CN115611300A - Method for preparing hydrotalcite in one step without solvent - Google Patents
Method for preparing hydrotalcite in one step without solvent Download PDFInfo
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- CN115611300A CN115611300A CN202211277650.1A CN202211277650A CN115611300A CN 115611300 A CN115611300 A CN 115611300A CN 202211277650 A CN202211277650 A CN 202211277650A CN 115611300 A CN115611300 A CN 115611300A
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- 238000000034 method Methods 0.000 title claims abstract description 41
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 title claims abstract description 29
- 229960001545 hydrotalcite Drugs 0.000 title claims abstract description 29
- 229910001701 hydrotalcite Inorganic materials 0.000 title claims abstract description 29
- 239000002904 solvent Substances 0.000 title claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 25
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 22
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 18
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000004202 carbamide Substances 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 12
- 230000007935 neutral effect Effects 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000013078 crystal Substances 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 9
- 239000012535 impurity Substances 0.000 abstract description 8
- 230000000052 comparative effect Effects 0.000 description 15
- 229910052760 oxygen Inorganic materials 0.000 description 9
- 239000000047 product Substances 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 7
- 239000011777 magnesium Substances 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 6
- 238000000227 grinding Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 4
- 239000001099 ammonium carbonate Substances 0.000 description 4
- 235000012501 ammonium carbonate Nutrition 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 230000005415 magnetization Effects 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910013553 LiNO Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003637 basic solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
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- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
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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
- C01G15/00—Compounds of gallium, indium or thallium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/20—Two-dimensional structures
- C01P2002/22—Two-dimensional structures layered hydroxide-type, e.g. of the hydrotalcite-type
-
- 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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/86—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by NMR- or ESR-data
-
- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a method for preparing hydrotalcite in one step without solvent, which comprises the following steps: 1) Physically mixing a mixed nitrate and urea to obtain a mixed raw material, wherein the mixed nitrate is a mixture of at least one monovalent or divalent nitrate and at least one trivalent nitrate, and the mixed nitrate contains at least one hydrated nitrate; 2) Placing the mixed raw material obtained in the step 1) into a reaction kettle, and placing the reaction kettle at 100-110 ℃ for heating reaction to obtain a reaction product; 3) Repeatedly washing the reaction product obtained in the step 2) with deionized water to be neutral, and drying to obtain the hydrotalcite. The method does not need to use external water as a solvent, and the hydrotalcite material prepared by the method has good crystal form, no impurity, rich sites, uniform size, stable structure and good industrial application prospect.
Description
Technical Field
The invention relates to a preparation method of hydrotalcite, in particular to a method for preparing hydrotalcite by one-step reaction without using any solvent, belonging to the technical field of inorganic materials.
Background
Hydrotalcite (LDHs) and hydrotalcite-like materials have been paid much attention to researchers because of their unique two-dimensional structures, and their adjustable compositions and morphologies, which have a wide application prospect in the fields of catalysis, ion exchange, carbon dioxide adsorption, flame retardation, polymer composites, drug release, and the like.
At present, the synthesis methods of LDHs mainly comprise a coprecipitation method, a hydrothermal method, a sol-gel method and a reconstruction method, and a large amount of aqueous solution is required to be used in the methods. In addition, the pH of the reaction system needs to be controlled at a specific value, and thus, an acidic or basic solution needs to be continuously added. Obviously, the above-mentioned conventional processes require the use of large amounts of water and additional chemicals, and also produce more waste streams which must be subjected to special treatments, such as dilution with water, which are clearly detrimental to sustainable development.
Mechanochemical synthesis has attracted considerable attention in order to reduce the use of water in the hydrotalcite synthesis process. Research shows that the LDHs can be synthesized by a mechanochemical method, but the LDHs without impurities are difficult to generate in one step by dry mechanical grinding, so a two-step method or water-adding grinding is usually adopted, the process is more complicated, and the LDHs are rarely applied to actual production.
Chinese patent CN201210179441.3 discloses a method for preparing hydrotalcite without adding water or with a small amount of water, which specifically comprises: fully grinding a mixture of divalent metal salt and trivalent metal salt to 60 meshes, transferring the mixture into a small kettle, then weighing urea or ammonium carbonate according to a proportion, adding the urea or ammonium carbonate into a large kettle, then placing the small kettle into the large kettle, adding water or not in the large kettle, then sealing the whole system, placing the system at 150-200 ℃ for reaction to obtain a hydrotalcite product, wherein the principle is that ammonium carbonate or urea is decomposed into ammonia and carbon dioxide at high temperature in a closed system, and the ammonia and the carbon dioxide are transferred to the surface of mixed salt through gas phase for reaction, and hydrothermally generating hydrotalcite with the assistance of crystal water.
