CN104984692A - Series connection apparatus for industrial large-batch stable preparation of quantum dots - Google Patents

Series connection apparatus for industrial large-batch stable preparation of quantum dots Download PDF

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Publication number
CN104984692A
CN104984692A CN201510087281.3A CN201510087281A CN104984692A CN 104984692 A CN104984692 A CN 104984692A CN 201510087281 A CN201510087281 A CN 201510087281A CN 104984692 A CN104984692 A CN 104984692A
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high pressure
quantum dot
ultra
maker
series connection
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CN201510087281.3A
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王建伟
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Fujian Yuanding New Material Technology Co., Ltd.
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王建伟
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Abstract

The present invention provides a series connection apparatus for industrial large-batch stable preparation of quantum dots, wherein the series connection apparatus comprises a plurality of ultra-high pressure reactors, the interfaces on both ends of all ultra-high pressure reactors are sequentially connected in series by connecting ultra-high pressure pipelines in a head-to-tail manner so as to form the tandem continuous production type equipment. According to the present invention, the technology of the use of the physical law enforcement intervention tissue growth mode of the ultra-high pressure mass transfer reaction to industrially prepare the quantum dots is used, such that the problem that the heat conduction and the mass transfer are changed during the quantum dot production in the heat reaction self-organization growth mode so as to cause the reaction result deviation is completely solved, the productivity, the quality, the product grade and the economic benefits are substantially improved, and the industrial production can be completely achieved.

