CN102671577A - Hydrothermal reaction system for inorganic nanoparticle synthesis - Google Patents
Hydrothermal reaction system for inorganic nanoparticle synthesis Download PDFInfo
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- CN102671577A CN102671577A CN2011102539520A CN201110253952A CN102671577A CN 102671577 A CN102671577 A CN 102671577A CN 2011102539520 A CN2011102539520 A CN 2011102539520A CN 201110253952 A CN201110253952 A CN 201110253952A CN 102671577 A CN102671577 A CN 102671577A
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Abstract
The invention discloses a hydrothermal reaction system for inorganic nanoparticle synthesis. The hydrothermal reaction system comprises a material mixing and pressurization system, a heating reaction system, a cooler and a filter which are sequentially connected, the material mixing and pressurization system comprises a material tank, a material transfer pump and an air pressurizer with a first agitator which are sequentially connected, and the outlet of the air pressurizer is connected with the inlet of the heating reaction system. Compared with the prior art, the hydrothermal reaction system adopts the air pressurizer with the first agitator, so that materials can be sufficiently mixed in the air pressurizer before entering the heating reaction system, consequently, the blockage of a reactor, which is caused by the ununiform mixing of the materials, is prevented, and meanwhile, the components of prepared inorganic nanoparticles are uniform. An experiment result shows that the components of the inorganic nanoparticles prepared by the hydrothermal reaction system for inorganic nanoparticle synthesis provided by the invention are uniform and that the dispersibility of the inorganic nanoparticles is good.
Description
Technical field
The present invention relates to nano material reactor technology field, more particularly, relate to the synthetic water thermal reaction apparatus of a kind of inorganic nano-particle.
Background technology
Inorganic nano-particle is meant material particles such as the metal of size between 1～100nm, pottery, semiconductor; Compare with the bulk solid material; Have tangible skin effect, small-size effect and macro quanta tunnel effect, be widely used in fields such as pottery, semiconductor, pigment and catalyst.According to the difference of purposes, the homogeneity of inorganic nano-particle, polymolecularity and appearance structure etc. become the key factor that influences the inorganic nano-particle serviceability.The preparation method of inorganic nano material commonly used comprises sol-gel process, conventional hydro-thermal method; Coprecipitation, vapor phase method and add moisture solution etc.; In these synthetic methods; Though sol-gel process, coprecipitation and add the mass preparation that the moisture solution can be used for material, the inorganic nano-particle that obtains are prone to reunite, and are difficult to obtain the even dispersed particle of nanoscale of good crystallinity; Higher costliness of the equipment of step conventional hydro-thermal method and security are relatively poor, are difficult to enlarge produce.
Adopt to synthesize with critical (subcritical) hydro-thermal method reacted inorganic nano material continuously and paid close attention to by more and more people; For example; Application number is that 03121941.1 Chinese patent document discloses a kind of continuous tubular type high-temperature high pressure water thermal reaction apparatus; This device adopts tubular type to circulate reactor, and this reactor is arranged on the high temperature circulation pump on the tubular reactor body mainly by the tubular reactor body of forced circulation; Be arranged in the high temperature circulation pump on the tubular reactor body; Be arranged at reacting body external heated device, be vertically mounted on reactor body external heated device, the gas wind indicator and the corresponding valve that are vertically mounted on the reactor body are formed.The duct route device of this device is complicated, and the preparation of product cycle is also long, is not suitable for large-scale production.
In addition; Application number a kind of hypercritical hydrothermal reaction device for continuously synthesizing inorganic nano particle that has been 200710037315.3 Chinese patent bibliographical information; This installs mainly by the material liquid induction system, reactor, and flash chamber and dry powder gatherer are formed; Wherein, the material liquid induction system is connected and composed by several high-pressure pumps side by side.Utilize in the process of said apparatus inorganic nano-particle, owing to mixed fully before the raw material entering reactor, and deliver into the material concentration difference in the reactor by each high-pressure pump, therefore, be prone to cause the obstruction of reactor; In addition, owing to mixed fully before the raw material entering reactor, thereby it is inhomogeneous to cause raw material to mix, and the uniform component property of the inorganic nano-particle of preparation is relatively poor.
