CN105107436B - A kind of method that film infiltration hydro-thermal continuously prepares nanometer oxide material - Google Patents
A kind of method that film infiltration hydro-thermal continuously prepares nanometer oxide material Download PDFInfo
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- CN105107436B CN105107436B CN201510509225.4A CN201510509225A CN105107436B CN 105107436 B CN105107436 B CN 105107436B CN 201510509225 A CN201510509225 A CN 201510509225A CN 105107436 B CN105107436 B CN 105107436B
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Abstract
The invention discloses the methods that a kind of film infiltration hydro-thermal continuously prepares nano-oxide, comprising the following steps: configuration metal salt solution and precipitant solution first;Film, which is carried out, by bimodulus permeability apparatus permeates hydro-thermal reaction;Washing;It is dry;It examines.The present invention is based on the thoughts that film infiltration and hydrothermal technique combine, salting liquid and precipitating reagent can be subjected to microring array reaction in micron even sub-micrometer scale using film osmosis process, pass through hydrothermal synthesis again, the nanometer oxide material that size tunable, monodisperse, crystallinity are high, particle diameter distribution is narrow can continuously be prepared, and realize continuous production, improve production efficiency.
Description
Technical field
The invention belongs to technical field of material chemistry, and in particular to a kind of film infiltration hydro-thermal continuously prepares the side of nano-oxide
Method.
Background technique
Currently, nano material is broadly that at least one dimension is in nanoscale range or by the scale in three-dimensional space
The general name for the ultrafine particles material that the substance of range is made of basic structural unit.Nanometer oxide material is a kind of high-precision
Thin inorganic nano material, since the substance of nano-scale has the skin effect totally different with macroscopic material, small-size effect, amount
Sub- dimensional effect, macro quanta tunnel effect and quantum confined effect have different from the light of common material, electricity, magnetic, heat, mechanics
With the performances such as machinery.The electricity that nanometer oxide material is widely used in due to its unique physical and chemical properties in recent years
The industry fields such as son, communication, aerospace, building, medical treatment.
The main preparation methods of nano material have the precipitation method, solvent (water) thermal method, microemulsion method, sol-gel method, heat point
Solution etc..The powder of hydro-thermal method preparation has many advantages, such as that grain growth is complete, partial size is small, is evenly distributed, particle agglomeration degree is small,
The presoma that hydro-thermal method nano materials obtain after needing to precipitate metal salt solution with precipitating reagent, which enters synthesis reactor, to carry out
Hydrothermal synthesis, therefore the mixed effect of salting liquid and precipitating reagent determines the quality of nano material after hydrothermal synthesis.Common two kinds
The mode that solution directly mixes easily causes undercompounding, particle agglomeration, partial size is not since its mixed-scale is in centimetres
It uniformly and can not continuous production.
Summary of the invention
The purpose of the present invention is to defect of the existing technology, a kind of combination is provided and uses for reference film infiltration and hydro-thermal skill
The method that the film infiltration hydro-thermal of the advantage of art continuously prepares nano-oxide.
Its technical solution is: a kind of method that film infiltration hydro-thermal continuously prepares nanometer oxide material, comprising the following steps:
1) metal salt solution and precipitant solution are configured first;
2) film is carried out by bimodulus permeability apparatus and permeates hydro-thermal reaction, by delivery pump respectively by metal salt solution and precipitating
Agent solution is defeated to be transported in the double ceramic membrane permeable reactive devices of immersion through metal salt solution entrance and precipitant solution entrance, and two kinds
Solution distinguishes permeation ceramic membrane under the effect of film pressure at both sides difference, controls temperature of reactor, two kinds of solution are respectively with droplet
Precipitation reaction occurs from micro-meter scale in the reactor for state, the slurry for completing reaction is passed through high-pressure delivery pump, into water
Thermal reaction apparatus, completes hydro-thermal reaction by heating zone, heat preservation zone and cooling area respectively, and hydro-thermal reaction equipment passes through conduction oil control
The temperature of three warm areas is made, the slurry after hydro-thermal is by ceramic-film tube after centrifugal pump pressurizes, and wherein slurry is passed through from ceramic-film tube
Enter washing procedure after the outflow of slurry outlet, foreign ion enters film permeable reactive device circular response after being discharged through fenestra;
3) it washs, the slurry after synthesis is continuously washed by ceramic membrane washing facility, until the impurity concentration in solution
< 500ppm;
4) dry, it is dried with spray dryer, control charging solid content 20 ~ 30%, 120 ~ 150 DEG C of outlet temperature;
5) it examines.
