CN1125672C - Jet coprecipitation device and method for preparing nano material - Google Patents
Jet coprecipitation device and method for preparing nano material Download PDFInfo
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- CN1125672C CN1125672C CN 00112586 CN00112586A CN1125672C CN 1125672 C CN1125672 C CN 1125672C CN 00112586 CN00112586 CN 00112586 CN 00112586 A CN00112586 A CN 00112586A CN 1125672 C CN1125672 C CN 1125672C
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- reaction vessel
- straight tube
- way pipe
- jet
- triangular flask
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- Expired - Fee Related
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- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 16
- 238000000975 co-precipitation Methods 0.000 title claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 35
- 239000002245 particle Substances 0.000 claims abstract description 29
- 238000005507 spraying Methods 0.000 claims abstract description 21
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 15
- 239000003513 alkali Substances 0.000 claims abstract description 3
- 150000003839 salts Chemical class 0.000 claims abstract description 3
- 239000000376 reactant Substances 0.000 claims description 17
- 230000006911 nucleation Effects 0.000 claims description 16
- 238000010899 nucleation Methods 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 12
- 238000005842 biochemical reaction Methods 0.000 claims description 9
- 239000012295 chemical reaction liquid Substances 0.000 claims description 9
- 238000001556 precipitation Methods 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 239000000084 colloidal system Substances 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract description 2
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 2
- 150000004706 metal oxides Chemical class 0.000 abstract description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 abstract 1
- 229910007486 ZnGa2O4 Inorganic materials 0.000 abstract 1
- 239000010419 fine particle Substances 0.000 abstract 1
- 229910001510 metal chloride Inorganic materials 0.000 abstract 1
- 239000011858 nanopowder Substances 0.000 abstract 1
- 150000002823 nitrates Chemical class 0.000 abstract 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 16
- 239000012530 fluid Substances 0.000 description 13
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 6
- 230000001476 alcoholic effect Effects 0.000 description 6
- 230000033001 locomotion Effects 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000000693 micelle Substances 0.000 description 5
- 238000009792 diffusion process Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(III) nitrate Inorganic materials [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001552 radio frequency sputter deposition Methods 0.000 description 2
- 238000005118 spray pyrolysis Methods 0.000 description 2
- 230000002123 temporal effect Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000333 cerium(III) sulfate Inorganic materials 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910000373 gallium sulfate Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000010349 pulsation Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000001119 stannous chloride Substances 0.000 description 1
- 235000011150 stannous chloride Nutrition 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Landscapes
- Physical Or Chemical Processes And Apparatus (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a spraying coprecipitation device and a method for preparing a nano material. One or more metal chlorides, sulfates, nitrates or other soluble salts, ammonia water, NaOH or other alkali are mixed in a device and sprayed into a reaction vessel, and ZnFe prepared by the method2O4、ZnGa2O4、SnO2The metal oxide particles are uniformly distributed and have fine particles, and nano powder of about 10 nanometers is generated.
Description
Affiliated technical field
The present invention relates to field of nano material preparation, particularly a kind of spraying codepostion device and method for preparing nano material.
These apparatus and method are improved traditional method-chemical coprecipitation for preparing nano material.The ZnFe for preparing with this method
2O
4, ZnGa
2O
4, SnO
2Tiny Deng metal oxide particle even size distribution, particle, produce the nanometer powder about 10 nanometers.
Background technology
Common preparation of nanomaterials has following several: sol-gal process, spray pyrolysis, RF sputtering method, chemical coprecipitation etc.
In these preparation methods, sol-gal process, spray pyrolysis, RF sputtering method etc. generally all need comparatively valuable equipment and complex process.And chemical coprecipitation has that equipment is cheap relatively, technology simple, the advantage such as easy of mixing, so occupy important position in the preparation of material.
