CN102671577B - Hydro-thermal reaction device is used in inorganic nano-particle synthesis - Google Patents
Hydro-thermal reaction device is used in inorganic nano-particle synthesis Download PDFInfo
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Abstract
The invention discloses a kind of inorganic nano-particle synthesis hydro-thermal reaction device, comprise the raw material mixing compression system, heated reaction system, cooling device and the filter that connect successively, described raw material mixing compression system comprises the raw material tank, the feedstock transportation pump that connect successively and has the air pressure of the first agitating device, and the outlet of described air pressure is connected with the entrance of heated reaction system.Compared with prior art, owing to present invention employs the air pressure with the first agitating device, raw material is fully mixed before entering heated reaction system in air pressure, avoid the obstruction of the reaction unit caused because raw material mixing is uneven, make the inorganic nano-particle uniform component of preparation simultaneously.Experimental result shows, utilizes inorganic nano-particle uniform component prepared by inorganic nano-particle synthesis hydro-thermal reaction device provided by the invention, favorable dispersibility.
Description
Technical field
The present invention relates to nano material reactor technology field, more particularly, relate to a kind of inorganic nano-particle synthesis hydro-thermal reaction device.
Background technology
Inorganic nano-particle refers to the material particles such as the metal of size between 1 ~ 100nm, pottery, semiconductor, compare with bulk solid material, there is obvious skin effect, small-size effect and macro quanta tunnel effect, be widely used in the fields such as pottery, semiconductor, pigment and catalyst.According to the difference of purposes, homogeneity, the polymolecularity and appearance structure etc. of inorganic nano-particle become the key factor affecting inorganic nano-particle serviceability.The preparation method of conventional inorganic nano material comprises sol-gel process, conventional hydrothermal method, coprecipitation, vapor phase method and hydrolyzable method etc., in these synthetic methods, although sol-gel process, coprecipitation and hydrolyzable method may be used for the extensive preparation of material, but the inorganic nano-particle obtained easily is reunited, be difficult to obtain the dispersed particle of nanoscale of good crystallinity; The higher costliness of equipment of step conventional hydrothermal method and security is poor, is difficult to expanding production.
Adopt the reaction of continuous synthesis critical (subcritical) hydro-thermal method to produce inorganic nano material to be paid close attention to by more and more people, such as, application number be 03121941.1 Chinese patent literature disclose a kind of continuous pipe type high-temperature high pressure water thermal reaction apparatus, this device adopts tubular circulation flow reactor, this reactor is primarily of the tubular reactor body of forced circulation, be arranged on the high temperature circulation pump on tubular reactor body, be arranged in the high temperature circulation pump on tubular reactor body, be arranged in the heater in reacting body outside, be vertically mounted on the heater of reactor body outside, be vertically mounted on the gas wind indicator on reactor body and corresponding valve composition.The duct route device of this device is complicated, and product manufacturing cycle is also long, is not suitable for large-scale production.
In addition, application number be 200710037315.3 Chinese patent literature report a kind of hypercritical hydrothermal reaction device for continuously synthesizing inorganic nano particle, this device is primarily of material liquid induction system, reactor, flash chamber and dry powder collector composition, wherein, material liquid induction system is connected and composed side by side by several high-pressure pumps.Utilize in the process of said apparatus inorganic nano-particle, due to raw material enter reactor before mixed fully, and it is different to deliver into material concentration in reactor by each high-pressure pump, therefore, easily causes the obstruction of reactor; In addition, due to raw material enter reactor before mixed fully, thus cause raw material mix uneven, the compositional uniformity of the inorganic nano-particle of preparation is poor.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of inorganic nano-particle synthesis hydro-thermal reaction device, avoids the obstruction of reaction unit, and the inorganic nano-particle uniform component of preparation.
In order to solve above technical problem, the invention provides a kind of inorganic nano-particle synthesis hydro-thermal reaction device, comprise the raw material mixing compression system, heated reaction system, cooling device and the filter that connect successively, described raw material mixing compression system comprises the raw material tank, the feedstock transportation pump that connect successively and has the air pressure of the first agitating device, and the outlet of described air pressure is connected with the entrance of heated reaction system.
Preferably, described raw material tank has the second agitating device.
