CN110589872A - Preparation method of single-layer zinc-aluminum hydrotalcite - Google Patents
Preparation method of single-layer zinc-aluminum hydrotalcite Download PDFInfo
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- CN110589872A CN110589872A CN201910807315.XA CN201910807315A CN110589872A CN 110589872 A CN110589872 A CN 110589872A CN 201910807315 A CN201910807315 A CN 201910807315A CN 110589872 A CN110589872 A CN 110589872A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/006—Compounds containing, besides zinc, two ore more other elements, with the exception of oxygen or hydrogen
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- 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
Abstract
A preparation method of single-layer zinc-aluminum hydrotalcite comprises the following steps: preparation of Zn (NO)3)2·6H2O and Al (NO)3)3·9H2The mixed solution of O is marked as solution A; preparing NaOH solution and recording the NaOH solution as solution B; preparing a boric acid solution, and recording the boric acid solution as a solution C; under the protection of inert gas, simultaneously dripping the solution A and the solution B into a reaction container, keeping the pH value of the system between 7 and 10, continuing stirring for 30 to 60min after dripping, carrying out suction filtration and washing, dispersing a filter cake into the solution C, stirring for 1 to 3h, carrying out suction filtration and washing, dispersing the filter cake into acetone, stirring for 1 to 3h, carrying out suction filtration and washing, and drying the filter cake to obtain single-layer zinc-aluminum hydrotalcite; the preparation method is simple, and the single-layer hydrotalcite with a good crystal form can be obtained; the interlayer spacing is firstly enlarged and then the laminated plate is stripped by utilizing the characteristic of the interchangeability of anions between hydrotalcite layers, so that the time for stripping the laminated plate is greatly shortened.
Description
(I) technical field
The invention relates to the technical field of catalysis, in particular to a preparation method of single-layer zinc-aluminum hydrotalcite.
(II) background of the invention
Hydrotalcite (LDHs) is a class of anionic clay materials with a layered structure, having the general formula: [ M ] A2+ 1-xM3+ x(OH)2]x+(An-)x/n·mH2O, wherein M2+Is Mg2+，Ni2+，Cu2+，Zn2+Divalent metal cations; m3+Is Al3+，Cr3+，Fe3 +An iso-trivalent metal cation; a. then-Being anions, e.g. CO3 2-，NO3 -，Cl-，SO4 2-Inorganic anions are subjected to plasma treatment, interlayer anions have adjustable denaturation, and different anions are introduced between layers through an ion exchange method. In addition, the hydrotalcite material has the characteristic of 'structure memory', namely, the single-layer hydrotalcite and the hydrotalcite calcined at a certain temperature are dispersed in the water solution, and the lamellar structure of the hydrotalcite can be recovered again.
In recent years, single-layered hydrotalcites have received much attention from researchers. Researches find that compared with the traditional hydrotalcite material, the surface of the single-layer hydrotalcite LDH exposes more abundant active crystal faces, oxygen defects and dislocations, and has higher catalytic performance. In addition, the single-layer hydrotalcite also has the characteristics of high conductivity, stable structure, high carrier migration speed, large specific surface area and the like, so that the single-layer hydrotalcite has wide research prospects.
Currently, the most common preparation method of the single-layered hydrotalcite is a top-down peeling and layering method. Namely, the hydrotalcite material is firstly synthesized and then dispersed into a solvent with strong polarity for stripping. Common solvents are butanol, CCl4Toluene, a mixed solution of DMF and ethanol, formamide, and the like. However, the conventional solvent stripping method has the disadvantages of insufficient stripping and long stirring reaction time (2-7 days).
According to the invention, by utilizing the exchangeable property of anions between hydrotalcite layers, anions with larger size are introduced between hydrotalcite layers to enlarge the interlayer spacing of the hydrotalcite, and then the hydrotalcite layers are dispersed in a strong polar solvent to strip the hydrotalcite layers, so that the single-layer hydrotalcite can be obtained finally.
Disclosure of the invention
The invention aims to provide a preparation method of single-layer hydrotalcite. Nitrate radical hydrotalcite is prepared through a coprecipitation method, and then nitrate radical among layers is converted into borate radical by fully utilizing the characteristic of interchangeability of anions among the layers of the hydrotalcite, so that the interlayer spacing is enlarged. And finally, dispersing the hydrotalcite with the borate intercalation in acetone for stripping to obtain the single-layer hydrotalcite.
