CN114920997A - High-conductivity polypyrrole gel and preparation method thereof - Google Patents
High-conductivity polypyrrole gel and preparation method thereof Download PDFInfo
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- 229920000128 polypyrrole Polymers 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000001879 gelation Methods 0.000 title description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 19
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 19
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 16
- 150000003839 salts Chemical class 0.000 claims abstract description 16
- 239000000178 monomer Substances 0.000 claims abstract description 14
- 229920001661 Chitosan Polymers 0.000 claims abstract description 13
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000001263 FEMA 3042 Substances 0.000 claims abstract description 11
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims abstract description 11
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 11
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- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 11
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims abstract description 11
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- 238000000034 method Methods 0.000 claims description 12
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- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 6
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 4
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 3
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 3
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 3
- FYWVMROQEMIMSK-UHFFFAOYSA-N butane-1-sulfonic acid;hydrogen sulfate;3-methyl-1h-imidazol-3-ium Chemical compound OS([O-])(=O)=O.C[N+]=1C=CNC=1.CCCCS(O)(=O)=O FYWVMROQEMIMSK-UHFFFAOYSA-N 0.000 claims description 3
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 3
- 238000004108 freeze drying Methods 0.000 claims description 3
- 239000002608 ionic liquid Substances 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 3
- FYMCOOOLDFPFPN-UHFFFAOYSA-K iron(3+);4-methylbenzenesulfonate Chemical compound [Fe+3].CC1=CC=C(S([O-])(=O)=O)C=C1.CC1=CC=C(S([O-])(=O)=O)C=C1.CC1=CC=C(S([O-])(=O)=O)C=C1 FYMCOOOLDFPFPN-UHFFFAOYSA-K 0.000 claims description 3
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- LIKZXCROQGHXTI-UHFFFAOYSA-M acid blue 25 Chemical compound [Na+].C1=2C(=O)C3=CC=CC=C3C(=O)C=2C(N)=C(S([O-])(=O)=O)C=C1NC1=CC=CC=C1 LIKZXCROQGHXTI-UHFFFAOYSA-M 0.000 claims description 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims description 2
- 229940012189 methyl orange Drugs 0.000 claims description 2
- YZORUOZKRBVLEG-UHFFFAOYSA-M sodium;4-[[4-(diethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(CC)CC)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 YZORUOZKRBVLEG-UHFFFAOYSA-M 0.000 claims description 2
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- KAIPKTYOBMEXRR-UHFFFAOYSA-N 1-butyl-3-methyl-2h-imidazole Chemical compound CCCCN1CN(C)C=C1 KAIPKTYOBMEXRR-UHFFFAOYSA-N 0.000 description 1
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- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
- C08J9/286—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum the liquid phase being a solvent for the monomers but not for the resulting macromolecular composition, i.e. macroporous or macroreticular polymers
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J9/0066—Use of inorganic compounding ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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Abstract
The invention discloses a high-conductivity polypyrrole gel and a preparation method thereof, and relates to the technical field of high polymer materials, wherein the high-conductivity polypyrrole gel comprises, by weight, 21-24 parts of carboxymethyl chitosan, 7-9 parts of a cross-linking agent, 6-8 parts of a pyrrole monomer, 6-9 parts of polyvinyl alcohol, 5-7 parts of a sulfur-based dye, 5-7 parts of tannic acid, 31-33 parts of a low-freezing-point medium, 12-14 parts of a trivalent iron salt, and 92-94 parts of deionized water. According to the high-conductivity polypyrrole gel, the holes of the gel are reduced through the carboxymethyl chitosan, the cross-linking agent and the polyvinyl alcohol, the overall density of the gel is improved, the conductivity of the gel is improved, and meanwhile, the conductivity of the gel is further improved through the trivalent ferric salt.
Description
Technical Field
The invention relates to the technical field of high polymer materials, and particularly relates to a high-conductivity polypyrrole gel and a preparation method thereof.