Summary of the invention
In view of this, the technical problem that the present invention will solve is to provide a kind of inorganic nano-particle to synthesize the water thermal reaction apparatus, has avoided the obstruction of reaction unit, and the inorganic nano-particle uniform component of preparation.
In order to solve above technical problem; The present invention provides a kind of inorganic nano-particle to synthesize the water thermal reaction apparatus; Comprise the raw material mixing compression system, heated reaction system, cooling device and the filter that connect successively; Said raw material mixing compression system comprises raw material tank, the former material conveying pump that connects successively and has the air pressurized device of first agitating device that the outlet of said air pressurized device links to each other with the inlet of heated reaction system.
Preferably, said raw material tank has second agitating device.
Preferably, said heated reaction system comprises preheater and reactor, and the entrance and exit of said preheater links to each other with reactor inlet with the outlet of said air pressurized device respectively, and the outlet of said reactor links to each other with the inlet of cooling device.
Preferably, said preheater and reactor have heating jacket respectively.
Preferably, also comprise the back of the body valve that is arranged between said heated reaction system and the cooling device.
Preferably, also comprise the pressure-regulating valve that is arranged between said cooling device and the filter.
Preferably, also comprise the spray-drying installation that links to each other with said filter outlet.
Preferably, said air pressurized device can realize that pressure is adjustable in 1～40MPa scope.
Preferably, said air pressurized device can realize that temperature is adjustable in 20～100 ℃ of scopes.
Preferably, said heated reaction system can realize that temperature is adjustable in 100～400 ℃ of scopes.
The present invention provides a kind of inorganic nano-particle to synthesize the water thermal reaction apparatus; Comprise the raw material mixing compression system, heated reaction system, cooling device and the filter that connect successively; Said raw material mixing compression system comprises raw material tank, the former material conveying pump that connects successively and has the air pressurized device of first agitating device that the outlet of said air pressurized device links to each other with the inlet of heated reaction system.Compared with prior art; Because the present invention has adopted the air pressurized device with first agitating device; Raw material is fully mixed in the air pressurized device before getting into heated reaction system; Avoided the obstruction reaction unit that causes, made the inorganic nano-particle uniform component of preparation simultaneously because raw material mixes inhomogeneous.Experimental result shows, utilizes the inorganic nano-particle uniform component of the synthetic water thermal reaction apparatus preparation of inorganic nano-particle provided by the invention, favorable dispersibility.
Description of drawings
Fig. 1 is the synthetic water thermal reaction apparatus structural representation of inorganic nano-particle disclosed by the invention;
Fig. 2 is the XRD figure of the embodiment of the invention 1 preparation inorganic nano-particle;
Fig. 3 is the scanning electron microscope diagram sheet of the inorganic nano-particle of the embodiment of the invention 1 preparation.
The specific embodiment
Carry out clear, intactly description in the face of the technical scheme in the embodiment of the invention down, obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills are not making the every other embodiment that is obtained under the creative work prerequisite, all belong to the scope of the present invention's protection.
The invention discloses the synthetic water thermal reaction apparatus of a kind of inorganic nano-particle; 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 raw material tank 101, the former material conveying pump 102 that connects successively and has the air pressurized device 103 of first agitating device 110 that the outlet of air pressurized device 103 links to each other with the inlet of heated reaction system.
