CN104709931A - Nanometer hydrotalcite-like compound preparation method - Google Patents
Nanometer hydrotalcite-like compound preparation method Download PDFInfo
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- CN104709931A CN104709931A CN201310690715.XA CN201310690715A CN104709931A CN 104709931 A CN104709931 A CN 104709931A CN 201310690715 A CN201310690715 A CN 201310690715A CN 104709931 A CN104709931 A CN 104709931A
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- reaction
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- hydrotalcite
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
- C01F7/784—Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
- C01F7/785—Hydrotalcite
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The present invention relates to a nanometer hydrotalcite-like compound preparation method, wherein a flowing focusing type microchannel reactor is adopted, and gas introducing microscopic mixing strengthening is performed to achieve the controllable preparation of the nanometer hydrotalcite-like compound. According to the preparation method, a water-soluble divalent metal salt raw material A<2+>X and a trivalent metal salt raw material B<3+>X are mixed according to a certain concentration, a soluble strong alkali or a mixture of a strong alkaline and a carbonate is prepared into an aqueous solution, the metal salt solution, gas and the alkaline solution concurrently enter from the three inlets of the flowing focusing type microchannel reactor, and are mixed and react in the microchannel, and the obtained precipitate is subjected to a hydrothermal treatment, centrifugation and drying so as to obtain the hydrotalcite-like compound material. According to the present invention, the obtained hydrotalcite-like compound has advantages of short residence time, high flux, controllable particle size, narrow particle size distribution, and the like; and compared with the conventional microchannel reactor, the microchannel reactor of the present invention has the following characteristics that: the gas inlet channel is additionally arranged on the structure, and the gas is introduced during the process, such that the mixing effect is further strengthened, the product particle size is uniform, and the clogging problem of the microchannel reactor in the nanometer material synthesis process can be solved.
Description
Technical field
The present invention relates to a kind of preparation method of nano hydrotalcite, particularly adopt flow focusing type micro passage reaction, by introducing the nano hydrotalcite preparation method of gas strengthening reaction process, belonging to field of nano material preparation.
Background technology
Layered double hydroxide (Layered Double Hydroxides, LDHs), is also called houghite, is the important anionic clay materials of a class.LDHs main body laminate is positively charged double-metal hydroxide, and interlayer is electronegative intercalant anion, and main body laminate institute is positively charged makes whole houghite molecule become electric neutrality with interlayer anion institute is electronegative.Because bulk in LDHs body layer plate metal composition, interlayer anion kind and quantity, layer etc. all has adjustable sex change, LDHs has broad application prospects in fields such as catalytic material, sorbing material, biology/medical materials.
For houghite, preparation method the most common in prior art is liquid-phase precipitation method, usually carries out in batch stirred tank reactor.Wang Rongtao etc. (functional materials, 2009,40 (12), 2119-2122) the nano-calcium carbonate root type magnesium aluminum-hydrotalcite that adopted liquid-phase precipitation method to prepare.Xie Xianmei etc. (chemistry of fuel journal, 2003,31 (6), 620-623) the NiMgAl ternary hydrotalcite that adopted liquid-phase precipitation method to prepare.But because microcosmic mixing efficiency in stirred-tank reactor is poor, temperature distributing disproportionation, in still, the nucleation rate of different positions differs comparatively large with growth rate, make conventional production methods exist Granularity Distribution inequality, batch between the problem such as poor repeatability.For batch stirred tank reactor, for reaching the Homogeneous phase mixing of microscopic units, taking often high energy consumption as cost, being unfavorable for industrial production.For make to prepare via liquid-phase precipitation method nano hydrotalcite homogeneous grain diameter, stable performance, microcosmic mixing can be strengthened in the urgent need to a kind of and conduct heat and there is the technology of less energy-consumption.
