CN110078916A - A kind of synthetic method of poly- 1,8- diaminonaphthalene nanotube - Google Patents
A kind of synthetic method of poly- 1,8- diaminonaphthalene nanotube Download PDFInfo
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- CN110078916A CN110078916A CN201910378961.9A CN201910378961A CN110078916A CN 110078916 A CN110078916 A CN 110078916A CN 201910378961 A CN201910378961 A CN 201910378961A CN 110078916 A CN110078916 A CN 110078916A
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- diaminonaphthalene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
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Abstract
The present invention provides one kind poly- 1, the synthetic method of 8- diaminonaphthalene nanotube, it is characterized in that, the following steps are included: 8- diaminonaphthalene and template are added in deionized water by 1, it is dispersed with stirring to form emulsion, in the emulsion prepared before hypochloric acid water solution is added with the speed of two seconds every drops, it is precipitated after being persistently stirred to react 6~12 hours, is dried to obtain poly- 1,8- diaminonaphthalene nanotube powder through washing after filtering.The present invention synthesizes poly- 1,8- diaminonaphthalene nanotube in full aqueous solution, and simple process, environmental pollution is small, product morphology stable structure.
Description
Technical field
The invention belongs to material chemistry technical fields, are related to a kind of synthetic method of poly- 1,8- diaminonaphthalene nanotube.
Background technique
Poly- 1,8- diaminonaphthalene is trapezoidal conjugation condensed ring macromolecule, has unique multifunctionality, in catalysis, electroluminescent change
There is potential application in the fields such as color, sensor.Electrochemical oxidation process and chemical oxidization method synthesis can be used in poly- 1,8- diaminonaphthalene,
Patent (CN1810853) discloses the chemical oxidation process for synthesizing poly- 1,8- diaminonaphthalene in organic solvent, patent (CN
The synthetic method that organic/water termination polymerize poly- 1,5-diaminonaphthalene nanotube 100503692C) is disclosed, the present invention is in aqueous solution
Middle poly- 1, the 8- diaminonaphthalene nanotube of oxidative synthesis.
Summary of the invention
The purpose of the present invention is to provide a kind of synthetic methods of poly- 1,8- diaminonaphthalene nanotube, which is characterized in that packet
It includes following steps: 1,8- diaminonaphthalene and template being added in deionized water, are dispersed with stirring to form emulsion, by hypochloric acid water
In the emulsion that solution is prepared before being added with the speed of two seconds every drops, precipitated after being persistently stirred to react 6~12 hours, mistake
Poly- 1,8- diaminonaphthalene nanotube powder is dried to obtain through washing after filter.
1,8- diaminonaphthalene concentration 1mmol/L~3mmol/L in mixed solution.
The template include α-naphthalenesulfonicacid, beta-naphthalenesulfonic-acid, 1,5-, bis- naphthalene sulfonic acids, in 2,4- dinitro naphthols -7- sulfonic acid
One kind, concentration 0.002mol/L~0.005mol/L in mixed solution.
Concentration 0.01mol/L~0.02mol/L in the hypochlorous acid mixed solution.
The washing is alternately washed with deionized water and ethyl alcohol, is used centrifuge to precipitate or filter each time after washing and is set
Standby to be filtered, filtration product is dispersed in deionized water or ethyl alcohol again, and repeated filtration is 7 until filtrate pH value, last
It is secondary to use ethanol washing with convenient and dry;The drying is dried in 50~80 DEG C of vacuum drying ovens, and vacuum drying condition is true
Reciprocal of duty cycle < 133Pa.
The present invention synthesizes poly- 1,8- diaminonaphthalene nanotube in full aqueous solution, and simple process, environmental pollution is small, product shape
Looks stable structure.
The contents of the present invention and feature have revealed that as above, however the present invention that describes of front only briefly or pertains only to this
The specific part of invention, feature of the invention may be more than what content disclosed herein was related to.Therefore, protection model of the invention
The revealed content of embodiment should be not limited to by enclosing, and should include the combination of all the elements embodied in different piece, with
And it is various without departing substantially from replacement and modification of the invention, and covered by claims of the present invention.
Detailed description of the invention
Fig. 1 is the stereoscan photograph that poly- 1,8- diaminonaphthalene nanotube is synthesized using (embodiment 1) of the invention.
Specific embodiment
Embodiment 1
By 2mmol/L 1,8- diaminonaphthalene and template are added in 100mL deionized water, are dispersed with stirring to form emulsion,
In the emulsion prepared before 100mL 0.02mol/L hypochlorous acid is added with the speed of two seconds every drops, it is persistently stirred to react 6
It is precipitated after~12 hours, is dried to obtain poly- 1,8- diaminonaphthalene nanotube powder as shown in Figure 1 through washing after filtering.
