CN108467484A - A kind of preparation method of polyaniline - Google Patents
A kind of preparation method of polyaniline Download PDFInfo
- Publication number
- CN108467484A CN108467484A CN201810337015.5A CN201810337015A CN108467484A CN 108467484 A CN108467484 A CN 108467484A CN 201810337015 A CN201810337015 A CN 201810337015A CN 108467484 A CN108467484 A CN 108467484A
- Authority
- CN
- China
- Prior art keywords
- solution
- polyaniline
- preparation process
- aniline
- aqueous
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
A kind of preparation method of polyaniline, belongs to polymeric material field, is prepared by the following method, aniline is scattered in aqueous resin solution, forms solution A；Oxidant is dissolved in the water, solution B is formed；Solution A is quickly mixed with solution B；Controlling reaction temperature exists（5~20）oBetween C, the reaction time exists（6~24）Between h, after the completion of polymerisation, filtering is dry after washing filter cake alkali cleaning, washing, alcohol, obtains polyaniline in eigenstate.Bronsted acid need not be added in the method that the present invention uses, and not only reduce corrosion of the acid to production equipment, be also greatly reduced the dosage of lye and water in post-processing stages, reduce the discharge of waste liquid.
Description
Technical field
The invention belongs to polymeric material fields, more particularly, to a kind of preparation method of polyaniline.
Background technology
Polyaniline is one of conducting function high molecular material of most commercial application prospect, the electrochemical properties of polyaniline
Stablize, Doping Mechanism is unique, can reach higher conductivity, and raw material is easy to get, preparation process is simple, in super capacitor
The fields such as device, anti-corrosion material, anti-static material, electronic shield material and absorbing material have boundless application prospect, quilt
It is considered most to be hopeful to obtain the conducting polymer of industrialized production in practice.
There are many synthetic method of polyaniline, and wherein chemical oxidative polymerization and electrochemical polymerization method are most widely used side
Method.Relative to common chemical synthesis, electrochemical method synthesizes special property polyaniline suitable for small lot；But consersion unit compared with
Chemical synthesis is complicated, production cost is higher, is difficult to form large-scale production.Chemical synthesis for electrochemical process,
It is relatively easy, suitable for high-volume synthesized polyaniline, easily industrializes, be always the main method for preparing polyaniline.Generally, it is considered that working as
When the acidity of system is sufficiently high, the oligomer that initial reaction stage generates dissolves in reaction system solution, and reactivity enhancing continues to join
With polymerisation, the longer polyaniline of strand is generated.Chemical synthesis is exactly in acid condition, to be added into aniline monomer
Strong oxidizer makes aniline monomer that oxidation polymerization occur and forms macromolecular chain.Chemical synthesis is simple for process, is suitable for criticizing on a large scale
Amount production；But used a large amount of acid in the reaction, to be used in last handling process in a large amount of ammonium hydroxide and excessive acid and
Progress polyaniline goes to adulterate, and generates a large amount of waste water, causes environmental pollution.Develop easy to operate, cost-effective, wastewater discharge
Small polyaniline production technology is the premise of polyaniline heavy industrialization.
Invention content
The technical problem to be solved by the present invention is to：One kind is provided to be produced on a large scale, reduce wastewater discharge, reduce dirt
The preparation method of the polyaniline of dye disperses aniline monomer using aqueous resin solution, and aqueous resin solution can be aniline monomer
It polymerize the particular space environment provided, and the oligomer generated in initial reaction stage can form hydrogen bond equimolecular with water-base resin
Intermolecular forces promote polymerisation to carry out, and generate polyaniline, so as to avoid the use of a large amount of Bronsted acids, reduce discharge of wastewater
Amount.
The present invention adopts the following technical scheme that：A kind of preparation method of polyaniline, it is characterized in that：It is by solution A and molten
Liquid B compositions, the solution A are made of aniline monomer and aqueous resin solution；The solution B is made of oxidant and water；
In the solution A, the mass ratio of aniline monomer and aqueous resin solution is (0.01~0.2):1.
