GB815940A - Improvements in or relating to photochemical chlorination apparatus - Google Patents
Improvements in or relating to photochemical chlorination apparatusInfo
- Publication number
- GB815940A GB815940A GB2495/57A GB249557A GB815940A GB 815940 A GB815940 A GB 815940A GB 2495/57 A GB2495/57 A GB 2495/57A GB 249557 A GB249557 A GB 249557A GB 815940 A GB815940 A GB 815940A
- Authority
- GB
- United Kingdom
- Prior art keywords
- tubes
- line
- benzene
- acetic anhydride
- pair
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/013—Preparation of halogenated hydrocarbons by addition of halogens
- C07C17/02—Preparation of halogenated hydrocarbons by addition of halogens to unsaturated hydrocarbons
-
- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/013—Preparation of halogenated hydrocarbons by addition of halogens
- C07C17/04—Preparation of halogenated hydrocarbons by addition of halogens to unsaturated halogenated hydrocarbons
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
<PICT:0815940/III/1> <PICT:0815940/III/2> <PICT:0815940/III/3> An apparatus suitable for the photo-chemical chlorination of benzene (see Group IV (b)) comprises a pair of parallel transparent tubes each of which is provided with cooling means and surrounded by a source of actinic light, a third tube connecting said pair of tubes at one end thereof and a fourth tube connecting said pair of tubes at their other ends, and a pump rotor in said fourth tube whereby liquid is circulated through said tubes. A plurality of pairs of tubes is preferably used in conjunction with a single pump: thus, in the illustrated apparatus, four pairs of tubes are provided and the reactants are introduced through line 113 into a central vertical well 112 with which each of said tubes communicates. The reactants are pumped by means of a rotor 116 into the upper of each pair of tubes (121, Fig. 1) and return to the well via the lower tubes. Each of the tubes comprises an inner transparent tube 122 containing U-tubes 127 (see Figs. 3 and 4) connected to headers 128 and 129 for circulation of a refrigerant, an outer reflector housing 126, and, between the housing and the inner tube, lamps 125 which supply the desired actinic light.ALSO:<p1> Hexachlorocyclohexane containing at least 20 per cent of the gamma-isomer is continuously produced in a photo-chemical apparatus (see Group III) from an initial mixture of benzene, acetic anhydride, carbon tetrachloride and chlorine at, e.g., 5 to -25 DEG C. As shown in Fig. 5, a reservoir 6, slightly pressurized by argon or helium, is provided for the benzeneacetic anhydride-carbon tetrachloride mixture, make-up quantities of benzene being added through line 8. The mixture passes via line 9 to the continuous reactor 12 together with chlorine from line 16, and circulates at a temperature of -10 DEG C., maintained by a refrigerant entering the apparatus by line 13, under the influence of actinic light. The product is withdrawn to a secondary illuminated reactor 20 where the chlorine is reduced to a trace and thence to a solvent preheater 18, after adding make-up quantities of acetic anhydride. Makeup benzene can also be added to line 25. The preheater 18 is operated at the boiling-point, e.g. 92 DEG C. at atmospheric pressure, and is equipped with a packed column 51 and reflux condenser 19; a small portion of the acetyl chloride and acetic acid formed in the reactors is thus converted to acetic anhydride, and hydrogen chloride is vented. The mixture is then passed to boiler 23 where the unreacted benzene together with acetic anhydride and carbon tetrachloride are volatilized and returned to reservoir 6 via receiver 28 kept under vacuum by a pump attached to line 32. The unvolatilized liquid in boiler 23 is withdrawn into stripper 36 and the product obtained therefrom. Solvent volatilized in the stripper is condensed and collected in evacuated receiver 42 and returned to the boiler. The product is a hot liquid containing acetic anhydride which is removed by stirring vigorously with water; the material obtained is in the form of fine pellets containing 28 per cent of gamma-isomer.
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US609295A US2870335A (en) | 1956-09-11 | 1956-09-11 | Apparatus for photochemical chlorination reactions |
Publications (1)
Publication Number | Publication Date |
---|---|
GB815940A true GB815940A (en) | 1959-07-01 |
Family
ID=24440176
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
GB2495/57A Expired GB815940A (en) | 1956-09-11 | 1957-01-23 | Improvements in or relating to photochemical chlorination apparatus |
Country Status (4)
Country | Link |
---|---|
US (1) | US2870335A (en) |
DE (1) | DE1097983B (en) |
FR (1) | FR1169423A (en) |
GB (1) | GB815940A (en) |
Family Cites Families (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US1735610A (en) * | 1926-10-25 | 1929-11-12 | Fred E Goodall | Apparatus for treating fluids with ultra-violet light |
US2436366A (en) * | 1943-11-22 | 1948-02-17 | Hooker Electrochemical Co | Processes for chlorination of hydrocarbons |
US2499129A (en) * | 1948-03-17 | 1950-02-28 | Allied Chem & Dye Corp | Photochemical manufacture of 1,1,1-difluorochloroethane |
US2572913A (en) * | 1949-04-21 | 1951-10-30 | Allied Chem & Dye Corp | Manufacture of fluorochloromethanes |
US2622205A (en) * | 1949-05-10 | 1952-12-16 | Ethyl Corp | Apparatus for chlorination reactions |
US2656313A (en) * | 1949-05-10 | 1953-10-20 | Ethyl Corp | Photochemical production of benzene hexachloride |
US2622105A (en) * | 1949-05-10 | 1952-12-16 | Ethyl Corp | Process for manufacture of benzene hexachloride |
US2628260A (en) * | 1949-05-31 | 1953-02-10 | Dow Chemical Co | Catalyzed and continuous addition chlorination of benzene |
US2608660A (en) * | 1950-06-13 | 1952-08-26 | Heyden Chemical Corp | Apparatus for halogenation |
US2688592A (en) * | 1950-10-21 | 1954-09-07 | Diamond Alkali Co | Photochemical process for preparing carbon tetrachloride |
US2662186A (en) * | 1952-01-23 | 1953-12-08 | Ethyl Corp | Two-stage photochemical reactor |
FR1066893A (en) * | 1953-01-23 | 1954-06-10 | Ethyl Corp | Improvements to two-phase photochemical reactors |
GB750502A (en) * | 1953-04-22 | 1956-06-20 | Columbia Southern Chem Corp | Improvements in or relating to preparation of benzene hexachloride |
-
1956
- 1956-09-11 US US609295A patent/US2870335A/en not_active Expired - Lifetime
-
1957
- 1957-01-23 GB GB2495/57A patent/GB815940A/en not_active Expired
- 1957-03-13 FR FR1169423D patent/FR1169423A/en not_active Expired
- 1957-09-09 DE DEST12943A patent/DE1097983B/en active Pending
Also Published As
Publication number | Publication date |
---|---|
FR1169423A (en) | 1958-12-29 |
US2870335A (en) | 1959-01-20 |
DE1097983B (en) | 1961-01-26 |
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