The metal salt solution can be inorganic salt solution, including nitrate, chloride, sulfate etc.;Metal salt is molten
Liquid may be organic metal salting liquid, including alkyl metal cpd and arylide compound etc., metallic solution concentration
For 0.1~2.0mol/L.
The bimodulus permeability apparatus includes that the double ceramic membrane permeable reactive devices of immersion and its metal salt solution being equipped with enter
Mouth and precipitant solution entrance, hydro-thermal reaction device and its heating zone being equipped with, heat preservation zone and cooling area, ceramic-film tube, high pressure
Delivery pump, centrifugal pump, said modules pass through placed in series.
The precipitant solution is ammonium hydrogen carbonate, sodium hydroxide, potassium hydroxide, sodium carbonate and ammonium hydroxide etc., and precipitating reagent is molten
Liquid concentration is 0.2~10mol/L, and the feed rate of the metal salt solution and precipitant solution is 200~1000L/ (m2
h)。
The double ceramic membrane permeable reactive devices of the immersion of the bimodulus permeability apparatus and washing are aluminium oxide with ceramic membrane
And zirconia composite ceramics, membrane tube aperture and washing are 10~200m with membrane tube aperture.
The reaction temperature of the bimodulus permeability apparatus is 20~50 DEG C.
The hydro-thermal reaction device uses high pressure hydrothermal synthesis device, and material is zirconium material, nickel material or titanium etc..
Hydro-thermal reaction device is heated up and is cooled down by conduction oil, and the heating rate of hydrothermal synthesis is 0.5~10 DEG C/min, drop
Warm rate is 1~10 DEG C/min, and holding temperature is 120~250 DEG C.
The concentration of the foreign ion is 0.1~8mol/L.
The pressure limit that the slurry pressurizes through centrifugal pump is 1~6MPa;After synthesis into ceramic membrane slurry pass through from
The pressure limit of heart pump pressurization is 1~6MPa, and cross-flow rate is 1.0~5.0m/s.
It, can be by salting liquid and heavy using film osmosis process the present invention is based on film infiltration and the thought that combines of hydrothermal technique
Shallow lake agent carries out microring array reaction in micron even sub-micrometer scale, then by hydrothermal synthesis, can continuously prepare size tunable,
The nanometer oxide material that monodisperse, crystallinity are high, particle diameter distribution is narrow, and realize continuous production, improve production efficiency.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of reversed film infiltration hydrothermal reactor of the invention;
Wherein, 1, the double ceramic membrane permeable reactive devices of immersion, 1-1, metal salt solution entrance, 1-2, precipitant solution enter
Mouthful, 2, hydro-thermal reaction device, 2-1, heating zone, 2-2, heat preservation zone, 2-3, cooling area.3, slurry outlet, 4, ceramic-film tube, 5,
High-pressure delivery pump, 6, centrifugal pump.
Fig. 2 is the stereoscan photograph of 1ZnO sample of the embodiment of the present invention;
Fig. 3 is the stereoscan photograph of 2TiO2 sample of the embodiment of the present invention;
Fig. 4 is the transmission electron microscope photo of 3ZrO2 sample of the embodiment of the present invention;
Fig. 5 is the transmission electron microscope photo of 4BaTiO3 sample of the embodiment of the present invention.
