CN105749844A - Quantum dot nanomaterial synthetic apparatus - Google Patents
Quantum dot nanomaterial synthetic apparatus Download PDFInfo
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- CN105749844A CN105749844A CN201510266013.8A CN201510266013A CN105749844A CN 105749844 A CN105749844 A CN 105749844A CN 201510266013 A CN201510266013 A CN 201510266013A CN 105749844 A CN105749844 A CN 105749844A
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Abstract
The invention is intended to provide a quantum dot nanomaterial synthetic apparatus enabling large-scale production of a high-quality quantum dot nanomaterial, characterized by comprising one or more reaction units; each reaction unit comprises a reaction portion, a stirring portion, a feeding portion, a gas protection portion, a tail liquid collection portion, a heating portion and a lifting portion, the reaction portion resides above the heating portion, the stirring portion, the feeding portion, the gas protection portion and the tail liquid collection portion are disposed on the reaction portion, and the heating portion resides on the lifting portion; the tail liquid collection portions in the reaction units have two functions: first, serving as an inert gas outlet to keep constant pressure in a reaction system; second, recycling a first reaction product and low-boiling-point impurity in a solvent.The low-boiling-point impurity in the reaction product and low-boiling-point impurity produced during reaction can be cleared, and quantum yield of quantum dots can be increased; strict vacuum pretreatment is not required, and the apparatus is suitable for large-scale production.
Description
Technical field
The invention belongs to technology of quantum dots field, particularly relate to a kind of CdS quantum dots synthesizer.
Background technology
Quantum dot is a kind of nano-particle elementary composition by II-VI group or iii-v.Quantum dot is also called semiconductor nanocrystal, and when the stimulation being subject to light or electricity, quantum dot will send the light of a wavelength range, and the scope of emission spectrum and intensity are determined by composition material and the size shape of quantum dot.This characteristic makes quantum dot can be applied to the fields such as biological detection, false proof, LED, display and photoelectric device as luminescent material.
The method of currently the majority synthesis quantum dot all adopts organic high-temperature synthesis, in whole building-up process, operates comparatively laborious, contaminated environment.The CdO such as Peng instead of the dimethyl cadmium of toxicity height, poor stability, and this method also continues up to now.But CdO needs to carry out pre-treatment, just can using after the moisture generated being removed with the ligand reaction final vacuum such as oleic acid, the parts such as this operation is more complicated, oleic acid are likely to therefore generate dimer or trimer, affect the quality of quantum dot.
The synthesis condition of quantum dot requires very harsh, and quantum dot quality is probably tremendous influence by a certain factor slight variation, and just because of this, the yield of quantum dot cannot expand always on a large scale now, significantly hinders quantum dot large-scale application.
Summary of the invention
In order to solve above-mentioned technical problem, it is an object of the invention to provide a kind of energy large-scale production high-quality CdS quantum dots synthesizer, the quantum dot quantum productivity of its synthesis is high, half-peak width, and yield is big, and environmental friendliness, cost is low.
To achieve these goals, technical scheme is as follows:
The invention have the benefit that and employ tail washings collection portion in reaction unit, there are two effects in tail washings collection portion: first, as inert gas outlet, keeps reaction system air pressure constant；Second, reclaim the low boiling impurity in the first reactant and solvent.Reaction unit can be single reaction unit, it is also possible to is two or more reaction unit and is unified into one group, and synthesizer scale industrialization can produce high-quality CdS quantum dots.The present invention eliminates in quantum dot synthesis mode and in advance CdO is reacted 1-2h under a high vacuum with oleic acid, to remove the step of the water produced, simplifies operation.The present invention can the low boiling impurity that produces of low boiling impurity in cleaning reaction thing and reaction, improve the quantum yield of quantum dot；Do not need strict vacuum pre-treatment, be suitable for large-scale production.
Accompanying drawing explanation
Fig. 1 is the structural representation of the reaction unit of the present invention；
Fig. 2 is the structural representation in the tail washings collection portion of the present invention；
Fig. 3 is the two townhouse reaction unit structural representations of the present invention；
Fig. 4 is the four townhouse reaction unit structural representations of the present invention；
Fig. 5 is the six townhouse reaction unit structural representations of the present invention.
