Stock material or miscellaneous articles – Coated or structually defined flake – particle – cell – strand,... – Particulate matter
Patent
1997-03-11
2000-01-25
Moore, Margaret G.
Stock material or miscellaneous articles
Coated or structually defined flake, particle, cell, strand,...
Particulate matter
501 80, 501 81, 528 10, 528 31, 528 35, 528 33, B32B 516
Patent
active
060176296
DESCRIPTION:
BRIEF SUMMARY
The present invention relates to amorphous microporous oxidic solids based on organofunctional compounds of metals, transition metals and semiconductor elements and a process for their production and their use as adsorbents, for substance separation, as catalysts or catalyst carrier materials.
German patent applications DE-OS 2 155 281 and DE-OS 2 357 184 disclose the preparation of porous silicon dioxides by subjecting tetraalkoxysilanes or polyalkoxysiloxanes, optionally together with organoalkoxysilanes, to hydrolytic polycondensation.
Furthermore, it is known that porous solids can be produced by hydrothermal synthesis or according to the sol-gel process. The solids produced in this manner are, however, either X-crystalline or X-amorphous and have a small portion of micropores.
According to German patent application DE-AS 1 038 015, it is possible to produce crystalline aluminosilicate by intermixing sodium aluminate solution and sodium silicate solution under formation of gel and by crystallizing the same.
Amorphous aluminosilicates can be produced by analogy with the method described in German application 2 917 313. An aluminate solution and a silicate solution are combined there.
When the mixture is immediately fed into a precipitation oil, beaded bodies of amorphous aluminosilicate are formed.
The porous solids which have so far been known are often non-specific in their effect, hardly selective and sensitive to mechanical or chemical action, such as hydrolytic attack.
The following pore classes are used for characterizing the porous solids according to the IUPAC classification (dp=mean pore diameter).
______________________________________ micropores dp < 2 nm
mesopores 2 nm < dp < 50 nm
macropores dp > 50 nm
______________________________________
The pore distribution can be determined by using different known methods, e.g., by adsorbing gases and vapors and by evaluating the resulting sorption isotherms according to the Horwath-Kawazoe, BET or Kelvin method, especially for determining the micro- and mesopore distribution, or by mercurcy porosimetry for measuring the pore distribution of macropores and large mesopores.
It has been the object of the present invention to provide porous solids having a predominant portion of micropores and a process for producing the same.
In accordance with the invention, the object is achieved by microporous oxidic solids based on organofunctional compounds of metals, transition metals and/or semiconductor elements, preferably elements of the third and fourth main group and/or the fourth sub-group of the periodic system of elements, which solids were produced by tempering or calcining such compounds and have a pore size of 0.3 to 2 nm, a pore volume of 0.05 to 0.9 ml/g and a BET surface of 10 to 1000 m.sup.2 /g.
BRIEF DESCRIPTION OF THE DRAWINGS
The figures show the sorption isotherms and pore volume distribution curves of samples 4, 5 and 7, as shown in Table 1 below.
The microporous solids of the invention are X-amorphous.
In accordance with the invention, the microporous solids are produced by thermally decomposing organofunctional compounds, preferably elements of the third and fourth main group or the fourth sub-group of the periodic system of elements in the presence of ozone, oxygen and/or air at 100 to 600.degree. C., preferably at 200 to 500.degree. C.
The reaction can also take place at ambient temperature, which, however, will entail a prolongation of the reaction time.
Organofunctional compounds within the meaning of the present invention are preferably compounds containing silicon, titanium, hafnium, zircon, aluminum or germanium.
The starting compounds can generally be described by formula I third, fourth main group or the fourth sub-group of the periodic system of elements,
Moreover, in the above formula I, R can stand for non-metal-containing elements or chemical groups. Compounds of such an embodiment are, e.g., bis(3-triethoxysilylpropyl)tetrasulfane, 3-aminopropyl-triethoxysilane, phosphoric acid-p,p-dimethyl-trimeth
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Engelhard Corporation
Moore Margaret G.
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