CN106519287A - Preparation method of cellulose based conductive hydrogel - Google Patents
Preparation method of cellulose based conductive hydrogel Download PDFInfo
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- CN106519287A CN106519287A CN201611016038.3A CN201611016038A CN106519287A CN 106519287 A CN106519287 A CN 106519287A CN 201611016038 A CN201611016038 A CN 201611016038A CN 106519287 A CN106519287 A CN 106519287A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
- C08F251/02—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof on to cellulose or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0605—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0611—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring, e.g. polypyrroles
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- C—CHEMISTRY; METALLURGY
- 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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- C—CHEMISTRY; METALLURGY
- 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
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- 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
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L51/02—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to polysaccharides
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- C—CHEMISTRY; METALLURGY
- 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
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/052—Inducing phase separation by thermal treatment, e.g. cooling a solution
- C08J2201/0522—Inducing phase separation by thermal treatment, e.g. cooling a solution the liquid phase being organic
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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
- C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2351/02—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to polysaccharides
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- C—CHEMISTRY; METALLURGY
- 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
- C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
- C08J2479/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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Abstract
The invention discloses a preparation method of a cellulose based conductive hydrogel. The preparation method comprises the following steps: (1) dissolving microcrystalline cellulose (MCC) with 1-Butyl-3-methylimidazolium chloride, reacting in a N2 protective atmosphere, and adding N,N-methylenebisacrylamide and benzoyl peroxide to prepare a pure microcrystalline cellulose hydrogel; and (2) soaking the pure microcrystalline cellulose hydrogel obtained in the step (1) in a mixed solution of FeCl3 and sodium p-benzenesulfonate, and immersing in a pyrrole water solution to prepare the cellulose based conductive hydrogel. The cellulose based conductive hydrogel prepared by the method has the advantages of uniform stable network structure, excellent conductivity, swelling property and heat stability, favorable electric conductivity and favorable swelling property; and the equilibrium swelling rate can be up to about 500%.
Description
Technical field
The invention belongs to the preparation field of conductive hydrogel, and in particular to a kind of preparation side of cellulose base conductive hydrogel
Method.
Background technology
Conducting polymer hydrogel combines the excellent electrical and optical property of the unique performance of hydrogel and conducting polymer
Can, on the premise of remaining dimensionally-stable property, can have different electrical conductivity interval, therefore can apply to biological medicine,
The field such as tissue engineering material and biosensor.In recent years, with good biocompatibility, nontoxic, environmental friendliness, and have
The natural polymer of more active group is increasingly becoming the ideal material for preparing conductive hydrogel.But the mechanics of natural polymer
Performance is often poor.Cellulose has good biocompatibility, and biodegradable, contains substantial amounts of hydroxyl in its molecular structure
Ji Deng functional groups, can form hydrogel by physical crosslinking and the method being chemically crosslinked.As cellulose has very strong point
With intermolecular hydrogen bonding and the crystal structure closely piled up in sub, it is difficult to dissolve in usual vehicle, which has limited cellulose
Using.
Existing conductive hydrogel electrical conductivity is poor, and swellability and heat stability can not meet requirement.
The content of the invention
The present invention provides a kind of preparation method of cellulose base conductive hydrogel, and the hydrogel good conductivity of preparation, heat are steady
It is qualitative good.
The present invention is achieved by the following technical solutions.
