CN105778085A - Preparation method for polyaniline - Google Patents
Preparation method for polyaniline Download PDFInfo
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- CN105778085A CN105778085A CN201610181639.3A CN201610181639A CN105778085A CN 105778085 A CN105778085 A CN 105778085A CN 201610181639 A CN201610181639 A CN 201610181639A CN 105778085 A CN105778085 A CN 105778085A
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- Prior art keywords
- preparation
- solution
- polyaniline
- mixed
- aniline
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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
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
Abstract
The invention relates to a preparation method for polyaniline, which includes the following steps: aniline and dimethyl carbonate are mixed, and under the condition of agitation, calcium chloride is added, so that a first mixed solution is obtained; a sulfuric acid solution is dispersed into ethanol, and potassium ferricyanide is added and mixed, so that a second mixed solution is obtained; the first mixed solution and the second mixed solution are mixed, and react under 20DEG C to 25DEG C for2 to 6 hours, suction filtration is performed, a product is washed with deionized water and dried, and thereby the polyaniline is obtained. The materials of the preparation method are cheap, easily obtained, nontoxic and environmentally-friendly, the reaction process is simple, special reaction conditions are not needed, and the preparation method is suitable for mass production.
Description
Technical field
The present invention relates to the preparation method of a kind of polyaniline, belong to the field of chemical synthesis.
Background technology
Polyaniline is a kind of conventional conducting polymer composite, has low cost, high chemical stability, height are led
The advantage such as electrically, is one the most commercially valuable in numerous conducting polymer.By big at polyaniline
Introduce substituent group on strand or introduce different aniones by protonic acid doping, can be to polyaniline band
Come new character and application.Polyaniline has started to industrialized production and obtains actual application at present.
Polyaniline has the prospect that is widely applied very much, especially as anlistatig as a kind of conducting polymer
Material or alloy.But its synthesis step and method have weak point, as use toluene, chloroform, four
The poisonous inflammable and explosive solvents such as chlorination carbon, dichloromethane, have pollution, transport and produce and all deposit environment
In unstable factor, the reaction of prior art polyaniline mostly is less than 0 DEG C reaction, and the response time is long, temperature
Low, improve the productivity of polyaniline with this, product need to be in vacuum drying, and reaction condition is special, is unfavorable for big
Large-scale production.
Summary of the invention
The technical problem to be solved is to provide the preparation method of a kind of polyaniline, this preparation method
Cheaper starting materials is easy to get, nontoxic, environmentally friendly, and course of reaction is simple, it is not necessary to specific response condition, suitable
Close large-scale production.
The technical scheme is that the preparation method of a kind of polyaniline, bag
Include:
1) aniline is mixed with dimethyl carbonate, under agitation, add calcium chloride, obtain first and mix
Close solution；
2) sulfuric acid solution is disperseed in ethanol, add potassium ferricyanide mixing, obtain the second mixed solution；
3) by 1) the first mixed solution and 2 of obtaining) the second mixed solution mixing of obtaining, 20-25 DEG C
Reaction 2-6h, sucking filtration, product is washed with deionized, and is dried, obtains polyaniline.
On the basis of technique scheme, the present invention can also do following improvement.
Further, 1) in, the mol ratio of described aniline, dimethyl carbonate and calcium chloride is (1-3):
(1-9): (0.5-4).
Present inventor finds through a large amount of screening experiment, in conjunction with this system to use this step to provide the benefit that
Preparation Method, dimethyl carbonate can substitute existing solvent, dimethyl carbonate have environmental-protecting performance excellent,
Production has use conveniently, safely, pollute less, the advantage such as easy transport.
Further, 2) in, the mass concentration of described sulfuric acid solution is 98%, the mass concentration of ethanol
Being 75%, sulfuric acid solution is 1:(2-4 with the volume ratio of ethanol).
Further, 2) in, the sulphuric acid in described sulfuric acid solution is (1-5) with the mol ratio of aniline:
(2-7), the addition of the described potassium ferricyanide is used by aniline 0.1-1 times of quality.
Further, 3) in, described dry temperature is 40-80 DEG C, and the time is 2-7h.
The invention has the beneficial effects as follows:
This preparation method cheaper starting materials is easy to get, nontoxic or toxicity is little, environmentally friendly, overcomes existing skill
The raw materials used toxicity of art is big, shortcoming inflammable and explosive, big for environment pollution.
This preparation method course of reaction is simple, as long as can react at normal temperatures, the response time is short, it is not necessary to
Vacuum drying, cost-effective, it is suitable for large-scale production.
Detailed description of the invention
Principle and feature to the present invention are described below, and example is served only for explaining the present invention, and
Non-for limiting the scope of the present invention.
Embodiment 1
A kind of preparation method of polyaniline, including:
1) aniline is mixed with dimethyl carbonate, under agitation, add calcium chloride, obtain first and mix
Closing solution, the mol ratio of aniline, dimethyl carbonate and calcium chloride is 3:9:0.5.
2) sulfuric acid solution of mass concentration 98% is dispersed in the ethanol of mass concentration 75%, adds ferrum cyanogen
Changing potassium mixing, obtain the second mixed solution, sulfuric acid solution is 1:4 with the volume ratio of ethanol, and described sulphuric acid is molten
Sulphuric acid in liquid is 5:2 with the mol ratio of aniline, and the addition of the described potassium ferricyanide is quality used by aniline
0.1 times.
