CN116081671A - Porous double-metal hydroxide and preparation method and application thereof - Google Patents
Porous double-metal hydroxide and preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 229910000000 metal hydroxide Inorganic materials 0.000 title claims description 35
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims abstract description 90
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000012266 salt solution Substances 0.000 claims abstract description 53
- 239000012670 alkaline solution Substances 0.000 claims abstract description 52
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000000243 solution Substances 0.000 claims abstract description 50
- 239000004317 sodium nitrate Substances 0.000 claims abstract description 45
- 235000010344 sodium nitrate Nutrition 0.000 claims abstract description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims abstract description 42
- 239000008367 deionised water Substances 0.000 claims abstract description 33
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 33
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- 238000001035 drying Methods 0.000 claims abstract description 27
- 238000003756 stirring Methods 0.000 claims abstract description 21
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims abstract description 19
- 239000000725 suspension Substances 0.000 claims abstract description 19
- 238000000967 suction filtration Methods 0.000 claims abstract description 15
- 239000012065 filter cake Substances 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000011148 porous material Substances 0.000 claims abstract description 7
- 150000004692 metal hydroxides Chemical class 0.000 claims description 24
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 16
- 150000001768 cations Chemical class 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 10
- 239000011261 inert gas Substances 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 4
- -1 nitrate anions Chemical class 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- 239000003463 adsorbent Substances 0.000 claims description 2
- 230000036571 hydration Effects 0.000 claims description 2
- 238000006703 hydration reaction Methods 0.000 claims description 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 238000011049 filling Methods 0.000 description 10
- 238000005303 weighing Methods 0.000 description 10
- 239000013078 crystal Substances 0.000 description 9
- 238000001179 sorption measurement Methods 0.000 description 9
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 8
- 238000002425 crystallisation Methods 0.000 description 8
- 230000008025 crystallization Effects 0.000 description 8
- 239000011229 interlayer Substances 0.000 description 7
- 239000001569 carbon dioxide Substances 0.000 description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000004570 mortar (masonry) Substances 0.000 description 5
- 238000004448 titration Methods 0.000 description 5
- 239000002351 wastewater Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 125000000129 anionic group Chemical group 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- HEFNNWSXXWATRW-UHFFFAOYSA-N Ibuprofen Chemical compound CC(C)CC1=CC=C(C(C)C(O)=O)C=C1 HEFNNWSXXWATRW-UHFFFAOYSA-N 0.000 description 2
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000002734 clay mineral Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229960001680 ibuprofen Drugs 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 229910001425 magnesium ion Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000011895 specific detection Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- JQMFQLVAJGZSQS-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-N-(2-oxo-3H-1,3-benzoxazol-6-yl)acetamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)NC1=CC2=C(NC(O2)=O)C=C1 JQMFQLVAJGZSQS-UHFFFAOYSA-N 0.000 description 1
- CONKBQPVFMXDOV-QHCPKHFHSA-N 6-[(5S)-5-[[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]methyl]-2-oxo-1,3-oxazolidin-3-yl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C[C@H]1CN(C(O1)=O)C1=CC2=C(NC(O2)=O)C=C1 CONKBQPVFMXDOV-QHCPKHFHSA-N 0.000 description 1
- 229910003023 Mg-Al Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000004098 Tetracycline Substances 0.000 description 1
- 238000005815 base catalysis Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000036760 body temperature Effects 0.000 description 1
- 229910052599 brucite Inorganic materials 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 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 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 210000004051 gastric juice Anatomy 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910001701 hydrotalcite Inorganic materials 0.000 description 1
- 229960001545 hydrotalcite Drugs 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000000968 intestinal effect Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229960002180 tetracycline Drugs 0.000 description 1
- 229930101283 tetracycline Natural products 0.000 description 1
- 235000019364 tetracycline Nutrition 0.000 description 1
- 150000003522 tetracyclines Chemical class 0.000 description 1
- 238000011282 treatment Methods 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28059—Surface area, e.g. B.E.T specific surface area being less than 100 m2/g
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/10—Magnesium; Oxides or hydroxides thereof
-
- B01J35/613—
-
- B01J35/643—
-
- B01J35/647—
-
- B01J35/69—
-
- 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
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention relates to the technical field of inorganic material preparation, in particular to a porous bimetal hydroxide, a preparation method and application thereof, wherein the preparation method comprises the following preparation steps: dissolving magnesium nitrate and aluminum nitrate in deionized water to form a mixed salt solution, dissolving sodium nitrate in the deionized water to prepare a sodium nitrate solution, and dissolving sodium hydroxide in the deionized water to prepare an alkaline solution; adding alkaline solution into sodium nitrate solution until pH value is 10-11, adding mixed salt solution and alkaline solution into sodium nitrate solution under water bath condition under stirring, controlling pH value to be 10.5-12.5, adding mixed salt solution until pH value is controlled to be 10-11.5, and stirring to obtain suspension; washing the suspension with deionized water, performing suction filtration, and drying the obtained filter cake to obtain the porous bimetal hydroxide. The prepared porous bimetal hydroxide has the advantages of adjustable pore space, high quality and controllable crystallinity.