Embodiment 2
By 4mmol/L 1,8- diaminonaphthalene and template are added in 100mL deionized water, are dispersed with stirring to form emulsion,
In the emulsion prepared before 100mL 0.03mol/L hypochlorous acid is added with the speed of two seconds every drops, it is persistently stirred to react 6
It is precipitated after~12 hours, is dried to obtain poly- 1,8- diaminonaphthalene nanotube powder through washing after filtering.
Embodiment 3
By 6mmol/L 1,8- diaminonaphthalene and template are added in 100mL deionized water, are dispersed with stirring to form emulsion,
In the emulsion prepared before 100mL 0.04mol/L hypochlorous acid is added with the speed of two seconds every drops, it is persistently stirred to react 6
It is precipitated after~12 hours, is dried to obtain poly- 1,8- diaminonaphthalene nanotube powder through washing after filtering.
Claims (6)
1. a kind of synthetic method of poly- 1,8- diaminonaphthalene nanotube, which comprises the following steps: by 1,8- diamino
Naphthalene and template are added in deionized water, are dispersed with stirring to form emulsion, hypochloric acid water solution is added with the speed of two seconds every drops
It in the emulsion prepared before entering, is precipitated after being persistently stirred to react 6~12 hours, is dried to obtain poly- 1 through washing after filtering,
8- diaminonaphthalene nanotube powder.
2. a kind of synthetic method of poly- 1,8- diaminonaphthalene nanotube according to claim 1, it is characterised in that: described 1,8-
Diaminonaphthalene concentration 1mmol/L~3mmol/L in mixed solution.
3. a kind of synthetic method of poly- 1,8- diaminonaphthalene nanotube according to claim 1, it is characterised in that: the template
Agent includes one of α-naphthalenesulfonicacid, beta-naphthalenesulfonic-acid, 1,5-, bis- naphthalene sulfonic acids, 2,4- dinitro naphthols -7- sulfonic acid, in mixed solution
Concentration 0.002mol/L~0.005mol/L.
4. a kind of synthetic method of poly- 1,8- diaminonaphthalene nanotube according to claim 1, it is characterised in that: the secondary chlorine
Concentration 0.01mol/L~0.02mol/L in sour mixed solution.
5. a kind of synthetic method of poly- 1,8- diaminonaphthalene nanotube according to claim 1, it is characterised in that: described washes
Washing alternately is washed with deionized water and ethyl alcohol, is filtered, is filtered using centrifuge precipitating or pumping and filtering device each time after washing
Product disperses in deionized water or ethyl alcohol again, and repeated filtration is 7 until filtrate pH value, for the last time with ethanol washing with side
Just it dries;The drying is dried in 50~80 DEG C of vacuum drying ovens, and vacuum drying condition is vacuum degree < 133Pa.
6. prepared by a kind of synthetic method of poly- 1,8- diaminonaphthalene nanotube as claimed in any one of claims 1 to 5, wherein
Poly- 1,8- diaminonaphthalene nanotube.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1810853A (en) * | 2005-01-26 | 2006-08-02 | 同济大学 | Prepn process of poly-1,8-naphthalenediamine |
CN103772702A (en) * | 2012-10-18 | 2014-05-07 | 上海纳米技术及应用国家工程研究中心有限公司 | Poly 1-naphthylamine nano hollow structure and its preparation method |
US20160248099A1 (en) * | 2013-10-01 | 2016-08-25 | Imperial Innovations Limited | Oxygen reduction catalysts |
CN109517168A (en) * | 2018-11-08 | 2019-03-26 | 上海萃励电子科技有限公司 | A kind of synthetic method of poly- naphthalidine -7- sulfonic acid nanotube |
-
2019
- 2019-04-23 CN CN201910378961.9A patent/CN110078916A/en not_active Withdrawn
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1810853A (en) * | 2005-01-26 | 2006-08-02 | 同济大学 | Prepn process of poly-1,8-naphthalenediamine |
CN103772702A (en) * | 2012-10-18 | 2014-05-07 | 上海纳米技术及应用国家工程研究中心有限公司 | Poly 1-naphthylamine nano hollow structure and its preparation method |
US20160248099A1 (en) * | 2013-10-01 | 2016-08-25 | Imperial Innovations Limited | Oxygen reduction catalysts |
CN109517168A (en) * | 2018-11-08 | 2019-03-26 | 上海萃励电子科技有限公司 | A kind of synthetic method of poly- naphthalidine -7- sulfonic acid nanotube |
Non-Patent Citations (2)
Title |
---|
《新编危险物品安全手册》编委会: "《新编危险物品安全手册》", 30 April 2001, 化学工业出版社 * |
章家立 等: "聚萘二胺纳米材料的合成及其应用研究进展", 《化工进展》 * |
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