CN105439188A - Preparation method of hydrotalcite-like compound nanosheet - Google Patents
Preparation method of hydrotalcite-like compound nanosheet Download PDFInfo
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- CN105439188A CN105439188A CN201510769754.8A CN201510769754A CN105439188A CN 105439188 A CN105439188 A CN 105439188A CN 201510769754 A CN201510769754 A CN 201510769754A CN 105439188 A CN105439188 A CN 105439188A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
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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
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- C—CHEMISTRY; METALLURGY
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/36—Spheres fragmented
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The invention provides a preparation method of a hydrotalcite-like compound nanosheet. The preparation method of the hydrotalcite-like compound nanosheet comprises the following steps: firstly adding mixed metal salt and sodium hydroxide into an ampholytic surfactant solution in parallel flow, and after reaction is finished, putting into a hydrothermal kettle for carrying out hydrothermal treatment, so that an intercalation hydrotalcite-like compound is prepared; and then putting the intercalation hydrotalcite-like compound into an acid solution, so that the hydrotalcite-like compound nanosheet is obtained. The preparation method of the hydrotalcite-like compound nanosheet is simple in operation and applicable to large-scale production. The preparation method of the hydrotalcite-like compound nanosheet adopts no other organic matters except the ampholytic surfactant and organic acid, and the adopted solvents are in an aqueous phase and do less harm to the environment; meanwhile, the operation is simple, and the cost is low.
Description
Technical field
The present invention relates to hydrotalcite-like materials, specifically belong to a kind of hydrothermal preparing process of acrylic/hydrotalcite-like nano sheet.
Background technology
Houghite (HTlc), also known as layered double hydroxide (LDHs), it is the two-dimentional anionic clay materials of a class high-sequential, it has regular octahedron structure, adjacent octahedron is by being total to limit form layers, layer and layer ask that interlayer passes through hydrogen bond association to stacking with pushing up; Due to interchangeability and the cationic collocation property of laminate of its negatively charged ion, and the houghite compound of various difference composition can be synthesized.It is large that the composite oxides prepared with houghite compound roasting generally have specific surface area, thermostability is high, Active components distribution is even, sintering can be suppressed, have the features such as good stability, at present in redox, all show excellent catalytic performance in the reaction such as acid-base catalysis, thus cause people to pay close attention to more and more widely.But, owing to being filled with negatively charged ion between laminate and laminate spacing is less, so reactant cannot enter interlayer in catalytic process, and all laminate faces of houghite cannot be made all fully to be utilized.The acrylic/hydrotalcite-like nano sheet of individual layer made by the laminate be stacked by houghite by lift-off technology, make originally to be come out by the laminate face that interlayer anion is filled, for catalyzed reaction provides catalytic site, greatly can improve the utilization ratio of catalyzer like this, reduce the catalyzer cost in reaction.
About houghite lift-off technology, found by people such as Adachi-Pagano at first, in some organic solvents, peeling behavior is shown with the hydrotalcite that long-chain organic anion is modified, in butanols environment, vinylformic acid under certain temperature, is utilized to be peeled off by the Zn/Al-LDH that sodium lauryl sulphate is modified in reflux course.But the heating of this process need and organic solvent.
The people such as Naik utilizes toluene to achieve the delamination of the hydrotalcite-like materials to sodium lauryl sulphate intercalation subsequently.
Amino acid modified Mg/Al-LDH successfully successfully peels off by the people such as Hibino in methane amide afterwards.The people such as Wu utilize methane amide under hyperacoustic condition by Mg/Al-LDH success delamination.Liu Zhao equality people also utilizes methane amide successfully to obtain the nanometer sheet of large-size subsequently.Although without any the process heated and reflux, these methods are still carried out in organic solvent, although utilize methane amide delamination to be a kind of effective stripping means, acrylic/hydrotalcite-like nano sheet long storage time in methane amide can be dissolved.
Comprehensive above report, utilizes amphoterics to make intercalation houghite at present and the direct peeling behavior that occurs has no report to this method preparing acrylic/hydrotalcite-like nano sheet in water.