In Fig. 1,1, reacting part；2, mixing part；3, feeder；4, gas shield portion；5, tail washings collection portion；6, heating part；7, lifting unit；In Fig. 2,8, condensation reflux unit；9, receiving flask；10, gas outlet.
Embodiment one
As shown in Fig. 1 Fig. 2; reaction unit includes reacting part 1, mixing part 2, feeder 3, gas shield portion 4, tail washings collection portion 5, heating part 6 and lifting unit 7; reacting part 1 is positioned at above heating part 6; being provided with mixing part 2, feeder 3, gas shield portion 4 and tail washings collection portion 5 on reacting part 1, heating part 6 is positioned on lifting unit 7.Reacting part 1 is internal equipped with the first reactant, solvent and reflux, and feeder 3 is equipped with the second reactant, and what pass in gas shield portion 4 is noble gas.Tail washings collection portion 5 includes condensation reflux unit 8, receiving flask 9 and gas outlet 10；Condensation reflux unit 8 is the one in gas condensing mode, liquid condensing mode.The air inlet in gas shield portion 4 is placed in below the liquid level of reacting part 1, and gas outlet is positioned at outside reacting part 1, and gas shield portion 4 is containing gas flowmeter.Heating part 6 is one or several in resistance heating, oil bath heating, Electromagnetic Heating, microwave heating, Infrared Heating or LASER HEATING；Heating temperature range is 0-500 DEG C.Being connected to temperature sensor on heating part 6, temperature sensor is positioned at below the liquid level of reacting part 1.Reacting part 1 is glass kettle, pottery still or rustless steel still.Reacting part 1 be sized to 10mL-1000mL or 1L-50L or 50L-500L or 500L-1000L.Mixing part 2 is mechanical agitation or magnetic agitation.Feeder 3 is constant pressure funnel, syringe, constant flow pump or automatic sampler.Lifting unit 7 is hand-operated lifting platform or electric lifting platform.
The operating procedure of the present invention is: (1) precise the first reactant, solvent and reflux, puts into reacting part 1；(2) precise the second reactant, puts into feeder 3；(3) open mixing part 2, set specific rotation speeds constant；(4) pass into noble gas, set gas flow rate constant；(5), after question response portion 1 inner air is got rid of completely, heating is opened；(6) when temperature reaches setting value, open feeder 3 valve, make reactant enter reacting part 1 by regulation feed rate and participate in reaction；(7) after question response completes, open lifting unit 7, heating part 6 is separated with reacting part 1, cool down reacting part 1.
Gas shield portion 4 is containing the gas flowmeter controlling gas flow rate, and gas flow rate is unsuitable too fast, it is prevented that take away reactant or solvent；Gas flow rate should not be excessively slow, in order to avoid impurities left.
Condensation reflux unit 8, by liquid condensing tube or gas condensing tube condensation, flowing back into receiving flask 9, in order to avoid being discharged in air, polluting, and receiving flask 9 volume is more than the cumulative volume of reflux materials and impurity.
Embodiment two
As it is shown on figure 3, two reaction units are connected in parallel, form two townhouses.Wherein mixing part 2 is fixed in same casing, and heating part 6 merges together, and lifting unit 7 merges together, it is possible to lift simultaneously.
Embodiment three
As shown in Figure 4, four reaction units are connected in parallel, and form four townhouses.Wherein mixing part 2 is fixed in same casing, and heating part 6 merges together, and lifting unit 7 merges together, it is possible to lift simultaneously.
Embodiment four
As it is shown in figure 5, six reaction units are connected in parallel, form four townhouses.Wherein mixing part 2 is fixed in same casing, and heating part 6 merges together, and lifting unit 7 merges together, it is possible to lift simultaneously.
