CN207239157U - A kind of continuous device for preparing high solids content nano silver - Google Patents
A kind of continuous device for preparing high solids content nano silver Download PDFInfo
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- CN207239157U CN207239157U CN201721067330.8U CN201721067330U CN207239157U CN 207239157 U CN207239157 U CN 207239157U CN 201721067330 U CN201721067330 U CN 201721067330U CN 207239157 U CN207239157 U CN 207239157U
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Abstract
The utility model provides a kind of continuous device for preparing high solids content nano silver, it includes material container, impinging streams mixer, microwave reactor, ultrasound growth combination unit and ultrasonic agitation grower, the material container includes raw polyol container and multiple silver salt mixed liquor material containers, the raw polyol container, one silver salt mixed liquor material container is connected with the feed inlet of impinging streams mixer respectively, the discharge port of the impinging streams mixer is connected with microwave reactor, the outlet of the microwave reactor is connected with the entrance of ultrasound growth combination unit, the outlet of the ultrasound growth combination unit is connected with ultrasonic agitation grower.Using the technical solution of the utility model, with continuous, divisible forming core and growth course, the advantage such as precursor concentration is high, production efficiency is high, stability is good, controllability is strong, amplification is easy, particularly suitable for industrialization preparation uniformity and the good silver nano-grain of stability on a large scale.
Description
Technical field
The utility model belongs to metal nano material preparing technical field, more particularly to one kind continuously prepares high solids content and receives
The device of meter Yin.
Background technology
Silver nano-grain is drawn because of its unique physics, chemical property including conduction, heat conduction, sterilization and surface enhanced
All have broad application prospects in various fields including graceful, metal-enhanced fluorescence scattering, sensing, imaging etc..According to
The statistics of Project on Emerging Nanotechnologies issues in 2013, in 32 622 national the father-in-law
It is on sale that department shares 1814 kinds of commodity containing nano material, wherein the product containing silver nano material shares as many as 435 kinds, accounts for total
Several 24%.In recent years, as nano silver is gradually deep in the application and development of the frontiers such as sensing, imaging and flexible electronic device
Enter, and the nanosizing with the ag material used in conductive, heat conduction field, as be commercialized most ripe nano material it
One, the market prospects of nano silver material will be more wide.
The premise and material base of nano silver material large-scale commercial application necessarily high solids content nano-Ag particles
Prepare with scale.The advantages of preparation method of silver nano-grain can be divided into two kinds of Physical and chemical method at present, Physical is
Without solvent, impurity in products is few, but shortcoming is to be difficult to obtain the nano particle of a large amount of size uniforms, and energy in preparation process
Consumption is big, wastage of material is more, and equipment is complicated, expensive.And chemical method is more energy efficient, experiment condition is easier to control, prepared
Size and the pattern control of nano material are more effective, are to prepare the widest method of various Application of micron at present.System at present
The chemical method of standby nano-Ag particles mainly has hydrothermal synthesis method and photochemical method etc..
Hydrothermal synthesis method is in special closed reaction vessel, using water as reaction medium, is held by heating reaction
Device, creates a high temperature, the reaction environment of high pressure so that usual indissoluble or insoluble material are dissolved and recrystallized.Utilize this
Often crystallinity is high for the nano particle that method is prepared, good dispersion.But also there is some shortcomings, including reaction effect for hydro-thermal method
Not directly, growth information, the theoretical foundation that crystal can only be understood by the form and structure for generating crystal are perfect not enough, suitable
Relatively narrow, stronger to the dependence of production equipment etc. with scope, these factors limit the industrial applications of hydro-thermal method.
Photochemical method is in the presence of appropriate chemical substance, can be made by the laser irradiation for carrying out controllable to silver sol
It is standby go out a series of patterns it is silver nanostructured.Cardinal principle is exactly that the illumination of laser melts silver nano-grain surface so that table
Face atom rearranges, and a series of patterns are formed under the assistance of appropriate chemical substance.But the Yin Na for utilizing this method to prepare
Rice grain is often polydispersion, and pattern and dimensional homogeneity be not high.
But at present these methods also have one it is common the problem of, exactly in order to make final product that there is uniform shape
Looks and size, the concentration of presoma are usually no more than 0.1mol/L, cause the solid content of prepared nano silver colloidal sol very low, much
The needs of commercial applications are not reached.And these methods are all carried out using discrete mode, these discrete, nothings
Method splits forming core and growth course and the very low method of precursor concentration does not possess the condition of industrialized production nano silver,
A kind of necessary device that can continuously prepare high solids content silver nano-grain on a large scale of exploitation.