But in traditional chemical coprecipitation reaction, the mixing of reactant liquor is the mode that adopts titration.When the drop of a certain reactant liquor enters in another reactant liquor system, surrounded by another reactant liquor, molecular diffusion and nucleation are reflected at the drop surface carries out, the molecular amounts that can participate in reaction seldom, so the nucleation number is also less.The nucleus that forms diffuses into the reactant liquor system, and further growth is being carried out the one-tenth nuclear reaction again on other drop surfaces simultaneously, carries out simultaneously on the nucleation of crystal and the growth macroscopic view.In sum, the particle of this method growth, particle size can be bigger relatively, and the distribution of particle size can be compared broad.
Summary of the invention
The apparatus and method that the objective of the invention is traditional chemical coprecipitation technology is prepared material are improved, invented the spraying codepostion method, utilize this apparatus and method can prepare that particle size distribution is even, particle is tiny, produce the following nanometer powder of 10 nanometers.
For be evenly distributed degree and improve performance of the particle size that improves the preparation powder sample, reduce particle size, the present invention improves traditional preparation method-chemical coprecipitation, designed chemical spraying codepostion subtraction unit (as shown in Figure 1), purpose is the nucleation of crystal grain and growth course are separated, fast a large amount of nucleation, evenly growth.Technical scheme of the present invention is: a kind of injection chemical coprecipitation device, comprise reactant liquor triangular flask (1), straight tube (2), gas cylinder (3), flowmeter (4), three-way pipe (5), jet (6), reaction vessel (7), and it is characterized in that:
Two reactant liquor triangular flasks (1) are connected with gas cylinder (3) by straight tube (2), two reactant liquor triangular flasks (1) are connected with two flowmeters (4) by straight tube (2) again, the following three-way pipe (5) and the jet (6) of connecting of two flowmeters, wherein the diameter of three-way pipe (5) is 0.4cm, and jet (6) is inserted in the reaction vessel (7).
A kind ofly prepare the method for nano material, it is characterized in that with spraying codepostion device:
Adopt chloride, sulfate, nitrate or other solubility salts and ammoniacal liquor, NaOH or other alkali of one or more metals, in device, mix, spurt into reaction vessel, generate nano material;
In the spraying codepostion device, compressed air is by flowing along straight tube (2) fast by colloid in gas cylinder (3) the driving a reaction liquid triangular flask (1) and ammoniacal liquor, enter flowmeter (4), locate the concurrent biochemical reaction of rapid mixing at three-way pipe (5), mixed liquor generates the nanometer powder precipitation after jet (6) is injected reaction vessel (7).
Reactant liquor triangular flask (1) mixes in three-way pipe (5), and the time that the straight tube of flowing through (2) enters reaction vessel (7) is about 0.1s, and nucleation is reflected in the straight tube carries out, and the nucleus of formation enters reaction vessel, carries out growth course under uniform temperature and stirring condition;
The diameter of three-way pipe (5) is 0.4cm, flow 10ml/s, the kinematic viscosity v=0.897 of water * 10 when getting 25 ℃
-6m
2/ s, Reynolds number are 3.5 * 10
3, greater than critical Reynolds number, flow regime is a turbulent flow;
Injection method can separately carry out nucleation and growth course: abundant hybrid reaction in pipeline at first, a large amount of nucleation, continued growth in reaction vessel (7) then, thereby the particle that obtains that crystalline form is complete, particle is tiny, is evenly distributed.
The invention has the beneficial effects as follows: traditional chemical coprecipitation is improved, it is cheap not only to have inherited traditional chemical coprecipitation equipment price, the simple advantage of technical process, and in the methods of the invention, the one-tenth nuclear reaction of particle separates with the developmental process of particle, overcome the shortcoming of traditional chemical coprecipitation, thereby obtain that particle is tiny, nano material is evenly distributed.
Description of drawings is elaborated to embodiment below in conjunction with accompanying drawing.Fig. 1 is the spraying codepostion device of preparation nano material.Fig. 2 is the velocity variations of turbulent flow in the spraying codepostion method of preparation nano material.