Description
Technical Field
The invention relates to the technical field of inorganic material preparation, in particular to a porous bimetal hydroxide, a preparation method and application thereof.
Background
The double metal hydroxide has a layered structure similar to brucite, and has excellent physical and chemical properties, such as acid-base catalysis, redox catalysis, photoelectrochemistry and the like. Cations in the framework of the double metal hydroxide laminate can be matched with each other in different molar proportions and different types within a certain element range, so that the hydrotalcite type anionic clay mineral can flexibly regulate and control the anionic charge density of the metal laminate; on the other hand, the interlayer anions thereof can be exchanged or reassembled, and the above properties make the experimental study of the double metal hydroxide and the development of high added value in industrial production significant.
The basic structural formula of the double metal hydroxide is
At present, the molar ratio of the divalent metal salt to the trivalent metal salt of the prepared bimetal hydroxide is 1-5:1, and the layered bimetal hydroxide with the molar ratio of the divalent metal salt to the trivalent metal salt of 1:5-6 is also reported, because the nitrate-type sample is difficult to prepare, and the nitrate-type bimetal hydroxide sample with higher purity is not easy to obtain when the bimetal hydroxide is prepared by adopting a common method.
Disclosure of Invention
The invention mainly aims to provide a porous bimetal hydroxide, a preparation method and application thereof, and aims to solve the technical problems that the preparation method of the layered bimetal hydroxide with the molar ratio of divalent metal salt to trivalent metal salt of 1:5-6 in the prior art is less, and nitrate-type bimetal hydroxide with higher purity is not easy to obtain.
In order to achieve the above object, the present invention provides a method for preparing a porous bimetal hydroxide, comprising the following preparation steps: s1, dissolving magnesium nitrate and aluminum nitrate in deionized water to form a mixed salt solution, dissolving sodium nitrate in the deionized water to prepare a sodium nitrate solution, and dissolving sodium hydroxide in the deionized water to prepare an alkaline solution;
s2, dropwise adding the alkaline solution into the sodium nitrate solution until the pH value is 10-11, simultaneously dropwise adding the mixed salt solution and the alkaline solution into the sodium nitrate solution under the water bath condition while stirring, controlling the pH value to be 10.5-12.5, continuously dropwise adding the mixed salt solution until the pH value is controlled to be 10-11.5, and stirring to obtain a suspension;
s3, washing the suspension with deionized water, carrying out suction filtration, and drying a filter cake obtained by suction filtration to obtain the porous bimetal hydroxide.
