[go: up one dir, main page]
More Web Proxy on the site http://driver.im/

CN113787188B - Method for purifying silver nanowires by inorganic salting-out - Google Patents

Method for purifying silver nanowires by inorganic salting-out Download PDF

Info

Publication number
CN113787188B
CN113787188B CN202111044118.0A CN202111044118A CN113787188B CN 113787188 B CN113787188 B CN 113787188B CN 202111044118 A CN202111044118 A CN 202111044118A CN 113787188 B CN113787188 B CN 113787188B
Authority
CN
China
Prior art keywords
silver
silver nanowires
silver nanowire
flocculate
inorganic salt
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.)
Active
Application number
CN202111044118.0A
Other languages
Chinese (zh)
Other versions
CN113787188A (en
Inventor
卞永俊
高绪彬
郭云才
潘克菲
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nuovo Film Suzhou China Inc
Original Assignee
Nuovo Film Suzhou China Inc
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Nuovo Film Suzhou China Inc filed Critical Nuovo Film Suzhou China Inc
Priority to CN202111044118.0A priority Critical patent/CN113787188B/en
Publication of CN113787188A publication Critical patent/CN113787188A/en
Application granted granted Critical
Publication of CN113787188B publication Critical patent/CN113787188B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention discloses a method for purifying silver nanowires by inorganic salt, which comprises the following steps: (1) Adding water into the silver nanowire synthetic solution for dilution, then sequentially adding inorganic salt (supersaturated) and alkali to obtain a suspension, standing for layering, and separating to obtain flocculate; (2) Adding PVP and water into the flocculate to obtain silver nanowire dispersion liquid; (3) Adding inorganic salt (supersaturated) and alkali into the silver nanowire dispersion liquid to obtain flocculate again; and (4) repeating the steps (2) and (3) for a plurality of times, and dispersing the obtained flocculate in the aqueous solution of PVP to obtain the purified silver nanowire dispersion liquid. The purification method of the silver nanowires is simple to operate, low in cost, free of any organic solvent, small in harm to human bodies and environment in the operation process, low in requirements on production and operation environments, free of organic solvent in waste liquid, easy to process, capable of further reducing production cost, and suitable for purification treatment of large-scale silver nanowires.

