CN102976373A - Method for synthesizing monodisperse stable LDHs (layered double hydroxides) colloid nanocrystalline - Google Patents
Method for synthesizing monodisperse stable LDHs (layered double hydroxides) colloid nanocrystalline Download PDFInfo
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Abstract
The invention relates to a preparation method for synthesizing relatively strict monodisperse stable LDHs (layered double hydroxides) colloid nanocrystalline. The preparation method mainly comprises the following steps of: 1, synthesizing the LDHs through a colloid mill to obtain white slurry, then centrifugally washing three times, transferring to a hydrothermal kettle, re-crystallizing to obtain a stable colloid solution; 2, respectively preparing density gradient medium solutions with different densities; 3, sequentially adding quantitative gradient solutions according to different densities in a centrifugal tube for preparing a step type density gradient solution; 4, slowly adding the prepared colloid solution on the liquid level of the density gradient solution, centrifuging under a certain condition; and 5, since colloid nano particles with different sizes have different sedimentation rates in the density gradient solutions, after centrifugation is stopped, the colloid nano particles remain in the gradient solutions with different densities, so that an effective method for preparing the monodisperse LDH nanocrystalline is provided. The high-monodispersity nano material has great potential application on the aspects of medicines, genetic vectors, polymer/LDHs biological nano composite materials, LDH films and the like.
Description
Technical field
The present invention relates to by utilizing density gradient centrifugation to separate LDHs nanocrystallinely and study its performance, and the method for a kind of synthetic single stably dispersing LDHs colloid nanocrystalline that obtains belongs to inorganic nano material synthesis technology field.
Background technology
Hydrotalcite (Layered Double Hydroxides writes a Chinese character in simplified form into LDHs) is an anionoid type lamellar compound, and its chemical expression can be expressed as [M
2+ (1-x)M
3+ x(OH)] A
N- (x/n)﹒ mH
2O, wherein M
2+With M
3+Tool is metallic cation.If n=0 is neutrality and only depends on the Van der Waals interaction force to combine between laminate.Because M
3+The trace of (x=0.33-0.167) replace so that laminate with positive charge, and by the negatively charged ion (A between laminate
N-) combine, and negatively charged ion can be most inorganic, organic anion.Adjustable sex change because of its structure and performance, can be widely used in various fields and industry, [J. Am. Chem. Soc. 2010,132 (47): 16735-16736.] is in recent years especially owing to their huge potential application powers in fields such as catalysis, absorption, nano composite material and pharmaceutical carriers cause extensive concern.
Traditional synthetic method generally is by constant pH or passes through crystallization [the J. Phys. Chem B of certain hour after changing the pH co-precipitation again, 2010,114 (17): 5678-5685], the second particle coacervate that the LDHs material that these class methods obtain generally is comprised of thousands of Stacking for laminated plates, size is in 1-10 μ m scope, this has just limited the LDHs material as medicine, genophore, the performance applications such as polymer/LDHs biological nano matrix material and LDHs film, this will ask the nano material that obtains high single dispersity.At present, a lot of synthetic method (J. Mater. Chem about colloid LDHs suspension are arranged, 2006,16 (39): 3809-3813.), existing a kind of method prepares stable LDHs colloid nanocrystalline (J. Phys. Chem B, 2006,110 (34): 16923-16929.), can obtain the colloidal solution that different size distributes by the control temperature.But obtain the single LDHs of dispersion colloid nanocrystalline nano-scale easy to control, stable and remain a challenge.
Density gradient centrifugation is a kind of harmless to the nano particle that separates, exists settling ratio poor and particle is separated by size or pattern in density gradient solution according to different nano particles.This separation method can obtain the nano particle that resulting size is more single in same system [J. Am. Chem. Soc. 2010,132 (7): 2333-2337.; Angew. Chem. In. Ed. 2009,48 (5): 939-942.].And in previous work, we have successfully utilized density gradient centrifugation to separate nm gold particles, Graphene, CdS, C@FeCo etc., here we attempt that first density gradient centrifugation and nucleation-crystallization isolation method are prepared LDH colloid nanocrystalline solution and combine, contacting between the size of inquiring into LDH and the composition.Density gradient centrifugation for the size of LDH in the research same system and the relation between forming strong technical support is provided, for the fields such as biological nano composite material and LDHs film provide abundant material foundation, the nanocrystalline application and development of LDH there is great meaning.