Description

A kind of industrial mass stablizes the tandem arrangement preparing quantum dot
Technical field
The present invention relates to a kind of technology of superelevation pressure mass transfer reaction preparation of industrialization quantum dot, especially a kind of industrialization superelevation pressure mass transfer reaction stable mass prepares the tandem arrangement of quantum dot.
Background technology
Quantum dot, i.e. semiconductor nano.At the nanometer semiconductor structure that conduction band electron, valence band hole and exciton are held onto on three direction in spaces.Quantum dot, electron motion is all restricted at three dimensions, therefore sometimes referred to as " artificial atom ", " superlattices ", " hyperonic atom " or " quantum dot atom ".The size of quantum dot in all three dimensions usually than and form quantum dot material in exciton size little, such exciton is all subject to strong confinement in all three dimensions, thus shows character distinct with corresponding body phase material.The special optical property of quantum dot makes it play effect greatly in biochemistry, cell biology, genomics, proteomics, drug screening, photonic crystal, Eurytrema coelomatium, light seizure, laser, solar energy, display, illumination, the fields such as social economy such as dual-use.
The research of quantum dot is the science of forefront in the world today, and the growth of quantum dot and character become the focus of current whole world research, and its preparation mainly contains physical method and chemical method, is chemically main.Current, the soft chemical preparation process of quantum dot has two kinds: a kind of is adopt the method for colloid chemistry to synthesize in organic system, and another kind synthesizes in aqueous.The method preparing quantum dot the most frequently used is at present " thermal response self-organizing growth mode ".But the production of above-mentioned quantum dot is still based on the method in laboratory, and output is few, and general each reaction volume, at 5 ~ 50mL, can only meet at most the test of some laboratory research ranks and the needs of application test.In mass production, these conventional methods all encounter insoluble bottleneck: when carrying out " amplification " volume production, along with the expansion of reaction volume, in reaction system all can there is great change in the situation of heat transfer and reactant diffusion, cause reaction result generation deviation, the waste product often obtained or properties of product instability.Therefore, the achievement obtained in most of laboratory can not be converted into actual application, and can only rest on the stage of laboratory research, and the needs from suitability for industrialized production are far apart.
In view of this, inventor carries out application experiment in large quantities, and the suitability for industrialized production with regard to quantum dot conducts a research, and has this case to produce eventually.
Summary of the invention
The object of the present invention is to provide a kind of industrial mass to stablize the tandem arrangement preparing quantum dot, it has, and process matching be simple, apparatus compact conformation, easy for installation, stable performance, the feature such as multi-functional.
In order to reach above-mentioned purpose, the solution that the present invention adopts is:
Industrial mass stablizes the tandem arrangement preparing quantum dot, and its reaction unit is superelevation pressure mass transfer reaction device.
In order to enhance productivity, minimizing equipment takes up an area space, described superelevation pressure mass transfer reaction device is made up of some super high pressure reactors, and all super high pressure reactor two end interface ultrahigh pressure pipelines are end to end to be sequentially connected in series, and forms tandem continuous seepage type equipment.
Described all super high pressure reactors are arranged in a containment housing, install circulates temperature controlled device and regulate temperature in containment housing.
The super high pressure bend of described superelevation pressure mass transfer reaction device end connects a maker by air pulsing switch valve, to complete shaping and the emulsification of quantum dot mother liquor.
Described maker is arranged on the casing of an injection cooling fluid capable of circulation, and cooling fluid carries out pressure cooling to maker, controls break-make between maker and reactor by air pulsing switch valve.
The root of the present inventor's analysis conventional preparation method problem, have developed this superelevation pressure mass transfer reaction " Physical forces intervention to organize growth pattern " preparation of industrialization technology of quantum dots, its Core Superiority is that this is the strong mass transfer reaction process of a kind of gravity+speed+energy (G/S/J), produces superpower pressure effect, pulsation effect, void effect and uniform microcosmic melange effect under G/S/J drives.During work, reactant is constantly imported into super-pressure reaction zone, fully reacted, be then exported after maker shaping and emulsification in the strong mass transport process of super energy that reactant is produced by above-mentioned comprehensive effect, be quantum dot mother liquor, then purified by next process.This superelevation pressure mass transfer reaction device prepares quantum dot, thorough solution thermal response self-organizing growth mode heat transfer and reactant diffusion in volume production change and cause the offset issue of reaction result, substantially increase production capacity, quality, product specification and economic benefit, and can suitability for industrialized production be realized completely.
Below in conjunction with drawings and the specific embodiments, the present invention is described in further details.
Accompanying drawing explanation
Fig. 1 is process chart of the present invention;
Fig. 2 is structural representation of the present invention.
Detailed description of the invention
As shown in Figure 1, be process of the present invention, the steps include:
Step one, quantum dot raw material are carried out proportioning by solid, liquid ratio (ratio), this proportioning belongs to prior art; Raw material good for proportioning is carried out micronization process and emulsifying;
Step 2, the raw emulsion that will handle well, rise to 280Mpa with 280Mpa(from zero) pressure import super high pressure reactor, voltage stabilizing 1-10 minute;
In order to its catalytic reaction process can be accelerated further, in this step 2, heating system can be utilized to heat super high pressure reactor, temperature 250 ~ 300 DEG C;
Step 3, again pressure is increased be depressed into 350Mpa(and rise to 350Mpa from 280Mpa) after, voltage stabilizing 1-10 minute;
Step 4 and then pressure is increased be depressed into 620Mpa(and rise to 620Mpa from 350Mpa) after, pressurize, after 1 ~ 30 minute, derives generated quantum dot mother liquor.In order to improve its solvability and rate constant sooner, can continue to raise pressure, until the proof pressure of equipment;
The quantum dot mother liquor that this step 4 derives carries out shaping and emulsification through maker, and product crystalline form size can be made so more to optimize;
Step 5, purification step five quantum mother liquor.
As shown in Figure 2, a kind of industrial mass that the present invention discloses stablizes the tandem arrangement preparing quantum dot, super high pressure reactor 1 that is anticorrosive by several, high strength alloy steel forms (needing changeable depending on design production capacity and reaction time), more super high pressure reactor 1(can arrange and be arranged side by side) be arranged in a containment housing 2, control temperature control fluid (conduction oil) with circulates temperature controlled device in containment housing 2 to go out from temperature control fluid import 9 and then by temperature control fluid outlet 10, regulate temperature required.Each super high pressure reactor 1 liang of end interface ultrahigh pressure pipeline 3 is sequentially connected in series by headtotail, forms tandem continuous seepage type equipment.Whole device end pipeline connects a maker 4 by air pulsing switch valve 5, maker 4 is arranged on one and is equipped with in the casing 6 of circulating cooling liquid, circulating cooling liquid goes out from cooling liquid inlet 11 and then by cooling liquid outlet 12, carries out pressure cooling to maker 4.Maker 4 possesses shaping and emulsification function, and it is controlled by air pulsing switch valve 5, is mainly used in reacted material by deriving after micronization, shaping and emulsification, its crystalline form is more optimized.The superelevation pressure mass transfer reaction become by these component combinations above-mentioned prepares quantum point apparatus, super high pressure reactor 1 is imported from raw emulsion pipeline 7 under the hyperpressure up to 620 Mpa, the super high pressure reactor 1 be together in series is filled with one by one, under the strong mass transfer of the pressure effect of super-pressure, pulsation effect, void effect and uniform microcosmic mixing effect, impel raw emulsion to produce reaction in-situ in super high pressure reactor 1, be generated as quantum dot mother liquor.Then, by deriving after maker 4 shaping and emulsification, its crystalline form size is more optimized.The quantum dot mother liquor that being exported pipe 8 derives enters next procedure and purifies.