The air pressurized device 103 that the present invention adopts directly pressurizes through compressed air 112, rather than realizes pressurization through high-pressure pump.Compressed air is regulated pressure can make reaction pressure more steady; This pressure method can make the raw material slurry under pressurized state, evenly disperse, and this pressue device is in the form that does not influence feed particles; Make the inorganic nanoparticles of generation have polymolecularity; High crystalline, the characteristics of high homogeneity help the stable of production process and carry out.Air pressurized device 103 can realize that pressure is adjustable in 1～40MPa scope, and temperature is adjustable in 20～100 ℃ of scopes.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 pressurized device 103 is preferably 1～40MPa; The temperature of raw material is preferably less than 100 ℃ in the air pressurized device 103.When the temperature of raw material is greater than 100 ℃ in the air pressurized device 103, is prone to make raw material in pressurizer, to react, thereby causes the heterogeneity of final products particle.Because air pressurized device 103 has first agitating device 110; Thereby raw material is fully mixed in air pressurized device 103 before getting into heated reaction system; Avoided the obstruction reaction unit that causes because raw material mixes inhomogeneous, and the inorganic nano-particle uniform component for preparing.
Raw material pressurizes in air pressurized device 103 in the back entering heated reaction system; Heated reaction system comprises preheater 104 and reactor 105; The entrance and exit of preheater 104 links to each other with reactor 105 inlets with the outlet of air pressurized device 103 respectively, and the outlet of reactor 105 links to each other with the inlet of cooling device 107.Raw material through preheater 104, can guarantee that raw material is even at the high-pressure reactor interior reaction temperature before getting into reactor 105, avoid because the heterogeneity of reaction temperature causes the heterogeneity of product particle.Reactor 105 can realize that pressure is adjustable in 1～40MPa scope, and temperature is adjustable in 100～400 ℃ of scopes.In the course of work of hydro-thermal reaction device, the pressure of reactor 105 generally is controlled at 1～40MPa, this be since pressure too the young pathbreaker be difficult for making the raw material fast reaction, obtain the high product of purity, pressure is controlled by material also on the other hand.The hydrothermal temperature of reactor 105 preferably is controlled at 100～400 ℃; More preferably 200～350 ℃; This is because temperature makes the not high or reaction of the product crystallinity that obtains of reaction not exclusively easily less than 100 ℃; Temperature is prone to make the particle overgrowth during greater than 400 ℃, causes reuniting, thereby influence the homogeneous distribution of particle.For the control temperature, preheater 104 has heating jacket respectively with reactor 105, and promptly the shell at preheater 104 and reactor 105 all is equipped with heater and thermocouple.
In entire reaction course, the present invention can reach the purpose in control reaction time through regulating the liquor charging amount, utilizes this mode to control the Separation of Solid and Liquid that the reaction time can reduce variation of temperature and raw material slurry in the liquor charging process.Simultaneously, the excessive Separation of Solid and Liquid that causes easily of reactor inside diameter causes the heterogeneity of hydro-thermal reaction shape of particle and particle diameter simultaneously.
After raw material reacts in reactor 105,, feed then in the filter 108 and filter, obtain high dispersive through cooling device 107 coolings, 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 simultaneously said hydro-thermal reaction device have simple in structure, easy and simple to handle, cost is low and the production advantages of higher; And the preparation process of this inorganic nano-particle is a continuous process, is suitable for large-scale industrialization production.
In addition, between reactor 105 and cooling device 107, preferably be provided with back of the body valve 106 and be used for regulating pressure; Pressure-regulating valve (not shown) with atmosphere is housed on pipeline between cooling device 107 and the filter 108.The synthetic water thermal reaction apparatus of inorganic nano-particle provided by the invention also preferably includes the spray-drying installation that links to each other with filter 108 outlets, is inorganic nano-particle thereby obtain product.
The synthetic water thermal reaction apparatus of inorganic nano-particle provided by the invention can prepare various metal acidulants or metal water acid compound, also can prepare two or more composition metal acidulants or phosphide, for example, 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 at 5nm～1 μ m, and the controllable shapes of particle for example can be bar-shaped simultaneously, sheet, and square shape, fibrous, needle-like, spherical etc.
In order to further specify technical scheme of the present invention; Below in conjunction with embodiment the preferred embodiment of the invention is described; Describe just to further specifying feature and advantage of the present invention but should be appreciated that these, rather than to the restriction of claim of the present invention.
