GB634398A - Process of refining chloral by distillation - Google Patents
Process of refining chloral by distillationInfo
- Publication number
- GB634398A GB634398A GB1068247A GB1068247A GB634398A GB 634398 A GB634398 A GB 634398A GB 1068247 A GB1068247 A GB 1068247A GB 1068247 A GB1068247 A GB 1068247A GB 634398 A GB634398 A GB 634398A
- Authority
- GB
- United Kingdom
- Prior art keywords
- water
- chloral
- hydrate
- distillation
- per cent
- 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
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C45/82—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Crude chloral containing hydrochloric acid is fractionally distilled with sufficient water to keep the concentration of hydrochloric acid below about 15 per cent of the weight of water present in the still. The distillate, which contains the chloral in the form of the hydrate, is free from acid and may be dehydrated by azeotropic distillation, in an oxygen-free atmosphere, using benzene as water-entrainer. A column having an efficiency of about 14 theoretical plates is suitable for each stage of the process. In an example, 335 gallons of crude (40 per cent) chloral containing about 11 per cent hydrochloric acid was fractionally distilled with a total of 265 gallons of water, the water being added as necessary during the distillation to keep the concentration of hydrochloric acid below 15 per cent by weight of the water in the still. The distillate contained chloral hydrate, dichloroacetaldehyde hydrate and butylchloral hydrate. Towards the end of the distillation, the distillate was mainly water and this was used to dilute the next batch. The mixed hydrates were dehydrated by azeotropic distillation, using 60 gallons of benzene; most of the water from the decanter being discarded to waste. The last 5 per cent of the water, however, contained some chloral, and was collected for diluting another batch of crude. The dehydrated mixture was distilled without fractionation to separate butylchloral, which was left as residue. The distillate was fractionated using a reflux ratio of 10 : 1; benzene being recovered up to 88 DEG C., and a small middle fraction being taken off between 88 DEG and 97 DEG C., for addition to the final fractionation of a subsequent batch. Refined chloral boiling at 97 DEG C. was then collected at a reflux ratio of 3 : 1. During all the steps after the hydrate distillation, the system was vented to an atmosphere of dry nitrogen. In another example, the first stage of the process is carried out with continuous addition of water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB1068247A GB634398A (en) | 1947-04-22 | 1947-04-22 | Process of refining chloral by distillation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB1068247A GB634398A (en) | 1947-04-22 | 1947-04-22 | Process of refining chloral by distillation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| GB634398A true GB634398A (en) | 1950-03-22 |
Family
ID=9972334
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB1068247A Expired GB634398A (en) | 1947-04-22 | 1947-04-22 | Process of refining chloral by distillation |
Country Status (1)
| Country | Link |
|---|---|
| GB (1) | GB634398A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5558747A (en) * | 1993-06-25 | 1996-09-24 | Amvac Chemical Corporation | Process for azeotropic distillation of aqueous chloral mixtures |
| US20130157992A1 (en) * | 2011-12-20 | 2013-06-20 | Keith R. Latham | Sustained drug release and improved product stability using non-covalent particle coating methods |
-
1947
- 1947-04-22 GB GB1068247A patent/GB634398A/en not_active Expired
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5558747A (en) * | 1993-06-25 | 1996-09-24 | Amvac Chemical Corporation | Process for azeotropic distillation of aqueous chloral mixtures |
| US20130157992A1 (en) * | 2011-12-20 | 2013-06-20 | Keith R. Latham | Sustained drug release and improved product stability using non-covalent particle coating methods |
| US9526701B2 (en) * | 2011-12-20 | 2016-12-27 | Keith R. Latham | Sustained drug release and improved product stability using non-covalent particle coating methods |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US2380019A (en) | Azeotropic distillation | |
| US2465959A (en) | Recovery of nitromethane from aqueous alcoholic mixtures thereof | |
| US3180897A (en) | Process for the production of phenols | |
| US2360685A (en) | Azeotropic distillation | |
| GB634398A (en) | Process of refining chloral by distillation | |
| GB668853A (en) | Separating alpha and beta methyl naphthalene by azeotropic distillation | |
| US2720549A (en) | Recovery of phenol | |
| US2559247A (en) | Purification of chloral | |
| GB978746A (en) | Process for the recovery of phenols from impure aqueous solutions | |
| US1365048A (en) | And mortimer j | |
| US1688731A (en) | Dehydration of alcohols | |
| NO134111B (en) | ||
| US2623845A (en) | Distillation of wood carbonization | |
| US2401335A (en) | Recovery of diketones and related products from technical liquors containing diketones | |
| US2584325A (en) | Purification of alcohols | |
| US1950889A (en) | Process for the purification of tertiary butyl alcohol | |
| DE861248C (en) | Process for the production of styrene | |
| US2530325A (en) | Azeotropic distillation of mesitylene from isophorone | |
| US2809927A (en) | Separation of sec-butyl ether from polymeric hydrocarbons | |
| GB580102A (en) | Improvements in or relating to the fractional distillation of hydrocarbons | |
| US3058892A (en) | Separation of beta-bromoethylbenzene from alpha-bromoethylbenzene by distillation | |
| DE591195C (en) | Process for separating liquid mixtures of acetic anhydride, acetic acid and water | |
| GB762974A (en) | Dehydrating alcohols by extractive distillation | |
| GB577241A (en) | An improved process for the purification of organic liquids by fractional distillation | |
| GB918003A (en) | Process for the continuous fractional distillation of coal tar |