Summary of the invention
The synthetic method that the purpose of this invention is to provide the stable single LDHs of the dispersion colloid nanocrystalline of a kind of effective control, thus can well recently control the size of synthesizing the LDHs nanometer sheet by the regulation and control material.
For achieving the above object, the present invention adopts following technical scheme:
Single synthetic method of disperseing the LDHs colloid nanocrystalline that a kind of effective control is stable is characterized in that the concrete steps of the method are as follows:
1. the preparation of LDH colloid nanocrystalline is characterized in that the method carries out as follows:
Prepare the stable nanocrystalline colloidal solution of LDH:
A. will contain Mg
2+And Al
3+Mixing salt solution and NaOH solution pour simultaneously high speed rotating into colloidal mill in several minutes, can obtain slurries;
B. with the slurries of a gained through 5000-12000 rev/mins about centrifugal ten minutes, remove supernatant liquor, add deionized water and stirring to without the bulk particle, centrifugal, washing is twice again;
C. the precipitation with step b gained is dissolved in 40 mL deionized water for stirring to without the bulk particle, then pours in the water heating kettle in 80-150 ℃ of baking oven internal reaction 8-16 h.Obtain at last stable transparent colloidal solution.
2. the nanocrystalline density gradient centrifugation of LDHs is separated:
A. successively compound concentration different (they being that density is descending) and can make the LDH stable dispersion glycol/water density gradient medium solution, get successively isopyknic medium solution by the order from the high density to the lower concentration and add centrifuge tube and be mixed with gradient solution;
B. lentamente the stable transparent colloidal solution of a certain amount of step 1 gained is placed on the gradient solution of above-mentioned gained;
C. be 4-25 ℃ in temperature, rotating speed is 20000-50000 rev/mins, and the time is centrifugal under 10-30 minutes the condition, obtains a kind of colloidal nano dispersion liquid according to the nanoparticle size size distribution;
D. the colloidal nano dispersion liquid that obtains is taken out in batches from the top, finally obtain the nano particle of different size.
Mg in the technique scheme 1
2+/ Al
3+Molar ratio can by regulating in 1.5-3 scopes, can obtain different Mg
2+/ Al
3+Than stable LDH colloidal solution, their corresponding distribution of sizes is also different.
The present invention compared with prior art has the following advantages and the high-lighting effect: 1. density gradient centrifugation is applied in the analysis of LDHs colloid nanocrystalline of same system, is easy to obtain the narrower nanoparticle of distribution of sizes; 2. the distribution that is not of identical composition of the LDH nanometer sheet in same system, the size of nanometer sheet and form between exist certain relation, the size of composition regulation and control LDH nanoparticle that can be by raw material.
Characterization result is seen Fig. 1-5.
Fig. 1 is X ray powder diffraction (XRD) figure that stablizes MgAl – LDH colloid nanocrystalline among the embodiment one a), there is measurement result to see, the highest peak of the sample that the present invention is worth is respectively (003) (006) (012) San Tiaofeng, is the characteristic peak of hydrotalcite structure; B) be transmission electron microscope (TEM) figure of this sample, by the big or small slice heterogeneity of the visible MgAl-LDH nanometer sheet of Fig. 2, size mainly is distributed in 50 –, 300 nm.
Fig. 2 is that MgAl-LDH carries out the digital photograph that density gradient centrifugation (DGUS) is separated front and back among the embodiment one, especially the sample after separating, because this colloidal solution is clear solution, so utilize Tyndall effect to differentiate the distribution situation of LDH colloid in density gradient solution, then just can take out layer by layer the nano particle that is dispersed in the density gradient solution.
After Fig. 3 is the centrifugation of LDHs colloid nanocrystalline, the TEM photo of the different numbers of plies is respectively the 8th, the 10th, the 12nd, the 14th, the 16th layer TEM photo, corresponding is histogram and the Gauss curve fitting curve thereof of the lamella size of mathematical statistics, as seen the LDH nanometer sheet increases gradually from top to bottom.
Fig. 4 is the composition of LDH nanometer sheet of the case study on implementation one different numbers of plies and the linear relationship chart of corresponding size thereof, as seen along with Mg
2+/ Al
3+The increase of ratio, corresponding size also increases gradually.