Micro-Chemical Engineering Technology is the Environment Science field of the multi-crossed disciplines that early 1990s rises.The principal feature of this technology adopts characteristic dimension to realize various unit operation and reaction process in tens of microchannel to hundreds of micron dimension.Because channel size significantly reduces, Mass and heat transfer process is significantly strengthened, and can increase substantially the utilising efficiency of the energy and the throughput of unit volume in reaction process, realizes chemical process strengthening, microminiaturized and greenization.In recent years, utilize micro-Chemical Engineering Technology to prepare extensive concern that nano material has caused academia and industry member.But, in micro passage reaction, carry out report prepared by houghite less.Abello etc. (Advanced Materials, 2006,18 (18), 2436-2439) disclose a kind of method that small volume reactor prepares hydrotalcite, and this reactor outer wall is equipped with fixed blade, and rotor is equipped with in bottom, turns scooter 24000rpm.Carry out enhancing mixed by the liquid of outer wall knife cut high speed rotating during reaction, but there is agglomeration traits in gained hydrotalcite product.In addition because rotor high-speed rotates, energy consumption is high, is unfavorable for industrial production.Patent CN103011254A discloses a kind of preparation method adopting T-shaped micro passage reaction to prepare acrylic/hydrotalcite-like nano monolithic.Known, the channel size of micro passage reaction is tens of between hundreds of micron, and the problem using it for the challenge of nano material synthesis most how to solve blocking.Patent CN103011254A do not relate to about blockage problem discussion with how to solve the essence way of blockage problem, particularly when preparing carbonate form sodium rice hydrotalcite, material in microchannel is easy to blocking channel, and this patent does not relate to the synthesis of the carbonate form sodium rice hydrotalcite of material settling out.(the Industrial & engineering chemistry research such as Shirure, 2005,44 (15), 5500-5507) disclose a kind of method that narrow passage reactor prepares houghite, but products obtained therefrom particle diameter is all greater than 10 μm.Known, powder body material is only in nanoscale just can show with block diverse excellent properties, although and Shirure etc. prepare hydrotalcite-like materials by narrow passage microreactor, because houghite granularity is excessive, not there is practical value.Therefore, provide a kind of utilize micro passage reaction effectively to solve method that blockage problem can prepare again nano hydrotalcite material is core place of the present invention.
Summary of the invention
The object of the invention is to the shortcoming overcoming prior art existence, a kind of method utilizing micro passage reaction to prepare nano hydrotalcite material is provided, both can realize nano hydrotalcite material particle size and size distribution controlled synthesis and batch between duplication of production, the blockage problem in micro passage reaction can be solved again.To achieve these goals, adopt a kind of flow focusing type micro passage reaction to carry out continuous production, this flow focusing type micro passage reaction is with two liquid-inlets, a gas feed and an outlet; Its concrete technology step is as follows:
(1) by soluble divalent metal salt raw material A
2+x and trivalent metal salt raw material B
3+x presses A
2+with B
3+total mol ratio be more than or equal to 2:1, be less than or equal to 4:1 and be configured to metal salt solution, A in described metal salt solution
2+with B
3+total concn be 0.1-2.0mol/L; Wherein, A
2+can be Mg
2+, Ni
2+, Zn
2+, Cu
2+, Fe
2+, Co
2+, Ca
2+in one or more; B
3+can be Al
3+, Fe
3+, Co
3+, Mn
3+, Cr
3+, Ga
3+, In
3+in one or more; X is Cl
-, NO
3 -, SO
4 2-in one or more;
(2) one or more getting in sodium hydroxide, potassium hydroxide, ammoniacal liquor, sodium carbonate, salt of wormwood, volatile salt are configured to mixed ammonium/alkali solutions, hydroxide radical (OH in mixing solutions
-) or carbonate (CO
3 2-) or hydroxide radical (OH
-) and carbonate (CO
3 2-) total concn be 0.2-4.5mol/L;
(3) gases used is one or more in air, nitrogen, argon gas;
(4) metal salt solution prepared of described step (1) and (2) and mixed ammonium/alkali solutions enter from two liquid inlets respectively with same traffic; Gas then enters flow focusing type micro passage reaction with the 0.2-5 of liquid starting material total flux flow doubly from gas inlet; In inside reactor reaction channel, metal salt solution and mixed ammonium/alkali solutions are divided into independently liquid bullet by gas, and the two contacts, mixes and react in liquid bullet, and reaction gained houghite slurry flows out from the exit of reactor;
(5) step (4) gained houghite slurry is through hydrothermal treatment consists; Fully washed by throw out deionized water after hydrothermal treatment consists, centrifugal rear gained sample is nano hydrotalcite.