Background
Polypyrrole is a common conductive polymer. The pure pyrrole monomer is colorless oily liquid at normal temperature, is a C, N five-membered heterocyclic molecule, is slightly soluble in water and nontoxic, and the polypyrrole can be prepared from the pyrrole monomer by a chemical oxidation method or an electrochemical method. The chemical polymerization is to obtain conjugated long-chain molecules in a certain reaction medium by oxidizing monomers with an oxidant or by coupling metallorganics and simultaneously complete a doping process. The method has simple synthesis process and low cost, and is suitable for mass production. The product obtained when the polypyrrole is prepared by a chemical method is generally solid polypyrrole powder, namely the polypyrrole powder is difficult to dissolve in a general organic solvent, has poor mechanical properties and is difficult to process, and the polypyrrole can be used for biological, ion detection, super-capacitor and anti-static materials, modified electrodes of photoelectrochemical cells and electrode materials of storage batteries. In addition, the material can also be used as an electromagnetic shielding material and a gas separation membrane material, is used for electrolytic capacitors, electrocatalysis, conductive polymer composite materials and the like, and has wide application range;
in the prior art, due to the natural porous structure and the property of gel, the density of the gel is low, so that the polypyrrole gel material generally has the defect of low conductivity at present, the polypyrrole gel material is limited in multiple aspects to a great extent, and the preparation process is complicated, so that the polypyrrole gel material is not beneficial to large-scale popularization and use in industry and life.
Disclosure of Invention
The invention mainly aims to provide a high-conductivity polypyrrole gel and a preparation method thereof, so as to solve the problems in the background art.
In order to achieve the purpose, the invention adopts the technical scheme that: the high-conductivity polypyrrole gel comprises, by weight, 20-25 parts of carboxymethyl chitosan, 5-10 parts of a cross-linking agent, 5-10 parts of a pyrrole monomer, 5-10 parts of polyvinyl alcohol, 4-8 parts of a sulfur-based dye, 4-8 parts of tannic acid, 30-35 parts of a low-freezing-point medium, 10-15 parts of a ferric iron salt and 90-95 parts of deionized water.
Further, the coating comprises, by weight, 21-24 parts of carboxymethyl chitosan, 7-9 parts of a cross-linking agent, 6-8 parts of a pyrrole monomer, 6-9 parts of polyvinyl alcohol, 5-7 parts of a sulfur-based dye, 5-7 parts of tannic acid, 31-33 parts of a low-freezing-point medium, 12-14 parts of a ferric salt and 92-94 parts of deionized water.
Further, the cross-linking agent is one or two of dicumyl peroxide, benzoyl peroxide, di-tert-butyl peroxide and dicumyl peroxide.
Further, the polyvinyl alcohol is a polymer stabilizer, and the molecular weight of the polyvinyl alcohol is 70000-200000.
Further, the medium with the low freezing point is one or two of ionic liquid 1-butyl sulfonic acid-3-methylimidazole hydrogen sulfate trichloro iron salt, 1-butyl sulfonic acid-3-methylimidazole hydrogen sulfate and 1-butyl-3-methylimidazole tetrachloro iron salt.
Further, the ferric salt is one or two of ferric trichloride, ferric sulfate, ferric nitrate and ferric p-toluenesulfonate.
A preparation method of high-conductivity polypyrrole gel comprises the following steps:
step S1: mixing polyvinyl alcohol and deionized water at room temperature, stirring for 5-10min, fully mixing to obtain a high-molecular stabilizer solution, and then dividing the high-molecular stabilizer solution into two parts;
step S2: adding pyrrole monomer, sulfur-based dye and tannic acid into a part of the high molecular stabilizer solution, and stirring to react for 5-20min to obtain a first solution;
step S3: then adding trivalent ferric salt into the other part of the high molecular stabilizer solution, and stirring to dissolve the trivalent ferric salt to prepare a second solution;
step S4: quickly mixing the first solution and the second solution, fully stirring, adding carboxymethyl chitosan and a cross-linking agent, and then performing freeze-drying treatment to obtain a primary gel;
step S5: and placing the gel in a low freezing point medium at room temperature for oscillation treatment to obtain the high-conductivity polypyrrole gel.
Further, the mixed solution is injected into a sealed mold in the step S4, the mixed solution and the mold are frozen for 4-12 hours in an environment of-30 ℃ to-70 ℃, and then the gel is frozen and dried for 2 hours at-20 ℃.