Fig. 5 keeps the amount of substance of alkali number and total metallic element constant in the case study on implementation one, change the Mg of MgAl-LDH
2+/ Al
3+Mol ratio to 3.0, obtains the size distribution plot of corresponding stable LDH colloidal solution by 1.5 regulation and control.As seen along with Mg
2+/ Al
3+Increase, the peak position of distribution of sizes moves to right, overall LDH nanometer sheet has the trend of increase.
Description of drawings
Fig. 1 is the invention process case one synthetic not separated XRD of resulting MgAl-LDHs colloid nanocrystalline a); B) be the synthetic not separated TEM photo of resulting MgAl-LDHs colloid nanocrystalline
Fig. 2 is that the MgAl-LDHs colloid nanocrystalline that the invention process case one is synthesized passes through the digital photograph that density gradient centrifugation separates the front and back centrifuge tube.
Fig. 3 is the TEM figure that is in the nano particle of the different numbers of plies after the MgAl-LDH colloid nanocrystalline that synthesized of the invention process case one separates through density gradient centrifugation.
Fig. 4 is that the invention process case one is the Mg/Al mol ratio of the different numbers of plies (being the composition of the nanometer sheet of the different numbers of plies), and the linear relationship of lamella size and the corresponding number of plies shows to exist between composition and the LDHs nanometer sheet to contact.
Fig. 5 is that the invention process case one changes synthetic feed ratio, obtains the different nanometer sheet of distribution of sizes.
Embodiment
Embodiment one
1. prepare stable MgAl-LDH colloid nanocrystalline solution;
(1) 10 mL is contained 3 mmol MgCl
2With 1 mmol AlCl
3Mixing salt solution and the NaOH solution of 40 mL, 0.15 M pour simultaneously high speed rotating into colloidal mill in 10 min, obtain white slurries;
(2) with white slurries through 12,000 rpm; Centrifugal washing is three times under the 15min condition;
(3) add the 40mL deionized water and stirring to without the bulk particle, then import in the water heating kettle in 100 ℃ of baking oven internal reaction 10 h, obtain stable transparent colloidal solution;
2. density gradient centrifugation is separated:
(1) make density gradient: spent glycol and water are mixed with the aqueous solution of volume percent 20%, 40%, 60%, 80%, 100% ethylene glycol.From ethylene glycol, the solution of getting successively 2 mL slowly adds centrifuge tube, is mixed with gradient solution.
(2) the stable MgAl that 1 mL step 1 is prepared-LDH colloid nanocrystalline solution is added on the gradient liquid.
(3) 20 ℃, 100 * 10
-6Normal atmosphere, 30,000 rpm, high speed centrifugation under the 15 min conditions.
(4) utilize Tyndall effect differentiate to separate after the distribution situation of particle, the mixed solution after centrifugal is begun sucking-off with liquid-transfering gun from top layer, every layer of volume is 500 μ L.Finally obtain the nanocrystalline dispersion liquid of size Different L DH.
3. the LDH of different size distribution is synthetic
The amount and the Mg that keep NaOH
2+, Al
3+Mixing salt total amount of substance constant, change Mg
2+/ Al
3+Mol ratio (in 1.5-3 scopes all can) can obtain the different LDH colloid nanocrystalline solution of particle size distribution.Such as Fig. 5.
Embodiment two
1. prepare stable MgAl-LDH colloid nanocrystalline solution;
(1) 10 mL is contained 3 mmol MgCl
2With 1 mmol AlCl
3Mixing salt solution and the NaOH solution of 40 mL, 0.15 M pour simultaneously high speed rotating into colloidal mill in 10 min, obtain white slurries;
(2) with white slurries through 12,000 rpm; Centrifugal washing is three times under the 15 min conditions;
(3) add 40 mL deionized water and stirring to without the bulk particle, then import in the water heating kettle in 100 ℃ of baking oven internal reaction 10 h, obtain stable transparent colloidal solution;
2. density gradient centrifugation is separated:
(1) make density gradient: spent glycol and water are mixed with the aqueous solution of volume percent 20%, 40%, 60%, 80%, 100% ethylene glycol.From ethylene glycol, the solution of getting successively 0.8 mL slowly adds centrifuge tube, is mixed with gradient solution.
(2) the stable MgAl that 0.5 mL step 1 is prepared-LDH colloid nanocrystalline solution is added on the gradient liquid.