Technique scheme flow focusing type used micro passage reaction takes monolithic microchannel plate or the superposition of multi-disc microchannel plate to make; When adopting monolithic microchannel plate to make, reactor comprises two blocks of shroudings and a slice microchannel plate, be specially four microchannels be positioned on microchannel plate, i.e. two fluid inlet channel, gas inlet channel, the reaction channel be connected with intake vent respectively, intake vent is connected with three imports respectively, and reaction channel is connected with outlet; When adopting the superposition of multi-disc microchannel plate to make, reactor comprises two panels shrouding and three microchannel plates, is specially gas inlet channel, and one of two fluid inlet channel make respectively on another two panels microchannel plate; Another kind of fluid inlet channel and reaction channel then make on the 3rd microchannel plate; Conventional pore structure mode of connection is adopted to be communicated with intake vent and reaction channel.
Technique scheme gas inlet channel is between two fluid inlet channel, equal with two fluid inlet channel angles, and angle is 20-80 °;
Technique scheme gas inlet channel and fluid inlet channel measure-alike, hydraulic diameter is 0.2-1mm; Reaction channel hydraulic diameter and intake vent hydraulic diameter identical or different, be 0.2-1mm, reaction channel length is 10mm-200mm.
Another feature that the present invention realizes nano hydrotalcite method be control liquid slurry in described flow focusing type micro passage reaction the residence time at 0.01 second-time, to make described metal salt solution and mixed ammonium/alkali solutions short mix in microchannel.
The present invention compared with prior art, has that the residence time is short, flux is large, granularity is controlled and the advantage such as narrowly distributing.Owing to introducing gas, T-shaped or that Y type micro passage reaction is common blockage problem can be solved.The nano hydrotalcite material prepared, uniform particle diameter, good dispersion degree.
Accompanying drawing explanation
The flow focusing type micro passage reaction schematic diagram that Fig. 1, the present invention are used, is made by monolithic microchannel plate.
In figure, 1,2,3 are respectively liquid one (metal-salt/mixed base) intake vent, liquid two (mixed base/metal-salt) intake vent, gas inlet channel; 4 is reaction channel; 11,21,31,41 liquid one (metal-salt/mixed base) import, liquid two (mixed base/metal-salt) import, gas feed and reaction outlet is respectively.
The flow focusing type micro passage reaction schematic diagram that Fig. 2, the present invention are used, is superposed by multi-disc microchannel plate and makes.
In figure, A, B, C are respectively: a kind of fluid inlet channel and reaction channel plate, another kind of fluid inlet channel plate, gas inlet channel plate; 1,2,3 is liquid one (metal-salt/mixed base) intake vent, liquid two (mixed base/metal-salt) intake vent, gas inlet channel; 4 is reaction channel; 11,21,31,41 liquid one (metal-salt/mixed base) import, liquid two (mixed base/metal-salt) import, gas feed and reaction outlet is respectively; 5A, 5B are connecting hole.
The XRD figure of Fig. 3, the embodiment of the present invention 1.
The TEM figure of Fig. 4, the embodiment of the present invention 1.
The XRD figure of Fig. 5, the embodiment of the present invention 2.
The XRD figure of Fig. 6, the embodiment of the present invention 3.
Embodiment
Describe the present invention in detail by the following examples, but invention is not limited to following example.
Flow focusing type micro passage reaction in embodiment simply describes:
As shown in accompanying drawing 1, Fig. 2.Comprise two panels fluid inlet channel plate A, B, a slice gas inlet channel plate C, wherein, a slice fluid inlet channel plate and reaction channel are located at (A) on same plate.Article three, intake vent 1,2,3 hydraulic diameter is equal, and be all 600 microns, reaction channel is equal with intake vent hydraulic diameter.Gas inlet channel 3 and two fluid inlet channel 1,2 angles are equal is 60 °.The length of reaction channel 4 is 100 millimeters, i.e. the volume of reaction channel about 36 microlitre, then can be calculated the residence time of liquid slurry in micro passage reaction by liquid slurry flow.
Embodiment 1
Take the Mg (NO of 48.1g
3)
26H
2al (the NO of O and 23.4g
3)
39H
2o, is configured to the aqueous solution 500ml that metal ion total concn is 0.5mol/L.Take the Na of NaOH and 13.25g of 16g
2cO
3be configured to OH
-and CO
3 2-total concn is the aqueous solution 500ml of 1.05mol/L.Gas selects air, and flow is 100ml/min.Metal salt solution and alkaline solution all enter micro passage reaction with the flow of 150ml/min and contact, mix and react, and temperature of reaction is 80 DEG C. and get partly precipitated thing and load hydrothermal reaction kettle, at 150 DEG C, process 6h.Precipitate with deionized water after hydrothermal treatment consists fully washed, centrifuged pellet thing is nano-calcium carbonate root type MgAl hydrotalcite, and itself XRD and TEM characterization result respectively as shown in Figure 3, Figure 4.
