CN105936770A - Preparation method of aqueous polyaniline conductive printing ink - Google Patents
Preparation method of aqueous polyaniline conductive printing ink Download PDFInfo
- Publication number
- CN105936770A CN105936770A CN201610474122.3A CN201610474122A CN105936770A CN 105936770 A CN105936770 A CN 105936770A CN 201610474122 A CN201610474122 A CN 201610474122A CN 105936770 A CN105936770 A CN 105936770A
- Authority
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- China
- Prior art keywords
- electrically conductive
- conductive ink
- preparation
- aqueous polyanion
- acid
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- Granted
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- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229920000767 polyaniline Polymers 0.000 title abstract description 8
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 34
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 13
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 13
- 239000002253 acid Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 9
- 229920000447 polyanionic polymer Polymers 0.000 claims description 32
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- -1 DBSA Chemical compound 0.000 claims description 4
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 4
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 4
- 239000011975 tartaric acid Substances 0.000 claims description 4
- 235000002906 tartaric acid Nutrition 0.000 claims description 4
- MIOPJNTWMNEORI-GMSGAONNSA-N (S)-camphorsulfonic acid Chemical compound C1C[C@@]2(CS(O)(=O)=O)C(=O)C[C@@H]1C2(C)C MIOPJNTWMNEORI-GMSGAONNSA-N 0.000 claims description 3
- 239000005711 Benzoic acid Substances 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- 235000010233 benzoic acid Nutrition 0.000 claims description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 239000008117 stearic acid Substances 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 3
- 150000001412 amines Chemical class 0.000 claims 1
- 235000015165 citric acid Nutrition 0.000 claims 1
- 239000000853 adhesive Substances 0.000 abstract description 4
- 230000001070 adhesive effect Effects 0.000 abstract description 4
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 9
- 239000010408 film Substances 0.000 description 6
- 229940068984 polyvinyl alcohol Drugs 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 239000003973 paint Substances 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000012785 packaging film Substances 0.000 description 3
- 229920006280 packaging film Polymers 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 235000005979 Citrus limon Nutrition 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000011231 conductive filler Substances 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- PXFBZOLANLWPMH-UHFFFAOYSA-N 16-Epiaffinine Natural products C1C(C2=CC=CC=C2N2)=C2C(=O)CC2C(=CC)CN(C)C1C2CO PXFBZOLANLWPMH-UHFFFAOYSA-N 0.000 description 1
- 244000248349 Citrus limon Species 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
-
- 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)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Conductive Materials (AREA)
Abstract
The invention discloses a preparation method of an aqueous polyaniline conductive printing ink. The preparation method comprises the following steps: adding polyvinyl alcohol into water, mixing, then adding aniline and organic protonic acid, keeping on mixing, then slowly dropwise adding ammonium persulfate, and stirring to obtain the aqueous polyaniline conductive printing ink. The obtained aqueous polyaniline conductive printing ink has the advantages of stability, good toughness, high adhesive force, excellent conductive performance, environment-friendliness, and no pollution.
Description
Technical field
The present invention relates to technical field, particularly relate to the preparation method of a kind of aqueous polyanion electrically conductive ink.
Background technology
Electrically conductive ink, as a kind of specific function type electrically-conducting paint, has had the history of more than 50 year, previous
Electrically-conducting paint, based on oil-soluble, is divided into three types: inorganic materials electrically conductive ink, organic material system (gather
Compound) electrically conductive ink and composite material type electrically conductive ink.Domestic electrically conductive ink is main is to be applied to flexographic plate
Printing and intaglio printing produce, and the correlational study starting of electrically conductive ink technology is the most later, currently mainly with height
It is main that research and development are explored in school, institute.Recognize from the existing report to electrically conductive ink and research, currently,
The research and development of electrically conductive ink are substantially focused on solvent-borne type electrically conductive ink field, and the content increasing conductive filler is
Improve the modal way measure of the electric conductivity of ink, although this way can increase substantially ink
Electric conductivity, but in actual application, due to the too high levels of inorganic type conductive filler, cause
The character degradations such as the application performance of printed coating, total quality and stability of material, and coating is tough
Property and adhesive force poor, be easily caused product crackle and coming off.Meanwhile, oil-soluble electrically-conducting paint was producing
Cheng Zhong, often contaminative is serious, big to human toxicity, production operation danger coefficient high, and big in production
Amount uses oil-dissolving solvent that environmental pollution can be caused serious, is difficult to clear up after terminating.Along with the need producing industry
The development of summation society, environmental protection problem of increasing concern, the attention of environmental issue is strengthened by government,
A kind of non-harmful environment protecting water-based paint and production technology thereof it is badly in need of on material market.
The appearance of aqueous carbon dust ink such as PMMA/ carbon dust etc. can solve the problem that the problems referred to above, but to aqueous
The research of conductive printing ink from polyaniline is blank.