Specific embodiment
Referring to figs. 1 to 5, a kind of method that film infiltration hydro-thermal continuously prepares nanometer oxide material, comprising the following steps:
1) metal salt solution and precipitant solution are configured first;
2) film is carried out by bimodulus permeability apparatus and permeates hydro-thermal reaction, by delivery pump respectively by metal salt solution and precipitating
Agent solution is defeated to be transported to the double ceramic membrane permeable reactive devices 1 of immersion through metal salt solution entrance 1-1 and precipitant solution entrance 1-2
In, two kinds of solution distinguish permeation ceramic membrane under the effect of film pressure at both sides difference, control temperature of reactor, two kinds of solution are respectively with small
The state of drop, occurs precipitation reaction from micro-meter scale in the reactor, and the slurry for completing reaction is passed through high-pressure delivery pump
5, into hydro-thermal reaction device 2, hydro-thermal reaction is completed by heating zone 2-1, heat preservation zone 2-2 and cooling area 2-3 respectively, hydro-thermal is anti-
Equipment 2 is answered to control the temperature of three warm areas by conduction oil, the slurry after hydro-thermal passes through ceramic-film tube 4 after the pressurization of centrifugal pump 6,
Wherein slurry enters washing procedure from ceramic-film tube 4 after the outflow of slurry outlet 3, and foreign ion enters after being discharged through fenestra
Film permeable reactive device circular response;
3) it washs, the slurry after synthesis is continuously washed by ceramic membrane washing facility, until the impurity concentration in solution
< 500ppm;
4) dry, it is dried with spray dryer, control charging solid content 20 ~ 30%, 120 ~ 150 DEG C of outlet temperature;
5) it examines.
The metal salt solution can be inorganic salt solution, including nitrate, chloride, sulfate etc.;Metal salt is molten
Liquid may be organic metal salting liquid, including alkyl metal cpd and arylide compound etc., metallic solution concentration
For 0.1~2.0mol/L.
The bimodulus permeability apparatus includes that the double ceramic membrane permeable reactive devices 1 of immersion and its metal salt solution being equipped with enter
Mouth 1-1 and precipitant solution entrance 1-2, hydro-thermal reaction device 2 and its heating zone 2-1 being equipped with, heat preservation zone 2-2 and cooling area 2-
3, ceramic-film tube 4, high-pressure delivery pump 5, centrifugal pump 6, said modules pass through placed in series.
The precipitant solution is ammonium hydrogen carbonate, sodium hydroxide, potassium hydroxide, sodium carbonate and ammonium hydroxide etc., and precipitating reagent is molten
Liquid concentration is 0.2~10mol/L, and the feed rate of the metal salt solution and precipitant solution is 200~1000L/ (m2
h)。
The double ceramic membrane permeable reactive devices 1 of the immersion of the bimodulus permeability apparatus and washing are aluminium oxide with ceramic membrane
And zirconia composite ceramics, membrane tube aperture and washing are 10~200m with membrane tube aperture.
The reaction temperature of the bimodulus permeability apparatus is 20~50 DEG C.
The hydro-thermal reaction device 2 uses high pressure hydrothermal synthesis device, and material is zirconium material, nickel material or titanium etc..
Hydro-thermal reaction device 2 is heated up and is cooled down by conduction oil, and the heating rate of hydrothermal synthesis is 0.5~10 DEG C/min,
Rate of temperature fall is 1~10 DEG C/min, and holding temperature is 120~250 DEG C.
The concentration of the foreign ion is 0.1~8mol/L.
The pressure limit that the slurry pressurizes through centrifugal pump 6 is 1~6MPa;After synthesis into ceramic membrane slurry pass through from
The pressure limit of heart pump pressurization is 1~6MPa, and cross-flow rate is 1.0~5.0m/s.
