CN106363192B - A kind of continuous feed parallel reaction device of gold nanorods preparation and application - Google Patents
A kind of continuous feed parallel reaction device of gold nanorods preparation and application Download PDFInfo
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- CN106363192B CN106363192B CN201611009713.XA CN201611009713A CN106363192B CN 106363192 B CN106363192 B CN 106363192B CN 201611009713 A CN201611009713 A CN 201611009713A CN 106363192 B CN106363192 B CN 106363192B
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Abstract
The invention discloses a kind of continuous feed parallel reaction devices of gold nanorods preparation.Described device is made of reactant premixer, peristaltic pump, the reaction tube of multiple parallel interconnections and water bath with thermostatic control.The device can realize effective uniform amplification preparation of the gold nanorods of different draw ratios.Reaction mass is uniformly mixed in premixer, then it is transported in the reaction tube of multiple parallel interconnections and is reacted by peristaltic pump, it is interconnected between reaction tube by bottom pipe, by law of connected vessels mean allocation reactant, while the discharge pipe as reaction product.It since each reaction tube is small in size, is heated evenly in water bath with thermostatic control, ensure that the uniformity of the heat and mass in the case where standing reaction condition, to obtain the reaction product of uniform morphology and size.
Description
Technical field
The present invention relates to a kind of continuous feed parallel reaction device of gold nanorods preparation and application, metal nanometer material preparations
Field.
Technical background
In recent years, being constantly progressive with nanotechnology, application real time implementation, polymorphicization, the nothing increasingly of bio-imaging means
Damage, nontoxic, the room and time resolution ratio continuous improvement of bio-imaging technology, noble metal (gold, silver etc.) nano material auxiliary
Bio-imaging technology is increasingly becoming research hotspot.Gold nano-material shows the property and advantage to attract people's attention, wherein gold nano
Stick is due to its unique surface plasma resonance (surfaceplasmonresonance, SPR) property and good bio-compatible
Property is widely used in field of biomedicine.Compared to other gold nano structures, the peaks SPR of gold nanorods with draw ratio increasing
Height is near infrared region red shift.Since visible light is not easy to penetrate biological tissue, and the gold nanorods of high length-diameter ratio are near infrared region
Absorption and scattering power to light are all very strong, therefore imaging for the cancer of subcutaneous tissue and photo-thermal therapy are to select well
It selects.Gold nanorods have extensively in researchs such as pharmaceutical carrier, diagnosing tumor, laserthermia, photoacoustic imaging, Computed tomographies
General application.Meanwhile research finds that the size of gold nanorods and the difference of crystal structure have significant impact for application, it is right
Gold nanorods synthesis is effective to adjust the effect that decide its subsequent application study.Quickly, easy, batch prepares high yield, high
The gold nanorods of homogeneity, to ensuring that gold nanorods are extremely important in biomedical applications.
The synthesis control method of different size shape gold nanorods has very much, mainly include electrochemistry, photochemistry, template and
Crystal seed method.Wherein crystal seed method becomes most extensive, the most frequently used because it prepares simple, high quality, high yield and is easy to control draw ratio
Method.The basic principle that crystal seed method synthesizes gold nanorods is the system existing for silver ion and cetyl trimethylammonium bromide
In, a certain amount of gold nano seed (1.5-4nm) is added, by changing the additional amount of reducing agent, protective agent, crystal seed, gold chloride,
And addition sequence, system temperature, reaction speed etc. control the particle size and draw ratio of gold nanorods.However gold nanorods
Synthesis to preparation environment temperature and reductant concentration it is extremely sensitive.Mass transfer and small variation of conducting heat, gold nanorods are synthesizing
It is easy in the process to generate the by-products nanoparticles such as spherical, sheet, cone cell.Therefore it is carried out when by simple volume iodine
When prepared by batch, since reaction system is there are serious heating is inhomogenous, the problems such as heat and mass is inhomogenous, will lead to preparation institute
Obtained gold nanorods low yield, consistency is poor between batch, causes later product purification & isolation difficult, it is difficult to meet biomedicine and answer
It is required that.Therefore, the gold nanorods synthetic method batch for needing to develop new model prepares high-performance gold nanorods.
Summary of the invention
The purpose of the present invention is to solve heat and mass is uneven, easily leads to nanorod shaped in gold nanorods amplification preparation
Looks size is inhomogenous, batch between consistency difference problem.