Utility model content
For above technical problem, the utility model discloses a kind of continuous device for preparing high solids content nano silver, tool
There are continuous, divisible forming core and growth course, precursor concentration height, production efficiency is high, stability is good, controllability is strong, amplification is held
The advantage such as easy, the silver nano-grain good particularly suitable for industrializing extensive preparation uniformity and stability.
In this regard, the technical solution adopted in the utility model is：
A kind of continuous device for preparing high solids content nano silver, it includes material container, impinging streams mixer, microwave reaction
Device, ultrasound growth combination unit and ultrasonic agitation grower, the material container includes raw polyol container and multiple silver salt mix
Close liquid material container, the raw polyol container, a silver salt mixed liquor material container feed inlet with impinging streams mixer respectively
Connection, the discharge port of the impinging streams mixer are connected with microwave reactor, and outlet and the ultrasound of the microwave reactor are grown
The entrance connection of combination unit, the outlet of the ultrasound growth combination unit are connected with ultrasonic agitation grower；Wherein, it is described
Ultrasound growth combination unit includes at least two ultrasonic growing element and is in series, and each ultrasound growing element includes one
A ultrasound reactor and a silver salt mixed liquor material container, each in ultrasound growing element, silver salt mixed liquor material container
Outlet and the entrance of ultrasound reactor connect, the ultrasound reactor of adjacent two ultrasonic growing elements is connected with each other；
Raw material in the raw polyol container, silver salt mixed liquor material container is pumped into impinging streams mixer and is mixed
Close, obtain silver-colored seed colloidal sol then into microwave heating reaction is carried out in microwave reactor, the silver-colored seed heated by microwave
Colloidal sol is entered in the ultrasound reactor of ultrasound growth combination unit, while the silver salt mixed liquor raw material of ultrasonic growing element holds
The silver salt mixed liquor of device, which is also entered in ultrasound reactor, makes silver-colored seed further grow up, in ultrasound growth combination unit,
Silver-colored seed is flowed into ultrasonic agitation grower after multistage grows into the particle size of requirement, in ultrasound and is stirred double
The lower further reaction of recast, completely consumes silver salt raw material；Wherein, the silver salt mixed liquor for silver salt, surfactant and
The mixed solution of water.
Wherein, the impinging streams mixer combines the advantage of percussion flow and static mixer, can be two kinds of volume flows
The liquid being not much different, is realized using opposite high-speed impact and quickly mixed, the liquid after impingement mix is further mixed by static state
Clutch realizes more uniform mass transfer mixing.The mass transfer requirement of different liquid materials, such as mixed effect, incorporation time, mixed flow
Amount etc., can realize simply by the means such as liquid flowing speed, increase caliber size, extension duct length are improved, therefore hit
Hitting stream mixer has mass transfer mixing velocity is fast, mixing efficiency is high, flow is big, amplification is easy, continuous, stable, controllability is strong etc.
A variety of advantages.Particularly, there is no any dynamical element in whole mixer, there is prominent energy-saving effect.The percussion flow
Mixer can use the conventional impinging streams mixer of the prior art.
The ultrasound growth combination unit is the ultrasound growth combination unit of ultrasonic growing element composition, can be gone here and there as needed
Join multiple ultrasonic growing elements, Argent grain seed is obtained needing the nano-Ag particles of size by multistage growth.The ultrasound
The liquid flowed through in its groove can be ultrasonically treated by ripple reactor, and the high temperature and pressure produced using acoustic cavitation accelerates anti-
The progress answered, makes seed further react the larger-sized nano particle of generation.The ultrasound reactor is preferably to pop one's head in
Formula ultrasound reactor.
The ultrasonic agitation grower can be ultrasonic agitation growth groove, that is, container or ultrasonic agitation is stirred by ultrasonic
Groove, the growth for nano-Ag particles；On the one hand the device can make inflow herein under the double action of ultrasound and stirring
Raw material fully reacts, and on the other hand also has good peptizaiton to nano-Ag particles.
Further, it is equipped with corundum glass screw pipe in the microwave reactor.In microwave reactor, liquid stream is from spiral
Flowed through in pipe, can by adjusting microwave power, the caliber of helix tube and length and liquid flowing speed by microwave fast heating
The heating-up temperature and soaking time of convenient control liquid stream, realize to liquid stream it is quick, efficient, be evenly heated.Silver salt fills herein
Put and react under the action of microwave with alcohols, the small size generated under the protection of surfactant uniformly, stable is silver-colored
Seed of the colloidal sol as next one-step growth.