Summary of the invention
The acrylic/hydrotalcite-like nano sheet of preparing that the object of the invention is to exist for prior art peels off in organic solvent, easily cause environmental pollution, the problem that cost is higher, a kind of hydrothermal preparing process of acrylic/hydrotalcite-like nano sheet is provided, the method is not with an organic solvent, cost is lower, and the acrylic/hydrotalcite-like nano sheet of preparation can realize the two-sided of catalyzer laminate in catalyzed reaction and fully be utilized.
For achieving the above object, the technical scheme that the present invention takes is:
A preparation method for acrylic/hydrotalcite-like nano sheet, comprises the steps:
(1) preparation of intercalation houghite: by mixed salt solution and sodium hydroxide solution and stream joins in amphoterics solution, keep pH=8 ~ 11, after completion of the reaction, put into water heating kettle and carry out hydrothermal treatment consists, take out product afterwards, drying except anhydrating, obtaining intercalation houghite; The concentration of amphoterics solution is lower than the micelle-forming concentration of itself;
(2) acrylic/hydrotalcite-like nano sheet preparation: in whipping process, above-mentioned obtained intercalation houghite is put into the acid solution configured in advance, after completion of the reaction, leave standstill a moment, get upper strata translucent liquid, carry out high speed centrifugation, obtain acrylic/hydrotalcite-like nano sheet.
Mixing salt described in step (1) can be at least two kinds in aluminum nitrate, zinc nitrate, magnesium nitrate, cupric nitrate, and in mixed metal salt, the mol ratio of trivalent metal cation and divalent metal is 0.25 ~ 0.67 ︰ 1.
Amphoterics described in step (1) can be one or more in betaine type amphoteric surfac-tant, imidazoline type amphoterics, amino acid type amphoteric surface active agent.
Amphoterics solution, mixed salt solution and NaOH solution described in step (1) are all preferably used without CO
2water formulated.
Acid in acid solution described in step (2) can be hydrochloric acid, nitric acid, acetic acid, sulfuric acid or citric acid.
Acid solution described in step (2) is preferably used without CO
2water formulated.
Step (2) whole process is preferably without CO
2environment in carry out.
Material purity grade of the present invention can be technical pure, chemical pure, analytical pure etc.
Principle of the present invention is: when preparing houghite by hydrothermal method, and solution is alkaline environment, now can be intercalation in the middle of houghite laminate by the amphoterics of display anion characteristic; Subsequently intercalation houghite is put into acid solution, amphoterics display cats product characteristic, by houghite Delamination, can directly obtain acrylic/hydrotalcite-like nano sheet in aqueous by electrostatic repulsion.
Compared with prior art advantage of the present invention is: the present invention, except utilizing amphoterics and organic acid two kinds of organism, does not all use other organism and used solvent is aqueous phase, little to environmental hazard; Stripping process be all carry out under normal temperature and pressure and the reaction times shorter, simple to operate, cost is low.
Accompanying drawing explanation
Fig. 1 is the forming process schematic diagram of acrylic/hydrotalcite-like nano sheet
Fig. 2 is the XRD spectra of intercalation hydrotalcite-like nanometer sheet
Fig. 3 is the XRD spectra after the restructuring of acrylic/hydrotalcite-like nano sheet
Embodiment
Below in conjunction with drawings and Examples, the present invention will be described in detail.
Embodiment 1 (for Cu/Al acrylic/hydrotalcite-like nano sheet)
1) preparation of intercalation houghite
What the lauryl tetrahydroglyoxaline taking 0.28g put into 40mL removes CO
2water wiring solution-forming, under normal temperature, be that metal nitrate mixed salt solution (each material mol ratio is Cu:Al=1:0.25) and the concentration of 0.5mol/L is the sodium hydroxide solution of 0.5mol/L, and stream adds logical N by 50mL concentration
2octyl group aqueous solutions of betaine in, vigorous stirring, control about pH=8.Salts solution to be mixed dropwises, and stops the dropping of alkali lye.After continuing vigorous stirring 0.5h, put into water heating kettle, 75 DEG C, 24h carries out hydrothermal treatment consists.React complete, product is centrifugal, spends CO
2water washing several times, to neutral, suction filtration, vacuum drying, namely obtains intercalation hydrotalcite-like materials.
2) preparation of acrylic/hydrotalcite-like nano sheet
Take 0.30g intercalation hydrotalcite-like materials, put into rapidly the hydrochloric acid soln of the 100mLpH=1.5 configured in advance, without CO
2environment in after vigorous stirring 24h, leave standstill a moment, get upper strata translucent liquid and carry out high speed centrifugation separation (10000rpm, 15min), namely obtain houghite metal oxide nano-sheet.
