Process for preparing small size layered double hydroxide particles
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A double hydroxide and particle technology is applied in chemical instruments and methods, preparation of aluminum compounds, alkaline earth metal aluminates/alumina/aluminum hydroxide, etc. The effect of improving purity
Inactive Publication Date: 2018-01-02
SCG CHEM CO LTD
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Aging at elevated temperature not only increases production cost but also prolongs the production time required to obtain said LDH particles
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[0117] Materials and methods
[0118] Powder X-ray Diffraction (XRD). Powder X-ray diffraction patterns were recorded on a PANalytical X'Pert Pro instrument using a Cu anode and K-α1λ=1.540598 and K-α2λ=1.544426, using a K-α2 / K-α1 ratio of 0.5. The generator voltage (generator voltage) is set to 40kV, and the tube current is set at 0.01°s -1 The lower setting is 40mA from 3 to 70° with a slit size of 1°. The samples were pulverized into powder form and loaded onto stainless steel sample holders.
[0119] Thermogravimetric Analysis (TGA). Thermogravimetric analysis was performed using a Mettler Toledo TGA / DSC 1 system. About 20 mg of the sample was heated in a crucible from 25°C to 700°C at a rate of 5°C / min, and then left to cool.
[0120] Dynamic Light Scattering (DLS). Dynamic light scattering analysis was performed using a Malvern Zetasizer NanoZS from Begbroke Science Park as described. A small amount of the sample in paste form was completely dispersed in about 1...
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Abstract
A process for preparing particles of a layered double hydroxide of the general formula [Mp z+ M'q y+ (OH)2]a+(Xn-)a / n.bH2O (I) wherein Mz+ and M'y+ are metal cations or mixtures of metal cations, z =1 or 2; y = 3 or 4; p + q = 1; b = 0 to 10, Xn- is an anion, n is 1 to 5 and a is determined by p, q, y and z such that a = zp+yq-2 comprises (a) mixing, in aqueous solution, Mz+ cations, M'y+ cationsand Xn- anions, with a base; and (b) allowing the layered double hydroxide of formula (I) to precipitate from the solution mixed in step (a). Preferably, M is Li, Mg, Zn, Fe, Ni, Co, Cu, Ca, or a mixture of two or more. Preferably, y is 3 and M' is Al, Ga, In, Fe or a mixture of two or more thereof. Also provided are particles obtainable by the process, especially wherein M is Ca, M' is Al and Xn- is NO3-. Particles of a layered double hydroxide wherein the particles have a particle size of not greater than 2000 nm, preferably not greater than 300 nm and especially not greater than 100 nm, are also provided. The layered double hydroxides according to the invention are useful in certain applications, for example, as adsorbents, coatings and catalyst supports.
Description
technical field [0001] The present invention relates to a process for the preparation of layered double hydroxide (LDH) particles of very small size. Background technique [0002] Layered double hydroxides (LDHs) are a class of compounds that contain two metal cations and have a layered structure. A review of LDHs is provided in the literature X Duan and D.G. Evans eds. Structure and Bonding; Vol 119, 2005 Layered Double Hydroxides. The hydrotalcites, perhaps the best known example of LDHs, have been studied for many years. LDHs are capable of intercalating anions between the layers of the structure. WO 99 / 24139 discloses the use of LDHs to segregate anions, including aromatic and aliphatic anions. [0003] Due to the relatively high surface charge and hydrophilic properties of LDH, the particles or crystallites of conventionally synthesized LDH are usually highly agglomerated. As a result, when produced, LDHs agglomerate to form "stone-like", with large particle sizes u...
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