The preparation of nano particle usually has forming core and two stages of growth, if carried out in same reaction system, forming core
Vie each other, interact with growth, nano particle is prepared in a reaction vessel, forming core and growth course are blended in one
Rise, while progress there is chemical reaction, the generating of new nucleus, the growing of existing nucleus, the short grained complicated mistake such as reunite
Journey, causes the problems such as final product particle size distribution is wide, pattern is uneven, stability and uniformity are poor.Such as existing skill
The nano silver preparation methods such as the reduction method of art, hydrothermal synthesis method, polyol process, photochemical method, are all in an individually reaction
In container, silver salt, reducing agent, solvent, surfactant are uniformly mixed by a certain percentage, at then heated, illumination, reflux
Reason makes silver salt reduce to obtain nano-Ag particles.As it can be seen that the use of these methods is all the intermittent mode of production, in same reaction
Forming core and growth course can not be split in container, the nano-Ag particles Size Distribution being prepared is wide, the uniformity between batch and
Stability is poor.More important is in order to make final product have uniform pattern and size, the concentration of silver salt used is all very
It is low, no more than 0.1M.The nano silver colloidal sol being prepared, certainly exists very low solid content, product particle size distribution width, shape
The problems such as looks are uneven, stability and uniformity are poor.
Using the technical solution of the utility model, fully utilize fast microwave heat temperature raising, sound cavitation effect of ultrasonic wave,
The advantage of the selective desalination of reverse osmosis membrane, using the silver salt presoma of high concentration, by splitting forming core and growth course, is realized
It is prepared by the continuous-stable of high solids content nano silver.Using the preparation facilities of the utility model, can in microwave reactor by
The characteristics of microwave firing rate is fast, homogeneous heating prepares largely stable silver nanoparticle seed, in subsequent probe type ultrasonic
Silver-colored seed growth is grown up under the acoustic cavitation effect of ultrasonic wave in reactor, and obtained by multiple ultrasonic growing elements of connecting
The silver nano-grain of desired size.
As further improvement of the utility model, it is single that the ultrasound growth combination unit includes 2 ~ 10 ultrasound growths
Member.
As further improvement of the utility model, in the ultrasound growing element, silver salt mixed liquor material container passes through
The entrance of peristaltic pump and ultrasound reactor connects.
As further improvement of the utility model, the continuous device for preparing high solids content nano silver further includes reverse osmosis
Permeable membrane desalter, enrichment facility, waste liquid tank and silver sol storage container, the outlet of the ultrasonic agitation grower with it is anti-
The entrance connection of permeable membrane desalter, the outlet of the reverse osmosis membrane desalter and the entrance of enrichment facility, waste liquid tank connect
Connect, the outlet of the enrichment facility is connected with silver sol storage container.Wherein, the reverse osmosis membrane desalter is reverse osmosis membrane
The desalter of composition, can selectivity removing nano silver colloidal sol in inorganic salts, realize product purification.Using this technical side
Case, the solution of obtained silver nano-grain remove impurity through reverse osmosis membrane desalter, and concentrated device obtains more high solids content
Nano silver colloidal sol；Purified nano silver colloidal sol removes unnecessary solvent by enrichment facility again, can prepare silver
Mass fraction is the nano silver colloidal sol of the high solids content of 30%-80%, is stored in silver sol holding tank, and waste liquid and impurity are collected
In reject chute.
As further improvement of the utility model, the enrichment facility for vacuum distillation apparatus, filtration apparatus or other
Enrichment facility.
As further improvement of the utility model, the raw polyol container, silver salt mixed liquor material container pass through respectively
The feed inlet of peristaltic pump and impinging streams mixer connects.
As further improvement of the utility model, agitating device is equipped with the material container.
The continuous device for preparing high solids content nano silver of above-mentioned technical proposal is a set of company for being suitable for industrialized production
The continuous quick reaction system for preparing nano silver.The reaction system has that mixing is fast, heat temperature raising speed is fast, continuous-stable, controllable
Property strong, amplification easily, the advantages of good energy-conserving effect etc. is prominent.Particularly the reaction system has very strong universality, Neng Goushi
The industrialized production for requiring high chemical liquid phase to react is passed for many reaction speeds soon, to three.
When carrying out continuously preparing high solids content nano silver using above device, it comprises the following steps：
Step S1, the mixed solution of silver salt, surfactant and water is poured into silver salt mixed liquor material container, is carried out
Stirring；
Step S2, introduces percussion flow by the raw material in raw polyol container, one of silver salt mixed liquor material container and mixes
Mixed in clutch；Preferably, the raw material in the raw polyol container, one of silver salt mixed liquor material container is isometric
It is flowed into impinging streams mixer and is mixed.