Embodiment 2 (for Mg/Al acrylic/hydrotalcite-like nano sheet)
1) preparation of intercalation houghite
What 80mL put into by the octyl group trimethyl-glycine taking 0.30g removes CO
2water wiring solution-forming, under normal temperature, be that metal nitrate mixed salt solution (each material mol ratio is Mg:Al=3:2) and the concentration of 0.1mol/L is the sodium hydroxide solution of 0.1mol/L, and stream adds logical N by 100mL concentration
2octyl group aqueous solutions of betaine in, vigorous stirring, control about pH=10.Salts solution to be mixed dropwises, and stops the dropping of alkali lye.After continuing vigorous stirring 1h, put into water heating kettle, 85 DEG C, 20h carries out hydrothermal treatment consists.React complete, product is centrifugal, spends CO
2water washing several times, to neutral, suction filtration, vacuum drying, namely obtains intercalation hydrotalcite-like materials.
2) preparation of acrylic/hydrotalcite-like nano sheet
Take 0.15g intercalation hydrotalcite-like materials, put into rapidly the salpeter solution of 50mLpH=2, without CO
2environment in vigorous stirring after 2 days, leave standstill a moment, get the translucent solution in upper strata and carry out high speed centrifugation separation (10000rpm, 20min), namely obtain houghite metal oxide nano-sheet.
Embodiment 3 (for Zn/Al acrylic/hydrotalcite-like nano sheet)
1) preparation of intercalation houghite
What the dodecyl amino propionic acid taking 6.91g put into 120mL removes CO
2water wiring solution-forming, under normal temperature, be that metal nitrate mixed salt solution (each material is than being Zn:Al=7:3) and the concentration of 1mol/L is the sodium hydroxide solution of 0.5mol/L, and stream adds logical N by 150mL concentration
2the dodecyl amino propionic acid aqueous solution in, vigorous stirring, control about pH=11.Salts solution to be mixed dropwises, and stops the dropping of alkali lye.After continuing vigorous stirring 1.5h, put into water heating kettle, 95 DEG C, 18h carries out hydrothermal treatment consists.React complete, product is centrifugal, spends CO
2water washing several times, to neutral, suction filtration, vacuum drying, namely obtains intercalation hydrotalcite-like materials.
2) preparation of acrylic/hydrotalcite-like nano sheet
Take 0.5g intercalation hydrotalcite-like materials, put into rapidly the sulphuric acid soln of 100mLpH=1, without CO
2environment in vigorous stirring after 5 days, leave standstill a moment, get the translucent solution in upper strata and carry out high speed centrifugation separation (10000rpm, 10min), namely obtain houghite metal oxide nano-sheet.
Embodiment 4 (for Cu/Mg/Al acrylic/hydrotalcite-like nano sheet)
1) preparation of intercalation houghite
What the octyl group amphoteric imidazoline taking 0.614g put into 160mL removes CO
2water wiring solution-forming, under normal temperature, be that metal nitrate mixed salt solution (each material is than being Cu:Mg:Al=7:3:2.5) and the concentration of 0.1mol/L is the sodium hydroxide solution of 2mol/L, and stream adds logical N by 200mL concentration
2the octyl group amphoteric imidazoline aqueous solution in, vigorous stirring, control about pH=8.Salts solution to be mixed dropwises, and stops the dropping of alkali lye.After continuing vigorous stirring 0.5h, put into water heating kettle, 105 DEG C, 24h carries out hydrothermal treatment consists.React complete, product is centrifugal, spends CO
2water washing several times, to neutral, suction filtration, vacuum drying, namely obtains intercalation hydrotalcite-like materials.。
2) preparation of acrylic/hydrotalcite-like nano sheet
Take 0.15g intercalation hydrotalcite-like materials, put into rapidly the acetum of 100mLpH=1.5, without CO
2environment in after vigorous stirring 12h, leave standstill a moment, get the translucent solution in upper strata and carry out high speed centrifugation separation (10000rpm, 20min), namely obtain houghite metal oxide nano-sheet.