Preferably, described heated reaction system comprises preheater and reactor, and the entrance and exit of described preheater is connected with reactor inlet with the outlet of described air pressure respectively, and the outlet of described reactor is connected with the entrance of cooling device.
Preferably, described preheater and reactor have heating jacket respectively.
Preferably, the back of the body valve be arranged between described heated reaction system and cooling device is also comprised.
Preferably, the pressure-regulating valve be arranged between described cooling device and filter is also comprised.
Preferably, also comprise and export with described filter the spray-drying installation be connected.
Preferably, can to realize pressure adjustable within the scope of 1 ~ 40MPa for described air pressure.
Preferably, can to realize temperature adjustable within the scope of 20 ~ 100 DEG C for described air pressure.
Preferably, can to realize temperature adjustable within the scope of 100 ~ 400 DEG C for described heated reaction system.
The invention provides a kind of inorganic nano-particle synthesis hydro-thermal reaction device, comprise the raw material mixing compression system, heated reaction system, cooling device and the filter that connect successively, described raw material mixing compression system comprises the raw material tank, the feedstock transportation pump that connect successively and has the air pressure of the first agitating device, and the outlet of described air pressure is connected with the entrance of heated reaction system.Compared with prior art, owing to present invention employs the air pressure with the first agitating device, raw material is fully mixed before entering heated reaction system in air pressure, avoid the obstruction of the reaction unit caused because raw material mixing is uneven, make the inorganic nano-particle uniform component of preparation simultaneously.Experimental result shows, utilizes inorganic nano-particle uniform component prepared by inorganic nano-particle synthesis hydro-thermal reaction device provided by the invention, favorable dispersibility.
Accompanying drawing explanation
Fig. 1 is inorganic nano-particle synthesis hydro-thermal reaction apparatus structure schematic diagram disclosed by the invention;
Fig. 2 is the XRD figure that the embodiment of the present invention 1 prepares inorganic nano-particle;
Fig. 3 is the scanning electron microscope diagram sheet of inorganic nano-particle prepared by the embodiment of the present invention 1.
Detailed description of the invention
Be clearly and completely described the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
The invention discloses a kind of inorganic nano-particle synthesis hydro-thermal reaction device, as shown in Figure 1, comprise the raw material mixing compression system, heated reaction system, cooling device 107 and the filter 108 that connect successively, raw material mixing compression system comprises the raw material tank 101, the feedstock transportation pump 102 that connect successively and has the air pressure 103 of the first agitating device 110, and the outlet of air pressure 103 is connected with the entrance of heated reaction system.
Raw material tank 101 has the second agitating device 109, second agitating device 109 and is preferably mixer.Raw material enters this hydro-thermal reaction device through the entrance 111 of raw material tank 101, delivers in air pressure 103 after the second agitating device 109 stirs through outlet.Connected by feedstock transportation pump 102 between the outlet of raw material tank 101 and air pressure 103.In the course of work of hydro-thermal reaction device, the various raw materials modulated are put into raw material tank 101 by the entrance 111 of raw material tank 101, through the stirring of the second agitating device 109, be delivered in air pressure 103 by feedstock transportation pump 102 after mixing.
The air pressure 103 that the present invention adopts carries out direct weighting by compressed air 112, instead of realizes pressurization by high-pressure pump.Compressed air regulates pressure that reaction pressure can be made more steady, this pressure method can make raw material slurry dispersed under pressurised conditions, and, this pressue device is not affecting the form of feed particles, the inorganic nanoparticles of generation is made to have polymolecularity, high crystalline, the feature of high homogeneity, is conducive to the stable of production process and carries out.It is adjustable within the scope of 1 ~ 40MPa that air pressure 103 can realize pressure, and temperature is adjustable within the scope of 20 ~ 100 DEG C.Utilizing this hydro-thermal reaction device to prepare the inorganic nano-particle period of the day from 11 p.m. to 1 a.m, the pressure of air pressure 103 is preferably 1 ~ 40MPa; In air pressure 103, the temperature of raw material is preferably less than 100 DEG C.When the temperature of raw material is greater than 100 DEG C in air pressure 103, easily makes raw material react in pressurizer, thus cause the heterogeneity of final products particle.Because air pressure 103 has the first agitating device 110, thus raw material is fully mixed before entering heated reaction system in air pressure 103, avoid the obstruction of the reaction unit caused because raw material mixing is uneven, and the inorganic nano-particle uniform component prepared.
