13mg, be warming up to 80 DEG C, insulation reaction 2h terminates reaction, cool to room temperature, the nano-composite gel of graphene oxide grafting poly N-isopropyl acrylamide/acrylamide can be obtained.
Embodiment 2
In the dimethyl sulfoxide (DMSO) that 150mL is refining, add 0.2g graphene oxide, be transferred to after fully stirring and whipping appts, reflux and N are housed
2in the there-necked flask of entrance, there-necked flask is inserted in ultrasonic device and carry out ultrasonic 15min, graphene sheet layer is fully separated, add pre-dry RAFT reagent 0.4g, after stirring 15min, add 0.5gN, N'-diisopropylcarbodiimide and 0.2g1-hydroxy benzo triazole, stirred at ambient temperature 24h, after having reacted, revolve and steam except desolventizing, wash away excessive RAFT reagent with methylene dichloride, through vacuum-drying, graphene oxide grafts can be obtained, getting gained grafts 15mg joins in the deionized water of 30mL, abundant ultrasonic disperse, then 2,2'-Azobis(2,4-dimethylvaleronitrile) 0.03mg is added successively wherein, refining vinylformic acid 1.5g, n-hexadecane 0.2g, abundant ultrasonic disperse, add Sodium dodecylbenzene sulfonate 0.08g again, stir 1h, abundant ultrasonic disperse, logical nitrogen 15min, be warming up to 75 DEG C and start reaction, after continuing logical nitrogen 2h, add vinylformic acid 2g again, NIPA 1g, 2,2'-Azobis(2,4-dimethylvaleronitrile) 0.1mg, be warming up to 80 DEG C, insulation 2h terminates reaction, cool to room temperature, graphene oxide grafting poly N-isopropyl acrylamide/acrylic acid nano-composite gel can be obtained.
Embodiment 3
In the tetrahydrofuran (THF) that 150mL is refining, add 0.2g graphene oxide, be transferred to after fully stirring and whipping appts, reflux and N are housed
2in the there-necked flask of entrance, there-necked flask is inserted in ultrasonic device and carry out ultrasonic 15min, graphene sheet layer is fully separated, add pre-dry RAFT reagent 0.4g, after stirring 15min, add 0.5g1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride and 0.2g4-Dimethylamino pyridine, stirred at ambient temperature 24h, after having reacted, revolve and steam except desolventizing, wash away excessive RAFT reagent with methylene dichloride, through vacuum-drying, graphene oxide grafts can be obtained, getting gained grafts 20mg joins in the deionized water of 50mL, abundant ultrasonic disperse, then azo-bis-iso-dimethyl 0.03mg is added successively wherein, refining NIPA 0.75g, n-hexadecane 0.15g, abundant ultrasonic disperse, add Sodium dodecylbenzene sulfonate 0.05g again, stir 1.5h, abundant ultrasonic disperse, logical nitrogen 10min, be warming up to 80 DEG C and start reaction, after continuing logical nitrogen 2h, add azo-bis-iso-dimethyl 0.07mg again, NIPA 3.5g, be warming up to 85 DEG C, insulation 2h terminates reaction, cool to room temperature, the nano-composite gel of graphene oxide grafting poly N-isopropyl acrylamide can be obtained.
Claims (9)
1. a preparation method for Nanometer composite hydrogel, is characterized in that, comprises the following steps:
(1) preparation of surface of graphene oxide grafting RAFT reagent
Graphite oxide is dissolved in organic solvent, after abundant stirring, the ultrasonic graphene sheet layer that makes fully is separated, add dry RAFT reagent afterwards, stirred at ambient temperature 10 ~ 20min, then add dewatering agent and catalyzer, stirred at ambient temperature 15 ~ 24h, after having reacted, revolve and steam except desolventizing, wash away excessive RAFT reagent with methylene dichloride, remaining part is graphene oxide grafts, drying for standby under vacuum condition;
(2) the mini-emulsion polymerization reaction of surface of graphene oxide graft homopolymer
Get step (1) gained graphene oxide grafts to be added to the water, abundant ultrasonic disperse, then adds initiator wherein successively, monomer, n-hexadecane, abundant ultrasonic disperse, add emulsifying agent again, stir 1 ~ 1.5h, abundant ultrasonic disperse, logical nitrogen 10 ~ 15min, is warming up to 70 ~ 80 DEG C and starts reaction, continues logical nitrogen, after 2h, again add initiator and monomer, be warming up to 80 ~ 85 DEG C, insulation reaction 2h, cool to room temperature, can obtain Nanometer composite hydrogel.
2. the preparation method of Nanometer composite hydrogel as claimed in claim 1, is characterized in that: the organic solvent in described step (1) is DMF, dimethyl sulfoxide (DMSO) or tetrahydrofuran (THF).
3. the preparation method of Nanometer composite hydrogel as claimed in claim 1, it is characterized in that: the dewatering agent in described step (1) is N, N '-dicyclohexylcarbodiimide, N, N'-diisopropylcarbodiimide or 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride.
4. the preparation method of Nanometer composite hydrogel as claimed in claim 1, is characterized in that: the catalyzer in described step (1) is DMAP or 1-hydroxy benzo triazole.