Embodiment 1: the preparation of nano-ZnO
Compound concentration is 0.5mol/L zinc nitrate solution respectively and concentration is 0.4mol/L sodium hydroxide solution;
Film permeates hydro-thermal reaction.Metal salt solution and precipitant solution are transported to the double potteries of immersion respectively by delivery pump
In porcelain film permeable reactive device, two kinds of solution film pressure at both sides difference effect under respectively permeation ceramic membrane, control temperature of reactor, two
Respectively with the state of droplet precipitation reaction occurs from micro-meter scale in the reactor for kind solution;It will complete the slurry of reaction
By high-pressure delivery pump, into hydro-thermal reaction equipment, hydro-thermal reaction, control are completed by heating zone, heat preservation zone and cooling area respectively
Heating zone processed is warming up to 150 DEG C with 5 DEG C/min heating rate, keeps the temperature 150 DEG C/5h, is then cooled to room with 3 DEG C/min rate
Temperature;For slurry after hydro-thermal by ceramic-film tube after centrifugal pump pressurizes, wherein slurry enters washing procedure after membrane tube outflow, miscellaneous
Matter ion enters film permeable reactive device circular response after being discharged through fenestra.
Washing.Slurry after synthesis is continuously washed by ceramic membrane washing facility, until the nitrate concentration in solution
< 300ppm, Na ion concentration < 500ppm.
It is dried with spray dryer, control charging solid content 20 ~ 30%, 120 ~ 150 DEG C of outlet temperature.
It examines.
Embodiment 2: the preparation of nano TiO 2
Compound concentration is 1.0mol/L titanium tetrachloride solution respectively and concentration is 5mol/L ammonium hydroxide;
Film permeates hydro-thermal reaction.Metal salt solution and precipitant solution are transported to the double potteries of immersion respectively by delivery pump
In porcelain film permeable reactive device, two kinds of solution film pressure at both sides difference effect under respectively permeation ceramic membrane, control temperature of reactor, two
Respectively with the state of droplet precipitation reaction occurs from micro-meter scale in the reactor for kind solution;It will complete the slurry of reaction
By high-pressure delivery pump, into hydro-thermal reaction equipment, hydro-thermal reaction, control are completed by heating zone, heat preservation zone and cooling area respectively
Heating zone processed is warming up to 180 DEG C with 5 DEG C/min heating rate, keeps the temperature 180 DEG C/3h, is then cooled to room with 3 DEG C/min rate
Temperature;For slurry after hydro-thermal by ceramic-film tube after centrifugal pump pressurizes, wherein slurry enters washing procedure after membrane tube outflow, miscellaneous
Matter ion enters film permeable reactive device circular response after being discharged through fenestra.
Washing.Slurry after synthesis is continuously washed by ceramic membrane washing facility, until the foreign ion in solution is dense
Spend < 300ppm;
It is dried with spray dryer, control charging solid content 20 ~ 30%, 120 ~ 150 DEG C of outlet temperature.
It examines.
Embodiment 3: the preparation of nanometer Zirconia
Compound concentration is 0.8mol/L% zirconyl chloride solution respectively and concentration is 5mol/L ammonium hydroxide;
Film permeates hydro-thermal reaction.Metal salt solution and precipitant solution are transported to the double potteries of immersion respectively by delivery pump
In porcelain film permeable reactive device, two kinds of solution film pressure at both sides difference effect under respectively permeation ceramic membrane, control temperature of reactor, two
Respectively with the state of droplet precipitation reaction occurs from micro-meter scale in the reactor for kind solution;It will complete the slurry of reaction
By high-pressure delivery pump, into hydro-thermal reaction equipment, hydro-thermal reaction, control are completed by heating zone, heat preservation zone and cooling area respectively
Heating zone processed is warming up to 140 DEG C with 5 DEG C/min heating rate, keeps the temperature 140 DEG C/12h, is then cooled to room with 3 DEG C/min rate
Temperature;For slurry after hydro-thermal by ceramic-film tube after centrifugal pump pressurizes, wherein slurry enters washing procedure after membrane tube outflow, miscellaneous
Matter ion enters film permeable reactive device circular response after being discharged through fenestra.