The formation of layered double hydroxide mainly comprises two parts of crystal nucleus formation and growth, in the reaction process, the alkaline solution prepared by NaOH gradually releases OH < - > to react with metal ions in the mixed salt solution, and after the crystal nucleus is formed, the crystal nucleus is reacted for a period of time to enable the crystal nucleus to grow into a more complete crystal structure. In the scheme, the pH value is higher when the porous Mg-Al double metal hydroxide is generated and is controlled within the range of 10.5-12.5, impurities are easy to generate when the pH value is controlled to be improper, so that the scheme adopts an accurate slow-speed double-drop dripping method when the pH value is controlled, the drop dripping speed in the step S2 is controlled to be 5-15mL/min, if the drop dripping speed is too fast, incomplete nucleation of a later product is easy to be caused, and trivalent cations are favorably adhered to the formed Mg (OH) in the form of hydrated aggregates by the dripping method 2 On the regular octahedral crystal nucleus, isomorphous replacement is carried out, so that the growth rate of the crystal nucleus is accelerated, the proportion of trivalent metal cations in the skeleton laminate of the obtained nitrate-type porous bimetal hydroxide is controllable, the prepared porous bimetal hydroxide belongs to a porous clay mineral material, and the purity of a product obtained by adopting the method can reach more than 96 percent at present.
Wherein, when the mixed salt solution and the alkaline solution are simultaneously dripped into the sodium nitrate solution, the pH value is raised by 1 to 1.5 compared with the previous step, and then the pH value is relatively lowered by 0.5 to 1.5 compared with the previous step when the mixed salt solution is continuously dripped into the mixed salt solution.
Preferably, in step S1, the molar ratio of the magnesium nitrate to the aluminum nitrate is 1:5.2-6. The molar ratio of magnesium ions to aluminum ions is limited by limiting the molar ratio of magnesium nitrate to aluminum nitrate, the molar ratio of magnesium ions to aluminum ions is specifically 1:5.2-6, and the crystallinity of the composite material is controlled more finely by preparing porous double metal hydroxide with a small ratio range, so that the stacking layer number and the order of the product in the microscopic c-axis direction are controlled, and the properties of the material such as adsorption property and the like are controlled more precisely.
Preferably, in the step S1, the concentration of the mixed salt solution is 1-2.5mol/L, the concentration of the sodium nitrate solution is 1.6-2.6mol/L, and the concentration of the alkaline solution is 1-2.5mol/L.
Preferably, the molar ratio of the mixed salt solution, the alkaline solution and the sodium nitrate solution is 1:0.5-2:0.5-2. By limiting the molar ratio, the porous bimetal hydroxide with relatively good performance can be obtained, and when the alkaline solution is mixed with the salt solution and the alkaline solution in the above range, the limiting requirement of the pH value in the scheme can be met.
Preferably, in step S2, the water bath temperature is 70-90 ℃ and the water bath time is 36-72h. The proper water bath temperature and time can balance the formation rate and the growth rate of crystal nuclei, and is favorable for generating the laminar double metal hydroxide with better crystal form and single layer, so that the interlayer spacing is larger.
Preferably, in step S2, stirring is continued for more than 8 hours to obtain a suspension. Firstly, dropwise adding the alkaline solution, then, dropwise adding the mixed salt solution until the alkaline solution and the mixed salt solution are dropwise added, and continuously stirring for 8 hours to complete the reaction.
Preferably, in step S3, the drying temperature is 70-90 ℃ and the drying time is 12-24 hours. The drying is mainly used for reducing the water content in the filter cake, so that the prepared porous double-metal hydroxide has higher purity and better performance.
Preferably, step S1, step S2 and step S3 are all performed under the protection of inert gas. Under the protection of inert gas, the water and carbon dioxide in the air can not influence the reaction, so that the porous double-metal hydroxide with better performance is obtained.
In addition, the invention also provides a porous double-metal hydroxide, which is characterized by being prepared by the preparation method of any one of the porous double-metal hydroxide, and the chemical composition general formula is as follows:
wherein M is 2+ Is a divalent metal cation, M 3+ Is a trivalent metal cation, A n -nitrate anions, m being the hydration number, said molar ratio of divalent metal cations to trivalent metal cations being in the range 1:5.2-6.