5. the preparation method of Nanometer composite hydrogel as claimed in claim 1, it is characterized in that: in described step (2), initiator is Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile), azo-bis-iso-dimethyl, azo-bis-isobutyrate hydrochloride, azo two isobutyl imidazoline hydrochloride or 4,4 '-azo two (4-cyanopentanoic acid).
6. the preparation method of Nanometer composite hydrogel as claimed in claim 1, is characterized in that: the monomer in described step (2) is one in acrylamide, vinylformic acid, 4-vinylpridine, NIPA or its arbitrary combination.
7. the preparation method of Nanometer composite hydrogel as claimed in claim 1, it is characterized in that: in described step (1), the consumption of each component is as follows, the quality of graphene oxide: account for 0.2 ~ 10% of system total mass, the quality of RAFT reagent: account for 0.5 ~ 20% of system total mass, the quality of dewatering agent: account for 0.5 ~ 20% of system total mass, the quality of catalyzer: account for 0.1 ~ 5% of system total mass.
8. the preparation method of Nanometer composite hydrogel as claimed in claim 1, it is characterized in that: in described step (2), the consumption of each component is as follows, graphene oxide grafts 10 ~ 20mg, water 10 ~ 50mL, initiator first time consumption 0.03 ~ 0.07mg, initiator second time consumption 0.07 ~ 0.13mg, monomer first time consumption 0.75 ~ 1.5g, monomer second time consumption 2.25 ~ 4.5g, n-hexadecane 0.1 ~ 0.2g, emulsifying agent 0.05 ~ 0.1g.
9. the preparation method of Nanometer composite hydrogel as claimed in claim 1, is characterized in that: the emulsifying agent in described step (2) is Sodium dodecylbenzene sulfonate.
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Cited By (8)
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| CN105694066A (en) * | 2016-01-28 | 2016-06-22 | 湖南工业大学 | Self-healing biologically-friendly aquagel with excellent mechanical properties |
| CN106674545A (en) * | 2016-12-30 | 2017-05-17 | 合众（佛山）化工有限公司 | Compound hydrogel based on aqueous RAFT polymerization method |
| CN109277086A (en) * | 2018-09-20 | 2019-01-29 | 长安大学 | Uns-dimethylhydrazine adsorbent material, preparation method and applications in a kind of vehicle exhaust |
| CN109868340A (en) * | 2019-02-20 | 2019-06-11 | 常州市宝平不锈钢制品有限公司 | A kind of steel-making efficient carburant and preparation method thereof |
| CN110204991A (en) * | 2019-04-28 | 2019-09-06 | 西南石油大学 | A kind of efficient corrosion resisting h-BN/GO/ water-base epoxy composite material, preparation method and application |
| CN113272054A (en) * | 2018-11-26 | 2021-08-17 | 沙特阿拉伯石油公司 | Polymeric structures for adsorbents used to separate polar liquids from non-polar hydrocarbons |
| CN113563759A (en) * | 2021-07-14 | 2021-10-29 | 中国科学院山西煤炭化学研究所 | Graphene and nano-silver composite material and preparation method thereof |
| CN115403717A (en) * | 2022-08-23 | 2022-11-29 | 中国船舶重工集团公司第七二五研究所 | Antifouling gel particles and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105694066A (en) * | 2016-01-28 | 2016-06-22 | 湖南工业大学 | Self-healing biologically-friendly aquagel with excellent mechanical properties |
| CN106674545A (en) * | 2016-12-30 | 2017-05-17 | 合众（佛山）化工有限公司 | Compound hydrogel based on aqueous RAFT polymerization method |
| CN106674545B (en) * | 2016-12-30 | 2019-04-12 | 合众（佛山）化工有限公司 | A kind of composite water gel based on aqueous RAFT polymerization |
| CN109277086A (en) * | 2018-09-20 | 2019-01-29 | 长安大学 | Uns-dimethylhydrazine adsorbent material, preparation method and applications in a kind of vehicle exhaust |
| CN113272054A (en) * | 2018-11-26 | 2021-08-17 | 沙特阿拉伯石油公司 | Polymeric structures for adsorbents used to separate polar liquids from non-polar hydrocarbons |
| CN113272054B (en) * | 2018-11-26 | 2022-03-29 | 沙特阿拉伯石油公司 | Polymeric structures for adsorbents used to separate polar liquids from non-polar hydrocarbons |
| CN109868340A (en) * | 2019-02-20 | 2019-06-11 | 常州市宝平不锈钢制品有限公司 | A kind of steel-making efficient carburant and preparation method thereof |
| CN110204991A (en) * | 2019-04-28 | 2019-09-06 | 西南石油大学 | A kind of efficient corrosion resisting h-BN/GO/ water-base epoxy composite material, preparation method and application |
| CN113563759A (en) * | 2021-07-14 | 2021-10-29 | 中国科学院山西煤炭化学研究所 | Graphene and nano-silver composite material and preparation method thereof |
| CN115403717A (en) * | 2022-08-23 | 2022-11-29 | 中国船舶重工集团公司第七二五研究所 | Antifouling gel particles and preparation method thereof |
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Application publication date: 20151209 |