In the solution B, the mass ratio of oxidant and water is (0.1~0.5):1.
The molar ratio of oxidant is (0.1~1) in aniline monomer and solution B in the solution A:1.
The aniline monomer is aniline or anil.The anil is methyl anthranilate, adjacent ammonia
One or more of yl benzoic acid, adjacent diphenylamines, adjacent cyano-aniline, o-toluidine and o-chloraniline.
The water-base resin is latex of epoxy resin of aqueous phenolic aldehyde, aqueous bisphenol a epoxy resin emulsion.The aqueous phenol
Any one in formaldehyde epoxy resin lotion model K051, K-F051；The aqueous bisphenol a epoxy resin emulsion model
Any one in MU-618, MU-601, MU-607.
The oxidant is ammonium persulfate, potassium peroxydisulfate, sodium peroxydisulfate, hydrogen peroxide, ferric trichloride, manganese dioxide, height
The mixture of one or more of potassium manganate, carbonates peroxide.
The water is tertiary effluent or deionized water.
A kind of preparation method of polyaniline, characterized in that the preparation method includes the following steps：
Step 1: being (0.01~0.2) in mass ratio:1 weighs aniline monomer and aqueous resin solution, mixing, after stirring evenly
Obtain solution A；
Step 2: being (0.1~0.5) in mass ratio:1 weighs oxidant and water, and mixing obtains solution B after stirring evenly；
Step 3: being according to the molar ratio of aniline monomer and oxidant with solution B by solution A（0.1~1)：1 quickly mixing, control
Reaction temperature processed exists（5~20）oC carries out polymerisation；
Step 4: after polymerisation, filtering, by filter cake after alkali cleaning, washing, alcohol are washed respectively, drying obtains eigenstate polyphenyl
Amine.
By above-mentioned design scheme, the present invention can bring following advantageous effect：
1, aniline is dissolved in aqueous resin solution, promotes initial reaction stage using the interaction of water-base resin and Oligoanilines
Oligomer of phenylamine further polymerization forms the higher polyaniline of molecular weight and is reduced to avoid the use of a large amount of Bronsted acids
Loss to equipment, and the use of lye and water in later stage cleaning process is greatly reduced, reduce wastewater discharge.
2, technological process can be controlled rationally, easy to operate, be suitable for large-scale production.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further described.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to limit
The present invention.
Embodiment 1
The preparation method of the present embodiment includes the following steps：
25g aniline is dissolved in 250g epoxy resin of aqueous phenolic aldehyde solution K051, solution A is formed, 61g ammonium persulfates is dissolved in
In 612g deionized water, solution B is formed, solution A is quickly mixed with solution B,（5~20）oAfter being reacted 6 hours under C, filtering,
After filter cake is washed with ammonium hydroxide, deionized water, ethyl alcohol respectively, drying obtains polyaniline in eigenstate.
Embodiment 2
The preparation method of the present embodiment includes the following steps：
25g aniline is dissolved in 250g epoxy resin of aqueous phenolic aldehyde solution K-F051, solution A is formed, 49g potassium peroxydisulfates is dissolved
In 327g deionized water, solution B is formed, solution A is quickly mixed with solution B,（5~20）oAfter being reacted 6 hours under C, mistake
Filter, after filter cake is washed with ammonium hydroxide, deionized water, ethyl alcohol respectively, drying obtains polyaniline in eigenstate.
Embodiment 3
The preparation method of the present embodiment includes the following steps：
25g aniline is dissolved in the aqueous bisphenol a epoxy resin emulsion MU-618 of 250g, solution A is formed, by 61g ammonium persulfates
It is dissolved in 612g deionized waters, forms solution B, solution A is quickly mixed with solution B,（5~20）oIt is reacted 12 hours under C
Afterwards, it filters, after filter cake is washed with ammonium hydroxide, deionized water, ethyl alcohol respectively, drying obtains polyaniline in eigenstate.
