CN109897316A - A kind of preparation method of polyaniline/polyvinyl alcohol composite conducting gel - Google Patents
A kind of preparation method of polyaniline/polyvinyl alcohol composite conducting gel Download PDFInfo
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Abstract
The present invention relates to Functional polymer materials technology fields, particularly relate to a kind of preparation method of polyaniline/polyvinyl alcohol composite conducting gel.The present invention provides the multimeshed network compound hydrogel material of a kind of high strength and electric conductivity, using aziridine and glutaraldehyde as multiple crosslinking agent, using polyvinyl alcohol (PVA) hydrogel material as I network, in conjunction with the polyaniline hydrogel material being crosslinked using aziridine as Section II network, the characteristics of present invention makes full use of aziridine molecule not only and can react but also can be reacted with polyvinyl alcohol molecule with polyaniline molecule, polyaniline hydrogel molecules are formed using it as the gel cross-linkage factor to intert mutually with PVA molecule, polyaniline hydrogel aggregation is evenly distributed in PVA hydrogel network, improve the electric conductivity and mechanical strength of conductive hydrogel.Meanwhile the excellent properties of PVA hydrogel backbone ensure that the good flexibility of polyaniline/polyvinyl alcohol compound hydrogel material.
Description
Technical field
The present invention relates to Functional polymer materials technology fields, particularly relate to a kind of polyaniline/polyvinyl alcohol composite conducting
The preparation method of gel.
Background technique
Hydrogel is a kind of functional polymer material, by three-dimensional net structure macromolecule and fill in its network chain gap
Hydrone medium is constituted.Hydrogel is soft and flexible, can be swollen in water, and can generate to extraneous small stimulation significant
Response, there is intelligence, therefore cause extensive research in recent years.Research is concentrated mainly on the preparation of novel hydrogels and new
Hydrogel application field.Hydrogel is widely used, and can be used as drug controlled release material, tissue bulking material, artificial cartilage, change
Scholar-tyrant, light control material, biosensor, tissue cultures etc..
Polyaniline (PANI) is a kind of conducting polymer of p-type doping, though its discovery is later, because its is nontoxic, raw material is easy
It obtains, various structures, preparation is simple, environmental stability is good, electric conductivity is relatively good, different redox states correspond to different face
The advantages that color and obtain extensive concern and fast development.The main chain of conducting polymer is rigid, chain and interchain electron system phase
Interaction is stronger, does not melt so that conducting polymer is insoluble, it is difficult to process, significantly limit the practical application of conducting polymer.
Therefore, conductive hydrogel is made in conducting polymer, not only can solve the processability problems of material, but also gel can be had both
Thus the good mechanical performance of material, swelling behavior improve conducting polymer physics, chemical property, cause people in recent years
The big interest of plate.Engineering properties, swelling property and the conduction that conducting polymer hydrogel combines conventional polymer hydrogel are poly-
The unique physicochemical properties of object are closed, have been obtained just in fields such as electrochemical capacitor, micro- pattern electrochemical appliance and sensors
Step application.
Since the main chain rigidity of the polymer such as PANI is stronger, it is practically insoluble in common solvent, so by handing in solution
Connection conducting polymer realizes that the route of gelation is difficult to obtain conductive polymer gel.Therefore, general conductive hydrogel is by exhausted
The stephanoporate framework and electro-chemical activity packing material of edge are constituted.It is conducting polymer as conductive agent using polyaniline in having been reported
The conducting polymer hydrogel of preparation, insulation stephanoporate framework material have polyacrylic acid, polyacrylamide, polyvinyl alcohol, carboxylic first
Base cellulose etc..But the hydrogel conductivity of this method preparation is not very high, because in these conductive composite hydrogels
In, conducting polymer is present in the duct of matrix gel as dispersed phase, it is difficult to form a continuous electric conductivity net
Network.Meanwhile this two phase structure would generally weaken the overall mechanical properties of conductive plural gel.