Embodiment 5 (for Cu/Mg/Al acrylic/hydrotalcite-like nano sheet)
1) preparation of intercalation houghite
What 500mL put into by the octyldimethyl trimethyl-glycine taking 3.48g removes CO
2water wiring solution-forming, under normal temperature, be that metal nitrate mixed salt solution (each material is than being Cu:Mg:Al=7:3:3) and the concentration of 1.5mol/L is the sodium hydroxide solution of 1.5mol/L, and stream adds logical N by 50mL concentration
2octyldimethyl aqueous solutions of betaine in, vigorous stirring, control about pH=9.Salts solution to be mixed dropwises, and stops the dropping of alkali lye.After continuing vigorous stirring 1h, put into water heating kettle, 115 DEG C, 20h carries out hydrothermal treatment consists.React complete, product is centrifugal, spends CO
2water washing several times, to neutral, suction filtration, vacuum drying, namely obtains intercalation hydrotalcite-like materials.
2) preparation of acrylic/hydrotalcite-like nano sheet
Take 0.1g intercalation hydrotalcite-like materials, put into rapidly the hydrochloric acid soln of the 200mLpH=5 configured in advance, without CO
2environment in vigorous stirring after 3 days, leave standstill a moment, get the translucent solution in upper strata and carry out high speed centrifugation separation (10000rpm, 15min), namely obtain houghite metal oxide nano-sheet.
Embodiment 6 (for Cu/Zn/Al acrylic/hydrotalcite-like nano sheet)
1) preparation of intercalation houghite
What 100mL put into by the dodecyl oxyethyl group sultaine taking 0.57g removes CO
2water wiring solution-forming, under normal temperature, be that metal nitrate mixed salt solution (each material is than being Cu:Zn:Al=7:3:4) and the concentration of 1mol/L is the sodium hydroxide solution of 1.mol/L, and stream adds logical N by 50mL concentration
2dodecyl oxyethyl group sulfobetaines alkali aqueous solution in, vigorous stirring, control about pH=10.Salts solution to be mixed dropwises, and stops the dropping of alkali lye.After continuing vigorous stirring 0.5h, put into water heating kettle, 120 DEG C, 20h carries out hydrothermal treatment consists.React complete, product is centrifugal, spends CO
2water washing several times, to neutral, suction filtration, vacuum drying, namely obtains intercalation hydrotalcite-like materials.。
2) preparation of acrylic/hydrotalcite-like nano sheet
Take 0.15g intercalation hydrotalcite-like materials, put into rapidly the salpeter solution of the 100mLpH=1.5 configured in advance, without CO
2environment in vigorous stirring after 3 days, leave standstill a moment, get the translucent solution in upper strata and carry out high speed centrifugation separation (10000rpm, 20min), namely obtain houghite metal oxide nano-sheet.
Embodiment 7 (for Cu/Zn/Mg/Al acrylic/hydrotalcite-like nano sheet)
1) preparation of intercalation houghite
What the stearylamide propyl group amine oxide taking 1.66g put into 80mL removes CO
2water wiring solution-forming, under normal temperature, be that metal nitrate mixed salt solution (each material is than being Cu:Zn:Mg:Al=4:3:3:6) and the concentration of 0.5mol/L is the sodium hydroxide solution of 0.6mol/L, and stream adds logical N by 100mL concentration
2stearylamide propyl group amine oxide aqueous solution in, vigorous stirring, control about pH=9.Salts solution to be mixed dropwises, and stops the dropping of alkali lye.After continuing vigorous stirring 1h, put into water heating kettle, 100 DEG C, 24h carries out hydrothermal treatment consists.React complete, product is centrifugal, spends CO
2water washing several times, to neutral, suction filtration, vacuum drying, namely obtains intercalation hydrotalcite-like materials.
2) preparation of acrylic/hydrotalcite-like nano sheet
Take 1.5g intercalation hydrotalcite-like materials, put into rapidly the citric acid solution of the 500mLpH=1.5 configured in advance, without CO
2environment in after vigorous stirring 24h, leave standstill a moment, get the translucent solution in upper strata and carry out high speed centrifugation separation (10000rpm, 15min), namely obtain houghite metal oxide nano-sheet.