Preferably, the specific surface area of the porous bimetallic hydroxide is 15-95m 2 And/g, the pore diameter is 0.8-50nm. That is, the porous double metal hydroxide produced by the above process has a porous characteristic.
In addition, the invention also provides an application of the porous double-metal hydroxide, and the porous double-metal hydroxide has the characteristic of being porous, so that the porous double-metal hydroxide can be used as an adsorbent or a catalyst carrier, has a good adsorption effect on part of impurities, and can also be used as a catalyst carrier to play a good role in catalysis.
Compared with the prior art, the porous double metal hydroxide and the preparation method thereof have the following beneficial effects: the preparation method of the nitrate-type porous bimetal hydroxide with controllable pore channel characteristics is provided, the porous bimetal hydroxide is prepared by adopting a bimetal coprecipitation reaction method under the closed environment protected by inert gas, and conditions such as the reaction temperature of a system, the crystallization time of a mixed suspension liquid and the like are accurately controlled in the whole preparation process, so that the porous bimetal hydroxide with different performance indexes is prepared. The method controls the pore channel characteristics by adjusting the molar ratio range of divalent cations and trivalent cations (influencing the height of the interlayer micropore channel and the number of cationic charges in the interlayer domain), the pH value (influencing the crystallization degree) and the like. Wherein the microporous passageway is of a height that provides selective adsorption or selective passage of molecules or ions. The charge number can regulate and control the ion type contained between layers; the degree of crystallization can control the porosity and thus affect the adsorption capacity. The preparation method has the advantages of simple operation, low cost, good repeatability and short growth period; more importantly, the scheme realizes finer control of the crystallinity of the composite material by preparing the porous bimetal hydroxide with a small ratio range, so that the material performance of the composite material is more accurately controlled, and the prepared porous bimetal hydroxide has the advantages of adjustable pore space, high quality, controllable crystallinity and the like, can be used for separating and adsorbing gas, and can also be used for adsorbing and separating flame retardant materials, catalyst carriers, heavy metals or organic pollutants (such as organic volatile gas and the like) after different types of special treatments.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and that other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic structural diagram of a porous bimetallic hydroxide provided herein;
FIG. 2 is a porous bimetallic hydroxide X-ray diffraction pattern corresponding to example 1 and examples 5-1 to 5-4 provided herein;
FIG. 3 is a chemical diagram of the interlayer region of porous double metal hydroxide provided herein.
The realization, functional characteristics and advantages of the present application will be further described with reference to the embodiments, referring to the attached drawings.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In addition, the technical solutions of the embodiments may be combined with each other, but it is necessary to base that the technical solutions can be realized by those skilled in the art, and when the technical solutions are contradictory or cannot be realized, the combination of the technical solutions should be considered to be absent and not within the scope of protection claimed in the present invention.
A method for preparing porous double metal hydroxide, comprising the following steps:
s1, mixing magnesium nitrate and aluminum nitrate in a molar ratio, placing the mixture in an agate mortar, grinding the mixture to ensure that the granularity is thinned (the granularity is controlled to be 10-100 mu m), dissolving the mixture in 500-1500 mL of deionized water (the deionized water is boiled for more than 30 minutes and then used) to form a mixed salt solution, weighing sodium nitrate with the same mass as that of the magnesium nitrate, dissolving the sodium nitrate in the deionized water to prepare a sodium nitrate solution, weighing sodium hydroxide, dissolving the sodium nitrate in the deionized water to prepare an alkaline solution;
wherein the molar ratio of the magnesium nitrate to the aluminum nitrate is 1:5.2-6, the concentration of the mixed salt solution is 1-2.5mol/L, the concentration of the sodium nitrate solution is 1.6-2.6mol/L, and the concentration of the alkaline solution is 1-2.5mol/L;
s2, filling a sodium nitrate solution into a 2000mL three-neck flask, dropwise adding an alkaline solution until the pH value becomes 10-11, respectively filling the mixed salt solution and the alkaline solution into two 250mL titration funnels with controllable flow rates under a water bath condition, slowly dropwise adding the mixed salt solution and the alkaline solution into the three-neck flask (the mixed salt solution and the alkaline solution are dropwise added at the same time) while strongly stirring (the stirring speed is 150-450 rpm), controlling the pH value of the whole solution system in the three-neck flask to be 10.5-12.5, controlling the pH value to be 10-11.5 after the mixed salt solution is titrated, and continuing stirring for 8-36 hours to obtain a suspension;
wherein the mol ratio of the mixed salt solution to the alkaline solution to the sodium nitrate solution is 1:0.5-2:0.5-2, the water bath temperature is 70-90 ℃, and the water bath time is 36-72h;
s3, continuously stirring until crystallization is completed, washing the suspension liquid with deionized water from which carbon dioxide is removed for a plurality of times, carrying out suction filtration, and drying a filter cake obtained by suction filtration in a drying oven (the drying temperature is 70-90 ℃ and the drying time is 12-24 h) to obtain the porous bimetal hydroxide.
