CN108788178A - A kind of preparation method of the nano metal particles of good dispersion - Google Patents

A kind of preparation method of the nano metal particles of good dispersion Download PDF

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Publication number
CN108788178A
CN108788178A CN201810660297.2A CN201810660297A CN108788178A CN 108788178 A CN108788178 A CN 108788178A CN 201810660297 A CN201810660297 A CN 201810660297A CN 108788178 A CN108788178 A CN 108788178A
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China
Prior art keywords
gold nanoparticle
gold
preparation
oil
present
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CN201810660297.2A
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Chinese (zh)
Inventor
陈善勇
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Chongqing University of Arts and Sciences
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Chongqing University of Arts and Sciences
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Priority to CN201810660297.2A priority Critical patent/CN108788178A/en
Publication of CN108788178A publication Critical patent/CN108788178A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • 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

Abstract

The gold nanoparticle preparation method that stability is good, simple for process is prepared the present invention provides a kind of.It is comprised the concrete steps that:Gold chloride is added in edible oil, stirring at normal temperature is after five minutes, you can obtain gold nanoparticle.Relative to other preparation methods, the present invention prepares the edible oil for not being related to complicated chemical reaction system and using inexpensive safety, therefore its manufacturing cost substantially reduces.Meanwhile in the preparation process of the present invention, reaction time, reaction temperature, gold chloride concentration, edible oil access times influence very little to the size of final nano-particle, therefore preparation process does not need complicated reaction condition control, is convenient for industrial production.Gold nanoparticle good conductivity prepared by the present invention, can be in the industries extensive use such as electronic information.