Further, the S2 is one or two of methyl orange, ethyl orange and acid blue 25 as a sulfonic acid group dye.
The invention has the following beneficial effects:
the high-conductivity polypyrrole gel provided by the invention has the advantages that the holes of the gel are reduced through the carboxymethyl chitosan, the cross-linking agent and the polyvinyl alcohol, the overall density of the gel is improved, the conductivity of the gel is improved, meanwhile, the conductivity of the gel is further improved through the trivalent ferric salt, the high-conductivity polypyrrole gel prepared by the method has good conductivity and mechanical property, can tolerate a wider temperature range, is not easy to lose water and collapse, and is not easy to freeze and freeze.
Secondly, the preparation method of the high-conductivity polypyrrole gel has the advantages of wide raw material source, simple operation, easy industrial production, strong processing and using controllability and strong adaptability.
Of course, it is not necessary for any product in which the invention is practiced to achieve all of the above-described advantages at the same time.
Drawings
FIG. 1 is a flow chart of the preparation method of the high conductivity polypyrrole gel of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The high-conductivity polypyrrole gel comprises, by weight, 20-25 parts of carboxymethyl chitosan, 5-10 parts of a cross-linking agent, 5-10 parts of a pyrrole monomer, 5-10 parts of polyvinyl alcohol, 4-8 parts of a sulfur-based dye, 4-8 parts of tannic acid, 30-35 parts of a low-freezing-point medium, 10-15 parts of a ferric iron salt and 90-95 parts of deionized water.
The coating comprises, by weight, 21-24 parts of carboxymethyl chitosan, 7-9 parts of a cross-linking agent, 6-8 parts of a pyrrole monomer, 6-9 parts of polyvinyl alcohol, 5-7 parts of a sulfur-based dye, 5-7 parts of tannic acid, 31-33 parts of a low-freezing-point medium, 12-14 parts of a trivalent ferric salt and 92-94 parts of deionized water.
The cross-linking agent is one or two of dicumyl peroxide, benzoyl peroxide, di-tert-butyl peroxide and dicumyl hydroperoxide, the polyvinyl alcohol is a polymer stabilizer, and the molecular weight of the polyvinyl alcohol is 70000-200000.
The low freezing point medium is one or two of ionic liquid 1-butyl sulfonic acid-3-methylimidazole hydrogen sulfate ferric chloride salt, 1-butyl sulfonic acid-3-methylimidazole bisulfate and 1-butyl-3-methylimidazole tetrachloroferric salt, and the ferric salt is one or two of ferric chloride, ferric sulfate, ferric nitrate and ferric p-toluenesulfonate.
Example 2
A preparation method of high-conductivity polypyrrole gel comprises the following steps:
step S1: mixing polyvinyl alcohol and deionized water at room temperature, stirring for 5-10min, fully mixing to obtain a high-molecular stabilizer solution, and then dividing the high-molecular stabilizer solution into two parts;
step S2: adding pyrrole monomer, sulfur-based dye and tannic acid into a part of the high molecular stabilizer solution, and stirring to react for 5-20min to obtain a first solution;
step S3: then adding trivalent ferric salt into the other part of the polymer stabilizer solution, and stirring to dissolve the trivalent ferric salt to prepare a second solution;
step S4: quickly mixing the first solution and the second solution, stirring fully, adding carboxymethyl chitosan and a cross-linking agent, and then performing freeze-drying treatment to obtain a primary gel;
step S5: and placing the gel in a low freezing point medium at room temperature for vibration treatment to obtain the high-conductivity polypyrrole gel.
Example 3
Aiming at detecting the using effect of the ultra-white IXPE foam prepared by the method, the high-conductivity polypyrrole gel prepared by the method is selected, and preferably, the high-conductivity polypyrrole gel comprises, by weight, 21-24 parts of carboxymethyl chitosan, 7-9 parts of a cross-linking agent, 6-8 parts of a pyrrole monomer, 6-9 parts of polyvinyl alcohol, 5-7 parts of a sulfur-based dye, 5-7 parts of tannic acid, 31-33 parts of a low-freezing-point medium, 12-14 parts of a trivalent ferric salt and 92-94 parts of deionized water;
randomly taking commercial polypyrrole gel to compare with the high-conductivity polypyrrole gel, and setting A, B, C and four control groups D, wherein the A, B, C group is the commercial high-conductivity polypyrrole gel, the D group is the high-conductivity polypyrrole gel, the detection standard is the conductivity and the frost resistance of each foam in the same use environment and state, and the test conditions are shown in the following table.