Embodiment 2
Take the Mg (NO of 48.1g
3)
26H
2al (the NO of O, 11.7g
3)
39H
2fe (the NO of O and 12.6g
3)
39H
2o, is configured to the aqueous solution 500ml that metal ion total concn is 0.5mol/L.Take the Na of NaOH and 13.25g of 16g
2cO
3be configured to OH
-and CO
3 2-total concn is the aqueous solution 500ml of 1.05mol/L.Gas selects nitrogen, and flow is 20ml/min.Metal salt solution and alkaline solution all enter micro passage reaction with the flow of 100ml/min and contact, mix and react, and temperature of reaction is 80 DEG C. and get partly precipitated thing and load hydrothermal reaction kettle, at 100 DEG C, process 4h.Precipitate with deionized water after hydrothermal treatment consists fully washed, centrifuged pellet thing is nano-calcium carbonate root type MgAlFe hydrotalcite, and XRD figure spectrum analysis result such as the accompanying drawing 5 of this hydrotalcite shows.
Embodiment 3
Take the Mg (NO of 24.0g
3)
26H
2ni (the NO of O, 27.3g
3)
26H
2al (the NO of O, 11.7g
3)
39H
2fe (the NO of O and 12.6g
3)
39H
2o, is configured to the aqueous solution 500ml that metal ion total concn is 0.5mol/L.Take the Na of NaOH and 13.25g of 16g
2cO
3be configured to OH
-and CO
3 2-total concn is the aqueous solution 500ml of 1.05mol/L.Gas selects nitrogen, and flow is 150ml/min.Metal salt solution and alkaline solution all enter micro passage reaction with the flow of 150ml/min and contact, mix and react, and temperature of reaction is 80 DEG C. and get partly precipitated thing and load hydrothermal reaction kettle, at 100 DEG C, process 4h.Precipitate with deionized water after hydrothermal treatment consists fully washed, centrifuged pellet thing is nano-calcium carbonate root type MgNiFeAl hydrotalcite, and XRD figure spectrum analysis result such as the accompanying drawing 6 of this hydrotalcite shows.
Claims (4)
1. a preparation method for nano hydrotalcite, is prepared, it is characterized in that in two liquid-inlets, a gas feed and a flow focusing type micro passage reaction exported:
(1) by soluble divalent metal salt raw material A
2+x and trivalent metal salt raw material B
3+x presses A
2+with B
3+total mol ratio be more than or equal to 2:1, be less than or equal to 4:1 and be configured to metal salt solution, A in described metal salt solution
2+with B
3+total concn be 0.1-2.0mol/L; Wherein, A
2+can be Mg
2+, Ni
2+, Zn
2+, Cu
2+, Fe
2+, Co
2+, Ca
2+in one or more; B
3+can be Al
3+, Fe
3+, Co
3+, Mn
3+, Cr
3+, Ga
3+, In
3+in one or more; X is Cl
-, NO
3 -, SO
4 2-in one or more;
(2) one or more getting in sodium hydroxide, potassium hydroxide, ammoniacal liquor, sodium carbonate, salt of wormwood, volatile salt are configured to mixed ammonium/alkali solutions, hydroxide radical (OH in mixing solutions
-) or carbonate (CO
3 2-) or hydroxide radical (OH
-) and carbonate (CO
3 2-) total concn be 0.2-4.5mol/L;
(3) gases used is one or more in air, nitrogen, argon gas;
(4) metal salt solution prepared of described step (1) and (2) and mixed ammonium/alkali solutions enter from two liquid inlets respectively with same traffic; Gas then enters flow focusing type micro passage reaction with the 0.2-5 of liquid starting material total flux flow doubly from gas inlet; In inside reactor reaction channel, metal salt solution and mixed ammonium/alkali solutions are divided into independently liquid bullet by gas, and the two contacts, mixes and react in liquid bullet, and reaction gained houghite slurry flows out from the exit of reactor;
(5) step (4) gained houghite slurry is through hydrothermal treatment consists; Fully washed by throw out deionized water after hydrothermal treatment consists, centrifugal rear gained sample is nano hydrotalcite.