LiMnPO
4Atomic preparation
With the LiOH aqueous solution as lithium source, MnSO
4As source of iron, H
3PO
4As the phosphorus source, by Li: Fe: P=3: add in raw material tank, simultaneously at 1: 1; Add 25% (mol ratio) ascorbic acid solution as the reduction protection agent; After in raw material tank, fully mixing, be transported in the air pressurized device through former material conveying pump then, the compressed air pressure of air pressurized device is 30MPa; Evenly stir simultaneously; The raw material that process pressurization and homogenization were handled is 370 ℃ high-pressure reactor continuously through temperature, and reacted raw material obtains inorganic nano-particle through apparatus for supercooling and continuous filter unit.
The inorganic nano-particle of present embodiment preparation is carried out the XRD test respectively, scanning electron microscope test and distribution of particles test.Fig. 2 composes for the XRD figure that present embodiment prepares inorganic nano-particle, detects through XRD to show that final products are the single phase of LiMnPO4; As shown in Figure 3, be the surface sweeping electron microscope picture of the inorganic nano-particle of present embodiment preparation, as can be seen from the figure, and the LiMnPO4 good dispersion of present embodiment preparation, about 100 nanometers are bar-shaped; Its favorable dispersibility of distribution of particles test shows.
Embodiment 2
ZrO
2Atomic preparation
The ZnOCl of preparation 0.4mol
2Solution, the NaOH solution of 1mol;
Under the atmospheric pressure at room condition, with ZnOCl
2Solution adds in the raw material tank, drips NaOH solution, and PH is 11 in control; After in raw material tank, fully mixing, be transported in the air pressurized device through former material conveying pump then, the compressed air pressure of air pressurized device is 28MPa; Evenly stir simultaneously; The raw material that process pressurization and homogenization were handled is 400 ℃ high-pressure reactor continuously through temperature, and the raw material that has reacted obtains inorganic nano-particle through apparatus for supercooling and continuous filter unit.
Adopt and test with embodiment 1 identical method, the result shows that present embodiment prepares is the spherical ZrO of the 50nm of good dispersion
2
Embodiment 3
BaTiO
3Atomic preparation
Under the atmospheric pressure at room condition, with the BaNO of 0.44mol
3And 0.4TiCl
4Solution (in the ratio of metering than Ba/Ti=1.1) adds in the raw material tank, adds aqueous slkali NaOH, regulates pH value 13.2; After in raw material tank, fully mixing, be transported in the air pressurized device through former material conveying pump then, the compressed air pressure of air pressurized device is 25MPa; Evenly stir simultaneously; The raw material that process pressurization and homogenization were handled is 370 ℃ high-pressure reactor continuously through temperature, and the raw material that has reacted obtains inorganic nano-particle through apparatus for supercooling and continuous filter unit.
Adopt and test with embodiment 1 identical method, the result shows that present embodiment prepares is the sheet BaTiO of the 50nm of good dispersion
3Product.
Embodiment 4
Mg (OH)
2Atomic preparation
Under the atmospheric pressure at room condition, with 0.5mol MgCl
2Add in the raw material tank, add aqueous slkali NaOH then, regulate pH value 10.5; After in raw material tank, fully mixing, carry in the air pressurized device through feedstock pump then, the compressed air pressure of air pressurized device is 30MPa; Evenly stir simultaneously; The raw material that process pressurization and homogenization were handled is 400 ℃ high-pressure reactor continuously through temperature, and the raw material that has reacted obtains inorganic nano-particle through apparatus for supercooling and continuous filter unit.
Adopt and test with embodiment 1 identical method, the result shows that present embodiment prepares is the block Mg (OH) of the 80nm of good dispersion
2Product.