The technical scheme of the invention is as follows:
a preparation method of single-layer zinc-aluminum hydrotalcite comprises the following steps:
(1) preparation of Zn (NO)3)2·6H2O and Al (NO)3)3·9H2The mixed solution of O is marked as solution A; preparing 1-1.5 mol/L NaOH solution, and recording the NaOH solution as solution B; preparing 0.5-2 mol/L boric acid solution which is marked as solution C;
the solvent used to prepare solution A, B, C was redistilled water;
in the solution A, Zn2+And Al3+The ratio of the amounts of the substances (A) to (B) is 2 to 4: 1, Al3+The concentration of (A) is 1-10 mol/L;
the solution A, the solution B and the solution C have no special meaning, and are only used for distinguishing different solutions, namely, the solution A, the solution B and the solution C are marked as 'A', 'B' and 'C';
(2) inert gases (e.g. N)2) Under protection, simultaneously dripping the solution A and the solution B into a reaction container, keeping the pH value of the system between 7 and 10, continuously stirring for 30 to 60min after dripping, performing suction filtration and washing, dispersing a filter cake into the solution C, stirring for 1 to 3h, performing suction filtration and washing, dispersing the filter cake into acetone, stirring for 1 to 3h, performing suction filtration and washing, and drying the filter cake at 50 to 80 ℃ for 16 to 24h to obtain single-layer zinc-aluminum hydrotalcite (marked as single layer ZnAl-LDHs);
zn in the solution A2+And Al3+The ratio of the total amount of the substances to the amounts of NaOH in the solution B and boric acid in the solution C was 9: 3: 1;
the washing may be with redistilled water.
The single-layer zinc-aluminum hydrotalcite prepared by the invention can be used for photocatalytic degradation reaction and photocatalytic CO2Reduction, water decomposition and hydrogenation reactions.
The invention has the advantages that:
(1) the preparation method is simple, and the single-layer hydrotalcite with better crystal form can be obtained;
(2) the interlayer spacing is firstly enlarged and then the laminated plate is stripped by utilizing the characteristic of the interchangeability of anions between hydrotalcite layers, so that the time for stripping the laminated plate is greatly shortened.
(IV) description of the drawings
FIG. 1 is an XRD pattern of single layer zinc aluminum hydrotalcite of example 1;
fig. 2 is an XRD pattern of the single-layer structure of example 2 restored to zinc-aluminum hydrotalcite.
(V) detailed description of the preferred embodiments
The present invention is further illustrated by the following specific examples, but the scope of the invention is not limited thereto.
Example 1:
a preparation method of a single-layer zinc-aluminum hydrotalcite material comprises the following steps:
(1) 0.6mol of Zn (NO) is taken3)2·6H2O and 0.3mol of Al (NO)3)3·9H2Dissolving O in 100mL of redistilled water to prepare a solution A;
(2) dissolving 0.3mol of NaOH in 200mL of redistilled water to prepare solution B;
(3) dissolving 0.1mol of boric acid in 100mL of redistilled water to prepare a solution C;
(4) in N2Under the protection of (1), simultaneously dripping the solution A and the solution B into a round-bottom flask, and keeping the pH value of the solution between 7 and 10; stirring for 60min after dripping;
(5) after stirring, carrying out suction filtration, washing with 200mL of redistilled water to be neutral, dispersing a filter cake into the solution C, and stirring for 1 h;
(6) carrying out suction filtration on the obtained slurry, washing the slurry to be neutral by 200mL of redistilled water, dispersing a filter cake into 100mL of acetone, and stirring for 2 h;
(7) and after stirring, carrying out suction filtration, washing the mixture to be neutral by 200mL of redistilled water, and drying the mixture for 16 hours at 80 ℃ to obtain the single layer ZnAl-LDHs.
Example 2:
(1) taking 0.01mol of Na2CO3Dissolving in 100mL of deionized water to prepare a solution D;
(2) dispersing 1g of the prepared single-layer zinc-aluminum hydrotalcite in the solution D, and stirring for 3 h;
(3) and (3) carrying out suction filtration on the obtained slurry, washing the slurry to be neutral by using 200mL of redistilled water, and drying the slurry for 16h at the temperature of 80 ℃ to obtain the ZnAl-LDH-receiver.
Characterization of XRD
A Shimadzu XRD-6000X-ray powder diffractometer is adopted, wherein the characteristic parameters are set as follows: cu target, Kalpha ray, lambda of 0.15405nm, angle range of 5-70 deg, and scanning speed of 4 deg/min.
As can be seen from the XRD spectrogram of single layer ZnAl-LDHs, the (003) characteristic peak of the hydrotalcite does not appear in the sample, which indicates the successful synthesis of the single-layer hydrotalcite; in addition, the XRD pattern of ZnAl-LDH-receiver shows the characteristic peaks of hydrotalcite (003), (006) and (009) with good peak shapes, which indicates that single layer ZnAl-LDHs is dispersed in Na2CO3After the solution, the structure of the hydrotalcite is recovered, and the synthesis of the single-layer hydrotalcite is further proved.