(step S1, step S2 and step S3 are all performed under the protection of inert gas)
The porous bimetallic hydroxide in this embodiment can adsorb anionic type impurities or molecules in organic wastewater, such as phenol; or drug molecules or ions in wastewater containing ibuprofen, tetracycline and the like generated in the artificial drugs. Of course, the adsorption of the anions is not limited to the above, and some macromolecules can be adsorbed by porous double metal hydroxide.
In addition, the porous double-metal hydroxide can be used as a carrier in the ibuprofen slow-release capsule, and the external skeleton frame of the porous double-metal hydroxide is utilized to play a role in protecting, so that the release speed of the medicine in gastric juice or intestinal environment of a human body is greatly reduced, and then the body temperature of the human body is gradually reduced under long-acting control.
As shown in FIG. 3, FIG. 3 shows the chemical characteristics of the interlayer region of the nitrate-type porous bimetal hydroxide with controllable pore channel characteristics, wherein d 003 Represents the interlayer spacing of the porous bimetallic hydroxide in the nanoscale, d in this embodiment 003 0.8-0.9nm.
The following description of the embodiments of the present invention will be presented in further detail with reference to the examples, which should be understood as being merely illustrative of the present invention and not limiting.
Example 1
A preparation method of porous double metal hydroxide, comprising the following steps (the following steps S1, S2 and S3 are all carried out under the protection of inert gas):
s1, mixing magnesium nitrate and aluminum nitrate according to a molar ratio of 1:5.2, grinding and thinning in a mortar, dissolving in 500mL of deionized water to form a mixed salt solution, wherein the concentration of the mixed salt solution is 1mol/L, weighing sodium nitrate which is the same as the magnesium nitrate in mass and dissolving in the deionized water to prepare a sodium nitrate solution, the concentration of the sodium nitrate solution is 2mol/L, weighing sodium hydroxide and dissolving in the deionized water to prepare an alkaline solution, and the concentration of the alkaline solution is 1mol/L;
s2, filling a sodium nitrate solution into a three-neck flask, dropwise adding an alkaline solution until the pH value becomes 10.5, respectively filling the mixed salt solution and the alkaline solution into two titration funnels with controllable flow rates under the water bath condition (the water bath temperature is 90 ℃ and the water bath time is 72 h), slowly dropwise adding the mixed salt solution and the alkaline solution into the three-neck flask while strongly stirring, controlling the pH value of the whole solution system in the three-neck flask to be 11, controlling the pH value to be 10 after the mixed salt solution is titrated, and continuing stirring for 24h until crystallization is completed to obtain a suspension; wherein the molar ratio of the mixed salt solution to the alkaline solution to the sodium nitrate solution is 1:1:2;
s3, washing the suspension liquid for 3 times by using deionized water from which carbon dioxide is removed, performing suction filtration, and drying a filter cake obtained by suction filtration in an oven (the drying temperature is 85 ℃ and the drying time is 24 hours) to obtain the porous bimetal hydroxide.