Summary of the invention
The technical problem existed based on background technology, the present invention proposes a kind of aqueous polyanion electrically conductive ink
Preparation method, gained aqueous polyanion electrically conductive ink is stable, and toughness and adhesive force are good, and electric conductivity is excellent,
And environmental protection, pollution-free.
The preparation method of a kind of aqueous polyanion electrically conductive ink that the present invention proposes, comprises the steps: poly-
After vinyl alcohol is added to the water mixing, adds aniline and organic proton acid continues mixing, be then slowly added dropwise
Ammonium sulfate, stirring obtains aqueous polyanion electrically conductive ink.
Preferably, the mol ratio of aniline and organic proton acid is 0.04～0.05:0.003～0.019.
Preferably, organic proton acid is camphorsulfonic acid, DBSA, tartaric acid, benzoic acid, lemon
Lemon acid or stearic acid.
Preferably, the mol ratio of aniline and Ammonium persulfate. is 0.04～0.05:0.03～0.04.
Preferably, the weight ratio of aniline and polyvinyl alcohol is 3.72～4.65:25～35.
Preferably, comprise the steps: to add polyvinyl alcohol mixing 0.5～1.0h in 80～90 DEG C of water, quiet
Put to clear, add aniline and organic proton acid continues mixing 5～10min, then drip over cure
Acid ammonium, rate of addition is 14～18g/h, and stirring 3.5～4.5h obtains aqueous polyanion electrically conductive ink.
Preferably, the weight ratio of polyethylene alcohol and water is 1～3:1.
Gained aqueous polyanion electrically conductive ink of the present invention is stable, and toughness and adhesive force are good, and electric conductivity is excellent,
Resistance is 0.64M Ω, and its surface conductivity is 1.6 × 10-6s/cm, and affine with water, contact angle up to
17.67 °, environmental protection, pollution-free.
Detailed description of the invention
Below, by specific embodiment, technical scheme is described in detail.
Embodiment 1
The preparation method of a kind of aqueous polyanion electrically conductive ink that the present invention proposes, comprises the steps: poly-
After vinyl alcohol is added to the water mixing, adds aniline and camphorsulfonic acid continues mixing, be then slowly added dropwise over cure
Acid ammonium, stirring obtains aqueous polyanion electrically conductive ink.
Embodiment 2
The preparation method of a kind of aqueous polyanion electrically conductive ink that the present invention proposes, comprises the steps: poly-
After vinyl alcohol is added to the water mixing, then continue mixed by molar part 0.04 part of aniline of addition and 0.019 part of tartaric acid
Closing, be then slowly added dropwise Ammonium persulfate., stirring obtains aqueous polyanion electrically conductive ink.
Embodiment 3
The preparation method of a kind of aqueous polyanion electrically conductive ink that the present invention proposes, comprises the steps: mole
After polyvinyl alcohol is added to the water mixing by part, then add 0.05 part of aniline and 0.003 part of tartaric acid by molar part
Continuing mixing, be then slowly added dropwise Ammonium persulfate., stirring obtains aqueous polyanion electrically conductive ink.
Embodiment 4
The preparation method of a kind of aqueous polyanion electrically conductive ink that the present invention proposes, comprises the steps: poly-
Vinyl alcohol adds and mixes 1.0h in 80 DEG C of water, then adds 0.042 part of aniline and 0.013 part of citric acid by molar part
Continuing mixing, be then slowly added dropwise 0.032 part of Ammonium persulfate., rate of addition is 15g/h, and stirring obtains aqueous
Conductive printing ink from polyaniline.
Embodiment 5
The preparation method of a kind of aqueous polyanion electrically conductive ink that the present invention proposes, comprises the steps: poly-
Vinyl alcohol adds and mixes 0.5h in 90 DEG C of water, stands to clear, then adds 0.045 part by molar part
Aniline and 0.01 part of DBSA continue mixing 8min, and the weight ratio of aniline and polyvinyl alcohol is 4:
30, then 0.035 part of Ammonium persulfate. of dropping, rate of addition is 16g/h, and stirring 4h obtains aqueous polyanion to be led
Electricity ink.
Prepare aqueous polyanion electrically conductive ink thin film: prepare application device, choose one piece of proper area, cleaning
Glass plate, a piece of plastic packaging film is fixed, in plastic cup, dips appropriate reaction solution by Glass rod,
Spreading upon on plastic packaging film, the 100nm coated face of spreader is selected in this test, then by spreader, makes
Solution is uniformly spread out, by with smearing the plastic packaging film of solution, is placed on and is dried at shady and cool natural air drying after 24 hours,
Take off and obtain aqueous polyanion electrically conductive ink thin film.
The contact angle of detection aqueous polyanion electrically conductive ink thin film, matched group is selected polyaniline/PVA film, is sent out
The contact angle of existing polyaniline/PVA film is 52.14 °, and embodiment 1-5 gained aqueous polyanion electrically conductive ink
Film contacts angle generally the least, be below 40 °, wherein embodiment 5 gained aqueous polyanion electrically conductive ink
Film contacts angle be 17.67 °.