Raw material enters in heated reaction system after pressurizeing in air pressure 103, heated reaction system comprises preheater 104 and reactor 105, the entrance and exit of preheater 104 is connected with reactor 105 entrance with the outlet of air pressure 103 respectively, and the outlet of reactor 105 is connected with the entrance of cooling device 107.Raw material by preheater 104, can ensure that raw material is even at high-pressure reactor interior reaction temperature before entering reactor 105, avoids because the heterogeneity of reaction temperature causes the heterogeneity of product particle.It is adjustable within the scope of 1 ~ 40MPa that reactor 105 can realize pressure, and temperature is adjustable within the scope of 100 ~ 400 DEG C.In the course of work of hydro-thermal reaction device, the pressure general control of reactor 105 at 1 ~ 40MPa, this be due to pressure too young pathbreaker not easily make raw material fast reaction, obtain the product that purity is high, on the other hand pressure also controls by material.The hydrothermal temperature of reactor 105 preferably controls at 100 ~ 400 DEG C, be more preferably 200 ~ 350 DEG C, this is that the product crystallinity easily making to be obtained by reacting is not high or reaction is incomplete because temperature is less than 100 DEG C, temperature easily makes particle overgrowth when being greater than 400 DEG C, cause reuniting, thus affect the homogeneous distribution of particle.In order to control control temperature, preheater 104 and reactor 105 have heating jacket respectively, namely at the shell of preheater 104 and reactor 105, heater and thermocouple are all housed.
In whole course of reaction, the present invention can reach by regulating liquor charging amount the object controlling the reaction time, utilizes which can reduce the change of temperature and the Separation of Solid and Liquid of raw material slurry in liquor charging process to control the reaction time.Meanwhile, reactor inside diameter is excessive easily causes Separation of Solid and Liquid, causes the heterogeneity of hydro-thermal reaction shape of particle and particle diameter simultaneously.
Raw material cools through cooling device 107 after reacting in reactor 105, and then pass in filter 108 and filter, obtain high dispersive, the inorganic nano-particle of high crystallization, this filter 108 is preferably continuous filter unit.The continuous filter unit that this device adopts can reduce the operation of engineering, improve the production of whole device, make described hydro-thermal reaction device have structure is simple, easy and simple to handle, cost is low and production advantages of higher simultaneously, and, the preparation process of this inorganic nano-particle is a continuous print process, is suitable for industrialization large-scale production.
In addition, between reactor 105 and cooling device 107, be preferably provided with back of the body valve 106 be used for regulating pressure; The pressure-regulating valve (not shown) communicated with air pipeline is equipped with between cooling device 107 and filter 108.Inorganic nano-particle synthesis hydro-thermal reaction device provided by the invention also preferably includes and exports with filter 108 spray-drying installation be connected, thus obtains product and inorganic nano-particle.
Inorganic nano-particle synthesis hydro-thermal reaction device provided by the invention can prepare various metal acid compound or metal water acid compound, also can prepare two or more composition metal acidulants or phosphide, such as, and Fe
2o
3, Fe
3o
4, Mn
3o
4, TiO
2, Mg (OH)
2, Al
2o
3, SnO
2, MnFe
2o
4, BaFe
12o
19, BaTiO
3, ZrO
2, WO
3, CeO
2, ZnO, Y
2o
3, La
2o
3, MoO
3, Co
3o
4, NiO, LiCoO
2, LiFePO
4, LiMnPO
4, Li
2mnSiO
4, Li
2feSiO
4, LiTi
2(PO
4)
3, Li
3v
2(PO
4)
3deng compound, the particle diameter of particle is in 5nm ~ 1 μm, and the controlled shape of particle, such as, can be bar-shaped simultaneously, sheet, square, threadiness, and needle-like is spherical etc.
In order to further illustrate technical scheme of the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just for further illustrating the features and advantages of the present invention, instead of limiting to the claimed invention.