In Fig. 1, compressed air is by gas cylinder 3 driving a reaction liquid triangular flasks 1 (colloid and ammonia Water) flow along straight tube 2 fast, enter flowmeter 4, concurrent in three-way pipe 5 place's rapid mixing Biochemical reaction, mixed liquor are injected reaction vessel 7 by jet 6 at last, generate nanometer powder Precipitation.
In the spraying codepostion device of preparation nano material, reactant liquor triangular flask 1 is at three-way pipe 5 The middle mixing, the time that the straight tube 2 of flowing through enters reaction vessel 7 is about 0.1s. During this period of time enough Reactant liquor fully mixes and reaction mutually. Therefore nucleation reacts completely and carries out in straight tube 2. Shape The nucleus that becomes enters reaction vessel 7, carries out growth course under uniform temperature and stirring condition. Spray Shooting method can separately carry out nucleation and growth course, abundant hybrid reaction in pipeline at first, A large amount of nucleation, then continued growth in reaction vessel. Adopt this method, can obtain crystalline substance The particle that shape is complete, particle is tiny, be evenly distributed.
Fig. 2 is the velocity variations of turbulent flow in the spraying codepostion method of preparation nano material. In chemical spraying codepostion method, finding when the three-way pipe place is mixed has turbulent flow to exist, according to stream It is many little micelles that the theory of mechanics, DIFFUSION IN TURBULENCE can make fluid breakup. Different micelles Component be different, under extreme situation, contacted two micelles are respectively two kinds of reactions The pure component of liquid. Molecular diffusion makes component react by the border between the micelle. Micelle more Little, provide the area of molecular diffusion more big, be conducive to the carrying out of accelerated reaction. Thereby participate in anti-The molecular amounts of answering is a lot, so the nucleation number also increases. The nucleus that forms enters from jet The reactant liquor system is grown, thereby nucleation and the growth of crystal are separately carried out. So this The particle of method growth, particle size can be smaller relatively, and the distribution of particle size can be compared More even.
In hydrodynamics, the fluid motion that no matter is produced by the sort of mode, because of velocity magnitude not With, take physical properties of fluids and geometrical condition into consideration, two kinds of different shapes will appear in fluid motion Attitude: laminar flow and turbulent flow. In both cases, the immanent structure of fluid motion and showing VELOCITY DISTRIBUTION, resistance law etc. are fully different.
During laminar flow, the fluid particle by space each point in the pipeline has definite speed, if stream The flow of body by straight tube be temporal evolution not, and the speed of each point will be not in time yet in the pipe so Change. Then different during turbulent flow, by managing the fluid particle speed of interior each point, have certain with Machine, though the temporal evolution not of the fluid flow by straight tube, the fluid speed of each point in the pipe Degree is but with the pulsation of higher Frequency generated all directions, as shown in Figure 2. Different flow regimes has the different characteristics of motion, therefore needs the flow state to declare Not. When certain fluid flows in the pipeline of a fixed-caliber, there is a critical speed Ucr, Less than this speed, flow regime is laminar flow; Greater than this speed, mobile transition is turbulent flow. Critical Speed is relevant with caliber d with viscosity, mu, the density p of fluid, is made up of these four physical quantitys Dimensionless number NRe is called Reynolds number:
Reynolds number can be used for judging the state of fluid motion, when Reynolds number equals critical value, and layer Stream is turbulent flow with transition. Usually get for the critical Reynolds number during Fluid Flow in A in the pipe on the engineering Be 2100.
The experiment condition of spraying codepostion method is: three-way pipe diameter 0.4cm, flow 10ml/s, water movement viscosity v=0.897 * 10 when getting 25 ℃-6m
2/ s, as calculated, Reynolds number is 3.5 * 103, Greater than critical Reynolds number, flow regime is turbulent flow.