Make use-case one
In the present embodiment, protective gas is argon, and condensing unit is water condensing tube, and reacting part 1 is 100mL glass flask, and heater is resistance heating, and lifting platform is hand-operated lifting platform, and agitating device is mechanical agitation.To prepare CdSeS alloy quantum dot, specifically comprise the following steps that
(1) pass into argon with 50mL/min speed, get rid of air in reacting part 1；
(2) after 15min, accurately weighing 1.28gCdO, 11.28g oleic acid, 40mL octadecylene joins 1,600 turn/min of reacting part stirring；
(3) tri octyl phosphine (0.632g selenium and 0.064g sulfur are dissolved in 5.92g tri octyl phosphine) being dissolved with Se and S is joined in constant pressure funnel, get rid of air 15min with argon；
(4) begin to warm up, control programming rate, when temperature reaches 298 DEG C after 65min, rapidly join liquid in constant pressure funnel.Now temperature is reduced to 290 DEG C；
(5) keep 290 DEG C of 3.5min, then reduce lifting platform, stop heating, be cooled to room temperature；
(6) wash three times by ethanol/toluene dissolution/precipitation repeatedly, then vacuum drying；
(7) in receiving flask, liquid carries out separatory, weighs upper strata fraction and the weight of lower floor's fraction respectively.
Use Gangdong spectrofluorophotometer F-380 and ultraviolet spectrophotometer SP-756PC test result:
| Numbering | Wavelength (nm) | Half-peak breadth (nm) | Quantum yield | Upper strata fraction (g) | Lower floor's fraction (g) | Yield (g) |
| 1# | 616.8 | 31.89 | 79% | 0.10g | 0.17 | 0.35 |
(note: in table, quantum yield represents quantum dot light transformation efficiency, numerical value more high conversion is more big)
Upper strata fraction is the low boiling organic impurities in raw material, and lower floor's fraction is the CdO water generated with elaidin reaction.Existing quantum dot synthesis mode is required in advance CdO is reacted 1-2h under a high vacuum with oleic acid, to remove the water produced.The present embodiment eliminates this step, operates simpler, is conducive to large-scale production.
Make use-case two:
Protective gas is argon, and condensing unit is water condensing tube, and reflux materials is toluene, and reacting part is 100mL glass flask, and heater is resistance heating, and lifting platform is hand-operated lifting platform, and agitating device is mechanical agitation.To prepare CdSeS alloy quantum dot, specifically comprise the following steps that
(1) pass into argon with 50mL/min speed, get rid of air in reacting part；
(2) after 15min, accurately weighing 1.28gCdO, 11.28g oleic acid, 40mL octadecylene, 10g toluene, join reacting part, 600r/min stirs；
(3) tri octyl phosphine (0.632g selenium and 0.064g sulfur are dissolved in 5.92g tri octyl phosphine) being dissolved with Se and S is joined in constant pressure funnel 12, get rid of air 15min with argon；
(4) begin to warm up, control programming rate, when temperature reaches 298 DEG C after 65min, rapidly join liquid in constant pressure funnel.Now temperature is reduced to 290 DEG C；
(5) keep 290 DEG C of 3.5min, then reduce lifting platform, stop heating, be cooled to room temperature；
(6) wash three times by ethanol/toluene dissolution/precipitation repeatedly, then vacuum drying；
(7) in receiving flask, liquid carries out separatory, weighs upper strata fraction and the weight of lower floor's fraction respectively.
Use Gangdong spectrofluorophotometer F-380 and ultraviolet spectrophotometer SP-756PC test result:
| Numbering | Wavelength (nm) | Half-peak breadth (nm) | Quantum yield | Upper strata fraction (g) | Lower floor's fraction (g) | Yield (g) |
| 2# | 615.2 | 32.15 | 87% | 10.50g | 0.20 | 0.36 |
Upper strata fraction is the mixing of toluene and low boiling impurity, and low boiling impurity has 0.5g, and more a lot of than to exceed in embodiment one, this is that toluene takes more polymictic reason out of with low boiling impurity azeotropic.Owing to impurity reduces, corresponding quantum yield also increases.
Above by embodiment being described in detail the present invention, but described content is only presently preferred embodiments of the present invention, it is impossible to be considered the practical range for limiting the present invention.All equalizations made according to the present patent application scope change and improvement etc., all should still belong within the patent covering scope of the present invention.
Claims (10)
1. a CdS quantum dots synthesizer; it is characterized in that being made up of one or more reaction units; described reaction unit includes reacting part, mixing part, feeder, gas shield portion, tail washings collection portion, heating part and lifting unit; described reactive site is above described heating part; being provided with described mixing part, feeder, gas shield portion and tail washings collection portion on described reacting part, described heating part is positioned on described lifting unit.
2. a kind of CdS quantum dots synthesizer as claimed in claim 1, it is characterised in that described tail washings collection portion includes condensation reflux unit, receiving flask and gas outlet；Described condensation reflux unit is the one in gas condensing mode, liquid condensing mode.