For achieving the above object, the present invention adopts the following technical scheme:
A kind of continuous feed parallel reaction device of gold nanorods preparation, reactant are uniformly mixed in premixer, so
It is transported in the reaction tube of multiple parallel interconnections and is reacted by peristaltic pump afterwards, to realize effectively uniform amplification preparation.
The premixer with churned mechanically three necks glass round bottom reaction flask by forming, capacity 0.5-2L.
It is conveyed and is assigned to after reactant mixing and reacted in the reaction tube of multiple parallel interconnections, reaction tube is configurable
5-20, each reaction tube inlet amount 20-50mL.
It is interconnected between the reaction tube of multiple parallel interconnections by bottom pipe, and anti-by law of connected vessels mean allocation
Answer object, while the discharge pipe as reaction product.
The reaction tube of multiple parallel interconnections is placed in thermostat water bath, and reaction temperature is can be controlled between -50 DEG C of room temperature.
A kind of continuous feed parallel reaction device using gold nanorods preparation synthesizes the gold nanorods of different draw ratios
Method, comprising the following steps:
(1) by 0.5mmol/L gold chloride 5mL-15mL and 0.2mol/L cetyl trimethylammonium bromide solution 5mL-
After 15mL mixing, freshly prepd 10mmol/mL ice sodium borohydride solution 0.6mL-1.8mL, after being sufficiently stirred, solution colour is added
The gold kind for becoming brown color, uses after standing 2h at room temperature；
(2) 0.1mol/L cetyl trimethylammonium bromide solution 0.25L-1L is added in reactant premixer, with
After sequentially add 0.01mol/L chlorauric acid solution 12.5mL-60mL, a certain amount of 0.01mol/L silver nitrate solution 1mL-24mL,
And 0.1mol/L quinol solution 17.5mL-70mL, it is eventually adding gold kind of 6mL-24mL, is sufficiently mixed by mechanical stirring
Uniformly；
(3) the uniformly mixed material of reacted object premixer is distributed flat to 5-20 25mL or 50mL by peristaltic pump
In row parallel connection reaction tube, feeding quantity 25-50mL in each reactor.Control water bath with thermostatic control temperature at 27 DEG C and maintains 12h to fill
Divide the growth for completing nanometer rods；
(4) after reaction, gold nanorods are collected by discharge port, and finished product is placed in -4 DEG C, made excessive in solution
Cetyl trimethylammonium bromide crystallize and be precipitated, and pass through low-speed centrifugal or come to remove extra cetyl trimethyl
Ammonium bromide, resulting gold nanorods can be placed in -4 DEG C of long-term preservations.
Beneficial effect
The present invention is uniformly controlled reaction temperature by continuous feed premixer, parallel connection reaction tube and thermostat water bath
Degree realizes different draw ratios, it is seen that the batch preparation for the gold nanorods that light to near-infrared absorption is continuously adjusted.This method passes through
Multiple reactors are parallel, successfully solve gold nanorods batch production when, directly amplify volume preparation there are heat and mass not
Uniformly, gold nanorods yield caused by easily leading to is lower, it is inhomogenous size easily occurs, and there are a large amount of spherical nanoparticle pairs
The problem of product.The unified pretreatment of reaction mass and unified temperature control, parallel connection reaction tube can amplify production volume, again
It can guarantee that liquid heat transfer is uniform in controlled volume, can get the gold nanorods of high quality.The device can be used for batch and prepare difference
Draw ratio, difference absorb the gold nanorods of (draw ratio is absorbed and is continuously adjusted from 650nm to 1060nm from 1.5 to 7), and highest is set
Meter theoretical yield is about 1L, and concentration is 0.1mg/mL gold nanorods, has significant amplification effect than conventional preparation volume 25mL, and
And have many advantages, such as good product consistency, size uniformity.
Feature in aspects above of the present invention can be freely combined within the scope of the invention, as long as the technology after combination
Scheme is fallen in connotation of the invention, and application method is not limited by its sequence.