Step S3, when there is liquid to be flowed out from microwave reactor, opens microwave and is heated, heating time 0.5-
30min, heating-up temperature are 50-100 DEG C；
Step S4, when in the ultrasound reactor that the silver-colored seed colloidal sol in microwave reactor flows to ultrasound growth combination unit
When, ultrasonic wave is opened, and the silver salt mixed liquor raw material in the silver salt mixed liquor material container of the ultrasound growing element is incorporated into
Reacted in ultrasound reactor, silver-colored seed is grown up；
Step S5, in ultrasound growth combination unit, silver-colored seed is flowed into after multistage grows into the particle size of requirement
It is stirred by ultrasonic in growing container, is further reacted under the double action of ultrasound and stirring, completely consume silver salt raw material；
The product of step S6, step S5 generation is flowed into reverse osmosis membrane desalter, is flowed into after elimination reaction impurity dense
In compression apparatus, after concentration, the solid content of silver sol reaches 30%-80%, and the silver sol after concentrating flows into silver sol and deposits
High solids content nano silver is made in storage container.
Further, the silver salt is at least one of silver nitrate, silver acetate.
Further, the concentration of the silver salt in the silver salt mixed liquor is 0.1mol/L-5mol/L.
Further, the alcohol is one or more mixtures in methanol, ethanol, ethylene glycol, glycerine.
Further, the surfactant is aliphatic acid, Sodium Polyacrylate, polyacrylic acid, polyvinylpyrrolidone, the moon
In cinnamic acid, cellulose, citric acid, sodium citrate, oleyl amine, hydroxyethyl cellulose, hexadecyltrimethylammonium chloride one in or
A variety of mixtures；
Further, the water is distilled water or ultra-pure water.
Further, in step S2, the raw polyol container, the raw material of silver salt mixed liquor material container flow into percussion flow and mix
Flow velocity in clutch is 0.1-50L/min.
Further, in step S5, in the ultrasound growth combination unit, the salt mixed liquor in each ultrasound growing element
The flow velocity that the raw material flow of material container enters ultrasound reactor is 0.1-30L/min.
Compared with prior art, the beneficial effects of the utility model are：
First, using the technical solution of the utility model, fully utilize that microwave heat temperature raising is fast, the acoustic cavitation of ultrasonic wave
The advantage of effect etc. is by the continuous mode of production, using the silver salt presoma of high concentration, by splitting forming core and growth course,
Prepared by the continuous-stable for realizing high solids content nano silver, it is with continuous, divisible forming core and growth course, precursor concentration
The advantages such as height, production efficiency are high, stability is good, controllability is strong, amplification is easy, particularly suitable for industrializing extensive prepare unanimously
Property and the good silver nano-grain of stability.
Second, the technical solution of the utility model is with technique is simple, operation controlling is strong, nano-Ag particles Size Distribution
Narrow, a variety of advantages such as product property is stable, easy volume production, energy consumption are low, have very strong Industrialized conditions and prospect.
3rd, the reaction system and preparation method of the technical solution of the utility model also have very strong universality, also fit
For other similar nano materials that wet chemistry reaction can be used to prepare, include but not limited to nano metal gold, nickel, copper etc. and receive
The preparation of rice grain.The silver nano-grain prepared using the device of the utility model have size uniform, pattern uniformly, size
Adjustable, the characteristics of solid content is high, impurity is few.
Brief description of the drawings
Fig. 1 is a kind of structure diagram of the continuous device for preparing high solids content nano silver of the utility model embodiment 1.
Fig. 2 is the structure diagram of ultrasonic growing element in the utility model embodiment 1.
Fig. 3 is the TEM figures of the silver nano-grain prepared in the embodiment of the present invention 2.
Fig. 4 is the TEM figures of the silver nano-grain prepared in the embodiment of the present invention 3.
Fig. 5 is the TEM figures of the silver nano-grain prepared in the embodiment of the present invention 4.
Reference numeral includes：
1- raw polyol dissolving tanks, the first peristaltic pumps of 2-, 3- impinging streams mixers, the second peristaltic pumps of 4-, 5- microwave reactors,
6- the first silver salt mixed liquor dissolution of raw material grooves, 7- probe type ultrasonic reactors, the 3rd peristaltic pumps of 8-, 9- the second silver salt mixed liquors
Dissolution of raw material groove, 10- ultrasound growth combination units, 11- ultrasonic agitation growth grooves, 12- reverse osmosis membrane desalters, 13- concentrations
Device, 14- reject chutes, 15- silver sol holding tanks.
Embodiment
The preferably embodiment of the utility model is described in further detail below.