Embodiment 4
The preparation method of the present embodiment includes the following steps：
25g aniline is dissolved in the aqueous bisphenol a epoxy resin emulsion MU-601 of 250g, solution A is formed, by 49g potassium peroxydisulfates
It is dissolved in 327g deionized waters, forms solution B, solution A is quickly mixed with solution B,（5~20）oIt is reacted 12 hours under C
Afterwards, it filters, after filter cake is washed with ammonium hydroxide, deionized water, ethyl alcohol respectively, drying obtains polyaniline in eigenstate.
Claims (10)
1. a kind of preparation process of polyaniline, characterized in that include the following steps：
Step 1: being (0.01~0.2) in mass ratio:1 weighs aniline monomer and aqueous resin solution, and is mixed, and stirs
Solution A is obtained after mixing；
Step 2: being (0.1~0.5) in mass ratio:1 weighs oxidant and water, and mixing obtains solution B after stirring evenly；
Step 3: being according to the molar ratio of aniline monomer and oxidant with solution B by solution A（0.1~1)：1 quickly mixing, control
Reaction temperature processed exists（5~20）oC carries out polymerisation；
Step 4: after polymerisation, filtering, by filter cake after alkali cleaning, washing, alcohol are washed respectively, drying obtains eigenstate polyphenyl
Amine.
2. a kind of preparation process of polyaniline according to claim 1, it is characterised in that：Aniline described in its step 1
Monomer is aniline or anil, and the anil is methyl anthranilate, ortho-aminobenzoic acid, adjacent hexichol
One or more of amine, adjacent cyano-aniline, o-toluidine and o-chloraniline.
3. a kind of preparation process of polyaniline according to claim 1, it is characterised in that：Aqueous tree described in its step 1
Fat is latex of epoxy resin of aqueous phenolic aldehyde, aqueous bisphenol a epoxy resin emulsion, the latex of epoxy resin of aqueous phenolic aldehyde model
For any one in K051, K-F051；Described aqueous bisphenol a epoxy resin emulsion model MU-618, MU-601, MU-
Any one in 607.
4. a kind of preparation process of polyaniline according to claim 1, it is characterised in that：Aniline described in its step 1
The mass ratio of monomer and aqueous resin solution is (0.01~0.2):1.
5. a kind of preparation process of polyaniline according to claim 1, it is characterised in that：Oxidation described in its step 2
Agent is ammonium persulfate, potassium peroxydisulfate, sodium peroxydisulfate, hydrogen peroxide, ferric trichloride, manganese dioxide, potassium permanganate, carbonates mistake
The mixture of one or more of oxide.
6. a kind of preparation process of polyaniline according to claim 1, it is characterised in that：Oxidation described in its step 2
The mass ratio of agent and water is (0.1~0.5):1.
7. a kind of preparation process of polyaniline according to claim 1, it is characterised in that：Aniline described in its step 3 with
The molar ratio of oxidant is（0.1~1）：1.
8. a kind of preparation process of polyaniline according to claim 1, it is characterised in that：Reaction temperature described in its step 3
Degree is（5~20）oC。
9. a kind of preparation process of polyaniline according to claim 1, it is characterised in that：When reaction described in its step 3
Between be（6~24）h.