Description

A kind of preparation method of the nano metal particles of good dispersion
The present invention is that application No. is the division Shens of the patent of invention on 30 days November 2016 201611090880.1, applying date Please.
Technical field
The invention belongs to nano metal particles preparing technical fields, and in particular to a kind of preparation side of gold nanoparticle Method.
Background technology
In previous report, gold nanoparticle is mainly anti-in organic solvent by using gold chloride and some reducing agents (Chem.Mater.2007,19,719-726 should be obtained;Chem.Mater.2011,23, 3312–3317;Nano Lett.2016,16,617-623).The price of gold chloride is very high, and the price of chemicals and organic solvent is also higher, this causes The manufacturing cost of final gold nanoparticle is very high, significantly impacts its application.Meanwhile these report preparation methods be also required to compared with The long reaction time, be unfavorable for it is quick, prepare gold nanoparticle on a large scale.Finally, organic solvent and organic chemical pollute environment, Its processing cost and the reaction environment brought pollute for reduction gold nanoparticle manufacturing cost, Protection personnel safety It is all unfavorable.To solve these problems and the application of gold nanoparticle is promoted, finds simple, cheap, quick, free of contamination gold nano Particle preparation method is just very necessary.
Invention content
Present invention aims at provide a kind of to prepare that stability is good, preparation method of gold nanoparticle simple for process.
The object of the invention is realized by following technical solution:
A kind of preparation method of gold nanoparticle, as follows:
(1) it takes a certain amount of edible oil to be added in a container to stir;
(2) and then by gold chloride it is added in edible oil, stirring to reaction terminates;The concentration range of the gold chloride is 0.01-0.30 grams of gold chloride/20 milliliter edible oil;
(3) after standing, edible oil is gone, is then cleaned, pure gold nanoparticle is obtained.
Edible oil used in the present invention includes soybean oil, corn oil, peanut oil, rapeseed oil, linseed oil, grape seed oil, purple Soviet Union's oil, walnut oil, apricot kernel oil, Seabuckthorn Oil, evening primrose oil, borage oil, sesame oil, sunflower oil, cottonseed oil, small oil, fire Sesame oil, siritch, camellia seed oil, peony seed oil, palm oil, walnut oil, coconut oil, olive oil etc..In use, can be independent A kind of oil can also be the mixing of two or more oil.Container used includes vial, stainless steel cauldron, glass The popular responses device such as reaction kettle, beaker, conical flask.After oil is added in container, stirring is opened.Then it is being kept stirring In the case of, gold chloride is added in oil, gold chloride dissolves and begins with solid generation immediately, and solution colour becomes black from transparent Brown.
Reaction time, reaction temperature, gold chloride concentration, edible oil access times influence the size of final gold nanoparticle Very little.In 5-180 minutes, 10-150 DEG C, the oily range in 0.01-0.30 grams of gold chloride/20 milliliter, the gold nanoparticle of acquisition Size it is essentially the same.Meanwhile edible oil access times do not have influence substantially on its size, and within 5 times, Jenner's grain of rice of acquisition The size of son remains unchanged.The size of final gold nanoparticle is between 300nm to 700nm.
After reaction, a few minutes are stood, gold nanoparticle is deposited to container bottom completely.Supernatant liquor is poured into one In a bottle, preserves, remain next use.Then the solvent that can dissolve edible oil is added, after stirring a few minutes, supernatant liquor is inclined ?.It is repeated several times this process, you can obtain pure gold nanoparticle.
The solvent of cleaning edible oil of the invention used be ethyl alcohol, isopropanol, methanol, acetone, one kind in ethyl acetate or Several mixing.
The present invention has the following advantages:(1) in addition to gold chloride and edible oil, other reactive materials are not required to, reaction is simple, pacifies Entirely;(2) whole process is other than reaction vessel and blender, need not be purified by centrifugation by other instruments, pair sets Standby requirement is very low;(3) reaction time, reaction temperature, gold chloride concentration, edible oil access times are to final gold nanoparticle Size influence very little, preparation process is easily controlled, the gold nanoparticle size uniformity of acquisition;(4) in addition to gold chloride, other Cost is negligible, and total production procedure is quick, inexpensive, pollution-free, facilitates industrial production.
Generally speaking, relative to pervious method, the present invention prepares the edible oil using inexpensive safety, manufacturing cost, Post processing cost substantially reduces.Importantly, in preparation process of the present invention, time, temperature, concentration are to final nano-particle Size influence very little, it can be used repeatedly for edible oil, therefore the preparation of gold nanoparticle of the present invention need not accurately control instead Condition is answered, This further reduces the manufacturing costs of gold nanoparticle.These advantages make gold nanoparticle of the present invention in valence Great competitive advantage on lattice, can be in the industries extensive use such as electronic information.
Description of the drawings
Fig. 1:The SEM image of final gold nanoparticle;
Fig. 2:Different gold chloride concentration (Fig. 2 (a), Fig. 2 (b), Fig. 2 (c), Fig. 2 (d), Fig. 2 (e)) are respectively 0.02 gram, 0.05 gram, 0.10 gram, 0.15 gram, 0.20 gram of gold chloride be dissolved in 20 milliliters of edible oils) to the shadow of final gold nanoparticle size It rings;
Fig. 3:Edible oil reuses number (Fig. 3 (a), Fig. 3 (b), Fig. 3 (c) are respectively 1,2,3 time) to final Jenner The influence of rice corpuscles size;
Fig. 4:Differential responses temperature (Fig. 4 (a), Fig. 4 (b), Fig. 4 (c), Fig. 4 (d), Fig. 4 (e), Fig. 4 (f) be respectively 30 DEG C, 50 DEG C, 70 DEG C, 90 DEG C, 110 DEG C, 130 DEG C) influence to final gold nanoparticle size;
Fig. 5:The differential responses time, (Fig. 5 (a), Fig. 5 (b), Fig. 5 (c), Fig. 5 (d), Fig. 5 (e), Fig. 5 (f), Fig. 5 (g) were respectively It is 5 minutes, 0.5 hour, 1 hour, 1.5 hours, 2 hours, 2.5 hours, 3 hours) influence to final gold nanoparticle size.
Specific implementation mode
Embodiment:
20ml rapeseed oils (supermarket's purchase) and a stirrer are added into a beaker, opens stirring.Then 0.10g is weighed Gold chloride is quickly poured into rapeseed oil.Gold chloride dissolves immediately, occurs insoluble solid in solution at once, and solution colour is from saturating It is bright to become dark brown;
Stirring after five minutes, stops stirring.3 minutes are stood, gold nanoparticle is made to sink to the bottom completely.Then by the vegetable seed on upper layer Oil is gone.It is subsequently added into 20ml ethyl alcohol, stirring after five minutes removes solution;
Above-mentioned ethyl alcohol cleaning process is in triplicate, you can pure gold nanoparticle is obtained, in golden yellow.SEM tests are aobvious Show its size between 300-580nm.
Presently preferred embodiments of the present invention described in detail above.It should be appreciated that those skilled in the art are without wound The property made labour, which according to the present invention can conceive, makes many modifications and variations.All technician in the art Yi Benfa Bright design passes through the available experiment of logical analysis, reasoning, or a limited experiment and technology on the basis of existing technology Scheme, all should be in the protection domain being defined in the patent claims.