Washing.Slurry after synthesis is continuously washed by ceramic membrane washing facility, until the foreign ion in solution is dense
Spend < 300ppm;
It is dried with spray dryer, control charging solid content 20 ~ 30%, 120 ~ 150 DEG C of outlet temperature.
It examines.
Embodiment 4: the preparation of nano-BaTiO_3 powder
The mixed solution of titanium tetrachloride and barium chloride is prepared according to molar ratio Ba/Ti=1.05 ~ 1.5, titanium tetrachloride concentration is
1.0mol/L titanium tetrachloride solution;Compound concentration is 5mol/L ammonium hydroxide;
Film permeates hydro-thermal reaction.Metal salt solution and precipitant solution are transported to the double potteries of immersion respectively by delivery pump
In porcelain film permeable reactive device, two kinds of solution film pressure at both sides difference effect under respectively permeation ceramic membrane, control temperature of reactor, two
Respectively with the state of droplet precipitation reaction occurs from micro-meter scale in the reactor for kind solution;It will complete the slurry of reaction
By high-pressure delivery pump, into hydro-thermal reaction equipment, hydro-thermal reaction, control are completed by heating zone, heat preservation zone and cooling area respectively
Heating zone processed is warming up to 210 DEG C with 5 DEG C/min heating rate, keeps the temperature 210 DEG C/6h, is then cooled to room with 3 DEG C/min rate
Temperature;For slurry after hydro-thermal by ceramic-film tube after centrifugal pump pressurizes, wherein slurry enters washing procedure after membrane tube outflow, miscellaneous
Matter ion enters film permeable reactive device circular response after being discharged through fenestra;
Washing.Slurry after synthesis is continuously washed by ceramic membrane washing facility, until the foreign ion in solution is dense
Spend < 300ppm;
It is dried with spray dryer, control charging solid content 20 ~ 30%, 120 ~ 150 DEG C of outlet temperature;
It examines.
What has been described above is only a preferred embodiment of the present invention, it is noted that for those of ordinary skill in the art
For, without departing from the concept of the premise of the invention, various modifications and improvements can be made, belongs to guarantor of the invention
Protect range.
Claims (10)
1. a kind of method that film infiltration hydro-thermal continuously prepares nanometer oxide material, it is characterised in that: the following steps are included:
1) metal salt solution and precipitant solution are configured first;
2) film is carried out by double film permeability apparatus permeate hydro-thermal reaction, it is respectively that metal salt solution and precipitating reagent is molten by delivery pump
Liquid is defeated to be transported in the double ceramic membrane permeable reactive devices of immersion through metal salt solution entrance and precipitant solution entrance, two kinds of solution
The permeation ceramic membrane respectively under the effect of film pressure at both sides difference, controls temperature of reactor, two kinds of solution respectively with the state of droplet,
Precipitation reaction occurs from micro-meter scale in the reactor, the slurry for completing reaction is passed through into high-pressure delivery pump, it is anti-into hydro-thermal
Device is answered, completes hydro-thermal reaction by heating zone, heat preservation zone and cooling area respectively, hydro-thermal reaction equipment passes through conduction oil control three
The temperature of a warm area, the slurry after hydro-thermal is by ceramic-film tube after centrifugal pump pressurizes, and wherein slurry is from ceramic-film tube through slurry
Enter washing procedure after outlet outflow, foreign ion enters film permeable reactive device circular response after being discharged through fenestra;
3) it washs, the slurry after synthesis is continuously washed by ceramic membrane washing facility, until the impurity concentration in solution <
500ppm;
4) dry, it is dried with spray dryer, control charging solid content 20~30%, 120~150 DEG C of outlet temperature;
5) it examines;
Wherein, the heating rate of the hydro-thermal reaction is 0.5~10 DEG C/min, and rate of temperature fall is 1~10 DEG C/min, holding temperature
It is 120~250 DEG C;
The pressure limit that the slurry pressurizes through centrifugal pump is 1~6MPa.