Detailed description of the invention
Fig. 1 is the continuous feed parallel reaction device of gold nanorods preparation
(1. reactant premixers；2. mechanical stirring；3. peristaltic pump；4. feed pipe；5. reaction feed mouth；6. reaction
Pipe；7. reaction tube connecting pipe；8. discharge port；9. constant temperature waters pot)
Fig. 2 is the electromicroscopic photograph that 10 25mL continuous feed parallel reaction devices prepare gold nanorods, respectively absorption peak
710nm+10nm, draw ratio 3.0 (a)；Absorption peak 810nm+10nm (b), draw ratio 3.6；Absorption peak 1020+10nm, draw ratio
It is 5.8 (c)
Fig. 3 is the electromicroscopic photograph and ultra-violet absorption spectrum that 20 25mL continuous feed parallel reaction devices prepare gold nanorods
Figure, respectively absorption peak 710nm+10nm, draw ratio 3.0 (a)；Absorption peak 810nm+10nm, draw ratio 3.6 (b)；Absorption peak
1020+10nm, draw ratio are 5.8 (c)；There are different suctions slave visible region to near-infrared region prepared by parallel reaction device
Receive the uv absorption spectra (d) of Au nanometer rods
Fig. 4 is the electromicroscopic photograph that 20 50mL continuous feed parallel reaction devices prepare gold nanorods, respectively absorption peak
660nm+10nm, draw ratio 1.4 (a)；Absorption peak 865nm+10nm, draw ratio 4.0 (b)；Absorption peak 1050+10nm, draw ratio
It is 6.0 (c)
Specific embodiment:
In the following with reference to the drawings and specific embodiments, the present invention is furture elucidated, it should be understood that these embodiments are only used for
It is bright the present invention rather than limit the scope of the invention, after reading this disclosure, those skilled in the art is to of the invention
The modification of various equivalent forms falls within claims hereof limited range.
The continuous feed parallel reaction device that in the present invention prepared by gold nanorods by premixer, parallel connection reaction tube with
And thermostat water bath composition.Premixer has churned mechanically three necks glass round bottom reaction flask, and reactant is being pre-mixed wherein
It is conveyed and is assigned to after being mixed evenly and reacted in the reaction tube for being placed in multiple parallel interconnections of thermostat water bath.Reaction temperature
Degree can be controlled in room temperature between 50 DEG C.Device is as shown in Figure 1, include following part: 1. reactant premixers；2. machinery stirs
It mixes；3. peristaltic pump；4. feed pipe；5. reaction feed mouth；6. reaction tube；7. reaction tube connecting pipe；8. discharge port；9. constant temperature
Waters pot.
1,10 25mL continuous feed parallel reaction device of embodiment prepares gold nanorods
Preparation facilities is by 0.5L reactant premixer, 10 25mL parallel connection reaction tubes and 1 thermostat water bath
Composition.Preparation process is as follows:
(1) gold chloride (0.5mmol/L, 5mL) and cetyl trimethylammonium bromide solution (0.2mol/L, 5mL) is mixed
After conjunction, freshly prepd ice sodium borohydride solution (10mmol/mL, 0.6mL) is added, after being sufficiently stirred, solution colour becomes pale brown
The gold kind of color, uses after standing 2h at room temperature.
(2) in reactant premixer be added 0.1mol/L cetyl trimethylammonium bromide solution 0.25L, then according to
Secondary addition 0.01mol/L chlorauric acid solution 12.5mL, a certain amount of silver nitrate solution and 0.1mol/L quinol solution
17.5mL is eventually adding 6mL gold kind, is sufficiently mixed uniformly by mechanical stirring.
(3) the uniformly mixed material of reacted object premixer, is distributed anti-to 10 25mL parallel connections by peristaltic pump
Ying Guanzhong, feeding quantity 25mL in each reactor.Control water bath with thermostatic control temperature at 27 DEG C and maintains 12h sufficiently to complete nanometer rods
Growth.
(4) after reaction, gold nanorods are collected by discharge port, and finished product is placed in -4 DEG C, made excessive in solution
Cetyl trimethylammonium bromide crystallize and be precipitated, and pass through low-speed centrifugal or come to remove extra cetyl trimethyl
Ammonium bromide, resulting gold nanorods can be placed in -4 DEG C of long-term preservations.
250mL can be obtained by above-mentioned preparation facilities, concentration is 0.1mg/mL gold nanorods solution, yield about 90%.?