Claims (7)
1. a preparation method for acrylic/hydrotalcite-like nano sheet, is characterized in that, comprises step as follows:
(1) preparation of intercalation houghite: adopt hydrothermal method, by mixed salt solution and sodium hydroxide solution and stream joins in amphoterics solution, keep pH=8 ~ 11, after completion of the reaction, put into water heating kettle and carry out hydrothermal treatment consists, taking out product afterwards, drying except anhydrating, obtain intercalation houghite; The concentration of amphoterics solution is lower than the micelle-forming concentration of itself;
(2) acrylic/hydrotalcite-like nano sheet preparation: in whipping process, above-mentioned obtained intercalation houghite is put into the acid solution configured in advance, after completion of the reaction, leave standstill a moment, get upper strata translucent liquid, carry out high speed centrifugation, obtain acrylic/hydrotalcite-like nano sheet.
2. the preparation method of a kind of acrylic/hydrotalcite-like nano sheet as claimed in claim 1, it is characterized in that, mixing salt described in step (1) is at least two kinds in aluminum nitrate, zinc nitrate, magnesium nitrate, cupric nitrate, and in mixed metal salt, the mol ratio of trivalent metal cation and divalent metal is 0.25 ~ 0.67 ︰ 1.
3. the preparation method of a kind of acrylic/hydrotalcite-like nano sheet as claimed in claim 1, it is characterized in that, the amphoterics described in step (1) is one or more in betaine type amphoteric surfac-tant, imidazoline type amphoterics, amino acid type amphoteric surface active agent.
4. the preparation method of a kind of acrylic/hydrotalcite-like nano sheet as claimed in claim 1, is characterized in that, amphoterics solution, mixed salt solution and NaOH solution described in step (1) are all used without CO
2water formulated.
5. the preparation method of a kind of acrylic/hydrotalcite-like nano sheet as claimed in claim 1, is characterized in that, the acid in the acid solution described in step (2) is hydrochloric acid, nitric acid, acetic acid, sulfuric acid or citric acid.
6. the preparation method of a kind of acrylic/hydrotalcite-like nano sheet as claimed in claim 1, is characterized in that, the acid solution described in step (2) is used without CO
2water formulated.
7. the preparation method of a kind of acrylic/hydrotalcite-like nano sheet as claimed in claim 1, is characterized in that, step (2) whole process is without CO
2environment in carry out.
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Cited By (6)
| 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 |
| WO2018138512A1 (en) * | 2017-01-27 | 2018-08-02 | University College Cardiff Consultants Ltd | Catalyst suitable for methanol synthesis |
| CN110433764A (en) * | 2019-08-13 | 2019-11-12 | 浙江理工大学 | A kind of double-hydroxide preparation method for fluorine absorption |
| CN110898796A (en) * | 2019-11-27 | 2020-03-24 | 清华大学深圳国际研究生院 | Preparation method of magnetic layered double hydroxide, magnetic layered double hydroxide and application thereof |
| CN112176338A (en) * | 2020-09-04 | 2021-01-05 | 重庆大学 | Preparation method of ZnAL-LDHs film with amino acid ion intercalation |
| CN113234254A (en) * | 2021-04-27 | 2021-08-10 | 台州学院 | Intercalated hydrotalcite flame-retardant smoke suppressant and preparation method thereof |
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| CN102786927A (en) * | 2012-08-24 | 2012-11-21 | 北京化工大学 | 4-hydroxy coumarin intercalated hydrotalcite blue-light composite luminescence material and preparation method thereof |
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Cited By (6)
| 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 |
| WO2018138512A1 (en) * | 2017-01-27 | 2018-08-02 | University College Cardiff Consultants Ltd | Catalyst suitable for methanol synthesis |
| CN110433764A (en) * | 2019-08-13 | 2019-11-12 | 浙江理工大学 | A kind of double-hydroxide preparation method for fluorine absorption |
| CN110898796A (en) * | 2019-11-27 | 2020-03-24 | 清华大学深圳国际研究生院 | Preparation method of magnetic layered double hydroxide, magnetic layered double hydroxide and application thereof |
| CN112176338A (en) * | 2020-09-04 | 2021-01-05 | 重庆大学 | Preparation method of ZnAL-LDHs film with amino acid ion intercalation |
| CN113234254A (en) * | 2021-04-27 | 2021-08-10 | 台州学院 | Intercalated hydrotalcite flame-retardant smoke suppressant and preparation method thereof |
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| CN105439188B (en) | 2017-10-17 |
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