Claims (2)

1. a kind of preparation method of gold nanoparticle, which is characterized in that as follows:
(1)Rapeseed oil is added in a container with stirrer and is stirred;
(2)Then it weighs gold chloride to be added in above-mentioned rapeseed oil, is stirred to react 5 minutes, stops stirring;The gold chloride it is dense Spend ranging from 0.01 gram of gold chloride/20 milliliter rapeseed oil;
(3)After said mixture standing is deposited to bottom in 3 minutes completely to gold nanoparticle, upper layer rapeseed oil is gone, is connect It and is cleaned with the alcohol solvent that 20ml or so is added, stirring after five minutes removes solution;Above-mentioned ethyl alcohol cleaning process is in triplicate Gold nanoparticle of the present invention is made.
2. gold nanoparticle preparation method as described in claim 1, it is characterised in that:The step(2)The temperature of the reaction Ranging from 10-150 DEG C.
CN201810660297.2A 2016-11-30 2016-11-30 A kind of preparation method of the nano metal particles of good dispersion Withdrawn CN108788178A (en)

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CN201611090880.1A CN106607594B (en) 2016-11-30 2016-11-30 A kind of quick, low cost gold nanoparticle preparation method
CN201810660297.2A CN108788178A (en) 2016-11-30 2016-11-30 A kind of preparation method of the nano metal particles of good dispersion

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113523297A (en) * 2021-07-13 2021-10-22 广州萃普生物科技有限公司 Method for preparing nano-silver by using peony extract

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* Cited by examiner, † Cited by third party
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WO2009140694A2 (en) * 2008-05-16 2009-11-19 Verutek Technologies, Inc. Green synthesis of nanometals using plant extracts and use thereof
CN103194616B (en) * 2013-04-08 2014-07-30 吉林大学 Method for preparing copper nanocrystalline
CN104174870B (en) * 2014-08-29 2016-08-24 北京工业大学 A kind of method utilizing Semen Vitis viniferae green syt nano zero valence iron and application thereof
CN104923804B (en) * 2015-07-02 2017-07-25 吉林大学 A kind of preparation method of nickel nano particle
CN105127442A (en) * 2015-08-20 2015-12-09 扬州大学 Method for synthesizing nano-silver colloid with green coffee bean extract as reducing agent
CN105665733A (en) * 2015-11-24 2016-06-15 鲁东大学 Method for preparing graphite-like C3N4/nano-silver antibacterial composite in environmental-friendly mode
CN105750562A (en) * 2016-04-21 2016-07-13 太原理工大学 Method for green synthesis of nanometer zero-valent iron suspension liquid with peels or seed kernels
CN105965031B (en) * 2016-07-21 2017-11-14 上海理工大学 A kind of method that nanogold particle is prepared using matrimony vine leaching liquor

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113523297A (en) * 2021-07-13 2021-10-22 广州萃普生物科技有限公司 Method for preparing nano-silver by using peony extract

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