Specific embodiment embodiment 1: the ZnFe of spraying codepostion method preparation
2O
4:
Respectively be dissolved in alcoholic solution by certain molar ratio soluble-salt ferric nitrate and dissolvable oxides zinc oxide, mix then in the triangular flask 1 of embedded device, adding concentration in another triangular flask 1 is the ammoniacal liquor of 0.1mol/L, compressed air flows along straight tube 2 fast by gas cylinder 3 driving a reaction liquid (mixed liquor and ammoniacal liquor) then, flow into flowmeter 4, in the concurrent biochemical reaction of three-way pipe 5 rapid mixing, mixed liquor is spurted into reaction vessel 7 by jet 6 at last and is generated precipitation.With its oven dry, sintering, the result of test is about 10 nanometers then.Embodiment 2: the ZnGa of spraying codepostion method preparation
2O
4:
Respectively be dissolved in alcoholic solution by certain molar ratio soluble-salt gallium sulfate and dissolvable oxides zinc oxide, mix then in the triangular flask 1 of embedded device, adding concentration in another triangular flask 1 is the ammoniacal liquor of 0.1mol/L, compressed air flows along straight tube 2 fast by gas cylinder 3 driving a reaction liquid (mixed liquor and ammoniacal liquor) then, flow into flowmeter 4, in the concurrent biochemical reaction of three-way pipe 5 rapid mixing, mixed liquor is injected reaction vessel 7 by jet 6 at last and is generated precipitation.Then with its oven dry, sintering, test found that particle size is about 10 nanometers.Embodiment 3: the Zn of spraying codepostion method preparation
2SnO
4:
Respectively be dissolved in alcoholic solution by certain molar ratio soluble-salt stannous chloride and dissolvable oxides zinc oxide, mix then in the triangular flask 1 of embedded device, adding concentration in another triangular flask 1 is the ammoniacal liquor of 0.1mol/L, compressed air flows along straight tube 2 fast by gas cylinder 3 driving a reaction liquid (mixed liquor and ammoniacal liquor) then, flow into flowmeter 4, in the concurrent biochemical reaction of three-way pipe 5 rapid mixing, mixed liquor is injected reaction vessel 7 by jet 6 at last and is generated precipitation.Then with its oven dry, sintering, test found that particle size is about 15 nanometers.Embodiment 4: the Fe of spraying codepostion method preparation
2O
3:
The soluble-salt ferric nitrate is dissolved in the alcoholic solution, then in the triangular flask 1 of embedded device, adding concentration in another triangular flask 1 is the ammoniacal liquor of 0.1mol/L, compressed air flows along straight tube 2 fast by gas cylinder 3 driving a reaction liquid (comprising ammoniacal liquor) then, flow into flowmeter 4, in the concurrent biochemical reaction of three-way pipe 5 place's rapid mixing, mixed liquor is injected reaction vessel 7 by jet 6 at last and is generated precipitation.Then with its oven dry, sintering, test found that particle size is about 15 nanometers.Embodiment 5: the CeO of spraying codepostion method preparation
2:
The soluble-salt cerous sulfate is dissolved in the alcoholic solution, then in the triangular flask 1 of embedded device, adding concentration in another triangular flask 1 is the ammoniacal liquor of 0.1mol/L, compressed air flows along straight tube 2 fast by gas cylinder 3 driving a reaction liquid (comprising ammoniacal liquor) then, flow into flowmeter 4, in the concurrent biochemical reaction of three-way pipe 5 place's rapid mixing, mixed liquor is injected reaction vessel 7 by jet at last and is generated precipitation.Then with its oven dry, sintering, test found that particle size is about 15 nanometers.Embodiment 6: the SnO of spraying codepostion method preparation
2:
The inferior tin of solubility chlorination is dissolved in the alcoholic solution, then in the triangular flask 1 of embedded device, adding concentration in another triangular flask 1 is the NaOH of 0.1mol/L, compressed air flows along straight tube 2 fast by gas cylinder 3 driving a reaction liquid (comprising NaOH) then, flow into flowmeter 4, in the concurrent biochemical reaction of three-way pipe 5 place's rapid mixing, mixed liquor is injected reaction vessel 7 by jet 6 at last and is generated precipitation.Then with its oven dry, sintering, test found that particle size is about 10 nanometers.