Embodiment 1
As depicted in figs. 1 and 2, a kind of continuous device for preparing high solids content nano silver, it includes material container, percussion flow
It is mixer 3, microwave reactor 5, ultrasound growth combination unit 10, ultrasonic agitation growth groove 11, reverse osmosis membrane desalter 12, dense
Compression apparatus 13, waste liquid tank 14 and silver sol holding tank 15, the material container includes raw polyol dissolving tank 1 and multiple silver salt mix
Liquid material container is closed, the silver salt mixed liquor material container includes at least the first silver salt mixed liquor dissolution of raw material groove 6 and the second silver medal
Salt mixed liquor dissolution of raw material groove 9；The raw polyol dissolving tank 1 is connected by the feed inlet of the first peristaltic pump 2 and impinging streams mixer 3
Connect, the first silver salt mixed liquor raw material tank is connected by the second peristaltic pump 4 with the feed inlet of impinging streams mixer 3, described to hit
The discharge port for hitting stream mixer 3 is connected with microwave reactor 5, and outlet and the ultrasound growth of the microwave reactor 5 combine the unit
10 entrance connection, the outlet of the ultrasound growth combination unit 10 are connected with ultrasonic agitation growth groove 11.The ultrasonic agitation
Growth groove 11 outlet be connected with the entrance of reverse osmosis membrane desalter 12, the outlet of the reverse osmosis membrane desalter 12 with it is dense
Entrance, the waste liquid tank 14 of compression apparatus 13 connect, and the outlet of the enrichment facility 13 is connected with silver sol holding tank 15.
As depicted in figs. 1 and 2, the ultrasound growth combination unit 10 includes at least two ultrasonic growing element string
Connection forms, and each ultrasound growing element is by a probe type ultrasonic reactor 7 and a silver salt mixed liquor material container i.e. the
Disilver salt mixed liquor dissolution of raw material groove 9 forms, and in each ultrasound growing element, the second silver salt mixed liquor dissolution of raw material groove 9 goes out
Mouth is connected by the 3rd peristaltic pump 8 with the entrance of probe type ultrasonic reactor 7, the probe of adjacent two ultrasonic growing elements
Formula ultrasound reactor 7 is connected with each other.Agitating device is equipped with the material container, corundum is equipped with the microwave reactor 5
Glass screw pipe；The enrichment facility 13 is vacuum distillation apparatus, filtration apparatus or other enrichment facilities.
Preferably, the ultrasound growth combination unit 10 includes 2 ~ 10 ultrasonic growing elements.The ultrasound growing element
In, each second silver salt mixed liquor dissolution of raw material groove 9 is connected by peristaltic pump with the entrance of probe type ultrasonic reactor 7.
Each device links together as shown in Figure 1 by more than, just constitutes and a set of is suitable for the continuous fast of industrialized production
Speed prepares the reaction system of nano silver.
The continuous preparation for preparing high solids content nano silver is carried out using above device, is comprised the following steps：
Step S1, the first silver salt mixed liquor dissolution of raw material groove 6 is poured into by the mixed solution of silver salt, surfactant and water
In the second silver salt mixed liquor dissolution of raw material groove 9, start blender and be thoroughly mixed.The silver salt is silver nitrate, acetic acid
One kind in silver, its concentration range is between 0.1mol/L-5mol/L.The alcohol be methanol, ethanol, ethylene glycol, propane diols,
One or more in butanediol, hexylene glycol, neopentyl glycol, Diethylene Glycol, dipropylene glycol, glycerine, polyethylene glycol
Mixture；Surfactant is aliphatic acid, Sodium Polyacrylate, polyacrylic acid, polyvinylpyrrolidone, laurate, cellulose, lemon
In lemon acid, sodium citrate, oleyl amine, hydroxyethyl cellulose, hexadecyltrimethylammonium chloride one in or a variety of mixtures, it is affiliated
Water be distilled water or ultra-pure water；
Step S2, opens the first peristaltic pump 2, the second peristaltic pump 4 by raw polyol dissolving tank 1, the first silver salt mixed liquor raw material
Raw material in dissolving tank 6 is incorporated into impinging streams mixer 3 and is mixed, and realizes the Quick uniform mixing of material.Raw polyol is molten
The fluid flow control range in groove 1, the first silver salt mixed liquor dissolution of raw material groove 6 is solved in 0.1-50L/min；
Step S3, when there is liquid to be flowed out from microwave reactor 5, opens microwave and is heated, heating time 0.5-
30min, heating-up temperature are 50-100 DEG C；
Step S4, when the silver-colored seed colloidal sol in microwave reactor 5 flows to the probe type ultrasonic of ultrasound growth combination unit 10
When in ripple reactor 7, ultrasonic wave is opened, and it is former by the second silver salt mixed liquor of the ultrasound growing element to open the 3rd peristaltic pump 8
Expect the silver salt mixed liquor raw material in dissolving tank 9（The concentration of silver salt is 0.1mol/L-5mol/L）It is anti-to be incorporated into probe type ultrasonic
Answer and reacted in device 7, silver-colored seed is grown up；
Step S5, in ultrasound growth combination unit 10, silver-colored seed flows into after multistage grows into the particle size of requirement
Into ultrasonic agitation growing container, further reacted under the double action of ultrasound and stirring, completely consume silver salt raw material；
The product of step S6, step S5 generation is flowed into reverse osmosis membrane desalter 12, is flowed into after elimination reaction impurity
In enrichment facility 13, after concentration, the solid content of silver sol reaches 30%-80%, and it is molten that the silver sol after concentrating flows into silver
High solids content nano silver is made in glue holding tank 15.