Embodiment 1
LiMnPO
4atomic preparation
Using the LiOH aqueous solution as lithium source, MnSO
4as source of iron, H
3pO
4as phosphorus source; add in raw material tank by Li: Fe: P=3: 1: 1; simultaneously; add 25% (mol ratio) ascorbic acid solution as reduction protection agent; after being fully uniformly mixed in raw material tank; then feedstock transportation transport pump is passed through in air pressure; the compressed air pressure of air pressure is 30MPa; uniform stirring simultaneously; raw material through pressurization and homogenization process continues through the high-pressure reactor that temperature is 370 DEG C; reacted raw material, through apparatus for supercooling and continuous filter unit, obtains inorganic nano-particle.
The inorganic nano-particle prepared by the present embodiment carries out XRD test respectively, scanning electron microscope test and distribution of particles test.Fig. 2 is the XRD collection of illustrative plates that the present embodiment prepares inorganic nano-particle, detects show that final products are LiMnPO4 single-phase through XRD; As shown in Figure 3, be the Scanning Electron microscope photograph of inorganic nano-particle prepared by the present embodiment, as can be seen from the figure, LiMnPO4 good dispersion prepared by the present embodiment, about 100 nanometers, in bar-shaped; Distribution of particles test shows its favorable dispersibility.
Embodiment 2
ZrO
2atomic preparation
The ZnOCl of preparation 0.4mol
2solution, the NaOH solution of 1mol;
Under atmospheric pressure at room condition, by ZnOCl
2solution adds in raw material tank, drip NaOH solution, control PH is 11, after being fully uniformly mixed in raw material tank, then pass through feedstock transportation transport pump in air pressure, the compressed air pressure of air pressure is 28MPa, uniform stirring simultaneously, raw material through pressurization and homogenization process continues through the high-pressure reactor that temperature is 400 DEG C, and the raw material reacted, through apparatus for supercooling and continuous filter unit, obtains inorganic nano-particle.
Adopt the method identical with embodiment 1 to test, result shows, the spherical ZrO of the 50nm for good dispersion prepared by the present embodiment
2.
Embodiment 3
BaTiO
3atomic preparation
Under atmospheric pressure at room condition, by the BaNO of 0.44mol
3and 0.4TiCl
4solution (in the ratio of metering than Ba/Ti=1.1) adds in raw material tank, add aqueous slkali NaOH, regulate pH value 13.2, after being fully uniformly mixed in raw material tank, then feedstock transportation transport pump is passed through in air pressure, the compressed air pressure of air pressure is 25MPa, uniform stirring simultaneously, raw material through pressurization and homogenization process continues through the high-pressure reactor that temperature is 370 DEG C, the raw material reacted, through apparatus for supercooling and continuous filter unit, obtains inorganic nano-particle.
Adopt the method identical with embodiment 1 to test, result shows, the sheet BaTiO of the 50nm for good dispersion prepared by the present embodiment
3product.
Embodiment 4
Mg (OH)
2atomic preparation
Under atmospheric pressure at room condition, by 0.5mol MgCl
2add in raw material tank, then aqueous slkali NaOH is added, regulate pH value 10.5, after being fully uniformly mixed in raw material tank, then by feedstock pump conveying air pressure, the compressed air pressure of air pressure is 30MPa, uniform stirring simultaneously, raw material through pressurization and homogenization process continues through the high-pressure reactor that temperature is 400 DEG C, and the raw material reacted, through apparatus for supercooling and continuous filter unit, obtains inorganic nano-particle.
Adopt the method identical with embodiment 1 to test, result shows, the block Mg (OH) of the 80nm for good dispersion prepared by the present embodiment
2product.
Embodiment 5
MnFe
2o
4atomic preparation
Under atmospheric pressure at room condition, by 2mol/LMn (NO
3)
2with 2mol/L Fe (NO
3)
3solution (in the ratio of metering than Mn/Fe=1: 2.5) adds in raw material tank, adds aqueous slkali NaOH, regulates pH value 13.2.After being fully uniformly mixed in raw material tank, then be transported in air pressure by feedstock pump, the compressed air pressure of air pressure is 28MPa, uniform stirring simultaneously, raw material through pressurization and homogenization process continues through the high-pressure reactor that temperature is 400 DEG C, the raw material reacted, through apparatus for supercooling and continuous filter unit, obtains inorganic nano-particle.
