CN109231244A - A kind of preparation method and application of potassium hydroxide etch magnalium hydrotalcite - Google Patents

A kind of preparation method and application of potassium hydroxide etch magnalium hydrotalcite Download PDF

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Publication number
CN109231244A
CN109231244A CN201811111321.3A CN201811111321A CN109231244A CN 109231244 A CN109231244 A CN 109231244A CN 201811111321 A CN201811111321 A CN 201811111321A CN 109231244 A CN109231244 A CN 109231244A
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CN
China
Prior art keywords
potassium hydroxide
magnalium hydrotalcite
hydrotalcite
hydroxide etch
reaction kettle
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Application number
CN201811111321.3A
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Chinese (zh)
Inventor
冯艳艳
李彦杰
杨地
叶广源
潘柳东
廖燕华
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Guilin University of Technology
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Guilin University of Technology
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Publication date
Application filed by Guilin University of Technology filed Critical Guilin University of Technology
Priority to CN201811111321.3A priority Critical patent/CN109231244A/en
Publication of CN109231244A publication Critical patent/CN109231244A/en
Withdrawn legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/78Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
    • C01F7/784Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
    • C01F7/785Hydrotalcite
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06Solid 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
    • B01J20/08Solid 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
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02CCAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00Capture or disposal of greenhouse gases
    • Y02C20/40Capture or disposal of greenhouse gases of CO2

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses a kind of preparation method and applications of potassium hydroxide etch magnalium hydrotalcite.Etching method is used to be removed the aluminium species in magnalium hydrotalcite to form nano pore using potassium hydroxide, to improve the specific surface area inside hydrotalcite.By scanning electron microscope as can be seen that occurring duct on the magnalium hydrotalcite nanoscale twins of potassium hydroxide etch, and the fractal dimension of sheet surfaces and fringe region increases.Preparation process of the present invention is simple, obtained potassium hydroxide etch magnalium hydrotalcite, has biggish effective ratio area, is capable of providing more active adsorption sites, has biggish application prospect in terms of carbon dioxide adsorption and trapping.

Description

A kind of preparation method and application of potassium hydroxide etch magnalium hydrotalcite
Technical field
The present invention relates to a kind of preparation method of hydrotalcite-based compound, especially a kind of potassium hydroxide etch magnalium neatly The preparation method and application of stone.
Background technique
Hydrotalcite is by two or more positively charged complex metal hydroxide mainboard layers and for the layer of balancing charge Between anion and hydrone composition.Due to hydrotalcite have special structure and physicochemical properties, such as interlayer anion can Exchangeability, Modulatory character, acid-base property, the memory effect of mainboard layer cation etc., so that it is outstanding in various fields effect.Especially It is magnalium hydrotalcite, due to properties such as its excellent alkalinity, adsorptivity, thermal stability, nontoxicitys, in catalyst carrier, inhales It has a good application prospect in the fields such as enclosure material, environment-friendly materials, functional material, pharmaceutical carrier, in recent years by people's Extensive concern.
The preparation method of magnalium hydrotalcite mainly has coprecipitation, hydro-thermal method, sol-gel method, ion-exchange at present With roasting thermal reduction etc..For magnalium hydrotalcite prepared by these methods, internal effective ratio area is smaller, in conduct Limited sorption capacity when carbon dioxide absorber.Therefore, in conjunction with the amphotericity of aluminium compound, the present invention is utilized using etching method Potassium hydroxide removes to form nano pore the aluminium species in magnalium hydrotalcite, thus improve its it is internal using than Surface area.
Summary of the invention
The purpose of the present invention is removed to aluminium species using potassium hydroxide to prepare potassium hydroxide etch magnalium neatly Stone material, it is internal using specific surface area, the more adsorption sites of exposure, so as to improve magnalium hydrotalcite to two to improve it The absorption property of carbonoxide.
Specific steps of the invention are as follows:
(1) 1.366 g magnesium nitrates and 1.0 g aluminum nitrates are placed in 70 mL distilled water, stirring is until solid is completely dissolved.
(2) 4.32 g urea are added in step (1) acquired solution, continue to stir, dissolve urea all.
(3) step (2) acquired solution is transferred in the reaction kettle of 100 mL polytetrafluoroethyllining linings, reaction kettle is placed in 120 oC baking oven reacts 12 hours, to be cooled to room temperature after reaction.Products therefrom is subjected to decompression suction filtration, is washed with distillation It washs 5~6 times.
(4) step (3) products therefrom is transferred in the potassium hydroxide solution that 75 mL concentration are 0.5 mol/L, later It is placed on magnetic stirring apparatus and stirs 10 minutes.
(5) solidliquid mixture obtained by step (4) is transferred in the reaction kettle of 100 mL polytetrafluoroethyllining linings, will be reacted Kettle is placed in 95oC reacts 2 hours, is cooled to room temperature after reaction.
(6) step (5) products therefrom is centrifuged, after being washed with distilled water 5~6 times, then is washed with dehydrated alcohol It washs 2~3 times;Sample is 80 after washingo6 hours are dried under C to get potassium hydroxide etch magnalium hydrotalcite.
Obtained potassium hydroxide etch magnalium hydrotalcite can apply to carbon dioxide adsorption and trapping.
Preparation process of the present invention is simple, obtained potassium hydroxide etch magnalium hydrotalcite, has biggish effective ratio table Area is capable of providing more active adsorption sites, has biggish application prospect in terms of carbon dioxide adsorption and trapping.
Detailed description of the invention
Fig. 1 is the technology path schematic diagram that the embodiment of the present invention prepares potassium hydroxide etch magnalium hydrotalcite.
Fig. 2 is not lose made from potassium hydroxide etch magnalium hydrotalcite (a) obtained by the embodiment of the present invention and comparative example Carve the scanning electron microscope (SEM) photograph of magnalium hydrotalcite (b).
Specific embodiment
Embodiment:
(1) 1.366 g magnesium nitrates and 1.0 g aluminum nitrates are placed in 70 mL distilled water, stirring is until solid is completely dissolved.
(2) 4.32 g urea are added in step (1) acquired solution, continue to stir, dissolve urea all.
(3) step (2) acquired solution is transferred in the reaction kettle of 100 mL polytetrafluoroethyllining linings, reaction kettle is placed in 120 oC baking oven reacts 12 hours, to be cooled to room temperature after reaction.Products therefrom is subjected to decompression suction filtration, is washed with distillation It washs 5 times.
(4) by step (3) products therefrom be transferred to 75 mL concentration be 0.5 mol/L potassium hydroxide solution in, postposition In being stirred 10 minutes on magnetic stirring apparatus.
(5) solidliquid mixture obtained by step (4) is transferred in the reaction kettle of 100 mL polytetrafluoroethyllining linings, will be reacted Kettle is placed in 95oC reacts 2 hours, is cooled to room temperature after reaction.
(6) step (5) products therefrom is centrifuged, after being washed with distilled water 5 times, then with dehydrated alcohol washs 3 It is secondary;Sample is 80 after washingo6 hours are dried under C to get potassium hydroxide etch magnalium hydrotalcite.
Fig. 2 (a) is the scanning electron microscope (SEM) photograph of potassium hydroxide etch magnalium hydrotalcite, it can be seen that the magnesium of potassium hydroxide etch Occurs duct on aluminum hydrotalcite nano piece layer, and the fractal dimension of sheet surfaces and fringe region increases, and can be carbon dioxide Absorption provides more adsorption activity positions.
Obtained potassium hydroxide etch magnalium hydrotalcite can apply to carbon dioxide adsorption and trapping.
Comparative example:
(1) 1.366 g magnesium nitrates and 1.0 g aluminum nitrates are placed in 70 mL distilled water, stirring is until solid is completely dissolved.
(2) 4.32 g urea are added in step (1) acquired solution, continue to stir, dissolve urea all.
(3) step (2) acquired solution is transferred in the reaction kettle of 100 mL polytetrafluoroethyllining linings, reaction kettle is placed in 120 oC baking oven reacts 12 hours, to be cooled to room temperature after reaction.Products therefrom is subjected to decompression suction filtration, is washed with distillation After washing 5 times, then washed 3 times with dehydrated alcohol.Sample is 80 after washingo6 hours are dried under C to get magnalium neatly is not etched Stone.
The scanning electron microscope (SEM) photograph of magnalium hydrotalcite is not etched as shown in Fig. 2 (b), the magnalium water without potassium hydroxide etch processing Smooth regular hexagon flaky nanometer structure is presented in talcum.
Pass through the control of embodiment and comparative example, it will thus be seen that use the resulting potassium hydroxide of preparation method of the invention Etching magnalium hydrotalcite has special appearance structure and biggish specific surface area, has potential carbon dioxide adsorption and trapping Application prospect.