Description

Method for purifying silver nanowires by inorganic salting-out
Technical Field
The invention relates to the technical field of silver nanowire purification, in particular to a method for purifying silver nanowires by inorganic salting out.
Background
The silver nanowire has good conductivity, excellent light transmission, bending resistance, length-diameter ratio effect and the like, and has wide application prospects in the fields of flexible electronic devices, catalysis, antibiosis and the like. At present, the polyol method is a mainstream preparation method of silver nanowires due to the advantages of simple operation, high yield, large-scale production and the like, but a certain amount of silver nanoparticles are mixed in the silver nanowire synthetic solution prepared by the method, and the byproducts can seriously affect the photoelectric properties of the silver nanowires and usually purify the silver nanowire synthetic solution.
The existing purification methods of the silver nanowire synthetic solution mainly comprise a centrifugal sedimentation method, an organic solvent precipitation method and the like. The centrifugal sedimentation method is used for strictly controlling the centrifugal time and speed, if the centrifugal time or speed is insufficient, the silver nanoparticles and the silver nanowires are difficult to separate, and if the centrifugal speed is too high and the centrifugal time is too long, the silver nanoparticles are easy to settle together with the silver nanowires, so that the separation and purification effects are difficult to achieve by the centrifugal sedimentation method, and the silver nanowires are easy to agglomerate to form blocks which are difficult to disperse after multiple centrifugal operations; in addition, by utilizing the dissolving property of polyvinylpyrrolidone (PVP), PVP poor solvents such as acetone, ethyl acetate and petroleum ether are added into the silver nanowire synthetic solution to separate out PVP which plays a role in dispersing silver nanowires, further, silver nanowires are agglomerated into flocculent precipitate and are settled, and the number of nanoparticles in the silver nanowire synthetic solution is obviously reduced by repeated settlement for a plurality of times.
Disclosure of Invention
In order to solve the problems, the invention provides a method for purifying silver nanowires by inorganic salting out, which reduces the solubility of PVP (polyvinyl pyrrolidone) by adding inorganic salt and alkali into a silver nanowire synthetic solution, so that the PVP is separated out to lose the effect of dispersing the silver nanowires, and the silver nanowires are agglomerated into flocculent separated out to achieve the effect of separating the silver nanowires from silver nanoparticles.
The invention provides the following technical scheme:
the invention provides a method for purifying silver nanowires by using inorganic salt, which comprises the following steps:
(1) Adding water into the silver nanowire synthetic solution to dilute to obtain a diluent, then sequentially adding inorganic salt and alkali into the diluent to obtain a suspension, standing for layering, and separating to obtain flocculate; the inorganic salt is added to supersaturation;
(2) Dispersing the flocculate into PVP and water to obtain silver nanowire dispersion liquid;
(3) Adding inorganic salt and alkali into the silver nanowire dispersion liquid in sequence, standing and layering to obtain flocculate again; the inorganic salt is added to supersaturation;
(4) And (4) repeating the steps (2) and (3) for at least 5 times to obtain the purified silver nanowire floc.
Further, in the step (1), the solid content of silver in the diluent is 0.05 to 0.3wt%.
Further, the water is preferably purified water.
Further, the inorganic salt includes one or more of sodium chloride, potassium chloride, ammonium chloride, sodium bromide, potassium bromide, ammonium bromide, sodium carbonate, potassium carbonate, ammonium carbonate, sodium bicarbonate, potassium bicarbonate, ammonium bicarbonate, sodium sulfate, potassium sulfate, ammonium sulfate, sodium sulfite, potassium sulfite, ammonium sulfite, sodium nitrate, potassium nitrate, ammonium nitrate, sodium nitrite, potassium nitrite, and ammonium nitrite.
Further, the alkali comprises one or more of sodium hydroxide, potassium hydroxide, lithium hydroxide, calcium hydroxide and ammonia water, and the addition of the alkali can reduce the solubility of PVP in water and promote the precipitation of PVP.
Further, in the step (1), the amount of the base added is 1 to 10wt% of the diluent.
Further, in the steps (1) and (3), the standing time is 3-30min.
Further, in the step (2), the PVP is added in an amount of 0.01-0.5wt% of the silver nanowire dispersion liquid.
Further, when the ratio of the content of the silver particles to the total content of silver in the silver nanowire synthetic solution is less than 30%, repeating for 5-10 times; when the ratio is 30-50%, repeating for 10-20 times; when the ratio is more than 50%, repeating for no less than 20 times.
Compared with the prior art, the invention has the beneficial effects that: the invention adopts inorganic salt and alkali to reduce the solubility of PVP in the silver nanowire synthetic solution, so that PVP is separated out to lose the action of dispersing the silver nanowires, the silver nanowires are agglomerated into flocculent separation, and the effect of separating the silver nanowires and silver nanoparticles is achieved.
Drawings
FIG. 1 is an optical microscope photograph (500 Xmagnification) of a silver nanowire synthetic fluid in example 1;
FIG. 2 is an optical microscopic image (500X magnification) of silver nanoparticles separated by the sedimentation treatment in example 1;
fig. 3 is an optical microscope photograph (500 × magnification) of the silver nanowire dispersion after purification in example 1.
Detailed Description
The present invention is further described below in conjunction with the drawings and the embodiments so that those skilled in the art can better understand the present invention and can carry out the present invention, but the embodiments are not to be construed as limiting the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The experimental procedures used in the following examples are conventional ones unless otherwise specified, and the materials, reagents and the like used therein are commercially available.
Example 1
In this example, the silver nanowires in the silver nanowire synthetic solution are purified by the following steps:
(1) Adding 20kg of deionized water into 5kg of silver nanowire synthetic stock solution with the solid content of silver of 0.4% for dilution to obtain silver nanowire mixed solution, adding 9kg of sodium chloride into the silver nanowire mixed solution while stirring until the sodium chloride is not completely dissolved, then adding 5kg of 33% sodium hydroxide aqueous solution, standing for 10min, and after layering in the mixed solution, extracting non-flocculates in the mixed solution to obtain flocculates;
(2) Adding 1kg of PVP with the concentration of 5% into the flocculate, supplementing purified water to 25kg, and uniformly stirring to redisperse the flocculated and settled silver nanowires to obtain silver nanowire dispersion liquid;
(3) Adding 9kg of sodium chloride into the silver nanowire dispersion liquid while stirring, adding 4kg of sodium hydroxide aqueous solution diluted by 33% aqueous solution, standing for 3min, and after layering in the mixed liquid, extracting non-flocculate in the mixed liquid to obtain flocculate;
(4) And (4) repeating the operations of the steps (2) and (3) for 8 times to obtain the purified silver nanowire.
The 500x optical micrographs of the silver nanowire synthesis stock solution, the separated silver nanoparticles and the purified silver nanowire dispersion solution of this example are shown in fig. 1 to 3, respectively; as can be seen from fig. 1, the silver nanowire synthesis stock solution contains a large amount of silver nanoparticles, and the silver nanowires shown in fig. 3 are obtained by the above-mentioned multiple sedimentation separation, only a very small amount of silver nanoparticles remain, and the purified silver nanowires still have good dispersibility.
Example 2
In this example, the silver nanowires in the silver nanowire synthetic solution are purified by the following steps:
(1) Adding 20kg of deionized water into 5kg of silver nanowire synthetic stock solution with the solid content of silver of 0.4% for dilution to obtain silver nanowire mixed solution, adding 8.5kg of potassium chloride into the silver nanowire mixed solution while stirring until the potassium chloride is not completely dissolved, adding 5kg of 33% potassium hydroxide aqueous solution, standing for 10min, after layering in the mixed solution, pumping out non-flocculates in the mixed solution, and obtaining flocculates;
(2) Adding 1kg of PVP with the concentration of 5% into the flocculate, supplementing purified water to 25kg, and uniformly stirring to redisperse the flocculated and settled silver nanowires to obtain silver nanowire dispersion liquid;
(3) Adding 8.5kg of potassium chloride into the silver nanowire dispersion liquid while stirring, adding 4kg of potassium hydroxide aqueous solution diluted by 33% aqueous solution, standing for 3min, and after layering in the mixed solution, extracting non-flocculates in the mixed solution to obtain flocculates;
(4) And (4) repeating the operations of the steps (2) and (3) for 10 times to obtain the purified silver nanowire.
Through the operations of multiple times of sedimentation and dispersion, the silver nanoparticles in the synthetic stock solution are basically removed, thereby realizing the purification of the silver nanowires.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.