Embodiment 2
The continuous reaction system and method provided using embodiment 1 prepares nano silver, comprises the following steps：
A certain amount of ethylene glycol is placed in raw polyol dissolving tank 1, a certain amount of silver nitrate, ultra-pure water and polyethylene pyrrole
Pyrrolidone is added to every in the first silver salt mixed liquor dissolution of raw material groove 6, ultrasound growth combination unit 10 according to a certain percentage
In second silver salt mixed liquor dissolution of raw material groove 9 of a ultrasound growing element, stirring 30min makes it fully dissolve mixing；Wherein,
The concentration of the silver nitrate of one silver salt mixed liquor dissolution of raw material groove 6 is 0.5mol/L.It is each super in ultrasound growth combination unit 10
The concentration of silver nitrate in second silver salt mixed liquor dissolution of raw material groove 9 of sound growing element is 0.1mol/L.
The first peristaltic pump 2 and the second peristaltic pump 4 are opened, sets flow as 1L/min, makes 1 and first silver medal of raw polyol dissolving tank
Mixing liquid in salt mixed liquor dissolution of raw material groove 6 is flowed into impinging streams mixer 3 in equal volume, mixes material Quick uniform
Close.
When there is liquid to be flowed out from microwave reactor 5, microwave heating is opened at once, material is in microwave reactor 5
Heating time is set as 10min, and temperature control is at 60 DEG C.
When the silver-colored seed colloidal sol in microwave reactor 5 is flowed in probe type ultrasonic reactor 7, ultrasonic wave and the are opened
Three peristaltic pumps 8, with 0.5L/min by the silver nitrate in the second silver salt mixed liquor dissolution of raw material groove 9（0.1mol/L）Solution introducing,
Silver-colored seed is set to grow up.The silver sol grown up in probe type ultrasonic reactor 7 enters the probe of next ultrasonic growing element
In formula ultrasound reactor 7, ultrasonic wave and peristaltic pump are opened, with the flow velocity of same 0.5L/min by the second silver salt mixed liquor raw material
Silver nitrate solution in dissolving tank 9（0.1mol/L）Introduce, silver-colored seed is further grown up.In this way, grow combination dress in ultrasound
In putting 10, after ultrasonic growing element of the silver-colored seed by 3 series connection grows into required particle size, ultrasonic agitation life is flowed into
In elongated slot, further react runs out of silver nitrate under the double action of ultrasound and stirring.The product ultimately generated flows into instead
In permeable membrane desalter 12, it is flowed into after elimination reaction impurity in enrichment facility 13.After concentration, silver sol flows into silver
In colloidal sol holding tank 15, final silver sol is obtained, Argent grain size is in 20nm or so, solid content 30%.Fig. 3 is this example
The silver nano-grain TEM figures of preparation, it can be seen that the uniform particle sizes of the silver nano-grain obtained.
Embodiment 3
The continuous reaction system and method provided using embodiment 1 prepares nano silver, comprises the following steps：
A certain amount of ethylene glycol and ethanol are placed in raw polyol dissolving tank 1, a certain amount of silver acetate, ultra-pure water and lemon
Lemon acid trisodium is added in the first silver salt mixed liquor dissolution of raw material groove 6, ultrasound growth combination unit 10 according to a certain percentage
In second silver salt mixed liquor dissolution of raw material groove 9 of each ultrasound growing element, stirring 30min makes it fully dissolve mixing.Wherein,
The concentration of the silver acetate of first silver salt mixed liquor dissolution of raw material groove 6 is 2mol/L.It is each super in ultrasound growth combination unit 10
The concentration of silver acetate in second silver salt mixed liquor dissolution of raw material groove 9 of sound growing element is 1mol/L.
The first peristaltic pump 2 and the second peristaltic pump 4 are opened, sets flow as 6L/min, makes 1 and first silver medal of raw polyol dissolving tank
Mixing liquid in salt mixed liquor dissolution of raw material groove 6 is flowed into impinging streams mixer 3 in equal volume, mixes material Quick uniform
Close.