Claims (2)

1. a kind of preparation method of potassium hydroxide etch magnalium hydrotalcite, it is characterised in that specific steps are as follows:
(1) 1.366 g magnesium nitrates and 1.0 g aluminum nitrates are placed in 70 mL distilled water, stirring is until solid is completely dissolved;
(2) 4.32 g urea are added in step (1) acquired solution, continue to stir, dissolve urea all;
(3) step (2) acquired solution is transferred in the reaction kettle of 100 mL polytetrafluoroethyllining linings, reaction kettle is placed in 120oC baking oven reacts 12 hours, to be cooled to room temperature after reaction;Products therefrom is subjected to decompression suction filtration, is washed with distilled water 5 ~6 times;
(4) by step (3) products therefrom be transferred to 75 mL concentration be 0.5 mol/L potassium hydroxide solution in, be placed on It is stirred 10 minutes on magnetic stirring apparatus;
(5) solidliquid mixture obtained by step (4) is transferred in the reaction kettle of 100 mL polytetrafluoroethyllining linings, reaction kettle is set In 95oC reacts 2 hours, is cooled to room temperature after reaction;
(6) step (5) products therefrom is centrifuged, after being washed with distilled water 5~6 times, then wash 2 with dehydrated alcohol~ 3 times;Sample is 80 after washingo6 hours are dried under C to get potassium hydroxide etch magnalium hydrotalcite.
2. the application of the potassium hydroxide etch magnalium hydrotalcite prepared method according to claim 1, it is characterised in that the hydrogen Potassium oxide etching magnalium hydrotalcite can apply to carbon dioxide adsorption and trapping.
CN201811111321.3A 2018-09-23 2018-09-23 A kind of preparation method and application of potassium hydroxide etch magnalium hydrotalcite Withdrawn CN109231244A (en)

Priority Applications (1)

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CN201811111321.3A CN109231244A (en) 2018-09-23 2018-09-23 A kind of preparation method and application of potassium hydroxide etch magnalium hydrotalcite

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811111321.3A CN109231244A (en) 2018-09-23 2018-09-23 A kind of preparation method and application of potassium hydroxide etch magnalium hydrotalcite

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115709070A (en) * 2022-11-08 2023-02-24 北京化工大学 Photocatalyst for carbon dioxide reduction reaction and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115709070A (en) * 2022-11-08 2023-02-24 北京化工大学 Photocatalyst for carbon dioxide reduction reaction and preparation method thereof

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