Claims (6)

1. A method for purifying silver nanowires by inorganic salting out is characterized by comprising the following steps:
(1) Adding water into the silver nanowire synthetic solution to dilute to obtain a diluent, then sequentially adding inorganic salt and alkali into the diluent to obtain a suspension, standing for layering, and separating to obtain flocculate; the inorganic salt is added to supersaturation;
(2) Adding PVP and water into the flocculate to obtain silver nanowire dispersion liquid;
(3) Adding inorganic salt and alkali into the silver nanowire dispersion liquid in sequence, standing and layering to obtain flocculate again; the inorganic salt is added to supersaturation;
(4) Repeating the steps (2) and (3) for at least 5 times to obtain purified silver nanowires;
the inorganic salt is sodium chloride or potassium chloride, and the alkali is sodium hydroxide or potassium hydroxide.
2. The method for purifying silver nanowires by inorganic salting out according to claim 1, wherein in the step (1), the solid content of silver in the dilution liquid is 0.05-0.3wt%.
3. The method for inorganic salting-out purification of silver nanowires according to claim 1, wherein in the step (1), the amount of the alkali added is 1-10wt% of the diluent.
4. The method for purifying silver nanowires by inorganic salting out according to claim 1, wherein in the steps (1) and (3), the standing time is 3-30min.
5. The method for inorganic salting-out purification of silver nanowires according to claim 1, wherein in the step (2), PVP is added in an amount of 0.01-0.5wt% of the silver nanowire dispersion.
6. The method for purifying silver nanowires by inorganic salting out as claimed in claim 1, wherein when the ratio of the content of silver particles to the total content of silver in the silver nanowire synthetic solution is less than 30%, repeating the steps for 5-10 times; when the ratio is 30-50%, repeating for 10-20 times; when the ratio is more than 50%, repeating for no less than 20 times.
CN202111044118.0A 2021-09-07 2021-09-07 Method for purifying silver nanowires by inorganic salting-out Active CN113787188B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111044118.0A CN113787188B (en) 2021-09-07 2021-09-07 Method for purifying silver nanowires by inorganic salting-out

