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Method for preparing magnesium-based layered composite metal hydroxide through high-pressure continuous feeding technology

A feeding technology and composite metal technology, which is applied in the field of inorganic functional material preparation, can solve the problems of large ion concentration, large solubility difference, uneven product composition and structure, and achieve the effect of eliminating volume effect and ensuring uniformity.

Inactive Publication Date: 2014-05-28
BEIJING UNIV OF CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Due to the large difference in solubility between brucite and aluminum hydroxide, it is very easy to cause Mg(OH) 2 Local Mg during nucleation on aluminum hydroxide surface in ionic form 2+ Excessive ion concentration and uneven product composition

Method used

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  • Method for preparing magnesium-based layered composite metal hydroxide through high-pressure continuous feeding technology
  • Method for preparing magnesium-based layered composite metal hydroxide through high-pressure continuous feeding technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Step A: the total mass is 30kg, and the molar ratio is 2:1 Mg(OH) 2 and Al(OH) 3 were added to 60kg of deionized water, and pretreated by a sand mill to make Mg(OH) 2 and Al(OH) 3 Slurry, take 10kg Mg(OH) 2 and all Al(OH) 3 The slurry is added into the autoclave;

[0015] Step B: heat up to the reaction temperature of 120°C, and use the plunger pump to remove the remaining Mg(OH) 2 The slurry was injected into the autoclave at a rate of 0.5L / min, while CO was introduced at a rate of 10ml / min 2 , reacted for 6h under stirring conditions, stopped the aeration, and dried the obtained product at 70°C for 8 hours to obtain the molecular formula Mg 4 al 2 (OH) 12 CO 3 4H 2 Magnesium-based layered composite metal hydroxides of O.

[0016] The XRD-6000 X-ray powder diffractometer of Shimadzu Corporation was used to characterize the crystal structure of the product. figure 1 It is an XRD spectrum. It can be seen from the figure that Mg appears at around 2θ=11.7°, 23....

Embodiment 2

[0019] Step A: the total mass is 30kg, and the molar ratio is 3:1 Mg(OH) 2 and Al(OH) 3 , were added to 60kg deionized water, and pretreated by a sand mill to make Mg(OH) 2 and Al(OH) 3 Slurry, take 10kgMg(OH) 2 and all Al(OH) 3 The slurry is added into the autoclave;

[0020] Step B: Add 22.5kg of boric acid, heat up to 100°C under stirring, discharge the air through the exhaust valve, continue to heat up to 200°C, and drain the remaining Mg(OH) through the plunger pump 2 The slurry was injected into the autoclave at a rate of 0.5 L / min, reacted for 24 hours, and the obtained product was dried at 70°C for 8 hours to obtain B with a Mg / Al ratio of 3. 3 o 3 (OH) 4 - Intercalated magnesium-based layered composite metal hydroxides.

Embodiment 3

[0022] Step A: the total mass is 30kg, and the molar ratio is 4:1 Mg(OH) 2 and Al(OH) 3 were added to 60kg of deionized water, and pretreated by a sand mill to make Mg(OH) 2 and Al(OH) 3 Slurry, take 5kgMg(OH) 2 and all Al(OH) 3 The slurry is added into the autoclave;

[0023] Step B: Add 34.8kg of phthalic acid, heat up to a reaction temperature of 120°C under stirring, and pump the remaining Mg(OH) 2 The slurry was injected into the autoclave at a rate of 0.5L / min, reacted for 8 days, and the obtained product was dried at 70°C for 8 hours to obtain the molecular formula Mg 8 al 2 (OH) 20 (C 8 h 4 o 4 )·4H 2 Magnesium-based layered composite metal hydroxides of O.

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Abstract

The invention discloses a method for preparing magnesium-based layered composite metal hydroxide through a high-pressure continuous feeding technology, and belongs to the technical field of preparation of inorganic functional materials. According to the reaction principle of clean production technologies, the method creatively adopts the high-pressure continuous feeding technology to add higher-solvability Mg(OH)2 into a reaction system in a reaction process to prepare the layered composite metal hydroxide with homogeneous structural compositions. A plunger pump is adopted to continuously feed Mg(OH)2 into a reaction kettle, so as to eliminate a volume effect in a magnification process and ensure the homogeneity of the compositions and the structure of the product at each stage. Due to overhigh Mg<2+> concentration, a basic magnesium carbonate or residual Al(OH)3 characteristic peak can appear on the XRD (X-Ray Diffraction). The product with high Mg / Al ratio, prepared by the method, is free of the basic magnesium carbonate or residual Al(OH)3 characteristic peak or other peaks.

Description

Technical field: [0001] The invention belongs to the technical field of preparation of inorganic functional materials, and in particular relates to a method for preparing magnesium-based layered composite metal hydroxide by adopting a high-pressure continuous feeding technology. 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-x m 3+ x (OH) 2 ]A n- x / n mH 2 O, where M 2+ , M 3+ represent divalent and trivalent metal cations, respectively, 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 a series of materials with special structures and properties. [0003] The patent (200710062650.9) pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F7/00
Inventor 林彦军王桂荣李凯涛段雪闻陈法谭徐昌
Owner BEIJING UNIV OF CHEM TECH