(3) 20 ℃, 100 * 10
-6Normal atmosphere, 50,000 rpm, high speed centrifugation under the 10 min conditions.
(4) utilize Tyndall effect differentiate to separate after the distribution situation of particle, the mixed solution after centrifugal is begun sucking-off with liquid-transfering gun from top layer, every layer of volume is 200 μ L.Finally obtain the nanocrystalline dispersion liquid of size Different L DH.
Embodiment three
1. prepare stable MgAl-LDH colloid nanocrystalline solution;
(1) 10 mL is contained 3 mmol MgCl
2With 1 mmol AlCl
3Mixing salt solution and the NaOH solution of 0.15 M of 40 mL pour simultaneously high speed rotating into colloidal mill in 10 min, obtain white slurries;
(2) with white slurries through 12,000 rpm; Centrifugal washing is three times under the 15 min conditions;
(3) add 40 mL deionized water and stirring to without the bulk particle, then import in the water heating kettle in 80 ℃ of baking oven internal reaction 16 h, obtain stable transparent colloidal solution;
2. density gradient centrifugation is separated:
(1) make density gradient: spent glycol and water are mixed with the aqueous solution of volume percent 20%, 40%, 60%, 80%, 100% ethylene glycol.From ethylene glycol, the solution of getting successively 2 mL slowly adds centrifuge tube, is mixed with gradient solution.
(2) the stable MgAl that 1 mL step 1 is prepared-LDH colloid nanocrystalline solution is added on the gradient liquid.
(3) 20 ℃, 100 * 10
-6Normal atmosphere, 30,000 rpm, high speed centrifugation under the 15 min conditions.
(4) utilize Tyndall effect differentiate to separate after the distribution situation of particle, the mixed solution after centrifugal is begun sucking-off with liquid-transfering gun from top layer, every layer of volume is 500 μ L.Finally obtain the nanocrystalline dispersion liquid of size Different L DH.
Embodiment four
1. prepare stable MgAl-LDH colloid nanocrystalline solution;
(1) 10 mL is contained 2 mmol MgCl
2With 1 mmol AlCl
3Mixing salt solution and the NaOH solution of 40 mL, 0.15 M pour simultaneously high speed rotating into colloidal mill in 10 min, obtain white slurries.
(2) with white slurries through 12,000 rpm; Centrifugal washing is three times under the 15min condition;
(3) add the 40mL deionized water and stirring to without the bulk particle, then import in the water heating kettle in 100 ℃ of baking oven internal reaction 10 h, obtain stable transparent colloidal solution;
2. density gradient centrifugation is separated:
(1) make density gradient: spent glycol and water are mixed with the aqueous solution of volume percent 20%, 40%, 60%, 80%, 100% ethylene glycol.From ethylene glycol, the solution of getting successively 2 mL slowly adds centrifuge tube, is mixed with gradient solution.
(2) the stable MgAl that 1 mL step 1 is prepared-LDH colloid nanocrystalline solution is added on the gradient liquid.
(3) 20 ℃, 100 * 10
-6Normal atmosphere, 30,000 rpm, high speed centrifugation under the 20 min conditions.
(4) utilize Tyndall effect differentiate to separate after the distribution situation of particle, the mixed solution after centrifugal is begun sucking-off with liquid-transfering gun from top layer, every layer of volume is 500 μ L.Finally obtain the nanocrystalline dispersion liquid of size Different L DH.
Embodiment five
1. prepare stable MgAl-LDH colloid nanocrystalline solution;
(1) 10 mL is contained 3 mmol MgCl
2With 1 mmol AlCl
3Mixing salt solution and the NaOH solution of 40 mL, 0.15 M pour simultaneously high speed rotating into colloidal mill in 10 min, obtain white slurries;
(2) with white slurries through 12,000 rpm; Centrifugal washing is three times under the 15 min conditions;
(3) add 40 mL deionized water and stirring to without the bulk particle, then import in the water heating kettle in 100 ℃ of baking oven internal reaction 8 h, obtain stable transparent colloidal solution;
2. density gradient centrifugation is separated:
(1) make density gradient: spent glycol and water are mixed with the aqueous solution of volume percent 20%, 40%, 60%, 80%, 100% ethylene glycol.From ethylene glycol, the solution of getting successively 2 mL slowly adds centrifuge tube, is mixed with gradient solution.
