GB808101A - Process for obtaining pure trimethylolpropane - Google Patents
Process for obtaining pure trimethylolpropaneInfo
- Publication number
- GB808101A GB808101A GB33625/55A GB3362555A GB808101A GB 808101 A GB808101 A GB 808101A GB 33625/55 A GB33625/55 A GB 33625/55A GB 3362555 A GB3362555 A GB 3362555A GB 808101 A GB808101 A GB 808101A
- Authority
- GB
- United Kingdom
- Prior art keywords
- trimethylolpropane
- raffinate
- cyclohexanol
- treated
- solvent
- 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
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/86—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by liquid-liquid treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/14—The ring being saturated
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
Pure trimethylolpropane is obtained from the aqueous reaction mixture obtained by alkaline condensation of butyraldehyde with formaldehyde, by treating the reaction mixture with a partially water-miscible solvent consisting of a monohydric aliphatic, cycloaliphatic or araliphatic alcohol containing 4-8 carbon atoms thus forming an aqueous phase and an organic phase, organic impurities going into the organic phase and the trimethylolpropane being distributed between the aqueous and organic phases. If a minor amount of solvent is used the bulk of the trimethylolpropane remains in the aqueous phase and the organic impurities, together with a small amount of trimethylolpropane pass into the organic phase. The bulk of the trimethylolpropane can be obtained from the aqueous solution by treating it with a greater quantity of the same or a different solvent as defined above. The small quantity of trimethylol propane can be recovered from the organic phase by washing with water or with a trimethylolpropane-free raffinate obtained at the end of the working process. If a major amount of the solvent is used the trimethylolpropane and organic impurities go into the organic phase. The bulk of the solvent is distilled off and the remaining extract is treated with water or a trimethylolpropane-free raffinate so that the trimethylol propane goes into the aqueous phase and the organic impurities remain behind in the solvent. In the examples: (a) a solution of trimethylolpropane obtained by the alkaline condensation of butyraldehyde and formaldehyde is treated with a minor proportion of iso-octanol to give an extract layer containing small amounts of trimethylolpropane and iso-octanol and organic impurities and a raffinate containing the major part of the trimethylolpropane; the iso-octanol is reclaimed from the extract layer by distillation; the raffinate layer is treated with a large quantity of iso-octanol, thereby giving an extract containing the bulk of the trimethylolpropane, which is obtained by evaporating the extract solution and may be further purified by distillation; and (b) a solution of trimethylolpropane obtained by the alkaline condensation of butyraldehyde and formaldehyde is treated with a major quantity of cyclohexanol thus forming an extract layer containing most of the trimethylolpropane and cyclohexanol and a raffinate containing small amounts of trimethylolpropane and cyclohexanol; the extract layer is distilled to give cyclohexanol, trimethylolpropane and a residue containing a further quantity of trimethylolpropane; the residue is treated with a major portion of the raffinate from the first extraction and a minor amount of cyclohexanol is added; the raffinate so obtained may be treated with a further quantity of cyclohexanol or may be added to some fresh crude condensation solution.
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE808101X | 1954-11-23 |
Publications (1)
Publication Number | Publication Date |
---|---|
GB808101A true GB808101A (en) | 1959-01-28 |
Family
ID=6723014
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
GB33625/55A Expired GB808101A (en) | 1954-11-23 | 1955-11-23 | Process for obtaining pure trimethylolpropane |
Country Status (1)
Country | Link |
---|---|
GB (1) | GB808101A (en) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1999020586A1 (en) * | 1997-10-16 | 1999-04-29 | Celanese International Corporation | Process improvement to produce low color trimethylolpropane |
EP1848679A1 (en) * | 2006-03-07 | 2007-10-31 | LG Chem. Ltd. | Method for preparing trimethylolpropane |
EP2167450A1 (en) * | 2007-06-18 | 2010-03-31 | Perstorp Specialty Chemicals AB | Method for extraction in a process for production of a di, tri or polyhydric alcohol |
CN103467252A (en) * | 2013-09-05 | 2013-12-25 | 百川化工(如皋)有限公司 | Method for increasing purity of di-trimethylolpropane |
-
1955
- 1955-11-23 GB GB33625/55A patent/GB808101A/en not_active Expired
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1999020586A1 (en) * | 1997-10-16 | 1999-04-29 | Celanese International Corporation | Process improvement to produce low color trimethylolpropane |
EP1848679A1 (en) * | 2006-03-07 | 2007-10-31 | LG Chem. Ltd. | Method for preparing trimethylolpropane |
EP1848679A4 (en) * | 2006-03-07 | 2010-06-09 | Lg Chemical Ltd | Method for preparing trimethylolpropane |
EP2167450A1 (en) * | 2007-06-18 | 2010-03-31 | Perstorp Specialty Chemicals AB | Method for extraction in a process for production of a di, tri or polyhydric alcohol |
EP2167450A4 (en) * | 2007-06-18 | 2010-08-04 | Perstorp Specialty Chem Ab | Method for extraction in a process for production of a di, tri or polyhydric alcohol |
CN103467252A (en) * | 2013-09-05 | 2013-12-25 | 百川化工(如皋)有限公司 | Method for increasing purity of di-trimethylolpropane |
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