Claims (4)

1. an industrial mass stablizes the tandem arrangement preparing quantum dot, it is characterized in that: be made up of some super high pressure reactors, all super high pressure reactor two end interface ultrahigh pressure pipelines are end to end to be sequentially connected in series, and forms tandem continuous seepage type equipment.
2. a kind of industrial mass stablizes the tandem arrangement preparing quantum dot as claimed in claim 1, it is characterized in that: described all super high pressure reactors are arranged in a containment housing, installs the circulates temperature controlled device for regulating temperature in containment housing.
3. a kind of industrial mass stablizes the tandem arrangement preparing quantum dot as claimed in claim 1, it is characterized in that: the ultrahigh pressure pipeline of described superelevation pressure mass transfer reaction device end connects a maker by air pulsing switch valve.
4. a kind of industrial mass stablizes the tandem arrangement preparing quantum dot as claimed in claim 3, it is characterized in that: described maker is arranged on the casing of an injection cooling fluid capable of circulation, controls break-make between maker and reactor by air pulsing switch valve.
CN201510087281.3A 2015-02-25 2015-02-25 Series connection apparatus for industrial large-batch stable preparation of quantum dots Pending CN104984692A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1776284A (en) * 2005-11-25 2006-05-24 许宏 Pressure and ultrahigh pressure generating method and device
CN1944266A (en) * 2006-10-25 2007-04-11 国家纳米技术与工程研究院 Method for preparing zinc sulfide nano crystal particles using high pressure fluid mill
US20090162658A1 (en) * 2007-12-13 2009-06-25 Sud Chemie Ag Process for the preparation of nanocrystalline hydrotalcite compounds
CN102076405A (en) * 2008-04-28 2011-05-25 南吉耐克斯纳米技术股份有限公司 Instrument and process for nanoparticles production in continuous flow mode
CN103820846A (en) * 2014-02-17 2014-05-28 中国科学技术大学 Multifunctional device based on hydrothermal method for growing nano materials
WO2014153570A2 (en) * 2013-03-15 2014-09-25 Transtar Group, Ltd New and improved system for processing various chemicals and materials
CN204656495U (en) * 2015-02-25 2015-09-23 王建伟 A kind of industrial mass stablizes the tandem arrangement preparing quantum dot

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1776284A (en) * 2005-11-25 2006-05-24 许宏 Pressure and ultrahigh pressure generating method and device
CN1944266A (en) * 2006-10-25 2007-04-11 国家纳米技术与工程研究院 Method for preparing zinc sulfide nano crystal particles using high pressure fluid mill
US20090162658A1 (en) * 2007-12-13 2009-06-25 Sud Chemie Ag Process for the preparation of nanocrystalline hydrotalcite compounds
CN102076405A (en) * 2008-04-28 2011-05-25 南吉耐克斯纳米技术股份有限公司 Instrument and process for nanoparticles production in continuous flow mode
WO2014153570A2 (en) * 2013-03-15 2014-09-25 Transtar Group, Ltd New and improved system for processing various chemicals and materials
CN103820846A (en) * 2014-02-17 2014-05-28 中国科学技术大学 Multifunctional device based on hydrothermal method for growing nano materials
CN204656495U (en) * 2015-02-25 2015-09-23 王建伟 A kind of industrial mass stablizes the tandem arrangement preparing quantum dot

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