Adopt the method identical with embodiment 1 to test, result shows, the square MnFe of the 100nm for good dispersion prepared by the present embodiment
2o
4product.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (5)
1. a MnFe
2o
4the hydro-thermal reaction device of particulate synthesis, it is characterized in that: comprise the raw material mixing compression system, heated reaction system, cooling device 107 and the filter 108 that connect successively, raw material mixing compression system comprises the raw material tank 101, the feedstock transportation pump 102 that connect successively and has the air pressure 103 of the first agitating device 110, and the outlet of air pressure 103 is connected with the entrance of heated reaction system; Raw material tank 101 has the second agitating device 109; Air pressure 103 carries out direct weighting by compressed air 112, instead of realizes pressurization by high-pressure pump; Raw material enters in heated reaction system after pressurizeing in air pressure 103, heated reaction system comprises preheater 104 and reactor 105, the entrance and exit of preheater 104 is connected with reactor 105 entrance with the outlet of air pressure 103 respectively, and the outlet of reactor 105 is connected with the entrance of cooling device 107; Raw material cools through cooling device 107 after reacting in reactor 105, then passes in filter 108 and filters, obtain high dispersive, the inorganic nano-particle of high crystallization; Between reactor 105 and cooling device 107, be provided with back of the body valve 106 be used for regulating pressure; The pressure-regulating valve communicated with air pipeline is equipped with between cooling device 107 and filter 108; Under atmospheric pressure at room condition, by 2mol/LMn (NO
3)
2with 2mol/L Fe (NO
3)
3solution, in the ratio of metering than Mn/Fe=1:2.5, add in raw material tank, add aqueous slkali NaOH, adjust ph is 13.2, after being fully uniformly mixed in raw material tank, then be transported in air pressure by feedstock pump, the compressed air pressure of air pressure is 28MPa, uniform stirring simultaneously, the raw material through pressurization and homogenization process continues through the high-pressure reactor that temperature is 400 DEG C, and the raw material reacted is through apparatus for supercooling and continuous filter unit, obtain inorganic nano-particle, this product is the square MnFe of the 100nm of good dispersion
2o
4product.
2. a MnFe as claimed in claim 1
2o
4the hydro-thermal reaction device of particulate synthesis, is characterized in that: the second agitating device 109 is mixer.
3. a MnFe as claimed in claim 1 or 2
2o
4the hydro-thermal reaction device of particulate synthesis, it is characterized in that: in order to control control temperature, preheater 104 and reactor 105 have heating jacket respectively.
4. a MnFe as claimed in claim 1
2o
4the hydro-thermal reaction device of particulate synthesis, is characterized in that: filter 108 is continuous filter unit.
5. a MnFe as claimed in claim 1
2o
4the hydro-thermal reaction device of particulate synthesis, is characterized in that: also comprise and export with filter 108 spray-drying installation be connected.
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| CN103920641B (en) * | 2013-01-12 | 2016-12-28 | 唐山兴铭科技有限公司 | A kind of industrialized unit producing nano-particle and technique thereof |
| CN109967010A (en) * | 2019-03-12 | 2019-07-05 | 柳州呈奥科技有限公司 | Process equipment is made in a kind of ATO of hydro-thermal method |
| CN114644329B (en) * | 2022-04-12 | 2023-07-07 | 深圳市沃伦特新能源有限公司 | Hydrothermal synthesis method of nano lithium iron manganese phosphate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101439875A (en) * | 2008-12-18 | 2009-05-27 | 东华大学 | Method for preparing alpha-Sb2O4 nano-rod by hydrothermal process |
| CN101530778A (en) * | 2009-03-09 | 2009-09-16 | 神农氏奈米科技有限公司 | Liquid nanocrystallization device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101439875A (en) * | 2008-12-18 | 2009-05-27 | 东华大学 | Method for preparing alpha-Sb2O4 nano-rod by hydrothermal process |
| CN101530778A (en) * | 2009-03-09 | 2009-09-16 | 神农氏奈米科技有限公司 | Liquid nanocrystallization device |
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