Aziridine crosslinker is to study at present more mature and effective room temperature crosslinking agent, the crosslinking of this kind of crosslinking agent are anti-
Answer speed fast, effect is obvious, it is formed by aziridine and three-functionality-degree or the condensation of the polyolcondensation product of higher functionality
's.Aziridine ring exists in structure compared with hightension, and activity is higher, and molecule, can be with carboxyl, amino under room temperature there are a large amount of groups
It is reacted with hydroxyl, generates insoluble reticular structure cross-linking products, can greatly improve the intensity of material.The present invention provides one
The multimeshed network compound hydrogel material of kind of high strength and electric conductivity, it is using aziridine and glutaraldehyde as compound
Crosslinking agent, using polyvinyl alcohol (PVA) hydrogel material as I network, in conjunction with the polyaniline water-setting glue material being crosslinked with aziridine
Material is used as Section II network, is a kind of compound hydrogel material with Multi-network.
Summary of the invention
The object of the present invention is to provide a kind of simple and easy preparations of flexible polyaniline conduction compound hydrogel material
Method, obtained material has good conductive property, mechanical strength and flexibility.
The technical scheme of the present invention is realized as follows:
A kind of preparation method of polyaniline/polyvinyl alcohol composite conducting gel, comprising the following steps:
(1) by weight will polyvinyl alcohol be added acidic aqueous solution in, stirred at a temperature of 85 DEG C~95 DEG C 2~4 hours until
Polyvinyl alcohol is completely dissolved to form homogeneous solution, cools to 20~30 DEG C, and aniline monomer is then added, and stirs 5~10min, then
Aziridine crosslinker, glutaraldehyde is added, stirs evenly, then pours into the mixture after stirring in mold, normal temperature crosslinked 5~
120min obtains the polyvinyl alcohol hydrogel containing aniline monomer；
(2) polyvinyl alcohol hydrogel that step (1) obtains is added in the acidic aqueous solution of ammonium persulfate and is reacted, controlled
Temperature is 0~40 DEG C, and the reaction time is 1.0~8.0 hours, obtains polyaniline/polyvinyl alcohol composite conducting hydrogel.
The parts by weight of polyvinyl alcohol and acidic aqueous solution are followed successively by 8~20 parts, 80~92 parts in the step (1).
In the step (1) parts by weight of aniline monomer be 2~5 parts, aziridine crosslinker, glutaraldehyde parts by weight successively
It is 0.1~0.5 part, 0.05~0.2 part.
In the step (2) parts by weight of the acidic aqueous solution of polyvinyl alcohol hydrogel and ammonium persulfate be 5~20 parts and
50~200 parts.
The polyvinyl alcohol is PVA1799 or PVA1797, wherein the degree of polymerization 1700 of PVA1799, alcoholysis degree 99%,
The degree of polymerization 1700 of PVA1797, alcoholysis degree 97%；Acidic aqueous solution is hydrochloric acid, sulfuric acid or p-methyl benzenesulfonic acid, and aziridine is handed over
Connection agent is trifunctional aziridine crosslinker.
The concentration of the acidic aqueous solution is 0.5~2mol/L, and the concentration of ammonium persulfate is 20~80g/L.
The beneficial effects of the present invention are:
1. the present invention uses aziridine and glutaraldehyde as multiple crosslinking agent first, the polyvinyl alcohol containing aniline monomer is prepared
Hydrogel, then the aniline monomer in gel network is polymerize, it obtains polyvinyl alcohol network and electrically conductive polyaniline network is mutual
Perforative hydrogel.Trifunctional aziridine used in the present invention exists in structure compared with hightension, active higher, molecule
It there are a large amount of groups, can be reacted with carboxyl, amino and hydroxyl under room temperature, generate insoluble reticular structure cross-linking products, it can be with
Greatly improve the intensity of material.
2. the present invention makes full use of aziridine molecule not only can react but also can be with poly- second with polyaniline molecule
The characteristics of enol molecule reacts forms polyaniline hydrogel molecules using it as the gel cross-linkage factor and PVA molecule is mutual
Interspersed, polyaniline hydrogel aggregation is evenly distributed in PVA hydrogel network, improves the electric conductivity of conductive hydrogel
And mechanical strength.Meanwhile the excellent properties of PVA hydrogel backbone ensure that polyaniline/polyvinyl alcohol compound hydrogel material is good
Good flexibility.Prepared used by the application polyaniline/polyvinyl alcohol compound hydrogel material method have it is easy to operate, at
This cheap advantage makes polyaniline/polyvinyl alcohol compound hydrogel material have wide application in flexible energy storage material field
Prospect.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Those of ordinary skill in the art's every other embodiment obtained under that premise of not paying creative labor, belongs to this hair
The range of bright protection.