Embodiment 5
MnFe
2O
4Atomic preparation
Under the atmospheric pressure at room condition, with 2mol/LMn (NO
3)
2With 2mol/L Fe (NO
3)
3Solution is (in measuring than Mn/Fe=1: 2.5 ratio) add in the raw material tank, add aqueous slkali NaOH, regulate pH value 13.2.After in raw material tank, fully mixing; Be transported in the air pressurized device through feedstock pump then; The compressed air pressure of air pressurized device is 28MPa, evenly stirs simultaneously, is 400 ℃ high-pressure reactor continuously through temperature through the raw material that pressurizes and homogenization was handled; The raw material that has reacted obtains inorganic nano-particle through apparatus for supercooling and continuous filter unit.
Adopt and test with embodiment 1 identical method, the result shows that present embodiment prepares is the square shape MnFe of the 100nm of good dispersion
2O
4Product.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be conspicuous concerning those skilled in the art, and defined General Principle can realize under the situation that does not break away from the spirit or scope of the present invention in other embodiments among this paper.Therefore, the present invention will can not be restricted to these embodiment shown in this paper, but will meet and principle disclosed herein and features of novelty the wideest corresponding to scope.
Claims (10)
1. an inorganic nano-particle synthesizes the water thermal reaction apparatus; Comprise the raw material mixing compression system, heated reaction system, cooling device and the filter that connect successively; It is characterized in that; Said raw material mixing compression system comprises raw material tank, the former material conveying pump that connects successively and has the air pressurized device of first agitating device that the outlet of said air pressurized device links to each other with the inlet of heated reaction system.
2. inorganic nano-particle according to claim 1 synthesizes the water thermal reaction apparatus, it is characterized in that said raw material tank has second agitating device.
3. inorganic nano-particle according to claim 1 synthesizes the water thermal reaction apparatus; It is characterized in that; Said heated reaction system comprises preheater and reactor; The entrance and exit of said preheater links to each other with reactor inlet with the outlet of said air pressurized device respectively, and the outlet of said reactor links to each other with the inlet of cooling device.
4. inorganic nano-particle according to claim 3 synthesizes the water thermal reaction apparatus, it is characterized in that said preheater and reactor have heating jacket respectively.
5. inorganic nano-particle according to claim 1 synthesizes the water thermal reaction apparatus, it is characterized in that, also comprises the back of the body valve that is arranged between said heated reaction system and the cooling device.
6. inorganic nano-particle according to claim 1 synthesizes the water thermal reaction apparatus, it is characterized in that, also comprises the pressure-regulating valve that is arranged between said cooling device and the filter.
7. inorganic nano-particle according to claim 1 synthesizes the water thermal reaction apparatus, it is characterized in that, also comprises the spray-drying installation that links to each other with said filter outlet.
8. according to the synthetic water thermal reaction apparatus of any described inorganic nano-particle of claim 1～7, it is characterized in that said air pressurized device can realize that pressure is adjustable in 1～40MPa scope.
9. according to the synthetic water thermal reaction apparatus of any described inorganic nano-particle of claim 1～7, it is characterized in that said air pressurized device can realize that temperature is adjustable in 20～100 ℃ of scopes.
10. according to the synthetic water thermal reaction apparatus of any described inorganic nano-particle of claim 1～7, it is characterized in that said heated reaction system can realize that temperature is adjustable in 100～400 ℃ of scopes.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103920641A (en) * | 2013-01-12 | 2014-07-16 | 唐山兴铭科技有限公司 | Industrial process for producing nano-particles |
| 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 |
| CN114644329A (en) * | 2022-04-12 | 2022-06-21 | 深圳沃伦特新能源科技有限公司 | Hydrothermal synthesis method of nano lithium ferric manganese phosphate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103920641A (en) * | 2013-01-12 | 2014-07-16 | 唐山兴铭科技有限公司 | Industrial process for producing nano-particles |
| 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 |
| CN114644329A (en) * | 2022-04-12 | 2022-06-21 | 深圳沃伦特新能源科技有限公司 | Hydrothermal synthesis method of nano lithium ferric manganese phosphate |
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