The gold nano size uniformity arrived, and different draw ratios, the Jenner that difference absorbs can be obtained by the amount of silver nitrate be added
Rice stick.As shown in Figure 2.Specifically, when 0.01mol/L silver nitrate be added is 2.5mL, morphological rules is obtained, absorption peak exists
710nm+10nm, the gold nanorods (a) that draw ratio is 3.0, be absorbed peak when 0.01mol/L silver nitrate is added and is 3.5mL
For 810nm+10nm, the gold nanorods (b) that draw ratio is 3.6, be absorbed peak when 0.01mol/L silver nitrate is added and is 5mL
For 1020+10nm, the gold nanorods (c) that draw ratio is 5.8.
2,20 25mL continuous feed parallel reaction devices of embodiment prepare gold nanorods
Preparation facilities is by 1L reactant premixer, 20 25mL parallel connection reaction tubes and 1 thermostat water bath group
At.Preparation process is as follows:
(1) by gold chloride (0.5mmol/L, 10mL) and cetyl trimethylammonium bromide solution (0.2mol/L, 10mL)
After mixing, freshly prepd ice sodium borohydride solution (10mmol/mL, 1.2mL) is added, after being sufficiently stirred, solution colour becomes palm fibre
The gold kind of yellow, uses after standing 2h at room temperature.
(2) in reactant premixer be added 0.1mol/L cetyl trimethylammonium bromide solution 0.5L, then according to
Secondary addition 0.01mol/L chlorauric acid solution 25mL, a certain amount of silver nitrate solution and 0.1mol/L quinol solution
35mL is eventually adding 12mL gold kind, is sufficiently mixed uniformly by mechanical stirring.
(3) the uniformly mixed material of reacted object premixer, is distributed anti-to 20 25mL parallel connections by peristaltic pump
Ying Guanzhong, feeding quantity 25mL in each reactor.Control water bath with thermostatic control temperature at 27 DEG C and maintains 12h sufficiently to complete nanometer rods
Growth.
(4) after reaction, gold nanorods are collected by discharge port, and finished product is placed in -4 DEG C, made excessive in solution
Cetyl trimethylammonium bromide crystallize and be precipitated, and pass through low-speed centrifugal or come to remove extra cetyl trimethyl
Ammonium bromide, resulting gold nanorods can be placed in -4 DEG C of long-term preservations.
Can be obtained 500mL by above-mentioned preparation facilities, concentration is 0.1mg/mL gold nanorods solution, yield about 90% with
On.Obtained gold nano size uniformity, and different draw ratios can be obtained by the amount of silver nitrate be added, difference absorbs
Gold nanorods.As shown in Figure 3.Specifically, when 0.01mol/L silver nitrate be added is 5mL, morphological rules is obtained, is absorbed
Peak is absorbed in 710nm+10nm, the gold nanorods (a) that draw ratio is 3.0 when 0.01mol/L silver nitrate is added and is 7mL
Peak is 810nm+10nm, and the gold nanorods (b) that draw ratio is 3.6 are absorbed when 0.01mol/L silver nitrate is added and is 10mL
Peak is 1020+10nm, the gold nanorods (c) that draw ratio is 5.8.Change 0.01mol/L silver nitrate additional amount 1mL to 12mL it
Between adjust, can be obtained from visible region to near-infrared region with different absorptions Au nanometer rods (d).
3,20 50mL continuous feed parallel reaction devices of embodiment prepare gold nanorods
Preparation facilities is by 2L reactant premixer, 20 50mL parallel connection reaction tubes and 1 thermostat water bath group
At.Preparation process is as follows:
(1) by gold chloride (0.5mmol/L, 15mL) and cetyl trimethylammonium bromide solution (0.2mol/L, 15mL)
After mixing, freshly prepd ice sodium borohydride solution (10mmol/mL, 1.8mL) is added, after being sufficiently stirred, solution colour becomes palm fibre
The gold kind of yellow, uses after standing 2h at room temperature.
(2) 0.1mol/L cetyl trimethylammonium bromide solution 1L is added in reactant premixer, then successively
0.01mol/L chlorauric acid solution 50mL, a certain amount of silver nitrate solution and 0.1mol/L quinol solution 70mL is added,
It is eventually adding 24mL gold kind, is sufficiently mixed uniformly by mechanical stirring.