Embodiment 1
A kind of preparation method of polyaniline/polyvinyl alcohol composite conducting gel, comprising the following steps:
8 grams of polyvinyl alcohol 1799 are added in the aqueous hydrochloric acid solution of 92 grams of 0.5mol/L, 2 hours are stirred at a temperature of 95 DEG C directly
It is completely dissolved to form homogeneous solution to polyvinyl alcohol；Solution is cooled to 30 DEG C, 2 grams of aniline monomer is added to it, stirs 5min,
0.1 gram of aziridine crosslinker, 0.2 gram of glutaraldehyde are added, is stirred evenly；Then it pours the mixture into mold, it is normal temperature crosslinked
5min obtains the PVA hydrogel containing aniline monomer.
By 10 grams of PVA hydrogel obtained containing aniline monomer be immersed in the aqueous hydrochloric acid solutions of 100 grams of ammonium persulfates into
Row reaction controls 0 DEG C of temperature, and the reaction time is 8.0 hours, obtains polyaniline/polyvinyl alcohol composite conducting hydrogel.Wherein cross
The concentration of ammonium sulfate is 20g/L, and the concentration of aqueous hydrochloric acid solution is 0.5mol/L.This composite hydrogel tensile strength is 1.3 Mpa,
Conductivity is 0.07 S/m.
Embodiment 2
A kind of preparation method of polyaniline/polyvinyl alcohol composite conducting gel, comprising the following steps:
20 grams of polyvinyl alcohol 1797 are added in the aqueous hydrochloric acid solution of 80 grams of 1mol/L, 85 DEG C degree under stir 4 hours until
Polyvinyl alcohol is completely dissolved to form homogeneous solution；Solution is cooled to 20 DEG C, 5 grams of aniline monomer is added to it, stirs, 10min,
0.5 gram of aziridine crosslinker, 0.05 gram of glutaraldehyde are added, is stirred evenly；Then it pours the mixture into mold, it is normal temperature crosslinked
120min obtains the PVA hydrogel containing aniline monomer.
By 20 grams of PVA hydrogel obtained containing aniline monomer be immersed in the aqueous hydrochloric acid solutions of 200 grams of ammonium persulfates into
Row reaction controls 0 DEG C of temperature, and the reaction time is 8.0 hours, obtains polyaniline/polyvinyl alcohol composite conducting hydrogel.Wherein cross
The concentration of ammonium sulfate is 80g/L, and the concentration of aqueous hydrochloric acid solution is 1mol/L.This composite hydrogel tensile strength is 2.8 Mpa, electricity
Conductance is 0.36 S/m.
Embodiment 3
A kind of preparation method of polyaniline/polyvinyl alcohol composite conducting gel, comprising the following steps:
15 grams of polyvinyl alcohol 1799 are added in the aqueous sulfuric acid of 85 grams of 1mol/L, 85 DEG C degree under stir 4 hours until
Polyvinyl alcohol is completely dissolved to form homogeneous solution；Solution is cooled to 25 DEG C, 4 grams of aniline monomer is added to it, stirs, 10min,
0.3 gram of aziridine crosslinker, 0.1 gram of glutaraldehyde are added, is stirred evenly；Then it pours the mixture into mold, it is normal temperature crosslinked
90min obtains the PVA hydrogel containing aniline monomer.
By 15 grams of PVA hydrogel obtained containing aniline monomer be immersed in the aqueous sulfuric acids of 200 grams of ammonium persulfates into
Row reaction controls 10 DEG C of temperature, and the reaction time is 4.0 hours, obtains polyaniline/polyvinyl alcohol composite conducting hydrogel.Wherein
The concentration of ammonium persulfate is 50g/L, and the concentration of aqueous sulfuric acid is 1mol/L.This composite hydrogel tensile strength is 2.1 Mpa,
Conductivity is 0.23 S/m.