Example 2
A preparation method of porous double metal hydroxide, comprising the following steps (the following steps S1, S2 and S3 are all carried out under the protection of inert gas):
s1, mixing magnesium nitrate and aluminum nitrate according to a molar ratio of 1:5.5, grinding and thinning in a mortar, dissolving in 800mL of deionized water to form a mixed salt solution, wherein the concentration of the mixed salt solution is 1mol/L, weighing sodium nitrate which is the same as the magnesium nitrate in mass and dissolving in the deionized water to prepare a sodium nitrate solution, the concentration of the sodium nitrate solution is 1.6mol/L, weighing sodium hydroxide and dissolving in the deionized water to prepare an alkaline solution, and the concentration of the alkaline solution is 1mol/L;
s2, filling a sodium nitrate solution into a three-neck flask, dropwise adding an alkaline solution until the pH value becomes 10.5, respectively filling the mixed salt solution and the alkaline solution into two titration funnels with controllable flow rates under the water bath condition (the water bath temperature is 75 ℃ and the water bath time is 72 h), slowly dropwise adding the mixed salt solution and the alkaline solution into the three-neck flask while strongly stirring, controlling the pH value of the whole solution system in the three-neck flask to be 12, controlling the pH value to be 10.5 after the mixed salt solution is titrated, and continuously stirring for 36h until crystallization is completed to obtain a suspension; wherein the molar ratio of the mixed salt solution, the alkaline solution and the sodium nitrate solution is 1: 1.6:1;
s3, washing the suspension liquid for 3 times by using deionized water from which carbon dioxide is removed, performing suction filtration, and drying a filter cake obtained by suction filtration in a drying oven (the drying temperature is 80 ℃ and the drying time is 24 hours) to obtain the porous bimetal hydroxide.
Example 3
A preparation method of porous double metal hydroxide, comprising the following steps (the following steps S1, S2 and S3 are all carried out under the protection of inert gas):
s1, mixing magnesium nitrate and aluminum nitrate according to a molar ratio of 1:6, grinding and thinning in a mortar, dissolving in 1000mL of deionized water to form a mixed salt solution, wherein the concentration of the mixed salt solution is 2.5mol/L, weighing sodium nitrate which is the same as the magnesium nitrate in mass and dissolving in the deionized water to prepare a sodium nitrate solution, the concentration of the sodium nitrate solution is 2.5mol/L, weighing sodium hydroxide and dissolving in the deionized water to prepare an alkaline solution, and the concentration of the alkaline solution is 2.5mol/L;
s2, filling a sodium nitrate solution into a three-neck flask, dropwise adding an alkaline solution until the pH value becomes 10.5, respectively filling the mixed salt solution and the alkaline solution into two titration funnels with controllable flow rates under the water bath condition (the water bath temperature is 80 ℃ and the water bath time is 72 h), slowly dropwise adding the mixed salt solution and the alkaline solution into the three-neck flask while strongly stirring, controlling the pH value of the whole solution system in the three-neck flask to be 11, controlling the pH value to be 10.5 after the mixed salt solution is titrated, and then continuously stirring for 24h until crystallization is completed to obtain a suspension; wherein the molar ratio of the mixed salt solution to the alkaline solution to the sodium nitrate solution is 1:1:1;
s3, washing the suspension liquid for a plurality of times by using deionized water from which carbon dioxide is removed, performing suction filtration, and drying a filter cake obtained by suction filtration in a drying oven (the drying temperature is 80 ℃ and the drying time is 24 hours) to obtain the porous bimetal hydroxide.