3) by 1) the first mixed solution and 2 of obtaining) the second mixed solution mixing of obtaining, then 0-25 DEG C
Start temperature ranges reaction 24h, course of reaction reaction heat inconspicuous reaction liquid temperature only raises
1-2℃.The reaction of Ammonium persulfate. one class oxidant will not be used as tradition, need cooling, not so react
System temperature raises 20-50 DEG C, and polyaniline chemical oxidation sucking filtration, product is washed with deionized, 40 DEG C
It is dried 4h, obtains polyaniline.
Reaction condition is gentle, it is not necessary to reaction heat cooling controls, and product property is stable, and batch reproducibility is good,
Be conducive to scale manufacturing.
Embodiment 2
A kind of preparation method of polyaniline, including:
1) aniline is mixed with dimethyl carbonate, under agitation, add calcium chloride, obtain first and mix
Closing solution, the mol ratio of aniline, dimethyl carbonate and calcium chloride is 1:4:1.
2) sulfuric acid solution of mass concentration 98% is dispersed in the ethanol of mass concentration 75%, adds ferrum cyanogen
Changing potassium mixing, obtain the second mixed solution, sulfuric acid solution is 1:2 with the volume ratio of ethanol, and described sulphuric acid is molten
Sulphuric acid in liquid is 5:2 with the mol ratio of aniline, and the addition of the described potassium ferricyanide is quality used by aniline
0.2 times.
3) by 1) the first mixed solution and 2 of obtaining) the second mixed solution mixing of obtaining, 25 DEG C are anti-
Answering 4h, sucking filtration, product is washed with deionized, 50 DEG C of dry 3h, obtains polyaniline.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all in the present invention
Spirit and principle within, any modification, equivalent substitution and improvement etc. made, should be included in this
Within bright protection domain.
Claims (5)
1. the preparation method of a polyaniline, it is characterised in that including:
1) aniline is mixed with dimethyl carbonate, under agitation, add calcium chloride, obtain first and mix
Close solution；
2) sulfuric acid solution is disperseed in ethanol, add potassium ferricyanide mixing, obtain the second mixed solution；
3) by 1) the first mixed solution and 2 of obtaining) the second mixed solution mixing of obtaining, 20-25 DEG C
Reaction 2-6h, sucking filtration, product is washed with deionized, and is dried, obtains polyaniline.
Preparation method the most according to claim 1, it is characterised in that 1) in, described aniline,
The mol ratio of dimethyl carbonate and calcium chloride is (1-3): (1-9): (0.5-4).
Preparation method the most according to claim 1, it is characterised in that 2) in, described sulphuric acid
The mass concentration of solution is 98%, and the mass concentration of ethanol is 75%, sulfuric acid solution and the volume ratio of ethanol
For 1:(2-4).
Preparation method the most according to claim 1, it is characterised in that 2) in, described sulphuric acid
Sulphuric acid in solution is (1-5) with the mol ratio of aniline: (2-7), the addition of the described potassium ferricyanide is
0.1-1 times of quality used by aniline.
Preparation method the most according to claim 1, it is characterised in that 3) in, described dry
Temperature be 40-80 DEG C, the time is 2-7h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610181639.3A CN105778085A (en) | 2016-03-28 | 2016-03-28 | Preparation method for polyaniline |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610181639.3A CN105778085A (en) | 2016-03-28 | 2016-03-28 | Preparation method for polyaniline |
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| Publication Number | Publication Date |
|---|---|
| CN105778085A true CN105778085A (en) | 2016-07-20 |
Family
ID=56391918
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610181639.3A Pending CN105778085A (en) | 2016-03-28 | 2016-03-28 | Preparation method for polyaniline |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101016412A (en) * | 2007-03-06 | 2007-08-15 | 中南大学 | Method of preparing lithium salt doping state polyaniline electrode material for super capacitor |
| CN102153747A (en) * | 2011-02-17 | 2011-08-17 | 中国科学院长春应用化学研究所 | Method for preparing hollow polyaniline microspheres |
| CN103214670A (en) * | 2013-03-05 | 2013-07-24 | 中国科学院长春应用化学研究所 | Aqueous polyaniline hollow microballoon and preparation method thereof |
| CN103539938A (en) * | 2013-08-27 | 2014-01-29 | 江苏科技大学 | Method for preparing ferricyanide doped polyaniline composite |
| CN103539943A (en) * | 2013-11-06 | 2014-01-29 | 中国科学院长春应用化学研究所 | Preparation method of polyaniline |
-
2016
- 2016-03-28 CN CN201610181639.3A patent/CN105778085A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101016412A (en) * | 2007-03-06 | 2007-08-15 | 中南大学 | Method of preparing lithium salt doping state polyaniline electrode material for super capacitor |
| CN102153747A (en) * | 2011-02-17 | 2011-08-17 | 中国科学院长春应用化学研究所 | Method for preparing hollow polyaniline microspheres |
| CN103214670A (en) * | 2013-03-05 | 2013-07-24 | 中国科学院长春应用化学研究所 | Aqueous polyaniline hollow microballoon and preparation method thereof |
| CN103539938A (en) * | 2013-08-27 | 2014-01-29 | 江苏科技大学 | Method for preparing ferricyanide doped polyaniline composite |
| CN103539943A (en) * | 2013-11-06 | 2014-01-29 | 中国科学院长春应用化学研究所 | Preparation method of polyaniline |
Non-Patent Citations (1)
| Title |
|---|
| 李进军等: "《绿色化学导论》", 31 August 2015, 武汉大学出版社 * |
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Application publication date: 20160720 |