Embodiment 4
A kind of preparation method of polyaniline/polyvinyl alcohol composite conducting gel, comprising the following steps:
12 grams of polyvinyl alcohol 1797 are added in the p-methyl benzenesulfonic acid aqueous solution of 88 gram of 0.8 mol/L, are stirred under 90 DEG C of degree
It mixes 3.5 hours to form homogeneous solution until polyvinyl alcohol is completely dissolved；Solution is cooled to 30 DEG C, aniline monomer 5 is added to it
Gram, 8 min are stirred, 0.4 gram of aziridine crosslinker, 0.15 gram of glutaraldehyde is added, stirs evenly；Then mould is poured the mixture into
In tool, normal temperature crosslinked 5min obtains the PVA hydrogel containing aniline monomer.
14 grams of PVA hydrogel obtained containing aniline monomer are immersed in the p-methyl benzenesulfonic acid of 150 grams of ammonium persulfates
Aqueous solution is reacted, and controls 30 DEG C of temperature, and the reaction time is 3.0 hours, obtains polyaniline/polyvinyl alcohol composite conducting water-setting
Glue.Wherein the concentration of ammonium persulfate is 40g/L, and the concentration of toluenesulfonic acid aqueous solution is 0.8 mol/L.This composite hydrogel is drawn
Stretching intensity is 1.9 Mpa, and conductivity is 0.29 S/m.
Embodiment 5
A kind of preparation method of polyaniline/polyvinyl alcohol composite conducting gel, comprising the following steps:
9 grams of polyvinyl alcohol 1799 are added in the aqueous sulfuric acid of 91 grams of 2mol/L, 4 hours are stirred under 85 DEG C of degree until poly-
Vinyl alcohol is completely dissolved to form homogeneous solution；Solution is cooled to 25 DEG C, to its be added 3 grams of aniline monomer, stir 7min, then plus
Enter 0.35 gram of aziridine crosslinker, 0.15 gram of glutaraldehyde, stirs evenly；Then it pours the mixture into mold, it is normal temperature crosslinked
5min obtains the PVA hydrogel containing aniline monomer.
By 15 grams of PVA hydrogel obtained containing aniline monomer be immersed in the aqueous sulfuric acids of 180 grams of ammonium persulfates into
Row reaction controls 25 DEG C of temperature, and the reaction time is 4.0 hours, obtains polyaniline/polyvinyl alcohol composite conducting hydrogel.Wherein
The concentration of ammonium persulfate is 70g/L, and the concentration of aqueous sulfuric acid is 2mol/L.This composite hydrogel tensile strength is 1.2 Mpa,
Conductivity is 0.13 S/m.
Embodiment 6
A kind of preparation method of polyaniline/polyvinyl alcohol composite conducting gel, comprising the following steps:
10 grams of polyvinyl alcohol 1799 are added in the p-methyl benzenesulfonic acid aqueous solution of 90 gram of 1.2 mol/L, are stirred under 88 DEG C of degree
It mixes 3.6 hours to form homogeneous solution until polyvinyl alcohol is completely dissolved；Solution is cooled to 30 DEG C, aniline monomer 4 is added to it
Gram, 7 min are stirred, 0.2 gram of aziridine crosslinker, 0.2 gram of glutaraldehyde is added, stirs evenly；Then mould is poured the mixture into
In tool, normal temperature crosslinked 90min obtains the PVA hydrogel containing aniline monomer.
12 grams of PVA hydrogel obtained containing aniline monomer are immersed in the p-methyl benzenesulfonic acid of 180 grams of ammonium persulfates
Aqueous solution is reacted, and controls 35 DEG C of temperature, and the reaction time is 2.0 hours, obtains polyaniline/polyvinyl alcohol composite conducting water-setting
Glue.Wherein the concentration of ammonium persulfate is 70g/L, and the concentration of toluenesulfonic acid aqueous solution is 1.2 mol/L.This composite hydrogel is drawn
Stretching intensity is 0.8 Mpa, and conductivity is 0.51 S/m.