Example 4
A preparation method of porous double metal hydroxide, comprising the following steps (the following steps S1, S2 and S3 are all carried out under the protection of inert gas):
s1, mixing magnesium nitrate and aluminum nitrate according to a molar ratio of 1:5.8, grinding and thinning in a mortar, dissolving in 600mL of deionized water to form a mixed salt solution, wherein the concentration of the mixed salt solution is 1.3mol/L, weighing sodium nitrate which is the same as the mass of the magnesium nitrate, dissolving in the deionized water to prepare a sodium nitrate solution, the concentration of the sodium nitrate solution is 2.6mol/L, weighing sodium hydroxide, dissolving in the deionized water to prepare an alkaline solution, and the concentration of the alkaline solution is 1.3mol/L;
s2, filling a sodium nitrate solution into a three-neck flask, dropwise adding an alkaline solution until the pH value becomes 11, respectively filling the mixed salt solution and the alkaline solution into two titration funnels with controllable flow rates under the water bath condition (the water bath temperature is 70 ℃ and the water bath time is 72 h), slowly dropwise adding the mixed salt solution and the alkaline solution into the three-neck flask while strongly stirring, controlling the pH value of the whole solution system in the three-neck flask to be 12.5, controlling the pH value to be 11.5 after the mixed salt solution is titrated, and then continuing stirring for 8h until crystallization is completed to obtain a suspension; wherein the molar ratio of the mixed salt solution to the alkaline solution to the sodium nitrate solution is 1:2:1;
s3, washing the suspension liquid for a plurality of times by using deionized water from which carbon dioxide is removed, performing suction filtration, and drying a filter cake obtained by suction filtration in a drying oven (the drying temperature is 80 ℃ and the drying time is 24 hours) to obtain the porous bimetal hydroxide.
Comparative example 1
The conditions in this comparative example were the same as in example 1, except that: the comparative example adopts the existing molar ratio of magnesium nitrate to aluminum nitrate (the molar ratio of the magnesium nitrate to the aluminum nitrate is adjusted within the range of 1-5:1), namely the magnesium nitrate is added in a large amount, and other preparation steps and parameters are consistent with those of the example 1, and the specific adjustment is as follows:
comparative example 2
The conditions in this comparative example were the same as in example 1, except that: in the step S2 of the comparative example, when the mixed salt solution and the alkaline solution were dropped into the sodium nitrate solution, the pH value of the whole solution system was controlled to 10, and the other preparation steps and parameters were the same as those of example 1.
Comparative example 3
The conditions in this comparative example were the same as in example 1, except that: the water bath temperature in step S2 of this comparative example was adjusted to 65 ℃, and the other preparation steps and parameters were the same as in example 1.
The porous double metal hydroxides prepared in examples 1 to 4 and comparative examples 1 to 3 were subjected to performance tests, and specific test results are shown in the following table:
note that, regarding the detection of the adsorption amount of phenol in wastewater: the ultraviolet spectrophotometer is used for measurement, so that the scheme is configured by a laboratory to simulate phenol in the wastewater, and the product of the scheme is directly put into the wastewater containing phenol during measurement. The purity in the above detection data is calculated from XRD patterns.
As is clear from the above table, the porous double metal hydroxide produced by the production method of the present embodiment has a porous characteristic. When the molar ratio of magnesium nitrate to aluminum nitrate is adjusted, the specific surface area and the adsorption quantity of phenol are greatly reduced, and the purity is also reduced; when the pH of the solution system was adjusted to 10, the specific surface area and the amount of adsorbed phenol were reduced drastically, and the purity was also reduced. The water bath temperature is also particularly important, and when the water bath temperature is too low, both the purity and the adsorption effect of phenol are reduced.
Example 5
The conditions in this example were the same as in example 1, except that: in this example, the molar ratio of the mixed magnesium nitrate to aluminum nitrate was adjusted to verify how the properties corresponding to the obtained porous double metal hydroxide could be adjusted after the molar ratio of the mixed magnesium nitrate to aluminum nitrate was adjusted, and the following preparation steps and parameters were consistent with those of example 1, except that:
| molar ratio of magnesium nitrate to aluminum nitrate | |
| Example 1-1 | 1∶5.2 |
| Example 5-1 | 1∶5.4 |
| Example 5-2 | 1∶5.6 |
| Examples 5 to 3 | 1∶5.8 |
| Examples 5 to 4 | 1∶6 |
| Examples 5 to 5 | 1∶4.5 |
| Examples 5 to 6 | 1∶6.2 |
The porous double metal hydroxide prepared in the embodiment is subjected to performance detection, and specific detection results are shown in the following table:
as can be seen from the examination data of the above table, when the molar ratio of magnesium nitrate to aluminum nitrate is in the range of 1:5.2-6, the effect is relatively good, and the specific surface area is 68.3m 2 The purity is above 80 percent, and the adsorption quantity of phenol is above 55.9 mg/g.
