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Sio2-layered double hydroxide microspheres and methods of making them

A hydroxide, layered double technology, applied in chemical instruments and methods, catalyst activation/preparation, silicon oxide, etc., can solve the problems of surface morphology LDH with small surface area, not allowing adjustment of LDH, etc.

Inactive Publication Date: 2017-08-29
SCG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Unfortunately, the reported method does not allow to tune the morphology of the surface of LDH and the product SiO 2 @LDH not much surface area

Method used

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  • Sio2-layered double hydroxide microspheres and methods of making them
  • Sio2-layered double hydroxide microspheres and methods of making them
  • Sio2-layered double hydroxide microspheres and methods of making them

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0186] Silica spheres (100 mg, 550 nm) were dispersed in deionized water (20 mL) using sonication. After 30min, the Na 2 CO 3(0.96 mmol) was added to the solution and sonicated for an additional 5 min to form solution A. Next, the Mg(NO 3 ) 2 ·6H 2 O(0.96mmol) and Al(NO 3 ) 3 9H 2 A solution of O (0.48 mmol) in water (19.2 mL) was added to solution A. The pH of the reaction solution was controlled to 10 by adding 1M NaOH. The resulting solid was collected by centrifugation at 4000 rpm for 5 min, then redispersed in deionized water (40 mL) and stirred for 1 h. Repeat collection and redispersion two more times. Then, the solid was washed with acetone (40 mL), then redispersed in acetone (40 mL) and stirred overnight. The solid was then dried under vacuum.

[0187] Before treatment with acetone, the SiO obtained in this example 2 @LDH has the formula:

[0188] (SiO 2 ) 0.04 @{[Mg 0.75 Al 0.25 (OH) 2 ](CO 3 ) 0.125 1.34(H 2 O)} 0.05

[0189] SiO obtained af...

Embodiment 2

[0206] To obtain a 1:1 Mg:Al LDH, the procedure described above in Example 1 was repeated except that Mg(NO 3 ) 2 ·6H 2 O(0.72mmol) and Al(NO 3 ) 3 9H 2 A solution of O (0.72 mmol) in water (19.2 mL) was added to solution A.

Embodiment 3

[0208] To obtain a 3:1 Mg:Al LDH, the procedure described above in Example 1 was repeated except that Mg(NO 3 ) 2 ·6H 2 O(1.08mmol) and Al(NO 3 ) 3 9H 2 A solution of O (0.36 mmol) in water (19.2 mL) was added to solution A.

[0209] Figure 12 SiO prepared by Mg:Al ratios of 1:1 (Example 2) and 3:1 (Example 3) are shown 2 XRD patterns of @LDH samples.

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PUM

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Abstract

A method of making silica-layered double hydroxide microspheres having the formula I : (i) wherein, Mz+ and M'y+ are two different charged metal cations; z = 1 or 2; y = 3 or 4; 0 < x < 0.9; b is 0 to 10; c is 0 to 10; P > 0, q > 0, Xn- is an anion; with n > 0 a = z(1-x) + xy-2; and the AMO-solvent is an 100% aqueous miscible organic solvent; comprises the steps: (a) contacting silica microspheres and a metal ion containing solution containing metal ions Mz+ and M'y+ in the presence of a base and an anion solution; (b) collecting the product; and (c) optionally treating the product with AMO-solvent and recovering the solvent treated material to obtain the silica-layered double hydroxide microspheres. Preferably, M in the formula I is Li, Mg, Ni or Ca. Preferably, M' in formula I is Al. The invention further provides silica-layered double hydroxide microspheres having the formula I. The silica-layered double hydroxide microspheres may be used as catalysts and / or catalyst supports.

Description

technical field [0001] The present invention relates to new SiO 2 Layered double hydroxide (LDH) microspheres (SiO 2 -layered doublehydroxide (LDH) microsphere) and preparation method thereof. Background technique [0002] Layered double hydroxides (LDHs) are a class of compounds that contain two or more metal cations and have a layered structure. A review of LDHs is provided in Structure and Bonding; Vol. 119, 2005 Layered Double Hydroxides ed. X Duan and D.G. Evans, ed. X Duan and D.G. Evans. Hydrotalcites have been studied for many years and are perhaps the best known examples of LDHs. LDHs can insert anions between the layers of the structure. [0003] In the literature by "core@shell" (for example by Teng et al., Nano Letters, 2003, 3, 261-264) or by "core / shell" (for example by J.Am.Chem Soc., 2001, 123, pp. 7961-7962 p.) describes core-shell particles. We use the "core@shell" name because it appears as the most commonly accepted abbreviation. [0004] SiO is de...

Claims

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Application Information

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IPC IPC(8): B01J20/10C01B33/12C09C1/30C01F7/785
CPCB01J20/103C01B33/12C09C1/3054C01P2006/12C01P2004/84C01P2004/62C01P2004/32C01P2002/72C01P2002/88C01P2002/86C01P2004/04C01P2004/03C01B33/18C01P2004/34C01P2004/80C09C1/405C01P2004/52C01F7/782C01F7/785B01J35/19B01J35/51B01J35/398B01J35/615B01J21/08B01J27/236B01J37/0221
Inventor 德莫特·奥黑尔陈春萍
Owner SCG CHEM CO LTD
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