Embodiment 7
A kind of preparation method of polyaniline/polyvinyl alcohol composite conducting gel, comprising the following steps:
18 grams of polyvinyl alcohol 1797 are added in the aqueous hydrochloric acid solution of 82 grams of 1.2mol/L, are stirred 2 hours at a temperature of 95 DEG C
Homogeneous solution is formed until polyvinyl alcohol is completely dissolved；Solution is cooled to 21 DEG C, is added 3 grams of aniline monomer to it, stirring
5min adds 0.3 gram of aziridine crosslinker, 0.1 gram of glutaraldehyde, stirs evenly；Then it pours the mixture into mold, room temperature
It is crosslinked 50min, obtains the PVA hydrogel containing aniline monomer.
By 12 grams of PVA hydrogel obtained containing aniline monomer be immersed in the aqueous hydrochloric acid solutions of 140 grams of ammonium persulfates into
Row reaction controls 8 DEG C of temperature, and the reaction time is 5.0 hours, obtains polyaniline/polyvinyl alcohol composite conducting hydrogel.Wherein cross
The concentration of ammonium sulfate is 45g/L, and the concentration of aqueous hydrochloric acid solution is 1.2mol/L.This composite hydrogel tensile strength is 2.3 Mpa,
Conductivity is 0.23 S/m.
Embodiment 8
A kind of preparation method of polyaniline/polyvinyl alcohol composite conducting gel, comprising the following steps:
14 grams of polyvinyl alcohol 1799 are added in the aqueous sulfuric acid of 86 gram of 1.6 mol/L, 4 hours are stirred under 85 DEG C of degree directly
It is completely dissolved to form homogeneous solution to polyvinyl alcohol；Solution is cooled to 25 DEG C, 4 grams of aniline monomer is added to it, stirs 8min,
0.4 gram of aziridine crosslinker, 0.15 gram of glutaraldehyde are added, is stirred evenly；Then it pours the mixture into mold, it is normal temperature crosslinked
30min obtains the PVA hydrogel containing aniline monomer.
By 15 grams of PVA hydrogel obtained containing aniline monomer be immersed in the aqueous sulfuric acids of 150 grams of ammonium persulfates into
Row reaction controls 10 DEG C of temperature, and the reaction time is 3.0 hours, obtains polyaniline/polyvinyl alcohol composite conducting hydrogel.Wherein
The concentration of ammonium persulfate is 50g/L, and the concentration of aqueous sulfuric acid is 1.6 mol/L.This composite hydrogel tensile strength is 1.8
Mpa, conductivity are 0.21 S/m.
Embodiment 9
A kind of preparation method of polyaniline/polyvinyl alcohol composite conducting gel, comprising the following steps:
14 grams of polyvinyl alcohol 1799 are added in the p-methyl benzenesulfonic acid aqueous solution of 84 gram of 0.9 mol/L, are stirred under 90 DEG C of degree
It mixes 3 hours to form homogeneous solution until polyvinyl alcohol is completely dissolved；Solution is cooled to 20 DEG C, is added 3 grams of aniline monomer to it,
8 min are stirred, 0.4 gram of aziridine crosslinker, 0.15 gram of glutaraldehyde is added, stirs evenly；Then mold is poured the mixture into
In, normal temperature crosslinked 40min obtains the PVA hydrogel containing aniline monomer.
12 grams of PVA hydrogel obtained containing aniline monomer are immersed in the p-methyl benzenesulfonic acid of 160 grams of ammonium persulfates
Aqueous solution is reacted, and controls 35 DEG C of temperature, and the reaction time is 2.0 hours, obtains polyaniline/polyvinyl alcohol composite conducting water-setting
Glue.Wherein the concentration of ammonium persulfate is 60g/L, and the concentration of toluenesulfonic acid aqueous solution is 0.9 mol/L.This composite hydrogel is drawn
Stretching intensity is 1.6 Mpa, and conductivity is 0.33 S/m.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of preparation method of polyaniline/polyvinyl alcohol composite conducting gel, it is characterised in that the following steps are included:
(1) by weight will polyvinyl alcohol be added acidic aqueous solution in, stirred at a temperature of 85 DEG C~95 DEG C 2~4 hours until
Polyvinyl alcohol is completely dissolved to form homogeneous solution, cools to 20~30 DEG C, and aniline monomer is then added, and stirs 5~10min, then
Aziridine crosslinker, glutaraldehyde is added, stirs evenly, then pours into the mixture after stirring in mold, normal temperature crosslinked 5~
120min obtains the polyvinyl alcohol hydrogel containing aniline monomer；
(2) polyvinyl alcohol hydrogel that step (1) obtains is added in the acidic aqueous solution of ammonium persulfate and is reacted, controlled
Temperature is 0~40 DEG C, and the reaction time is 1.0~8.0 hours, obtains polyaniline/polyvinyl alcohol composite conducting hydrogel.