Claims (3)
1. A preparation method of single-layer zinc-aluminum hydrotalcite is characterized by comprising the following steps:
(1) preparation of Zn (NO)3)2·6H2O and Al (NO)3)3·9H2The mixed solution of O is marked as solution A; preparing 1-1.5 mol/L NaOH solution, and recording the NaOH solution as solution B; preparing 0.5-2 mol/L boric acid solution which is marked as solution C;
in the solution A, Zn2+And Al3+The ratio of the amounts of the substances (A) to (B) is 2 to 4: 1, Al3+The concentration of (A) is 1-10 mol/L;
(2) under the protection of inert gas, simultaneously dripping the solution A and the solution B into a reaction container, keeping the pH value of the system between 7 and 10, continuing stirring for 30 to 60min after dripping, carrying out suction filtration and washing, dispersing a filter cake into the solution C, stirring for 1 to 3h, carrying out suction filtration and washing, dispersing the filter cake into acetone, stirring for 1 to 3h, carrying out suction filtration and washing, and drying the filter cake for 16 to 24h at the temperature of 50 to 80 ℃ to obtain single-layer zinc-aluminum hydrotalcite;
zn in the solution A2+And Al3+The total amount of the substances is equal to the amount of NaOH and the solution in the solution BThe mass ratio of boric acid in C is 9: 3: 1.
2. the method for preparing single-layer zinc-aluminum hydrotalcite according to claim 1, wherein in step (1), the solvent used for preparing solution A, B, C is redistilled water.
3. The method for preparing single-layer zinc-aluminum hydrotalcite according to claim 1, wherein in step (2), the washing is performed by redistilled water.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111153444A (en) * | 2020-01-14 | 2020-05-15 | 山东大学 | Method for rapidly preparing carbonate hydrotalcite-like single-layer nanosheets at low temperature |
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| CN103011254A (en) * | 2012-12-19 | 2013-04-03 | 青岛科技大学 | Preparation method for nanosheet of uniformly dispersed layered double hydroxides (LDHs) |
| CN104703918A (en) * | 2012-09-28 | 2015-06-10 | Scg化学有限公司 | Modification of layered double hydroxides |
| US20170107116A1 (en) * | 2014-03-27 | 2017-04-20 | Scg Chemicals Co., Ltd. | High surface area layered double hydroxides |
| CN108940307A (en) * | 2018-06-26 | 2018-12-07 | 浙江工业大学 | Golden cobalt dual-metal load zinc-aluminum hydrotalcite and the preparation method and application thereof |
| CN109641761A (en) * | 2016-06-17 | 2019-04-16 | Scg化学有限公司 | Layered double-hydroxide |
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Patent Citations (5)
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|---|---|---|---|---|
| CN104703918A (en) * | 2012-09-28 | 2015-06-10 | Scg化学有限公司 | Modification of layered double hydroxides |
| CN103011254A (en) * | 2012-12-19 | 2013-04-03 | 青岛科技大学 | Preparation method for nanosheet of uniformly dispersed layered double hydroxides (LDHs) |
| US20170107116A1 (en) * | 2014-03-27 | 2017-04-20 | Scg Chemicals Co., Ltd. | High surface area layered double hydroxides |
| CN109641761A (en) * | 2016-06-17 | 2019-04-16 | Scg化学有限公司 | Layered double-hydroxide |
| CN108940307A (en) * | 2018-06-26 | 2018-12-07 | 浙江工业大学 | Golden cobalt dual-metal load zinc-aluminum hydrotalcite and the preparation method and application thereof |
Non-Patent Citations (3)
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| WANG Q ET AL.: "Large-scale synthesis of highly dispersed layered double hydroxide powders containing delaminated single layer nanosheets", 《CHEMICAL COMMUNICATIONS》 * |
| 刘博: "《煤/水滑石矿物复合材料的制备及其性能研究》", 30 September 2018, 中国矿业大学出版社 * |
| 郑德等: "《稳定剂》", 30 June 2011, 国防工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111153444A (en) * | 2020-01-14 | 2020-05-15 | 山东大学 | Method for rapidly preparing carbonate hydrotalcite-like single-layer nanosheets at low temperature |
| CN111153444B (en) * | 2020-01-14 | 2022-02-15 | 山东大学 | Method for rapidly preparing carbonate hydrotalcite-like single-layer nanosheets at low temperature |
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Application publication date: 20191220 |