Table one is the use test comparison of 4 groups of foam:
| group of | A | B | C | D |
| Conductivity of electricity | Superior food | Is good | Good effect | Superior food |
| Freezing resistance | Is good | Youyou (an instant noodle) | Is good | Superior food |
As can be seen from the table I, the high-conductivity polypyrrole gel prepared by the method disclosed by the invention has the advantages of good comprehensive use effect, balanced conductivity and frost resistance, obvious use advantages compared with the commercially available high-conductivity polypyrrole gel, and higher popularization value.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise forms disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand the invention for and utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (9)
1. The high-conductivity polypyrrole gel is characterized by comprising, by weight, 20-25 parts of carboxymethyl chitosan, 5-10 parts of a cross-linking agent, 5-10 parts of a pyrrole monomer, 5-10 parts of polyvinyl alcohol, 4-8 parts of a sulfur-based dye, 4-8 parts of tannic acid, 30-35 parts of a low-freezing-point medium, 10-15 parts of a trivalent iron salt and 90-95 parts of deionized water.
2. The high-conductivity polypyrrole gel according to claim 1, wherein the gel comprises, by weight, 21-24 parts of carboxymethyl chitosan, 7-9 parts of a cross-linking agent, 6-8 parts of a pyrrole monomer, 6-9 parts of polyvinyl alcohol, 5-7 parts of a sulfur-based dye, 5-7 parts of tannic acid, 31-33 parts of a low-freezing-point medium, 12-14 parts of a ferric salt, and 92-94 parts of deionized water.
3. The highly conductive polypyrrole gel according to claim 2, wherein said crosslinking agent is one or two of dicumyl peroxide, benzoyl peroxide, di-t-butyl peroxide and dicumyl hydroperoxide.
4. The polypyrrole gel of claim 2, wherein the polyvinyl alcohol is a polymeric stabilizer, and the molecular weight of the polyvinyl alcohol is 70000-200000.
5. The high-conductivity polypyrrole gel according to claim 2, wherein said low freezing point medium is one or two of ionic liquid 1-butyl sulfonic acid-3-methylimidazole hydrogen sulfate trichloroiron salt, 1-butyl sulfonic acid-3-methylimidazole hydrogen sulfate and 1-butyl-3-methylimidazole tetrachloroiron salt.
6. The highly conductive polypyrrole gel according to claim 2, wherein the ferric salt is one or two of ferric chloride, ferric sulfate, ferric nitrate and ferric p-toluenesulfonate.
7. The preparation method of the high-conductivity polypyrrole gel is characterized by comprising the following steps:
step S1: mixing polyvinyl alcohol and deionized water at room temperature, stirring for 5-10min, fully mixing to obtain a high-molecular stabilizer solution, and then dividing the high-molecular stabilizer solution into two parts;
step S2: adding pyrrole monomer, sulfur-based dye and tannic acid into a part of the high molecular stabilizer solution, and stirring to react for 5-20min to obtain a first solution;
step S3: then adding trivalent ferric salt into the other part of the high molecular stabilizer solution, and stirring to dissolve the trivalent ferric salt to prepare a second solution;
step S4: quickly mixing the first solution and the second solution, fully stirring, adding carboxymethyl chitosan and a cross-linking agent, and then performing freeze-drying treatment to obtain a primary gel;
step S5: and placing the gel in a low freezing point medium at room temperature for vibration treatment to obtain the high-conductivity polypyrrole gel.
8. The method for preparing polypyrrole gel with high conductivity according to claim 7, wherein the mixed solution is injected into the sealed mold in step S4, and the mold is frozen at-30 ℃ to-70 ℃ for 4-12 h, and then the gel is freeze-dried at-20 ℃ for 2 h.
9. The method for preparing highly conductive polypyrrole gel according to claim 7, wherein said S2 is one or two of methyl orange, ethyl orange and acid blue 25 as sulfonic dye.
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