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111044118.0A CN113787188B (en) 2021-09-07 2021-09-07 Method for purifying silver nanowires by inorganic salting-out

Publications (2)

Publication Number Publication Date
CN113787188A CN113787188A (en) 2021-12-14
CN113787188B true CN113787188B (en) 2023-04-07

Family

ID=78879685

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111044118.0A Active CN113787188B (en) 2021-09-07 2021-09-07 Method for purifying silver nanowires by inorganic salting-out

Country Status (1)

Country Link
CN (1) CN113787188B (en)

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103394704B (en) * 2013-08-20 2015-09-30 纳米籽有限公司 Preparation method of high-purity gold nanobicones and composite nanomaterials thereof
KR20160147817A (en) * 2014-04-11 2016-12-23 챔프 그레이트 인터내셔널 코포레이션 Methods of controlling nanowire morphology
CN109434132A (en) * 2018-12-07 2019-03-08 陕西煤业化工技术研究院有限责任公司 A method of purifying ultra-fine silver nanowires
CN111217389A (en) * 2020-01-08 2020-06-02 苏州星烁纳米科技有限公司 Nanowire processing method and nanowire

Also Published As

Publication number Publication date
CN113787188A (en) 2021-12-14

Similar Documents

Publication Publication Date Title
CN109650350B (en) Method for large-scale preparation of polysaccharide modified nano-selenium and application
US10773312B2 (en) Preparation method for silver nanowires with uniform aspect ratio and nodes
CN103613182B (en) A kind of heavy metal high-polymer flocculating agent and application thereof
CN102101173A (en) Method for preparing novel large-scale oil-soluble nano silver
CN104108738B (en) A kind of method being prepared high pure spherical cupric oxide by bluestone waste
CN113787188B (en) Method for purifying silver nanowires by inorganic salting-out
CN1032703C (en) Copper removing method for nickel electrolysis anolyte
CN105883889B (en) A kind of method of industrialized production high-purity neodymium oxide
CN110814361A (en) Silver nanowire purification method
CN117285138B (en) Aluminum sulfate water treatment agent and preparation method thereof
CN110112411B (en) MnCO3Microspheres and method for preparing same
CN113714500B (en) Purification method of superfine silver nanowire
CN110408778B (en) Heavy rare earth precipitated by mixing sodium carbonate and sodium bicarbonate
CN112744811B (en) Large-sheet-diameter graphene oxide and preparation method thereof
CN1321200C (en) Method for separating copper, arsenic and zinc from copper-smelting high-arsenic flue dust sulphuric acid leach liquor
CN110422867B (en) Method for preparing dehydrated titanium gypsum and product prepared by method
CN1211285C (en) Method of preparing white magnesium chloride by reduction method
CN112934213A (en) Cerium dioxide nanosheet-carbon nanotube composite material for water treatment
CN1609225A (en) Method of processing fermented erythromycin liquid with modified chitosan
CN115740434B (en) A kind of silver nanowire and separation and purification method thereof
CN111777094B (en) Preparation method of nanoscale zinc oxide with controllable pile ratio
CN111482183A (en) Composite photocatalytic material and preparation method thereof
CN114620879B (en) Method for recycling silver nanowire production waste liquid
CN219546839U (en) Treatment of ternary precursor production wastewater device
CN117798372A (en) Method for synthesizing silver nanowires by converting particles

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
GR01 Patent grant
GR01 Patent grant