The method indeed solves the problems of large water consumption, serious pollution and the like existing in the traditional method, but has high requirements on equipment, if equipment with a large kettle sleeved with a small kettle is required to be adopted, and operation processes such as grinding pretreatment of metal salt and the like exist, the process is complex, the problem of overlarge reaction system pressure exists in order to completely decompose urea or ammonium carbonate to generate gas at a high temperature of more than 150 ℃, so that the method is still inconvenient and energy-saving, and the industrial large-scale production requirements are difficult to realize.
Disclosure of Invention
Aiming at the defects of large water consumption, high equipment requirement, complex process, impurities in the obtained hydrotalcite and the like of the existing hydrotalcite preparation method, the invention provides the hydrotalcite preparation method which has the advantages of simple process, low cost, strong operability, short production period and environmental friendliness.
The technical scheme for solving the technical problems is as follows:
a method for preparing hydrotalcite in one step without solvent comprises the following steps:
1) Physically mixing a mixed nitrate and urea to obtain a mixed raw material, wherein the mixed nitrate is a mixture of at least one monovalent or divalent nitrate and at least one trivalent nitrate, and the mixed nitrate contains at least one hydrated nitrate;
2) Placing the mixed raw materials obtained in the step 1) into a reaction kettle, and placing the reaction kettle at 100-110 ℃ for heating reaction to obtain a reaction product;
3) Repeatedly washing the reaction product obtained in the step 2) with deionized water to be neutral, and drying to obtain the hydrotalcite.
Preferably, the molar ratio of the mixed nitrate to urea is 1: (1-4).
Preferably, the molar ratio of the mono-or divalent nitrate salt to the trivalent nitrate salt is (0.5-4): 1.
preferably, the heating reaction time is 12-24h.
Preferably, the temperature of the drying is 60-80 ℃.
The technical principle of the invention is introduced as follows:
considering the raw materials again from the perspective of their composition, conventional methods for synthesizing LDHs usually use nitrate with crystal water as the metal source, such as Mg (NO) 3 ) 2 ·6H 2 O and Al (NO) 3 ) 3 ·9H 2 And O, the crystal water molecules are required to provide enough oxygen atoms and hydrogen atoms for the formation of LDHs, so that after nitrate with crystal water is physically blended with urea, in the subsequent heating process, the temperature rise can cause the dissolution of crystal water molecules, the nitrate and the urea can be dissolved in the crystal water dissolved out by the raw materials to form a concentrated solution, and the urea can generate hydrolysis due to the temperature rise to further generate an alkaline environment, so that metal ions are precipitated to finally generate a hydrotalcite material.
The preparation method provided by the invention has the beneficial effects that:
1) The crystal water carried by the raw material per se is dissolved out at the elevated temperature, so that sufficient oxygen and hydrogen atoms are provided for the generation of the hydrotalcite, no external water is needed as a solvent, and no additional chemical is needed to be provided for adjusting the pH of the system;
2) The hydrotalcite material prepared by the method has good crystal form, no impurity, rich sites, uniform size and stable structure;
3) The method has the advantages of simple process, low cost, low equipment requirement, strong operability, short manufacturing period, greenness, sustainability and good industrial application prospect.
Drawings
FIG. 1 is an XRD spectrum of the product obtained in examples 1-3;
FIG. 2 is an XRD spectrum of the products obtained in example 1, comparative example 1 and comparative example 2;
FIG. 3 is an SEM photograph of the products obtained in example 1, comparative example 1 and comparative example 2;
FIG. 4 shows the results of example 1, comparative example 1 and comparative example 2 1 H, solid NMR spectrum;
FIG. 5 is an XRD spectrum of the products obtained in examples 4-7.
Detailed Description
The principles and features of this invention are described below in conjunction with examples, which are included to illustrate the invention and not to limit the scope of the invention.