2. the preparation method of hydrotalcite according to claim 1, is characterized in that:
Described flow focusing type micro passage reaction takes monolithic microchannel plate or the superposition of multi-disc microchannel plate to make; When adopting monolithic microchannel plate to make, reactor comprises two blocks of shroudings and a slice microchannel plate, be specially four microchannels be positioned on microchannel plate, i.e. two fluid inlet channel, gas inlet channel, the reaction channel be connected with intake vent respectively, intake vent is connected with three imports respectively, and reaction channel is connected with outlet; When adopting the superposition of multi-disc microchannel plate to make, reactor comprises two panels shrouding and three microchannel plates, is specially gas inlet channel, and one of two fluid inlet channel make respectively on another two panels microchannel plate; Another kind of fluid inlet channel and reaction channel then make on the 3rd microchannel plate; Conventional pore structure mode of connection is adopted to be communicated with intake vent and reaction channel.
3. the preparation method of hydrotalcite according to claim 2, is characterized in that:
Described gas inlet channel is between two fluid inlet channel, equal with two fluid inlet channel angles, and angle is 20-80 °;
Gas inlet channel and fluid inlet channel measure-alike, hydraulic diameter is 0.2-1mm; Reaction channel hydraulic diameter and intake vent hydraulic diameter identical or different, be 0.2-1mm, reaction channel length is 10mm-200mm.
4. the preparation method of hydrotalcite according to claim 1, is characterized in that: control the residence time of liquid slurry in described flow focusing type micro passage reaction at 0.01 second-time.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105948085A (en) * | 2016-04-21 | 2016-09-21 | 巢湖学院 | Preparation method of magnetic hydrotalcite |
| CN107837782A (en) * | 2017-12-08 | 2018-03-27 | 中国科学院大连化学物理研究所 | A kind of method for passing through Nanoparticles Prepared by Precipitation using multichannel blender |
| CN107855091A (en) * | 2017-12-08 | 2018-03-30 | 中国科学院大连化学物理研究所 | A kind of method for passing through Nanoparticles Prepared by Precipitation using single channel blender |
| CN112023929A (en) * | 2019-11-22 | 2020-12-04 | 天津大学 | Preparation method and application of transition metal double hydroxide nano-film and carbon nano-tube composite material |
| CN112871103A (en) * | 2021-01-14 | 2021-06-01 | 浙江工业大学 | Preparation method of capillary microchannel reactor with internal coated hydrotalcite film |
| CN115532193A (en) * | 2022-10-19 | 2022-12-30 | 贵州大学 | Micro-reaction equipment for preparing nano titanium dioxide and using method |
| CN115624928A (en) * | 2022-11-01 | 2023-01-20 | 贵州大学 | Micro-reaction equipment for preparing nano cuprous iodide and using method |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105948085A (en) * | 2016-04-21 | 2016-09-21 | 巢湖学院 | Preparation method of magnetic hydrotalcite |
| CN107837782A (en) * | 2017-12-08 | 2018-03-27 | 中国科学院大连化学物理研究所 | A kind of method for passing through Nanoparticles Prepared by Precipitation using multichannel blender |
| CN107855091A (en) * | 2017-12-08 | 2018-03-30 | 中国科学院大连化学物理研究所 | A kind of method for passing through Nanoparticles Prepared by Precipitation using single channel blender |
| CN112023929A (en) * | 2019-11-22 | 2020-12-04 | 天津大学 | Preparation method and application of transition metal double hydroxide nano-film and carbon nano-tube composite material |
| CN112023929B (en) * | 2019-11-22 | 2021-12-03 | 天津大学 | Preparation method and application of transition metal double hydroxide nano-film and carbon nano-tube composite material |
| CN112871103A (en) * | 2021-01-14 | 2021-06-01 | 浙江工业大学 | Preparation method of capillary microchannel reactor with internal coated hydrotalcite film |
| CN115532193A (en) * | 2022-10-19 | 2022-12-30 | 贵州大学 | Micro-reaction equipment for preparing nano titanium dioxide and using method |
| CN115532193B (en) * | 2022-10-19 | 2024-04-12 | 贵州大学 | Micro-reaction equipment for preparing nano titanium dioxide and use method |
| CN115624928A (en) * | 2022-11-01 | 2023-01-20 | 贵州大学 | Micro-reaction equipment for preparing nano cuprous iodide and using method |
| CN115624928B (en) * | 2022-11-01 | 2024-04-12 | 贵州大学 | Micro-reaction equipment for preparing nano cuprous iodide and use method |
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| Publication number | Publication date |
|---|---|
| CN104709931B (en) | 2017-03-15 |
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