(3) the uniformly mixed material of reacted object premixer, is distributed anti-to 20 50mL parallel connections by peristaltic pump
Ying Guanzhong, feeding quantity 50mL in each reactor.Control water bath with thermostatic control temperature at 27 DEG C and maintains 12h sufficiently to complete nanometer rods
Growth.
(4) after reaction, gold nanorods are collected by discharge port, and finished product is placed in -4 DEG C, made excessive in solution
Cetyl trimethylammonium bromide crystallize and be precipitated, and pass through low-speed centrifugal or come to remove extra cetyl trimethyl
Ammonium bromide, resulting gold nanorods can be placed in -4 DEG C of long-term preservations.
1L can be obtained by above-mentioned preparation facilities, concentration is 0.1mg/mL gold nanorods solution, yield about 90% or more.?
The gold nano size uniformity arrived, and different draw ratios, the Jenner that difference absorbs can be obtained by the amount of silver nitrate be added
Rice stick.As shown in Figure 4.Specifically, when 0.01mol/L silver nitrate be added is 6mL, morphological rules is obtained, absorption peak exists
660nm+10nm, the gold nanorods (a) that draw ratio is 1.4, the peak that is absorbed when 0.01mol/L silver nitrate is added and is 16mL are
865nm+10nm, the gold nanorods (b) that draw ratio is 4.0, the peak that is absorbed when 0.01mol/L silver nitrate is added and is 22mL are
1050+10nm, the gold nanorods (c) that draw ratio is 6.0.
Claims (2)
1. a kind of continuous feed parallel reaction device of gold nanorods preparation, it is characterised in that reactant mixes in premixer
Uniformly, it is then transported in the reaction tube of multiple parallel interconnections and is reacted by peristaltic pump；
Premixer with churned mechanically three necks glass round bottom reaction flask by forming, capacity 0.5-2L；
It is conveyed and is assigned to after reactant mixing and reacted in the reaction tube of multiple parallel interconnections, reaction tube configures 5-20
It is a, each reaction tube inlet amount 20-50mL；
It is interconnected between the reaction tube of multiple parallel interconnections by bottom pipe, and by law of connected vessels mean allocation reactant, together
The discharge pipe of Shi Zuowei reaction product；
The reaction tube of multiple parallel interconnections is placed in thermostat water bath, and reaction temperature controls between -50 DEG C of room temperature.
2. the side that a kind of continuous feed parallel reaction device using gold nanorods preparation synthesizes the gold nanorods of different draw ratios
Method, which comprises the following steps: (1) by 0.5mmol/L gold chloride 5mL-15mL and 0.2mol/L cetyl front three
After base ammonium bromide solution 5mL-15mL mixing, freshly prepd 10mmol/mL ice sodium borohydride solution 0.6mL-1.8mL is added, fills
After dividing stirring, solution colour becomes the gold kind of brown color, uses after standing 2h at room temperature；(2) in reactant premixer
0.1mol/L cetyl trimethylammonium bromide solution 0.25L-1L is added, then sequentially adds 0.01mol/L chlorauric acid solution
12.5mL-60mL, 0.01mol/L silver nitrate solution 1mL-24mL and 0.1mol/L quinol solution 17.5mL-70mL,
It is eventually adding gold kind of 6mL-24mL, is sufficiently mixed uniformly by mechanical stirring；(3) the uniformly mixed object of reacted object premixer
Material, is distributed by peristaltic pump into 5-20 25mL parallel connection reaction tube, feeding quantity 25mL in each reaction tube；Control constant temperature
Bath temperature is at 27 DEG C and maintains 12h sufficiently to complete the growth of nanometer rods；(4) after reaction, gold is collected by discharge port
Nanometer rods, and finished product is placed in -4 DEG C, excessive cetyl trimethylammonium bromide crystallization in solution is precipitated, and by low
Speed centrifugation is filtered to remove extra cetyl trimethylammonium bromide, and resulting gold nanorods are placed in -4 DEG C of long-term preservations.
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| CN100549244C (en) * | 2006-08-22 | 2009-10-14 | 国家纳米科学中心 | A kind of rectangle bimetallic nano rod with gold nucleus and palladium shell and preparation method thereof |
| CN103624266B (en) * | 2012-08-28 | 2015-11-11 | 北京化工大学 | One changes gold nanorods draw ratio and reduces its Cytotoxic preparation method |
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