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Atom-economical preparation method of layered composite metal hydroxide
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A hydroxide and layered composite technology, which is applied in the preparation of oxides/hydroxides, etc., can solve the problems of unrecoverable structure, unavoidable by-product formation and washing process, and achieve the effect of protecting the environment and saving water resources
Active Publication Date: 2011-12-07
北京泰克来尔科技有限公司
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Generally speaking, the recovery of the structure is possible when the calcination temperature is below 500°C. When the calcination temperature is above 600°C, a calcination product with a spinel structure is formed, and the structure cannot be recovered permanently.
This method also requires the synthesis of LDHs precursors in advance, which cannot avoid the generation of by-products and the washing process
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Embodiment 1
[0029] Step A: Mg(OH) 2 and Al(OH) 3 by Mg 2+ / Al 3+ The molar ratio is mixed in a ratio of 3:1, and 10 g of the mixture is placed in 90 g of deionized water, and then added to the reactor;
[0030] Step B: Add 1.27g of ammonium bicarbonate and 10ml of ammonia water into the reactor, raise the temperature to 100°C, react for 2 hours, centrifuge the obtained product and directly dry it at 70°C for 8 hours to obtain the molecular formula Mg 6 Al 2 (OH) 12 CO 3 4H 2 LDHs product of O, namely MgAl-CO 3 -LDHs.
[0031] The crystal structure of the sample was characterized by XRD-6000 X-ray powder diffractometer from Shimadzu Corporation, Japan. figure 1 It is the XRD spectrogram of the sample obtained in Example 1. As can be seen from the figure, the 003, 006 and 009 crystal plane diffraction peaks reflecting the layered structure appear at 2θ=11.7°, 23.4° and 34.5° respectively. The peak shape of the diffraction peak is sharp, the baseline is low and flat, and no impurit...
Embodiment 2
[0034] Step A: Zn(OH) 2 , Mg(OH) 2 and Al(OH) 3 Press Zn 2+ :Mg 2+ : Al 3+ The molar ratio is mixed in a ratio of 1:3:2, and 15g of the mixture is placed in 80g of deionized water, and then added to the reactor;
[0035] Step B: Add 1.27g of ammonium bicarbonate and 20ml of ammonia water into the reactor, raise the temperature to 200°C, react for 1 hour, centrifuge the obtained product and directly dry it at 70°C for 8 hours to obtain the molecular formula ZnMg 3 Al 2 (OH) 12 CO 3 4H 2 O's LDHs products.
Embodiment 3
[0037] Step A: Ca(OH) 2 and Al(OH) 3 Press Ca 2+ :Al 3+ The molar ratio is mixed in a ratio of 3:1, and 20 g of the mixture is placed in 80 g of deionized water, and then added to the reactor;
[0038] Step B: Add 1.27g of ammonium bicarbonate and 30ml of ammonia water into the reactor, raise the temperature to 200°C, react for 1 hour, centrifuge the obtained product, and directly dry at 70°C for 8 hours to obtain the molecular formula Ca 4 Al 2 (OH) 12 CO 3 4H 2 O's LDHs products.
[0039] The elemental content of the samples was analyzed by a Shimadzu ICPS-7500 elemental analyzer. Elemental analysis shows that the sample prepared in Example 3 shows that Ca in the product: Al=3: 1, and does not contain Na in the product + and other hetero ions.
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Abstract
The invention discloses an atom-economic preparation method of a layered composite metal hydroxide, which belongs to the technical field of preparation of inorganic non-metallic functional materials. The invention uses metal hydroxide, ammonium salt and ammonia water as raw materials, and prepares layered composite metal hydroxide through atomic economical reaction in a reactor. The reaction process uses ammonium salt and ammonia water, which reduces the temperature of the reaction, making the reaction conditions more mild and easy to control; the ammonium salt used in the reaction and the ammonia in the ammonia water can be recovered in the post-treatment process; the reaction uses metal hydroxide The compound and the anion are the corresponding ammonium salts of An-, without using other raw materials such as NaOH, all raw materials participate in the reaction and generate the target product, and the atom economy is 100%, which belongs to a typical atom economy reaction. No by-products are generated in the production process of the invention, and the products can be dried to obtain pure products without washing, which greatly saves water resources and protects the environment.
Description
technical field [0001] The invention belongs to the technical field of preparation of inorganic non-metallic functional materials, in particular to an atom-economic preparation method of layered composite metal hydroxides. Background technique [0002] Layered double hydroxides (LDHs for short), also known as hydrotalcite, is a typical anionic layered material, and its chemical composition formula is [M 2+ 1 -xM 3+ x (OH) 2 ]A n- x / n mH 2 O, where M 2+ , M 3+ is a metal cation, A n- is an interlayer anion, x is M 3+ The mole fraction of ions, m is the number of crystal water. The element types and composition ratios of the main laminates of LDHs, and the types and quantities of interlayer objects can be adjusted in a wide range according to needs, so as to obtain materials with special structures and properties. The adjustable composition and structure of LDHs and the resulting multifunctionality make them a class of new materials with great research potential an...
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