10. a kind of preparation process of polyaniline according to claim 1, it is characterised in that：Cleaning described in its step 3
Medium is ammonium hydroxide, water and ethyl alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810337015.5A CN108467484A (en) | 2018-04-16 | 2018-04-16 | A kind of preparation method of polyaniline |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810337015.5A CN108467484A (en) | 2018-04-16 | 2018-04-16 | A kind of preparation method of polyaniline |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108467484A true CN108467484A (en) | 2018-08-31 |
Family
ID=63263143
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810337015.5A Pending CN108467484A (en) | 2018-04-16 | 2018-04-16 | A kind of preparation method of polyaniline |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108467484A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102336909A (en) * | 2011-07-05 | 2012-02-01 | 绍兴贝斯美化工有限公司 | Eigenstate poly 2,3-dimethylaniline preparation, and application of eigenstate poly 2,3-dimethylaniline in anti-corrosive paint |
| CN103980798A (en) * | 2014-05-14 | 2014-08-13 | 天津大学 | Doped-state polyaniline epoxy paint and preparation method thereof |
| CN106633047A (en) * | 2016-10-21 | 2017-05-10 | 南通绿业中试技术研究院有限公司 | Method for preparing polyaniline |
-
2018
- 2018-04-16 CN CN201810337015.5A patent/CN108467484A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102336909A (en) * | 2011-07-05 | 2012-02-01 | 绍兴贝斯美化工有限公司 | Eigenstate poly 2,3-dimethylaniline preparation, and application of eigenstate poly 2,3-dimethylaniline in anti-corrosive paint |
| CN103980798A (en) * | 2014-05-14 | 2014-08-13 | 天津大学 | Doped-state polyaniline epoxy paint and preparation method thereof |
| CN106633047A (en) * | 2016-10-21 | 2017-05-10 | 南通绿业中试技术研究院有限公司 | Method for preparing polyaniline |
Non-Patent Citations (2)
| Title |
|---|
| 于灵敏著: "《一维ZnO纳米线及其气敏特性》", 30 September 2014 * |
| 张学铭等: "《化学小辞典 第2版》", 31 August 1994 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101265255B (en) | Method for preparing benzoxazine intermediate containing triazine structure | |
| CN101519473B (en) | Method for preparing fluorine-containing modified amphoteric water-soluble polymer | |
| CN102911371B (en) | Hyperbranched polyester modified acrylic resin and preparation method thereof | |
| CN104069891B (en) | The preparation method of the immobilized HP catalyst of a kind of polymer microballoon | |
| CN101831053A (en) | Aqueous ultraviolet cured epoxy acrylic resin and preparation method thereof | |
| CN107188802A (en) | Using the method for the ionic liquid-catalyzed butyric ester of alcohol depolymerization 3 of bisgallic acid type | |
| CN101717464A (en) | Preparation method of carboxyl-terminated liquid fluorine polymer | |
| CN102229685A (en) | Polyvinyl alcohol and use of polyvinyl alcohol as dispersant | |
| CN103011200A (en) | Preparation method of high-concentration cyanamide solution | |
| CN104492495A (en) | Ionic liquid immobilized magnetic solid acid material catalyst and preparation method thereof | |
| CN107383284A (en) | A kind of ultraviolet, double tracer type concrete admixtures of fluorescence and preparation method thereof | |
| CN101514175B (en) | Method for producing tetramethylthiuram disulfide | |
| CN102533042B (en) | Preparation method of acrylic organic bentonite polyvinyl acetate emulsion paint | |
| CN101531762A (en) | Preparation of composite water absorbent material composed of silk fibroin/acrylic acid/acrylamide | |
| CN108467484A (en) | A kind of preparation method of polyaniline | |
| CN109053934A (en) | A kind of rare earth modified photoinitiator and preparation method | |
| CN104492482A (en) | Polymerized ionic liquid-silicon dioxide composite solid acid and preparation method thereof | |
| CN103804631A (en) | Polyketide with quaternized side chain and preparation method thereof as well as anion-exchange membrane | |
| CN104844455A (en) | Method used for catalyzed synthesis of tert-butyl acrylate | |
| CN104479136A (en) | Nonionic epoxy emulsifier and preparation method thereof | |
| CN103073521A (en) | Preparation method of rubber vulcanization accelerator N-tert-butyl-2-benzothiazole sulfonamide (NS) | |
| CN105175342A (en) | Ionic liquid and method for homogeneous phase-modified reed-reinforced PE (polyethylene) composite material thereof | |
| CN105384637A (en) | Method for degrading polyethylene glycol terephthalate under catalysis of polysubstituted sandwiched multi-metal oxygen cluster | |
| CN102604134B (en) | Cellulose based water-absorbing and oil-absorbing film and preparation method thereof | |
| CN109824891A (en) | A kind of synthetic method of polyaniline |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180831 |
|
| WD01 | Invention patent application deemed withdrawn after publication |