CN103435850A - Preparation method for sea squirt nano-cellulose conductive paper - Google Patents
Preparation method for sea squirt nano-cellulose conductive paper Download PDFInfo
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- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 10
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 239000004160 Ammonium persulphate Substances 0.000 claims description 3
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 3
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 3
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 239000004159 Potassium persulphate Substances 0.000 claims description 2
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 235000019394 potassium persulphate Nutrition 0.000 claims description 2
- VVWRJUBEIPHGQF-UHFFFAOYSA-N propan-2-yl n-propan-2-yloxycarbonyliminocarbamate Chemical compound CC(C)OC(=O)N=NC(=O)OC(C)C VVWRJUBEIPHGQF-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 150000003384 small molecules Chemical class 0.000 claims description 2
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
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- 229920000168 Microcrystalline cellulose Polymers 0.000 description 1
- 241000251576 Styela clava Species 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a preparation method for polyaniline-coated sea squirt nano-cellulose conductive paper through in situ polymerization. The method comprises the following steps: subjecting extracted sea squirt cellulose to acid hydrolysis so as to prepare a sea squirt nano-cellulose suspension; then fully mixing an aniline monomer with the suspension, adding an oxidizing agent and an acid-doped mixed liquor and carrying out in situ polymerization so as to prepare a polyaniline-coated sea squirt nano-cellulose suspension; and subjecting the polyaniline-coated sea squirt nano-cellulose suspension to drying and film formation so as to obtain the sea squirt nano-cellulose conductive paper. The sea squirt nano-cellulose conductive paper prepared by using the method has the characteristics high conductivity, low cost, a simple synthetic method, low toxicity, etc.
Description
Technical field
The invention belongs to conductive polymer composite and biomaterial preparation field, be specifically related to the technology of preparing of polyaniline-coated Ascidian nano-cellulose matrix material.
Background technology
The Ascidian Mierocrystalline cellulose is as a kind of novel environmentally friendly natural macromolecular material, has that degree of crystallinity is high, physical strength large and the special performance such as biocompatibility.Along with the concern of people to environment and resource problem, this elite clone also progressively becomes the focus of research.2010, Piao Guang wise man seminar [extracts Microcrystalline Cellulose and prepares the method for lyotropic cholesteryl liquid crystal in Ascidian, China, patent of invention, ZL201010217969.6,2012.3.14] related work that takes the lead in carrying out at home, adopt the method for sulphuric acid hydrolysis to prepare Styela clava nano-cellulose cholesteryl liquid crystal, the cellulosic utilization of Ascidian has been carried out to useful research and probe.
1977, [Shirakawa H., the Louis E. J. such as Shirakawa, MacDiarmid A. G., Chiang, C. K., Heeger A. J., J. Chem. Soc., Chem. Commun., 1977,578] reported that the polyacetylene after the doping has high conductivity, the traditional concept that polymer is isolator has been broken in this discovery, and the science researcher has carried out research extensively and profoundly to conducting polymer since then.Through the development of decades, the conjugated polymers that chemical stability is good is come out one after another, as [Johannes P., Stefan M., Chem. Rev., 2010,110:6260] such as polyaniline, polypyrrole, Polythiophenes.
Polyaniline is a kind of very promising conducting polymer composite, has good thermostability and chemical stability.But it is insoluble not molten, and the polyaniline finished product is powder, is difficult for being processed, and has limited its industrial application, by preparing Mierocrystalline cellulose/conductive polymer composite, can effectively overcome this shortcoming.
In recent years, in succession have with cotton cellulose [Mattoso L. H., Medeiros E. S., Baker D. A., et al.. Journal of nanoscience and nanotechnology, 2009,9 (5): 2917], bacteria cellulose [Luong N. D., Korhonen J. T., Soininen A. J., European Polymer Journal, 2012,49:335] for base material prepares the report of conducing composite material, but there is not yet the work that the Ascidian Mierocrystalline cellulose prepares conductive nano paper as base material of take.
The potential application of conductive paper has caused investigator's interest, as induction wallpaper, inductor block, other electron device etc.Electronic Paper can be applicable on the indicating meter of the high and low weight of intensity, less energy-consumption, is supplementing of information media Mierocrystalline cellulose paper.Paper is just playing the surrogate effect of electronic product as renewable resources, the output height of paper and the low-cost surrogate that also becomes other non-renewable base materials.On market, existing related products, generally adopt the deposition of conducting polymer on White Board to prepare conductive paper, need to produce by silk screen printing, intaglio printing, offset printing and ink jet printing or spin coating mode.But the conductive paper that this these methods are produced only has surface conductivity, there is no volume conduction, and production technique is comparatively complicated, and production unit is had relatively high expectations, and environmental pollution is larger.
The present invention take the Ascidian Mierocrystalline cellulose as base material, successfully prepared the conductive paper that polyaniline coats the Ascidian nano-cellulose fully.This method has that cost is low, processing method is simple, the specific conductivity high.
