ES291865A1 - PROCEDURE FOR THE SYNTHESIS OF FLUORINATED COMPOUNDS - Google Patents
PROCEDURE FOR THE SYNTHESIS OF FLUORINATED COMPOUNDSInfo
- Publication number
- ES291865A1 ES291865A1 ES0291865A ES291865A ES291865A1 ES 291865 A1 ES291865 A1 ES 291865A1 ES 0291865 A ES0291865 A ES 0291865A ES 291865 A ES291865 A ES 291865A ES 291865 A1 ES291865 A1 ES 291865A1
- Authority
- ES
- Spain
- Prior art keywords
- solution
- hour
- heat treatment
- trivalent chromium
- fluorine atoms
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 238000000034 method Methods 0.000 title abstract 2
- 230000015572 biosynthetic process Effects 0.000 title 1
- 150000001875 compounds Chemical class 0.000 title 1
- 238000003786 synthesis reaction Methods 0.000 title 1
- 238000010438 heat treatment Methods 0.000 abstract 5
- 239000003054 catalyst Substances 0.000 abstract 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 abstract 3
- 239000000243 solution Substances 0.000 abstract 3
- OJUUDWYPNQALHZ-UHFFFAOYSA-N 1-chloro-1,1,3,3,3-pentafluoropropan-2-one Chemical compound FC(F)(F)C(=O)C(F)(F)Cl OJUUDWYPNQALHZ-UHFFFAOYSA-N 0.000 abstract 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical class CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 abstract 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 abstract 2
- 150000001844 chromium Chemical class 0.000 abstract 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 abstract 2
- 125000001153 fluoro group Chemical group F* 0.000 abstract 2
- VBZWSGALLODQNC-UHFFFAOYSA-N hexafluoroacetone Chemical compound FC(F)(F)C(=O)C(F)(F)F VBZWSGALLODQNC-UHFFFAOYSA-N 0.000 abstract 2
- 239000011261 inert gas Substances 0.000 abstract 2
- 230000001376 precipitating effect Effects 0.000 abstract 2
- 239000000047 product Substances 0.000 abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 abstract 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract 1
- 239000000908 ammonium hydroxide Substances 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 229910052801 chlorine Inorganic materials 0.000 abstract 1
- 239000000460 chlorine Substances 0.000 abstract 1
- 239000011651 chromium Substances 0.000 abstract 1
- 229910052731 fluorine Inorganic materials 0.000 abstract 1
- 239000011737 fluorine Substances 0.000 abstract 1
- 238000004508 fractional distillation Methods 0.000 abstract 1
- 229910052736 halogen Inorganic materials 0.000 abstract 1
- 150000002367 halogens Chemical class 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 239000008188 pellet Substances 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- 239000011819 refractory material Substances 0.000 abstract 1
- 239000007858 starting material Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/61—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups
- C07C45/63—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by introduction of halogen; by substitution of halogen atoms by other halogen atoms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/26—Chromium
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A dichromium trioxide catalyst is made by precipitating hydrous chromic oxide from a solution of a trivalent chromium salt, e.g. by adding sodium or potassium hydroxide, or, preferably, ammonia gas or aqueous ammonium hydroxide, and subsequently heating it to 300-400 DEG C. for not less than one hour. For example, aqueous ammonia is added to a heated aqueous solution of Cr(NO3)3.9H2O to pH7, the solution is boiled and filtered hot, the precipitate hot water-washed and, dried by heating under vacuum or in an inert gas stream or in equipment with facilities for steam escape, at 100-200 DEG C. The partially dehydrated oxide is granulated to 4-20 mesh or pressed to pellets 3 mm. x 10 mm. and subjected to heat treatment at 300-400 DEG C. for a substantial period. The heat treatment may take place in an atmosphere consisting of water vapour and optionally an inert gas for at least two hours. The catalysts are substantially amorphous and have a surface area at least 5m2/g and usually above 50m2/g. Specification 794,075 is referred to.ALSO:Hexafluoroacetone, perfluorochloroacetone or a mixture thereof is made by contacting in the vapour phase at least one perhalogenated acetone containing two to five fluorine atoms and no halogen other than chlorine and fluorine at an elevated temperature up to 500 DEG C. with a dichromium trioxide catalyst obtained by precipitating hydrous chromic oxide from a solution of a trivalent chromium salt and subsequently heating it to 300 DEG -400 DEG C. for not less than one hour. The catalyst may be used in unsupported granular or pelleted form or supported on inert refractory material. The preferred starting materials are perhalogenated acetones containing two to four fluorine atoms. The process may be operated continuously and the products separated by fractional distillation. In examples using sym-tetrafluorodichloroacetone, 1,1,2 - trifluoro - 1,2,2 - tricloroacetone or pentafluorochloroacetone, the main products were CF3COCF3, CF3COCF2Cl, CF3 COCFCL2 and CF3COCL3 with CF2ClCoCCL3 in addition in the first two examples. Specification 794,075 is referred to.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US22644062A | 1962-09-26 | 1962-09-26 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| ES291865A1 true ES291865A1 (en) | 1964-01-01 |
Family
ID=22848916
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| ES0291865A Expired ES291865A1 (en) | 1962-09-26 | 1963-09-20 | PROCEDURE FOR THE SYNTHESIS OF FLUORINATED COMPOUNDS |
Country Status (6)
| Country | Link |
|---|---|
| BE (1) | BE637698A (en) |
| DE (1) | DE1199754B (en) |
| ES (1) | ES291865A1 (en) |
| FR (1) | FR1369785A (en) |
| GB (1) | GB994093A (en) |
| NL (1) | NL298216A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1036870A (en) * | 1964-07-08 | 1966-07-20 | Du Pont | Preparation of fluorinated perhaloaldehydes |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2807646A (en) * | 1955-03-14 | 1957-09-24 | Allied Chem & Dye Corp | Manufacture of chlorofluoroacetones |
| DE1057087B (en) * | 1955-03-14 | 1959-05-14 | Allied Chem | Process for the preparation of perchlorofluoroacetones |
-
0
- NL NL298216D patent/NL298216A/ unknown
- BE BE637698D patent/BE637698A/ unknown
-
1963
- 1963-09-20 FR FR948233A patent/FR1369785A/en not_active Expired
- 1963-09-20 DE DEA44107A patent/DE1199754B/en active Pending
- 1963-09-20 ES ES0291865A patent/ES291865A1/en not_active Expired
- 1963-09-25 GB GB3777463A patent/GB994093A/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| FR1369785A (en) | 1964-08-14 |
| DE1199754B (en) | 1965-09-02 |
| BE637698A (en) | |
| GB994093A (en) | 1965-06-02 |
| NL298216A (en) |
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