2. the preparation method of polyaniline/polyvinyl alcohol composite conducting gel according to claim 1, it is characterised in that: institute
It states the parts by weight of polyvinyl alcohol and acidic aqueous solution in step (1) and is followed successively by 8~20 parts, 80~92 parts.
3. the preparation method of polyaniline/polyvinyl alcohol composite conducting gel according to claim 1, it is characterised in that: institute
State aniline monomer in step (1) parts by weight be 2~5 parts, aziridine crosslinker, glutaraldehyde parts by weight be followed successively by 0.1~0.5
Part, 0.05~0.2 part.
4. the preparation method of polyaniline/polyvinyl alcohol composite conducting gel according to claim 1, it is characterised in that: institute
The parts by weight for stating the acidic aqueous solution of polyvinyl alcohol hydrogel and ammonium persulfate in step (2) are 5~20 parts and 50~200 parts.
5. the preparation method of polyaniline/polyvinyl alcohol composite conducting gel according to claim 1, it is characterised in that: institute
Stating polyvinyl alcohol is PVA1799 or PVA1797, wherein the degree of polymerization 1700 of PVA1799, alcoholysis degree 99%, the polymerization of PVA1797
Degree 1700, alcoholysis degree 97%；Acidic aqueous solution is hydrochloric acid, sulfuric acid or p-methyl benzenesulfonic acid, and aziridine crosslinker is trifunctional
Aziridine crosslinker.
6. the preparation method of polyaniline/polyvinyl alcohol composite conducting gel according to claim 5, it is characterised in that: institute
The concentration for stating acidic aqueous solution is 0.5~2mol/L, and the concentration of ammonium persulfate is 20~80g/L.
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Cited By (6)
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| CN111499884A (en) * | 2020-04-11 | 2020-08-07 | 上海理工大学 | Method for preparing conductive polyaniline hydrogel based on composite oxidant |
| CN112151816A (en) * | 2020-10-26 | 2020-12-29 | 中北大学 | Cobalt-based composite catalyst for direct methanol fuel cell anode and preparation method thereof |
| CN113325141A (en) * | 2021-07-13 | 2021-08-31 | 浙江农林大学 | Preparation method of high-sensitivity flexible gas sensing material for detecting ammonia gas at room temperature |
| CN113336971A (en) * | 2021-06-11 | 2021-09-03 | 东华大学 | Nano-structure polyaniline composite hydrogel and preparation method and application thereof |
| CN113372576A (en) * | 2021-05-25 | 2021-09-10 | 武汉工程大学 | Polyacid-polyaniline-glycerol-polyvinyl alcohol composite gel and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110563969A (en) * | 2019-09-23 | 2019-12-13 | 南京邮电大学 | self-healing conductive hydrogel, preparation method and application thereof |
| CN111499884A (en) * | 2020-04-11 | 2020-08-07 | 上海理工大学 | Method for preparing conductive polyaniline hydrogel based on composite oxidant |
| CN112151816A (en) * | 2020-10-26 | 2020-12-29 | 中北大学 | Cobalt-based composite catalyst for direct methanol fuel cell anode and preparation method thereof |
| CN113372576A (en) * | 2021-05-25 | 2021-09-10 | 武汉工程大学 | Polyacid-polyaniline-glycerol-polyvinyl alcohol composite gel and preparation method thereof |
| CN113336971A (en) * | 2021-06-11 | 2021-09-03 | 东华大学 | Nano-structure polyaniline composite hydrogel and preparation method and application thereof |
| CN113325141A (en) * | 2021-07-13 | 2021-08-31 | 浙江农林大学 | Preparation method of high-sensitivity flexible gas sensing material for detecting ammonia gas at room temperature |
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