Summary of the invention
The invention discloses a kind of method that method by in-situ polymerization prepares polyaniline-coated Ascidian nano-cellulose conductive paper.The method is that the Ascidian Mierocrystalline cellulose that extraction is obtained carries out the acid hydrolysis processing, prepares Ascidian nano-cellulose suspension.Then aniline monomer is fully mixed with this suspension, then add oxygenant to make it that home position polymerization reaction occur, prepare polyaniline/Ascidian nano-cellulose suspension.By above-mentioned polyaniline/Ascidian nano-cellulose suspension drying film-forming process, preparation Ascidian nano-cellulose conductive paper.
The preparation method of polyaniline/Ascidian nano-cellulose conductive paper comprises the following steps:
The Ascidian cellulose powder is mixed according to certain ratio with the vitriol oil, after mixing solutions is heated to magnetic agitation reaction certain hour, add a large amount of deionized water termination reactions, remove excessive acid in solution by centrifugal and dialysis again, obtain Ascidian nano-cellulose suspension after ultrasonication.Then aniline monomer is fully mixed with this suspension, dropwise add the dopant acid solution of oxygenant under condition of ice bath, the magnetic agitation reaction.The matrix material that obtains is removed to oxygenant and the small molecules polymkeric substance in system through alcohol wash, washing, then be dried film forming and just obtain Ascidian nano-cellulose conductive paper.
The accompanying drawing explanation
The digital photograph that Fig. 1 is polyaniline/Ascidian nano-cellulose conductive paper.
The scanning electronic microscope that Fig. 2 is the Ascidian nano-cellulose (SEM) photo
The SEM photo that Fig. 3 is polyaniline/Ascidian nano-cellulose conductive paper surface.
The polyaniline that discovery makes by present method in Fig. 1/Ascidian nano-cellulose conductive paper has good mechanical property.
Can find out that by Fig. 2 and Fig. 3 the length of Ascidian nano-cellulose is 0.5 ~ 1.5 μ m, diameter is 20 ~ 30nm.After compound, its length variations is little, but diameter is increased to 40 ~ 75nm.Being coated on the Ascidian nano-cellulose of polyaniline success is described.
Embodiment
Embodiment 1
(1) get the vitriol oil that 5g Ascidian Mierocrystalline cellulose is 64% with 175ml concentration and mix, at 45 ℃ of lower oil bath magnetic agitation reacting by heating 10h.
(2) add 800ml deionized water termination reaction, use the whizzer centrifugal treating, rotating speed is 12000rpm, removes supernatant liquor, with centrifugal again after washed with de-ionized water, and repetitive operation three times.
(3) till centrifugal sediment being packed in dialysis tubing and being neutrality with the deionized water dialysis to extraneous solution.
(4) with Ultrasonic cell smash, nano-cellulose suspension is carried out to supersound process, ultrasonic power is 25KHz, and ultrasonic power is 600W, and ultrasonic time is 8min, and the ultrasonic amplitude of fluctuation shank diameter is 6mm.
(5) get suspension 50ml after ultrasonication and the aniline monomer of 0.1ml and fully be uniformly mixed, dropwise add the mixing solutions 50ml of oxygenant ammonium persulphate (APS) and dopant acid hydrochloric acid, under condition of ice bath, magnetic agitation reaction 6h.
(6) reaction is washed with ethanol, distilled water after finishing, and then by its seasoning, can make polyaniline/Ascidian nano-cellulose conductive paper, and testing its specific conductivity is 2.0 * 10
-3s/cm.
Embodiment 2
The proportional range of the Mierocrystalline cellulose described in step (1) and the vitriol oil is 1g: 1ml ~ 1g: 200ml, and it is identical with embodiment 1 with step.
Embodiment 3
In step (1), the acid hydrolysis temperature is 0 ~ 80 ℃, and all the other steps are identical with embodiment 1.
Embodiment 4
In step (1), the acid hydrolysis time is 0.5 ~ 24h, and all the other steps are identical with embodiment 1.
Embodiment 5
In step (4), the ultrasonication power range is 100 ~ 1500W, and all the other steps are identical with embodiment 1.
Embodiment 6
In step (4), the ultrasonic treatment time scope is 1 ~ 180min, and all the other steps are identical with embodiment 1.
Embodiment 7
In step (5), oxygenant is iron trichloride, Potassium Persulphate, dibenzoyl peroxide, Diisopropyl azodicarboxylate, and all the other steps are identical with embodiment 1.
Embodiment 8
In step (5), dopant acid is Witco 1298 Soft Acid, tosic acid, sulfuric acid, nitric acid, perchloric acid, and all the other steps are identical with embodiment 1.
Embodiment 9
In step (5), the reaction times is 0.5 ~ 10h, and all the other steps are identical with embodiment 1.
Embodiment 10
In step (6), drying temperature is 20 ~ 80 ℃, and all the other steps are identical with embodiment 1.
Claims (8)
1. the preparation method of an Ascidian nano-cellulose conductive paper, its feature comprises the following steps:
Ascidian nano-cellulose suspension is fully mixed with aniline monomer, dropwise add the dopant acid solution of oxygenant under condition of ice bath, the magnetic agitation reaction.