A kind of preparation method of cellulose base conductive hydrogel, comprises the following steps：
（1）The preparation of pure microcrystalline cellulose hydrogel:Microcrystalline Cellulose is dissolved in chlorination -1- butyl -3- Methylimidazole .s,
Logical N2Protection, 100 DEG C of reaction 12h of constant temperature, is subsequently adding N,N methylene bis acrylamide and benzoyl peroxide, oily in 80 DEG C
The lower reaction 24h of bath, obtains microcrystalline cellulose hydrogel, microcrystalline cellulose hydrogel is taken out, and in immersion deionized water, magnetic force is stirred
Mix, change a water per 12h, stir 60h, obtain final product pure microcrystalline cellulose hydrogel；
（2）By step（1）The pure microcrystalline cellulose hydrogel for obtaining is immersed in the FeCl that concentration is 0.5mol/L3With to benzene
In the mixed solution of sodium sulfonate, 24h is soaked, gel is immersed after taking-up in pyrroles's aqueous solution of 0.15 mol/L, adjusted with HCl
The pH values of section solution react 6 h under ice bath between 6.0-6.5, and vacuum filtration is washed with deionized the water-setting for obtaining
After glue, by hydrogel lyophilization, Microcrystalline Cellulose-polypyrrole composite aquogel, i.e. cellulose base conductive hydrogel is obtained.
Above-mentioned steps（1）Middle Microcrystalline Cellulose, chlorination -1- butyl -3- Methylimidazole .s, N,N methylene bis acrylamide,
The mass ratio of benzoyl peroxide is 10: 80: 10: 1.
Advantages of the present invention：
The present invention is prepared for a kind of new cellulose base conductive hydrogel with chlorination -1- butyl -3- Methylimidazole .s as solvent,
The cellulose base conductive hydrogel possesses homogeneous, stable network structure, electric conductivity, swellability and heat stability excellent performance,
Electrical conductivity can reach 10-4 -10-3S/cm, the cellulose base conductive hydrogel of preparation have excellent swelling behavior, its balance
Swelling ratio can reach 500% or so.
Specific embodiment
With reference to specific embodiment, the present invention will be described in detail.
Embodiment 1
A kind of preparation method of cellulose base conductive hydrogel, comprises the following steps：
（1）The preparation of pure microcrystalline cellulose hydrogel:Microcrystalline Cellulose is dissolved in chlorination -1- butyl -3- Methylimidazole .s,
Logical N2Protection, 100 DEG C of reaction 12h of constant temperature, is subsequently adding N,N methylene bis acrylamide and benzoyl peroxide, oily in 80 DEG C
The lower reaction 24h of bath, obtains microcrystalline cellulose hydrogel, microcrystalline cellulose hydrogel is taken out, and in immersion deionized water, magnetic force is stirred
Mix, change a water per 12h, stir 60h, obtain final product pure microcrystalline cellulose hydrogel；
（2）By step（1）The pure microcrystalline cellulose hydrogel for obtaining is immersed in the FeCl that concentration is 0.5mol/L3With to benzene
In the mixed solution of sodium sulfonate, 24h is soaked, gel is immersed after taking-up in pyrroles's aqueous solution of 0.15 mol/L, adjusted with HCl
The pH values of section solution react 6 h under ice bath between 6.0-6.5, and vacuum filtration is washed with deionized the water-setting for obtaining
After glue, by hydrogel lyophilization, Microcrystalline Cellulose-polypyrrole composite aquogel, i.e. cellulose base conductive hydrogel is obtained.
Above-mentioned steps（1）Middle Microcrystalline Cellulose, chlorination -1- butyl -3- Methylimidazole .s, N,N methylene bis acrylamide,
The mass ratio of benzoyl peroxide is 10: 80: 10: 1.
Claims (2)
1. a kind of preparation method of cellulose base conductive hydrogel, it is characterised in that：Comprise the following steps：
（1）The preparation of pure microcrystalline cellulose hydrogel:Microcrystalline Cellulose is dissolved in chlorination -1- butyl -3- Methylimidazole .s,
Logical N2Protection, 100 DEG C of reaction 12h of constant temperature, is subsequently adding N,N methylene bis acrylamide and benzoyl peroxide, oily in 80 DEG C
The lower reaction 24h of bath, obtains microcrystalline cellulose hydrogel, microcrystalline cellulose hydrogel is taken out, and in immersion deionized water, magnetic force is stirred
Mix, change a water per 12h, stir 60h, obtain final product pure microcrystalline cellulose hydrogel；
（2）By step（1）The pure microcrystalline cellulose hydrogel for obtaining is immersed in the FeCl that concentration is 0.5mol/L3With to benzene
In the mixed solution of sodium sulfonate, 24h is soaked, gel is immersed after taking-up in pyrroles's aqueous solution of 0.15 mol/L, adjusted with HCl
The pH values of section solution react 6 h under ice bath between 6.0-6.5, and vacuum filtration is washed with deionized the water-setting for obtaining
After glue, by hydrogel lyophilization, Microcrystalline Cellulose-polypyrrole composite aquogel, i.e. cellulose base conductive hydrogel is obtained.