The Thin film conductive performance of detection embodiment 5 gained aqueous polyanion electrically conductive ink and mechanical performance, with poly-
Aniline/PVA film is as a control group；Wherein mechanical performance detection all uses 70.0mm × 20.0mm × 0.1
The rectangle sheet film of mm detects, and its result is as follows:
As seen from the above table: mechanical performance of the present invention is more or less the same with matched group, but electric conductivity exceptional,
It is applicable to electrically conductive ink field.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention not office
Being limited to this, any those familiar with the art is in the technical scope that the invention discloses, according to this
The technical scheme of invention and inventive concept thereof in addition equivalent or change, all should contain the protection in the present invention
Within the scope of.
Claims (7)
1. the preparation method of an aqueous polyanion electrically conductive ink, it is characterised in that comprise the steps: by
After polyvinyl alcohol is added to the water mixing, adds aniline and organic proton acid continues mixing, be then slowly added dropwise
Ammonium persulfate., stirring obtains aqueous polyanion electrically conductive ink.
The preparation method of aqueous polyanion electrically conductive ink the most according to claim 1, it is characterised in that benzene
The mol ratio of amine and organic proton acid is 0.04～0.05:0.003～0.019.
The preparation method of aqueous polyanion electrically conductive ink the most according to claim 1 or claim 2, it is characterised in that
Organic proton acid is camphorsulfonic acid, DBSA, tartaric acid, benzoic acid, citric acid or stearic acid.
4. according to the preparation method of aqueous polyanion electrically conductive ink described in any one of claim 1-3, its feature
Being, the mol ratio of aniline and Ammonium persulfate. is 0.04～0.05:0.03～0.04.
5. according to the preparation method of aqueous polyanion electrically conductive ink described in any one of claim 1-4, its feature
Being, the weight ratio of aniline and polyvinyl alcohol is 3.72～4.65:25～35.
6. according to the preparation method of aqueous polyanion electrically conductive ink described in any one of claim 1-5, its feature
It is, comprises the steps: to add polyvinyl alcohol 80～90 DEG C of water mix 0.5～1.0h, stand to clear
Clear bright after, add aniline and organic proton acid and continue mixing 5～10min, then drip Ammonium persulfate.,
Rate of addition is 14～18g/h, and stirring 3.5～4.5h obtains aqueous polyanion electrically conductive ink.
7. according to the preparation method of aqueous polyanion electrically conductive ink described in any one of claim 1-6, its feature
Being, the weight ratio of polyethylene alcohol and water is 1～3:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610474122.3A CN105936770B (en) | 2016-06-22 | 2016-06-22 | A kind of preparation method of aqueous polyanion electrically conductive ink |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610474122.3A CN105936770B (en) | 2016-06-22 | 2016-06-22 | A kind of preparation method of aqueous polyanion electrically conductive ink |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105936770A true CN105936770A (en) | 2016-09-14 |
| CN105936770B CN105936770B (en) | 2019-03-01 |
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Family Applications (1)
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| CN201610474122.3A Active CN105936770B (en) | 2016-06-22 | 2016-06-22 | A kind of preparation method of aqueous polyanion electrically conductive ink |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110628270A (en) * | 2019-08-29 | 2019-12-31 | 苏州世华新材料科技股份有限公司 | Conductive ink suitable for micro-gravure printing and preparation method thereof |
| CN114933827A (en) * | 2022-06-17 | 2022-08-23 | 中国船舶重工集团公司第七二五研究所 | Preparation method of low-solid-content high-conductivity water-based ink |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103496233A (en) * | 2013-09-27 | 2014-01-08 | 上海工程技术大学 | Preparation method of novel electrochromic double woven fabric |
| KR20160061278A (en) * | 2014-11-21 | 2016-05-31 | 롯데케미칼 주식회사 | Preparation method of conductive polymer complex and conductive polymer complex |
-
2016
- 2016-06-22 CN CN201610474122.3A patent/CN105936770B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103496233A (en) * | 2013-09-27 | 2014-01-08 | 上海工程技术大学 | Preparation method of novel electrochromic double woven fabric |
| KR20160061278A (en) * | 2014-11-21 | 2016-05-31 | 롯데케미칼 주식회사 | Preparation method of conductive polymer complex and conductive polymer complex |
Non-Patent Citations (2)
| Title |
|---|
| 王香琴等: "PANI/PVA共混薄膜的制备及表征", 《天津工业大学学报》 * |
| 王香琴等: "导电聚苯胺的制备及其表征", 《材料导报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110628270A (en) * | 2019-08-29 | 2019-12-31 | 苏州世华新材料科技股份有限公司 | Conductive ink suitable for micro-gravure printing and preparation method thereof |
| CN114933827A (en) * | 2022-06-17 | 2022-08-23 | 中国船舶重工集团公司第七二五研究所 | Preparation method of low-solid-content high-conductivity water-based ink |
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|---|---|
| CN105936770B (en) | 2019-03-01 |
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