When there is liquid to be flowed out from microwave reactor 5, microwave heating is opened at once, material is in microwave reactor 5
Heating time is set as 10min, and temperature control is at 70 DEG C.
When the silver-colored seed colloidal sol in microwave reactor 5 is flowed in probe type ultrasonic reactor 7, ultrasonic wave and the are opened
Three peristaltic pumps 8, with 2L/min by the silver acetate in the second silver salt mixed liquor dissolution of raw material groove 9（1mol/L）Solution introduces, makes silver
Seed is grown up.The sonde-type that the silver sol grown up in probe type ultrasonic reactor 7 enters next ultrasonic growing element surpasses
In sound wave reactor 7, ultrasonic wave and peristaltic pump are opened, with the flow velocity of same 2L/min by the second silver salt mixed liquor dissolution of raw material groove
Silver acetate solution in 9（1mol/L）Introduce, silver-colored seed is further grown up.In the example, the ultrasound growth combination unit 10
Include 5 ultrasonic growing elements.Ultrasound growth combination unit 10 in, silver-colored seed after 5 grades grow into required particle size,
It is flowed into ultrasonic agitation growth groove, silver acetate is run out of in ultrasound and further reaction under the double action of stirring.Finally
The product of generation is flowed into reverse osmosis membrane desalter 12, is flowed into after elimination reaction impurity in enrichment facility 13.By concentration
Afterwards, silver sol is flowed into silver sol holding tank 1518, obtains final silver sol, and Argent grain size is in 40nm or so, admittedly contain
Measure as 50%.Fig. 4 is the TEM figures of silver nano-grain prepared by this example, it can be seen that the particle diameter of the silver nano-grain obtained
Uniformly.
Embodiment 4
The continuous reaction system and method provided using embodiment 1 prepares nano silver, comprises the following steps：
A certain amount of glycerine is placed in raw polyol dissolving tank 1, a certain amount of silver nitrate, ultra-pure water and ethoxy are fine
Dimension element is added to each in the first silver salt mixed liquor dissolution of raw material groove 6, ultrasound growth combination unit 10 according to a certain percentage
In second silver salt mixed liquor dissolution of raw material groove 9 of ultrasonic growing element, stirring 30min makes it fully dissolve mixing.Wherein, first
The concentration of the silver nitrate of silver salt mixed liquor dissolution of raw material groove 6 is 3mol/L.Each ultrasound in ultrasound growth combination unit 10 is raw
The concentration of silver nitrate in second silver salt mixed liquor dissolution of raw material groove 9 of long unit is 1.5mol/L.
The first peristaltic pump 2 and the second peristaltic pump 4 are opened, sets flow as 30L/min, makes raw polyol dissolving tank 1 and first
Mixing liquid in silver salt mixed liquor dissolution of raw material groove 6 is flowed into impinging streams mixer 3 in equal volume, mixes material Quick uniform
Close.
When there is liquid to be flowed out from microwave reactor 5, microwave heating is opened at once, material is in microwave reactor 5
Heating time is set as 10min, and temperature control is at 80 DEG C；
When the silver-colored seed colloidal sol in microwave reactor 5 is flowed in probe type ultrasonic reactor 7, ultrasonic wave and the are opened
Three peristaltic pumps 8, with 10L/min by the silver nitrate solution in the second silver salt mixed liquor dissolution of raw material groove 9（1.5mol/L）Solution draws
Enter, silver-colored seed is grown up.The silver sol grown up in probe type ultrasonic reactor 7 enters the spy of next ultrasonic growing element
In head type ultrasonic ripple reactor 7, ultrasonic wave and peristaltic pump are opened, it is with the flow velocity of same 10L/min that the second silver salt mixed liquor is former
Expect the silver nitrate solution in dissolving tank 9（1.5mol/L）Introduce, silver-colored seed is further grown up.Ultrasound growth combination unit 10
Include 6 ultrasonic growing elements.Ultrasound growth combination unit 10 in, silver-colored seed after 6 grades grow into required particle size,
It is flowed into ultrasonic agitation growth groove, silver acetate is run out of in ultrasound and further reaction under the double action of stirring.Finally
The product of generation is flowed into reverse osmosis membrane desalter 12, is flowed into after elimination reaction impurity in enrichment facility 13.By concentration
Afterwards, silver sol is flowed into stirring holding tank, obtains final silver sol, Argent grain size is in 110nm or so, solid content
70%.Fig. 5 is silver nano-grain TEM figures prepared by this example, from figure 5 it can be seen that using this technical solution, the silver nanoparticle of acquisition
The uniform particle sizes of grain.