2. the matrix material that obtains is removed to oxygenant and the small molecules polymkeric substance in system through alcohol wash, washing, then be dried and just obtain polyaniline/Ascidian nano-cellulose conductive paper.
3. according to the preparation method of Ascidian nano-cellulose conductive paper claimed in claim 1, it is characterized in that the cellulosic length 100nm ~ 3000nm that is of a size of of described Ascidian, diameter 5 ~ 50nm.
4. according to the preparation method of Ascidian nano-cellulose conductive paper claimed in claim 1, it is characterized in that oxygenant used is ammonium persulphate, iron trichloride, Potassium Persulphate, dibenzoyl peroxide, Diisopropyl azodicarboxylate.
5. according to the preparation method of Ascidian nano-cellulose conductive paper claimed in claim 1, it is characterized in that dopant acid used is hydrochloric acid, Witco 1298 Soft Acid, tosic acid, sulfuric acid, nitric acid, perchloric acid.
6. according to the preparation method of Ascidian nano-cellulose conductive paper claimed in claim 1, it is characterized in that the home position polymerization reaction time is 0.5 ~ 10h, polymeric reaction temperature is-10 ~ 30 ℃.
7. according to the preparation method of Ascidian nano-cellulose conductive paper claimed in claim 1, the drying temperature that it is characterized in that Ascidian nano-cellulose conductive paper is 20 ~ 80 ℃.
8. according to the preparation method of Ascidian nano-cellulose conductive paper claimed in claim 1, the specific conductivity that it is characterized in that Ascidian nano-cellulose conductive paper is 10
-5~ 10 S/cm.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105218864A (en) * | 2015-09-07 | 2016-01-06 | 四川大学 | A kind of Electrochromic composite material based on nano-cellulose and device preparation method |
| CN105350400A (en) * | 2015-11-11 | 2016-02-24 | 无锡英普林纳米科技有限公司 | Conductive nano-paper |
| CN105536567A (en) * | 2015-12-25 | 2016-05-04 | 武汉大学 | Sea squirt nano cellulose ultrafiltration membrane as well as preparation method and application of sea squirt nano cellulose ultrafiltration membrane |
| CN107043441A (en) * | 2017-04-24 | 2017-08-15 | 武汉大学 | Ascidian Cellulose nanocrystal body/polyalcohol hydrogel and its preparation method and application |
| CN107474343A (en) * | 2017-07-31 | 2017-12-15 | 华南理工大学 | The method that one kettle way prepares ascidian nano micro crystal cellulose/rubber nano composite material |
| CN110960723A (en) * | 2019-11-04 | 2020-04-07 | 南方医科大学 | Preparation method and application of ascidian conductive hydrogel |
| WO2022261103A1 (en) * | 2021-06-09 | 2022-12-15 | Soane Materials Llc | Articles of manufacture comprising nanocellulose elements |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105218864A (en) * | 2015-09-07 | 2016-01-06 | 四川大学 | A kind of Electrochromic composite material based on nano-cellulose and device preparation method |
| CN105218864B (en) * | 2015-09-07 | 2018-07-03 | 四川大学 | A kind of Electrochromic composite material and device preparation method based on nano-cellulose |
| CN105350400A (en) * | 2015-11-11 | 2016-02-24 | 无锡英普林纳米科技有限公司 | Conductive nano-paper |
| CN105536567A (en) * | 2015-12-25 | 2016-05-04 | 武汉大学 | Sea squirt nano cellulose ultrafiltration membrane as well as preparation method and application of sea squirt nano cellulose ultrafiltration membrane |
| CN105536567B (en) * | 2015-12-25 | 2018-11-13 | 武汉大学 | A kind of ascidian nano-cellulose ultrafiltration membrane and its preparation method and application |
| CN107043441A (en) * | 2017-04-24 | 2017-08-15 | 武汉大学 | Ascidian Cellulose nanocrystal body/polyalcohol hydrogel and its preparation method and application |
| CN107474343A (en) * | 2017-07-31 | 2017-12-15 | 华南理工大学 | The method that one kettle way prepares ascidian nano micro crystal cellulose/rubber nano composite material |
| CN107474343B (en) * | 2017-07-31 | 2020-02-18 | 华南理工大学 | Method for preparing sea squirt nano microcrystalline cellulose/rubber nano composite material by one-pot method |
| CN110960723A (en) * | 2019-11-04 | 2020-04-07 | 南方医科大学 | Preparation method and application of ascidian conductive hydrogel |
| WO2022261103A1 (en) * | 2021-06-09 | 2022-12-15 | Soane Materials Llc | Articles of manufacture comprising nanocellulose elements |
| US11795420B2 (en) | 2021-06-09 | 2023-10-24 | Soane Materials Llc | Articles of manufacture comprising nanocellulose elements |
| US11932829B2 (en) | 2021-06-09 | 2024-03-19 | Soane Materials Llc | Articles of manufacture comprising nanocellulose elements |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20131211 |
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| RJ01 | Rejection of invention patent application after publication |