Example 1:
1) Mixing Mg (NO) 3 ) 2 ·6H 2 O and Al (NO) 3 ) 3 ·9H 2 Controlling the molar ratio of O to be 2, namely, physically blending 0.015mol and 0.045mol of urea to obtain a solid mixed raw material;
2) Transferring the mixed raw material obtained in the step 1) into a reaction kettle, and heating and reacting for 24 hours at 110 ℃ to obtain a reaction product;
3) Washing the reaction product obtained in the step 2) with deionized water to be neutral, and drying at 60 ℃ for 24h to obtain MgAl-LDHs, which is marked as a sample A;
example 2:
1) Mixing Mg (NO) 3 ) 2 ·6H 2 O and Al (NO) 3 ) 3 ·9H 2 Controlling the molar ratio of O to be 3;
2) Transferring the mixed raw material obtained in the step 1) into a reaction kettle, and heating and reacting at 110 ℃ for 12 hours to obtain a reaction product;
3) Washing the reaction product obtained in the step 2) with deionized water to be neutral, and drying at 60 ℃ for 24h to obtain MgAl-LDHs, which is marked as a sample B;
example 3:
1) Mixing Mg (NO) 3 ) 2 ·6H 2 O and Al (NO) 3 ) 3 ·9H 2 Controlling the molar ratio of O to be 4, namely, physically blending 0.015mol and 0.045mol of urea to obtain a solid mixed raw material;
2) Transferring the mixed raw material obtained in the step 1) into a reaction kettle, and heating and reacting for 24 hours at 110 ℃ to obtain a reaction product;
3) Washing the reaction product obtained in the step 2) to be neutral by using deionized water, and drying at 70 ℃ for 24 hours to obtain MgAl-LDHs, and marking as a sample C;
example 4:
1) Mixing Mg (NO) 3 ) 2 ·6H 2 O and Ga (NO) 3 ) 3 ·9H 2 Controlling the molar ratio of O to be 2, namely, physically blending 0.015mol and 0.045mol of urea to obtain a solid mixed raw material;
2) Transferring the mixed raw material obtained in the step 1) into a reaction kettle, and heating and reacting for 24 hours at 110 ℃ to obtain a reaction product;
3) Washing the reaction product obtained in the step 2) with deionized water to be neutral, and drying at 60 ℃ for 24h to obtain MgGa-LDHs, which is marked as a sample D;
example 5:
1) Mixing Co (NO) 3 ) 2 ·6H 2 O and Al (NO) 3 ) 3 ·9H 2 Controlling the molar ratio of O to be 2, namely, physically blending 0.015mol of the total O and 0.03mol of urea to obtain a solid mixed raw material;
2) Transferring the mixed raw material obtained in the step 1) into a reaction kettle, and heating for 24 hours at 110 ℃ to obtain a reaction product;
3) Washing the reaction product obtained in the step 2) with deionized water to be neutral, and drying at 80 ℃ for 24h to obtain CoAl-LDHs, and marking as a sample E;
example 6:
1) Reacting LiNO with a catalyst 3 And Al (NO) 3 ) 3 ·9H 2 Controlling the molar ratio of O to be 1;
2) Transferring the mixed raw material obtained in the step 1) into a reaction kettle, and heating for 24 hours at 110 ℃ to obtain a reaction product;
3) Washing the reaction product obtained in the step 2) to be neutral by using deionized water, and drying for 24 hours at the temperature of 60 ℃ to obtain LiAl-LDHs which is marked as a sample F;
example 7:
1) Zn (NO) 3 ) 2 ·6H 2 O and Al (NO) 3 ) 3 ·9H 2 Controlling the molar ratio of O to be 2;
2) Transferring the mixed raw material obtained in the step 1) into a reaction kettle, and heating for 24 hours at 100 ℃ to obtain a reaction product;
3) Washing the reaction product obtained in the step 2) to be neutral by using deionized water, and drying at 80 ℃ for 12h to obtain ZnAl-LDHs, and marking as a sample G;
comparative example 1:
1) Mixing Mg (NO) 3 ) 2 ·6H 2 O and Al (NO) 3 ) 3 ·9H 2 O is dispersed in 80mL of deionized water by controlling the molar ratio of 2 to 1 to be 0.015mol, and a mixed salt solution is prepared;
2) Dissolving 0.045mol of urea in the mixed salt solution obtained in the step 1) to obtain a mixed raw material;
3) Transferring the mixed raw material obtained in the step 2) into a reaction kettle, and heating at 110 ℃ for 24 hours to obtain a reaction product;
4) Washing the reaction product obtained in the step 3) with deionized water to be neutral, and drying at 60 ℃ for 24H to obtain MgAl-LDHs, which is marked as sample H.
Comparative example 2:
1) 2.565g of Mg (NO) 3 ) 2 ·6H 2 O and 1.876g of Al (NO) 3 ) 3 ·9H 2 Grinding O in mortar for 10-15 min, loading into small kettle, and weighing 3.360g (NH) 4 ) 2 CO 3 Adding into a large kettle.