2. the method that film infiltration hydro-thermal according to claim 1 continuously prepares nanometer oxide material, it is characterised in that:
The metal salt solution is inorganic salt solution, and the inorganic salts include nitrate, chloride or sulfate, or
The metal salt solution is organic metal salting liquid, and the organic metal salt includes alkyl metal cpd and aromatic radical
Metallic compound;
The metal salt solution concentration is 0.1~2.0mol/L.
3. the method that film infiltration hydro-thermal according to claim 1 continuously prepares nanometer oxide material, it is characterised in that: institute
The double film permeability apparatus stated include the double ceramic membrane permeable reactive device of immersion and its metal salt solution entrance and precipitating reagent that are equipped with
Solution inlet, hydro-thermal reaction device and its heating zone being equipped with, heat preservation zone and cooling area, ceramic-film tube, high-pressure delivery pump, centrifugation
Pump, said modules pass through placed in series.
4. the method that film infiltration hydro-thermal according to claim 1 continuously prepares nanometer oxide material, it is characterised in that: institute
The precipitating reagent stated be selected from ammonium hydrogen carbonate, sodium hydroxide, potassium hydroxide, sodium carbonate and ammonium hydroxide, precipitant solution concentration be 0.2~
The feed rate of 10mol/L, the metal salt solution and precipitant solution is 200~1000L/ (m2·h)。
5. the method that film infiltration hydro-thermal according to claim 1 or 3 continuously prepares nanometer oxide material, feature exist
It with ceramic membrane is aluminium oxide and oxidation in the double ceramic membrane permeable reactive devices of the immersion of: double film permeability apparatus and washing
Zirconium composite ceramics, membrane tube aperture and washing are 10~200m with membrane tube aperture.
6. the method that film infiltration hydro-thermal according to claim 3 continuously prepares nanometer oxide material, it is characterised in that: institute
The reaction temperature for the double film permeability apparatus stated is 20~50 DEG C.
7. the method that film infiltration hydro-thermal according to claim 3 continuously prepares nanometer oxide material, it is characterised in that: institute
The hydro-thermal reaction device stated uses high pressure hydrothermal synthesis device, and material is zirconium material, nickel material or titanium.
8. the method that film infiltration hydro-thermal according to claim 3 continuously prepares nanometer oxide material, it is characterised in that: water
Thermal reaction apparatus is heated up and is cooled down by conduction oil.
9. the method that film infiltration hydro-thermal according to claim 1 continuously prepares nanometer oxide material, it is characterised in that: institute
The concentration for the foreign ion stated is 0.1~8mol/L.
10. the method that film infiltration hydro-thermal according to claim 1 continuously prepares nanometer oxide material, it is characterised in that:
Pressure limit pressurize through centrifugal pump of slurry after the hydro-thermal into ceramic membrane is 1~6MPa, cross-flow rate for 1.0~
5.0m/s。
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Citations (3)
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CN103663508A (en) * | 2012-09-07 | 2014-03-26 | 中国科学院大连化学物理研究所 | Method for preparing low-specific surface area magnesium hydroxide flame retardant by using microchannel reactor |
CN103950967A (en) * | 2014-04-25 | 2014-07-30 | 南京工业大学 | Method for continuously preparing nanometer zinc oxide in membrane reactor |
CN104649333A (en) * | 2014-12-01 | 2015-05-27 | 马来鹏 | Method for continuously preparing nanometer Fe3O4 |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN103663508A (en) * | 2012-09-07 | 2014-03-26 | 中国科学院大连化学物理研究所 | Method for preparing low-specific surface area magnesium hydroxide flame retardant by using microchannel reactor |
CN103950967A (en) * | 2014-04-25 | 2014-07-30 | 南京工业大学 | Method for continuously preparing nanometer zinc oxide in membrane reactor |
CN104649333A (en) * | 2014-12-01 | 2015-05-27 | 马来鹏 | Method for continuously preparing nanometer Fe3O4 |
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