2. the preparation method of a kind of cellulose base conductive hydrogel according to claim 1, it is characterised in that：Step（1）
Middle Microcrystalline Cellulose, chlorination -1- butyl -3- Methylimidazole .s, N,N methylene bis acrylamide, the mass ratio of benzoyl peroxide are
10∶80∶10∶1。
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| CN201611016038.3A CN106519287A (en) | 2016-11-18 | 2016-11-18 | Preparation method of cellulose based conductive hydrogel |
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| CN201611016038.3A CN106519287A (en) | 2016-11-18 | 2016-11-18 | Preparation method of cellulose based conductive hydrogel |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108587023A (en) * | 2018-05-14 | 2018-09-28 | 西南交通大学 | A kind of preparation method of polypyrrole conductive hydrogel |
| CN108659237A (en) * | 2018-05-22 | 2018-10-16 | 中南林业科技大学 | A kind of electric conductivity with thermal tuning nanofiber composite hydrogel and its preparation method and application |
| CN109503765A (en) * | 2018-11-19 | 2019-03-22 | 华南理工大学 | The preparation method of cellulose ion conductive hydrogel and the hydrogel being prepared |
| CN111367007B (en) * | 2018-12-26 | 2021-07-06 | 深圳Tcl新技术有限公司 | Backlight module, light guide plate and preparation method of conductive hydrogel of light guide plate |
| CN113480824A (en) * | 2021-07-14 | 2021-10-08 | 金塑企业集团（上海）有限公司 | High-temperature-resistant oxygen-resistant polybutylene composite heating pipe and processing technology thereof |
-
2016
- 2016-11-18 CN CN201611016038.3A patent/CN106519287A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108587023A (en) * | 2018-05-14 | 2018-09-28 | 西南交通大学 | A kind of preparation method of polypyrrole conductive hydrogel |
| CN108659237A (en) * | 2018-05-22 | 2018-10-16 | 中南林业科技大学 | A kind of electric conductivity with thermal tuning nanofiber composite hydrogel and its preparation method and application |
| CN108659237B (en) * | 2018-05-22 | 2021-01-26 | 中南林业科技大学 | Nanofiber composite hydrogel with conductivity tuned with temperature as well as preparation method and application thereof |
| CN109503765A (en) * | 2018-11-19 | 2019-03-22 | 华南理工大学 | The preparation method of cellulose ion conductive hydrogel and the hydrogel being prepared |
| CN109503765B (en) * | 2018-11-19 | 2021-07-02 | 华南理工大学 | Preparation method of cellulose ion conductive hydrogel and hydrogel prepared by same |
| CN111367007B (en) * | 2018-12-26 | 2021-07-06 | 深圳Tcl新技术有限公司 | Backlight module, light guide plate and preparation method of conductive hydrogel of light guide plate |
| US11300723B2 (en) | 2018-12-26 | 2022-04-12 | Shenzhen Tcl New Technology Co., Ltd. | Backlight module, light guide plate, and preparation method for conductive hydrogel of light guide plate |
| CN113480824A (en) * | 2021-07-14 | 2021-10-08 | 金塑企业集团（上海）有限公司 | High-temperature-resistant oxygen-resistant polybutylene composite heating pipe and processing technology thereof |
| CN113480824B (en) * | 2021-07-14 | 2022-01-11 | 金塑企业集团（上海）有限公司 | High-temperature-resistant oxygen-resistant polybutylene composite heating pipe and processing technology thereof |
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Application publication date: 20170322 |