Titanium oxide and alumina alkali metal compositions

A technology of oxides and compositions, applied in the field of porous metal oxide compositions, can solve the problems of incomplete mixing and not suitable for preparing Na/TiO2 and Na/NaCl

Inactive Publication Date: 2007-10-24
SIGNA CHEM INC +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to Furstner, this simple process is not very suitable for the preparation of Na / TiO 2 and Na / NaCl due to insufficient mixing

Method used

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  • Titanium oxide and alumina alkali metal compositions
  • Titanium oxide and alumina alkali metal compositions
  • Titanium oxide and alumina alkali metal compositions

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0077] Example 1: Exemplary Porous Metal Oxide. Calcination of porous TiO by Sachtleben Chemie in air at 600 °C 2 (Anatase) (29.5nm diameter pores, or 295_) and activated porous alumina of Almatis AC (358m 2 / g), and then cooled to room temperature. To these powders in a helium-filled glove box was added dropwise liquid Na 2 K onto the porous oxide in a stainless steel pan. The liquid alloy is quickly absorbed into the porous metal oxide. As long as the total concentration of metals does not exceed 30 wt%, the white powder becomes dark black in color and the mixture becomes a uniform loose powder. This provides a class 0 material sample, as shown in FIG. 5 .

Embodiment 2

[0078] Example 2: A distinctive feature of the Group 1 metal / porous metal oxide compositions of the present invention is their ability to generate pure hydrogen gas when added to water. The "reducing power" of the Group 1 metal / porous metal oxide composition was determined by adding water to the evacuated sample and collecting the hydrogen gas with a modified Toeppler pump. Reducing power is defined as the weight percent of the alkali metal or alloy used to produce the same amount of hydrogen. This was confirmed by collecting hydrogen gas produced by a known mass of material upon reaction with degassed water. Hydrogen gas was collected in a calibrated pipette with a modified Toeppler pump (mercury filled). This analysis was performed on every sample of reduced porous metal oxide, regardless of the grade of material. For example, if a 30 wt% sample of NaK in a class I porous metal oxide produces the same amount of hydrogen as that amount of NaK alone, the reducing power is 30...

Embodiment 3

[0079] Example 3: Preparation of Class I materials can be performed by continuously heating Class 0 materials to 150°C or by using higher melting alkali metals such as sodium and potassium. 14.0 g of degassed and calcined porous alumina was weighed and put together with 6.0 g of Na metal into a Parr stainless steel reactor equipped with a Teflon gasket seal. The combination of porous metal oxide and Na was heated while rotating the reactor upside down at 60 rpm, first to 105°C for 1 hour, then at 155°C overnight. The powder is loose, black and free flowing. Transformation 0 grade Na was also carried out 2 K-Al 2 o 3 、Na 2 K-TiO 2 and Na-TiO 2 A similar process to Class I material. For example, the DSC for 21 wt% material is shown in Figure 6.

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Abstract

The invention relates to Group 1 metal / silica gel compositions comprising silica gel and an alkali metal or an alkali metal alloy. The compositions of the inventions are described as Stage 0, I, II, and III materials. These materials differ in their preparation and chemical reactivity. Each successive stage may be prepared directly using the methods described below or from an earlier stage material. Stage 0 materials may, for example, be prepared using liquid alloys of Na and K which are rapidly absorbed by silica gel (porous Si02) under isothermal conditions, preferably at or just above room temperature, to form loose black powders that retain much of the reducing ability of the parent metals. When the low melting Group 1 metals are absorbed into the silica gel, a mild exothermic reaction produces Stage I material, loose black powders that are indefinitely stable in dry air. Subsequent heating to 400 DEG C produces Stage II materials, which are also loose black powders. Further heating above 400 DEG C forms Stage III material with release of some Group 1 metal. It is believed that Stage I, II and III materials represent reductions of the silica gel after absorption of the Group 1 metal. Preferred Group 1 metal / silica gel compositions of the invention are those containing sodium, potassium, or sodium-potassium alloys with sodium and sodium- potassium alloys being most preferred. Each stage of the Group 1 metal / silica gel composition of the invention may be used as a reducing agent reacting with a number of reducible organic materials in the same manner known for alkali metals and their alloys.

Description

field of invention [0001] The present invention relates to porous metal oxide compositions prepared by the interaction of alkali metals or alloys of these metals with porous titania or porous alumina. The composition has improved processing characteristics and maintains the reactivity of the neutral alkali metal or alloy. Background of the invention [0002] Those alkali metals and alloys of alkali metals in Group 1 of the periodic table are very reactive in their metallic or neutral state. Alkali metals and their alloys are very reactive to air and moisture and may spontaneously catch fire when exposed to these agents. To avoid the inherent hazards associated with their reactivity, neutral metals or alloys must often be stored in vacuum or in an inert liquid such as oil to avoid its exposure to air, which might cause oxidation or other reactions. Sodium metal, for example, is often stored in liquid paraffin oil, which must be removed before use in chemical reactions to av...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/00B01J23/02B01J23/04B01J23/08B01J20/00B01J21/04B01J31/00B01J37/00C07F1/02C01B3/08C07C17/25
CPCY02E60/36
Inventor M·勒芬费尔德J·L·戴
Owner SIGNA CHEM INC
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