Difluoromethylation of unsaturated compounds
US-9464087-B2 · Oct 11, 2016 · US
US9556079B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-9556079-B2 |
| Application number | US-73795609-A |
| Country | US |
| Kind code | B2 |
| Filing date | Sep 4, 2009 |
| Priority date | Sep 5, 2008 |
| Publication date | Jan 31, 2017 |
| Grant date | Jan 31, 2017 |
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A new chromium-containing fluorination catalyst is described. The catalyst comprises an amount of zinc that promotes activity. The zinc is contained in aggregates which have a size across their largest dimension of up to 1 micron. The aggregates are distributed throughout at least the surface region of the catalyst and greater than 40 weight % of the aggregates contain a concentration of zinc that is within ±1 weight % of the modal concentration of zinc in those aggregates.
Opening claim text (preview).
The invention claimed is: 1. A chromium-containing fluorination catalyst which comprises from 0.5 to 25% by weight of zinc based on the total weight of the catalyst, said zinc being contained in aggregates which have a size across their largest dimension of up to 1 micron and which are distributed throughout at least the surface region of the catalyst and wherein greater than 40 weight % of the zinc-containing aggregates contain a concentration of zinc that is within ±1 weight % of the modal concentration of zinc in the zinc-containing aggregates and, wherein the catalyst is amorphous or partially crystalline containing from 0.4 to 5% by weight of one or more crystalline compounds of chromium and/or one or more crystalline compounds of zinc. 2. A chromium-containing fluorination catalyst which comprises from 0.5 to 25% by weight of zinc based on the total weight of the catalyst, said zinc being contained in aggregates which have a size across their largest dimension of up to 1 micron and which are distributed throughout at least the surface region of the catalyst, wherein greater than 60 weight % of the zinc-containing aggregates contain a concentration of zinc that is within ±1 weight % of the modal concentration of zinc in the zinc-containing aggregates and wherein the catalyst is amorphous or partially crystalline containing from 0.1 to 50% by weight of one or more crystalline compounds of chromium and/or one or more crystalline compounds of zinc. 3. The catalyst of claim 2 , wherein greater than 80 weight % of the zinc-containing aggregates contain a concentration of zinc that is within ±2 weight % of the modal concentration of zinc in the zinc-containing aggregates. 4. The catalyst of claim 2 , wherein greater than 90 weight % of the zinc-containing aggregates contain a concentration of zinc that is within ±2 weight % of the modal concentration of zinc in the zinc-containing aggregates. 5. The catalyst of claim 2 , wherein the number of zinc-containing aggregates in each square millimeter of the catalyst surface or in each square millimeter of the catalyst bulk is within ±2 % of the mean number of zinc-containing aggregates per square millimeter of the catalyst surface or catalyst bulk. 6. The catalyst of claim 2 , wherein the zinc-containing aggregates have a size in the range of from 20 nm to 1 micron. 7. The catalyst of claim 2 wherein the catalyst has been subjected to a calcination process and then subsequently fluorinated. 8. The catalyst of claim 2 , wherein from 92.0 to 100% by weight of the chromium in the catalyst based on the total weight of said chromium is present as chromium (III). 9. The catalyst of claim 2 , further comprising one or more chromium (VI) compounds and wherein from 0.5 to 4.0 % by weight of the chromium in the catalyst based on the total weight of said chromium is present as chromium (VI). 10. The catalyst of claim 9 , wherein from 96.0 to 99.5% by weight of the chromium in the catalyst based on the total weight of said chromium is present as chromium (III). 11. The catalyst of claim 2 , wherein the zinc is present in the catalyst in an amount of from 1.0 to 6.0% by weight based on the total weight of the catalyst. 12. The catalyst of claim 2 , wherein the surface area of the catalyst is in the range of from 20 to 300 m 2 /g. 13. The catalyst of claim 2 , wherein the surface area of the catalyst is in the range of from 100 to 250 m 2 /g. 14. The catalyst of claim 2 , wherein the catalyst comprises one or more chromium (III) compounds selected from the group consisting of chromia, chromium (III) fluoride, fluorinated chromia and chromium (III) oxyfluorides. 15. The catalyst of claim 2 , wherein the catalyst contains from 0.4 to 5% by weight of one or more crystalline compounds of chromium and/or one or more crystalline compounds of zinc.
Scanning electron microscopy; Transmission electron microscopy · CPC title
X-ray diffraction · CPC title
Indexing scheme associated with group B01J35/00, related to the analysis techniques used to determine the catalysts form or properties · CPC title
Nanoparticles · CPC title
characterised by their crystalline properties, e.g. semi-crystalline (catalysts comprising carbon B01J21/18; molecular sieves B01J29/00) · CPC title
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