Claims (2)
1. one kind is sprayed the chemical coprecipitation device, comprises reactant liquor triangular flask (1), straight tube (2), gas cylinder (3), flowmeter (4), three-way pipe (5), jet (6), reaction vessel (7), it is characterized in that:
Two reactant liquor triangular flasks (1) are connected with gas cylinder (3) by straight tube (2), two reactant liquor triangular flask reactant liquors (1) are connected with two flowmeters (4) by straight tube (2) again, the following three-way pipe (5) and the jet (6) of connecting of two flowmeters, wherein the diameter of three-way pipe (5) is 0.4cm, and jet (6) is inserted in the reaction vessel (7).
2. one kind prepares the method for nano material with spraying codepostion device, it is characterized in that:
Adopt chloride, sulfate, nitrate or other solubility salts and ammoniacal liquor, NaOH or other alkali of one or more metals, in device, mix, spurt into reaction vessel, generate nano material;
In the spraying codepostion device, compressed air flows along straight tube (2) fast by colloid in gas cylinder (3) the driving a reaction liquid triangular flask (1) and ammoniacal liquor, enter flowmeter (4), locate the concurrent biochemical reaction of rapid mixing at three-way pipe (5), mixed liquor generates the nanometer powder precipitation after jet (6) is injected reaction vessel (7);
Reactant liquor triangular flask (1) mixes in three-way pipe (5), and the time that the straight tube of flowing through (2) enters reaction vessel (7) is about 0.1s, and nucleation is reflected in the straight tube carries out, and the nucleus of formation enters reaction vessel, carries out growth course under uniform temperature and stirring condition;
The diameter of three-way pipe (5) is 0.4cm, flow 10ml/s, the kinematic viscosity v=0.897 of water * 10 when getting 25 ℃
-6m
2/ s, Reynolds number are 3.5 * 10
3, greater than critical Reynolds number, flow regime is a turbulent flow;
Injection method can separately carry out nucleation and growth course: abundant hybrid reaction in pipeline at first, a large amount of nucleation, continued growth in reaction vessel (7) then, thereby the particle that obtains that crystalline form is complete, particle is tiny, is evenly distributed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00112586 CN1125672C (en) | 2000-09-27 | 2000-09-27 | Jet coprecipitation device and method for preparing nano material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00112586 CN1125672C (en) | 2000-09-27 | 2000-09-27 | Jet coprecipitation device and method for preparing nano material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1290572A CN1290572A (en) | 2001-04-11 |
| CN1125672C true CN1125672C (en) | 2003-10-29 |
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ID=4582438
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 00112586 Expired - Fee Related CN1125672C (en) | 2000-09-27 | 2000-09-27 | Jet coprecipitation device and method for preparing nano material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1125672C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100460102B1 (en) * | 2002-07-15 | 2004-12-03 | 한화석유화학 주식회사 | Method for preparing fine metal oxide particles |
| CN1883786B (en) * | 2005-06-24 | 2010-07-28 | 鸿富锦精密工业（深圳）有限公司 | Nanoparticle Synthesis Method |
| CN105645959B (en) * | 2015-12-25 | 2018-06-19 | 江苏师范大学 | Y2O3The spraying codepostion preparation method of base transparent ceramic powder |
| CN106977206A (en) * | 2017-02-22 | 2017-07-25 | 江苏师范大学 | Spraying codepostion prepares the continuation method of high dispersancy nano oxide powder |
| SG10201905946YA (en) * | 2019-06-26 | 2021-01-28 | Nat Univ Singapore | Systems and Methods for Fabricating Nanoparticles |
-
2000
- 2000-09-27 CN CN 00112586 patent/CN1125672C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1290572A (en) | 2001-04-11 |
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