2) Placing the small kettle into a large kettle, crystallizing for 1 day in a drying oven at 150 ℃, washing and filtering by using deionized water after the reaction is finished, and drying in a drying oven at 80 ℃ to obtain a product I;
(comparative example 2 MgAl-LDHs from example 1 in patent CN 201210179441.3)
The hydrotalcite products obtained in examples 1 to 7 and comparative examples 1 to 2 were subjected to a series of tests and analyses, the results of which are shown in FIGS. 1 to 5, and the spectral analyses were as follows:
1. from the XRD analysis of fig. 1, it can be seen that the samples a, B, and C prepared by the method of the present invention are all typical carbonate type magnesium aluminum hydrotalcite, and there is no impurity diffraction peak, which indicates that the method of the present invention is a new way to successfully prepare magnesium aluminum hydrotalcite with different metal molar ratios.
2. As can be seen from the analysis of fig. 2, sample a prepared by the method of the present invention has a similar crystal structure to sample H prepared in comparative example 1, has no impurity peak, and is a pure hydrotalcite phase, while hydrotalcite material I prepared in comparative example 2 has a significant impurity peak.
3. As can be seen from the analysis of fig. 3, the sample a prepared by the method of the present invention has a uniform size, and the particle size is significantly smaller than that of the sample H prepared in comparative example 1, the smaller particle size facilitates the introduction of more abundant edge sites, and the abundant edge sites facilitate the application of the material, in contrast, the hydrotalcite material I prepared in comparative example 2 has no significant lamellar structure and has significant amorphous morphology.
4. As can be seen from the analysis of FIG. 4, the solid nuclear magnetization of sample A prepared by the method of the present invention is comparable to the solid nuclear magnetization of products H and I obtained in the comparative example 1 The H spectrum shows more sites, and abundant sites have important significance for the application of materials, such as the application of the materials in the fields of adsorption and catalysis.
5. As can be seen from the analysis of FIG. 5, mgGa-LDHs, coAl-LDHs, liAl-LDHs and ZnAl-LDHs prepared by the method have good crystal forms and no impurities, which indicates that the method has certain universality in the preparation of hydrotalcite.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. A method for preparing hydrotalcite in one step without solvent is characterized by comprising the following steps:
1) Physically mixing a mixed nitrate and urea to obtain a mixed raw material, wherein the mixed nitrate is a mixture of at least one monovalent or divalent nitrate and at least one trivalent nitrate, and the mixed nitrate contains at least one hydrated nitrate;
2) Placing the mixed raw material obtained in the step 1) into a reaction kettle, and placing the reaction kettle at 100-110 ℃ for heating reaction to obtain a reaction product;
3) Repeatedly washing the reaction product obtained in the step 2) with deionized water to be neutral, and drying to obtain the hydrotalcite.
2. The method according to claim 1, wherein the molar ratio of mixed nitrate to urea is 1: (1-4).
3. The method according to claim 1 or 2, wherein the molar ratio of mono-or divalent nitrate to trivalent nitrate is (0.5-4): 1.
4. the method according to claim 1 or 2, wherein the heating reaction time is 12-24h.
5. The method according to claim 3, wherein the heating reaction time is 12-24h.
6. The method of claim 1, 2 or 5, wherein the drying temperature is 60-80 ℃.
7. The method according to claim 3, wherein the temperature of the drying is 60-80 ℃.
8. The method according to claim 4, wherein the temperature of the drying is 60-80 ℃.
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| CN103449378A (en) * | 2012-06-04 | 2013-12-18 | 华东师范大学 | Hydrotalcite preparation method |
| CN112919548A (en) * | 2021-03-09 | 2021-06-08 | 陕西科技大学 | Purple luster iron oxide flaky particles and preparation method thereof |
| CN113443650A (en) * | 2021-07-12 | 2021-09-28 | 苏州大学 | Method for preparing nano titanate by utilizing self-release of crystal water |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101746734A (en) * | 2008-12-01 | 2010-06-23 | 中国科学院过程工程研究所 | Hydrotalcite preparation method |
| CN103449378A (en) * | 2012-06-04 | 2013-12-18 | 华东师范大学 | Hydrotalcite preparation method |
| CN112919548A (en) * | 2021-03-09 | 2021-06-08 | 陕西科技大学 | Purple luster iron oxide flaky particles and preparation method thereof |
| CN113443650A (en) * | 2021-07-12 | 2021-09-28 | 苏州大学 | Method for preparing nano titanate by utilizing self-release of crystal water |
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