Above content is to combine specific preferred embodiment further detailed description of the utility model, it is impossible to
Assert that the specific implementation of the utility model is confined to these explanations.For the ordinary skill of the utility model technical field
For personnel, without departing from the concept of the premise utility, some simple deduction or replace can also be made, should all be regarded
To belong to the scope of protection of the utility model.
Claims (8)
- A kind of 1. continuous device for preparing high solids content nano silver, it is characterised in that：It includes material container, percussion flow mixing Device, microwave reactor, ultrasound growth combination unit and ultrasonic agitation grower, the material container include raw polyol container and Multiple silver salt mixed liquor material containers, the raw polyol container, a silver salt mixed liquor material container are mixed with percussion flow respectively The feed inlet connection of device, the discharge port of the impinging streams mixer are connected with microwave reactor, the outlet of the microwave reactor It is connected with the entrance of ultrasound growth combination unit, outlet and the ultrasonic agitation grower of the ultrasound growth combination unit connect Connect；Wherein, the ultrasound growth combination unit includes at least two ultrasonic growing element and is in series, each ultrasound life Long unit includes a ultrasound reactor and a silver salt mixed liquor material container, and in each ultrasound growing element, silver salt mixes Close the outlet of liquid material container and the entrance of ultrasound reactor connects, the ultrasonic response of adjacent two ultrasonic growing elements Device is connected with each other.
- 2. the continuous device for preparing high solids content nano silver according to claim 1, it is characterised in that：The ultrasound growth Combination unit includes 2 ~ 10 ultrasonic growing elements.
- 3. the continuous device for preparing high solids content nano silver according to claim 1, it is characterised in that：The ultrasound growth In unit, silver salt mixed liquor material container is connected by the entrance of peristaltic pump and ultrasound reactor.
- 4. the continuous device for preparing high solids content nano silver according to claim 3, it is characterised in that：It further includes reverse osmosis Permeable membrane desalter, enrichment facility, waste liquid tank and silver sol storage container, the outlet of the ultrasonic agitation grower with it is anti- The entrance connection of permeable membrane desalter, the outlet of the reverse osmosis membrane desalter and the entrance of enrichment facility, waste liquid tank connect Connect, the outlet of the enrichment facility is connected with silver sol storage container.
- 5. the continuous device for preparing high solids content nano silver according to claim 4, it is characterised in that：The raw polyol holds Device, silver salt mixed liquor material container are connected by the feed inlet of peristaltic pump and impinging streams mixer respectively.
- 6. the continuous device for preparing high solids content nano silver according to claim 5, it is characterised in that：The material container It is interior to be equipped with agitating device.
- 7. the continuous device for preparing high solids content nano silver according to claim 6, it is characterised in that：The microwave reaction Corundum glass screw pipe is equipped with device.
- 8. the continuous device for preparing high solids content nano silver according to claim 7, it is characterised in that：The enrichment facility For vacuum distillation apparatus, filtration apparatus or other enrichment facilities.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201721067330.8U CN207239157U (en) | 2017-08-24 | 2017-08-24 | A kind of continuous device for preparing high solids content nano silver |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201721067330.8U CN207239157U (en) | 2017-08-24 | 2017-08-24 | A kind of continuous device for preparing high solids content nano silver |
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| CN207239157U true CN207239157U (en) | 2018-04-17 |
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| CN201721067330.8U Active CN207239157U (en) | 2017-08-24 | 2017-08-24 | A kind of continuous device for preparing high solids content nano silver |
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| Country | Link |
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| CN (1) | CN207239157U (en) |
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Address after: 518000 Shenzhen Nanshan District Guangdong Province Yuehai Street 10 High-tech Nanjiu Road Shenzhen Bay Science and Technology Eco-Park 10 Skirt Building 5 Floor 14-A Patentee after: SHENZHEN GLOR NEW MATERIALS TECHNOLOGY Co.,Ltd. Address before: Room 201, Building A, Qianhai Road, Qianhai Shenzhen-Hong Kong Cooperation Zone, Shenzhen, Guangdong 518000 Patentee before: SHENZHEN GELUO OPTOELECTRONIC CO.,LTD. |
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Effective date of registration: 20221230 Address after: 518000 610b, South Block, 6th floor, Tairan Cangsong building, Tairan 6th Road, Tian'an community, Shatou street, Futian District, Shenzhen, Guangdong Patentee after: Shenzhen Yuanchi 3D Technology Co.,Ltd. Address before: 518000 Shenzhen Nanshan District Guangdong Province Yuehai Street 10 High-tech Nanjiu Road Shenzhen Bay Science and Technology Eco-Park 10 Skirt Building 5 Floor 14-A Patentee before: SHENZHEN GLOR NEW MATERIALS TECHNOLOGY Co.,Ltd. |