(2) the stable MgAl that 1 mL step 1 is prepared-LDH colloid nanocrystalline solution is added on the gradient liquid.
(3) 20 ℃, 100 * 10
-6Normal atmosphere, 30,000 rpm, high speed centrifugation under the 20 min conditions.
(4) utilize Tyndall effect differentiate to separate after the distribution situation of particle, the mixed solution after centrifugal is begun sucking-off with liquid-transfering gun from top layer, every layer of volume is 500 μ L.Finally obtain the nanocrystalline dispersion liquid of size Different L DH.
Claims (2)
- The synthetic method that colloid is nanocrystalline is characterized in that the concrete steps of the method are as follows:1.LDH the preparation of colloid nanocrystalline is characterized in that the method carries out as follows:Prepare the stable nanocrystalline colloidal solution of LDH:A. will contain Mg 2+And Al 3+Mixing salt solution and NaOH solution pour simultaneously high speed rotating into colloidal mill in several minutes, can obtain slurries;B. with the slurries of a gained through 5000-12000 rev/mins about centrifugal ten minutes, remove supernatant liquor, add deionized water and stirring to without the bulk particle, centrifugal, washing is twice again;C. the precipitation with step b gained is dissolved in 40 mL deionized water for stirring to without the bulk particle, then pours in the water heating kettle in 80-150 ℃ of baking oven internal reaction 8-16 h.Obtain at last stable transparent colloidal solution.
- 2.LDHs nanocrystalline density gradient centrifugation is separated:A. successively compound concentration different (they being that density is descending) and can make the LDH stable dispersion glycol/water density gradient medium solution, get successively isopyknic medium solution by the order from the high density to the lower concentration and add centrifuge tube and be mixed with gradient solution;B. lentamente the stable transparent colloidal solution of a certain amount of step 1 gained is placed on the gradient solution of above-mentioned gained;C. be 4-25 ℃ in temperature, rotating speed is 20000-50000 rev/mins, and the time is centrifugal under 10-30 minutes the condition, obtains a kind of colloidal nano dispersion liquid according to the nanoparticle size size distribution;D. the colloidal nano dispersion liquid that obtains is taken out in batches from the top, finally obtain the nano particle of different size.Mg in the technique scheme 1 2+/ Al 3+Molar ratio can by regulating in 1.5-3 scopes, can obtain different Mg 2+/ Al 3+Than stable LDH colloidal solution, their corresponding distribution of sizes is also different.
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CN102671589A (en) * | 2012-05-21 | 2012-09-19 | 北京化工大学 | Density gradient centrifugation method for analyzing nano grain surface reaction process |
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CN101554596A (en) * | 2009-05-22 | 2009-10-14 | 北京化工大学 | Method for preparing solid base catalyst with high specific surface by hybrid composite precursors |
CN101559401A (en) * | 2009-05-26 | 2009-10-21 | 北京化工大学 | Method for separating nano-particles at water-phase density gradient centrifugation rate |
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CN103723678A (en) * | 2013-12-23 | 2014-04-16 | 北京化工大学 | Method for switching media for nano-particles or separating same from one another according to sizes and/or shapes of nano-particles |
CN103723678B (en) * | 2013-12-23 | 2017-02-15 | 北京化工大学 | Method for switching media for nano-particles or separating same from one another according to sizes and/or shapes of nano-particles |
CN108689418A (en) * | 2018-07-26 | 2018-10-23 | 塔里木大学 | A kind of stratiform houghite raw powder's production technology |
CN111498810A (en) * | 2019-01-31 | 2020-08-07 | 北京卫蓝新能源科技有限公司 | Nano material dispersion liquid and preparation method thereof |
CN111498810B (en) * | 2019-01-31 | 2022-07-12 | 北京卫蓝新能源科技有限公司 | Nano material dispersion liquid and preparation method thereof |
CN110129815A (en) * | 2019-04-24 | 2019-08-16 | 北京大学深圳研究生院 | Modified TM-LDH nano material, preparation method and application |
CN110129815B (en) * | 2019-04-24 | 2020-10-16 | 北京大学深圳研究生院 | Modified TM-LDH nano material, preparation method and application thereof |
EP3792376A1 (en) | 2019-09-10 | 2021-03-17 | Vito NV | A process for producing mixed metal oxides and hydroxides |
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