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Process for producing high-purity hafnium amide
   
Document Number
US Patent 7319158
Issued Date
January 15, 2008
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Abstract
A process for producing a high-purity hafnium amide includes the steps of (a) adding a compound which contains a carbonyl group or sulfonyl group and is represented by the formula of A(O.sub.yXO.sub.nR.sub.f).sub.m (e.g., CF.sub.3SO.sub.3H, Hf(CF.sub.3SO.sub.3).sub.4, (CF.sub.3SO.sub.2).sub.2O, CF.sub.3CO.sub.2H, CH.sub.3SO.sub.3H, C.sub.6H.sub.5SO.sub.3H, and (CH.sub.3SO.sub.2).sub.2O), to a crude hafnium amide which is represented by the formula of Hf[N(R.sub.1)(R.sub.2)].sub.4, where each of R.sub.1 and R.sub.2 independently represents a methyl group or ethyl group, and which contains a zirconium component as an impurity; and (b) subjecting a product of the step (a) to a distillation under reduced pressure, thereby removing the zirconium component from the crude hafnium amide.
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Number of Claims:
10
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Published
January 15, 2008
Application Number
11/705,524
Filed
February 13, 2007
US Classification
556/51  
Int'l Classification
C07F   7/00   (20060101)  
Attorney/Law Firm
Priority Data
Feb 20, 2006 [JP] 2006-042934 Nov 20, 2006 [JP] 2006-312847 Jan 10, 2007 [JP] 2007-002547
USPTO Field of Search
556/51  
Related Patents
7518008 - Processes for producing hafnium complexes - Owned by Central Glass Company, Limited (Ube-shi,JP)

Disclosed are first to sixth processes for respectively producing hafnium tetra-tertiary-butoxide, tetrakis(acetylacetonato)hafnium, tetrakis(1-methoxy-2-methyl-2-propanolato)hafnium, hafnium tetra-tertiary-amyloxide, tetrakis(3-methyl-3-pentoxy)hafnium, and tetrakis(hexafluoroacetylacetonato)hafnium. The first process includes the steps of (a) adding a compound A(O.sub.yXO.sub.nRf).sub.m (e.g., CF.sub.3SO.sub.3H) to a crude hafnium amide Hf[N(R.sub.1)(R.sub.2)].sub.4; (b) subjecting a product of the step (a) to a distillation under reduced pressure; (c) adding a lithium alkylamide Li(NR.sub.3R.sub.4) to a fraction obtained by the step (b); (d) subjecting a product of the step (c) to a distillation under reduced pressure; (e) adding tertiary butanol to a fraction obtained by the step (d); and (f) subjecting a product of the step (e) to a distillation under reduced pressure. The tertiary butanol of the step (e) is replaced with acetylacetone, 1-methoxy-2-methyl-2-propanol, tertiary amyl alcohol, 3-methyl-3-pentanol, and hexafluoroacetylacetone in the second to six processes, respectively.

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