Example 6
The conditions in this example were the same as in example 1, except that: in this example, the respective dropping rates of the mixed salt solution and the alkaline solution were adjusted to change the pH value of the whole solution system in the three-necked flask, and the other preparation steps and parameters were the same as those in example 1, except that:
the porous double metal hydroxide prepared in the embodiment is subjected to performance detection, and specific detection results are shown in the following table:
as can be seen from the above table, when the pH of the solution system is changed, the performance of the product is changed, wherein the performance of the product obtained in example 1 is optimal.
The foregoing description is only of the preferred embodiments of the present invention and is not intended to limit the scope of the invention, and all equivalent structural changes made by the content of the present invention or direct/indirect application in other related technical fields are included in the scope of the present invention.
Claims (10)
1. The preparation method of the porous double metal hydroxide is characterized by comprising the following preparation steps:
s1, dissolving magnesium nitrate and aluminum nitrate in deionized water to form a mixed salt solution, dissolving sodium nitrate in the deionized water to prepare a sodium nitrate solution, and dissolving sodium hydroxide in the deionized water to prepare an alkaline solution;
s2, dropwise adding the alkaline solution into the sodium nitrate solution until the pH value is 10-11, simultaneously dropwise adding the mixed salt solution and the alkaline solution into the sodium nitrate solution under the water bath condition while stirring, controlling the pH value to be 10.5-12.5, continuously dropwise adding the mixed salt solution until the pH value is controlled to be 10-11.5, and stirring to obtain a suspension;
s3, washing the suspension with deionized water, carrying out suction filtration, and drying a filter cake obtained by suction filtration to obtain the porous bimetal hydroxide.
2. The method for producing a porous bimetal hydroxide according to claim 1, wherein in step S1, the molar ratio of said magnesium nitrate to said aluminum nitrate is 1:5.2-6.
3. The method for producing a porous double metal hydroxide according to claim 1, wherein in step S1, the concentration of the mixed salt solution is 1 to 2.5mol/L, the concentration of the sodium nitrate solution is 1.6 to 2.6mol/L, and the concentration of the alkaline solution is 1 to 2.5mol/L.
4. The method for producing a porous bimetal hydroxide according to claim 1, wherein in step S2, the molar ratio of said mixed salt solution, said alkaline solution and said sodium nitrate solution is 1:0.5-2:0.5-2.
5. The method for producing a porous bimetal hydroxide according to claim 1, wherein in step S2, the water bath temperature is 70 to 90 ℃ and the water bath time is 36 to 72 hours.
6. The method for producing a porous bimetal hydroxide according to claim 1, wherein in step S2, stirring is continued for 8 hours or more to obtain a suspension.
7. The method for producing a porous bimetal hydroxide according to claim 1, wherein in step S3, the drying temperature is 70 to 90 ℃ and the drying time is 12 to 24 hours.
8. The method for producing a porous bimetal hydroxide according to claim 1, wherein step S1, step S2 and step S3 are each performed under the protection of an inert gas.
9. A porous bimetallic hydroxide prepared by the method of any one of claims 1-8, having the chemical composition formula:
wherein M is 2+ Is a divalent metal cation, M 3+ Is a trivalent metal cation, A n- For nitrate anions, m is a hydration number, and the molar ratio of the divalent metal cations to the trivalent metal cations is in the range of 1:5.2-6;
the specific surface area of the porous double metal hydroxide is 15-95m 2 And/g, the pore diameter is 0.8-50nm.
10. Use of a porous bimetallic hydroxide according to claim 9 as an adsorbent or catalyst support.
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