3. a kind of CdS quantum dots synthesizer as claimed in claim 1, it is characterised in that the air inlet in described gas shield portion is placed in below the liquid level of described reacting part, and gas outlet is positioned at outside described reacting part, and gas flowmeter is contained in described gas shield portion.
4. a kind of CdS quantum dots synthesizer as claimed in claim 1, it is characterised in that being connected to temperature sensor on described heating part, described temperature sensor is positioned at below the liquid level of described reacting part.
5. a kind of CdS quantum dots synthesizer as described in claim 1 or 4, it is characterised in that described heating part is one or several in resistance heating, oil bath heating, Electromagnetic Heating, microwave heating, Infrared Heating or LASER HEATING；Heating temperature range is 0-500 DEG C.
6. a kind of CdS quantum dots synthesizer as claimed in claim 1, it is characterised in that described reacting part is glass kettle, pottery still or rustless steel still.
7. a kind of CdS quantum dots synthesizer as claimed in claim 1, it is characterised in that described reacting part is sized to 10mL-1000mL or 1L-50L or 50L-500L or 500L-1000L.
8. a kind of CdS quantum dots synthesizer as claimed in claim 1, it is characterised in that described mixing part is mechanical agitation or magnetic agitation.
9. a kind of CdS quantum dots synthesizer as claimed in claim 1, it is characterised in that described feeder is constant pressure funnel, syringe, constant flow pump or automatic sampler.
10. a kind of CdS quantum dots synthesizer as claimed in claim 1, it is characterised in that described lifting unit is hand-operated lifting platform or electric lifting platform.
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| CN201510266013.8A CN105749844A (en) | 2015-05-22 | 2015-05-22 | Quantum dot nanomaterial synthetic apparatus |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106995703A (en) * | 2017-04-21 | 2017-08-01 | 东莞市睿泰涂布科技有限公司 | Quantum dot nucleosynthesis device and quantum dot nucleosynthesis method |
| TWI595115B (en) * | 2016-08-17 | 2017-08-11 | 國立清華大學 | Non-contact reactor and nanocrystal fabrication system having the same |
| CN117339507A (en) * | 2023-08-29 | 2024-01-05 | 珠海奥博凯生物医药技术有限公司 | Compound synthesis equipment based on continuous flow reaction and method for preparing compound |
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| CN202143841U (en) * | 2011-07-08 | 2012-02-15 | 四川国和新材料有限公司 | Glass reaction kettle device |
| CN202741095U (en) * | 2012-07-25 | 2013-02-20 | 天津滨海新区庚海精细化工有限公司 | Electrical heating reaction kettle |
| CN104310327A (en) * | 2007-02-08 | 2015-01-28 | 斯泰拉化工公司 | Method of manufacturing phosphorous pentafluoride and hexafluorophosphate |
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2015
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Patent Citations (5)
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| WO2005102510A1 (en) * | 2004-04-20 | 2005-11-03 | Sanko Chemical Industry Co., Ltd. | Chemical reaction apparatus utilizing microwave |
| US20070114187A1 (en) * | 2005-11-16 | 2007-05-24 | Company United L O | Enhanced water removal from used lubricating oils (Pre-treatment of Used oils) |
| CN104310327A (en) * | 2007-02-08 | 2015-01-28 | 斯泰拉化工公司 | Method of manufacturing phosphorous pentafluoride and hexafluorophosphate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI595115B (en) * | 2016-08-17 | 2017-08-11 | 國立清華大學 | Non-contact reactor and nanocrystal fabrication system having the same |
| CN106995703A (en) * | 2017-04-21 | 2017-08-01 | 东莞市睿泰涂布科技有限公司 | Quantum dot nucleosynthesis device and quantum dot nucleosynthesis method |
| CN117339507A (en) * | 2023-08-29 | 2024-01-05 | 珠海奥博凯生物医药技术有限公司 | Compound synthesis equipment based on continuous flow reaction and method for preparing compound |
| CN117339507B (en) * | 2023-08-29 | 2024-06-11 | 珠海奥博凯生物医药技术有限公司 | Compound synthesis equipment based on continuous flow reaction and method for preparing compound |
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Application publication date: 20160713 |