DE263106C - - Google Patents
Info
- Publication number
- DE263106C DE263106C DENDAT263106D DE263106DA DE263106C DE 263106 C DE263106 C DE 263106C DE NDAT263106 D DENDAT263106 D DE NDAT263106D DE 263106D A DE263106D A DE 263106DA DE 263106 C DE263106 C DE 263106C
- Authority
- DE
- Germany
- Prior art keywords
- hydrochloric acid
- dichlorohydrin
- monochlorohydrin
- gas stream
- experiment
- 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.)
- Active
Links
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- DEWLEGDTCGBNGU-UHFFFAOYSA-N 1,3-dichloropropan-2-ol Chemical compound ClCC(O)CCl DEWLEGDTCGBNGU-UHFFFAOYSA-N 0.000 claims description 7
- SSZWWUDQMAHNAQ-UHFFFAOYSA-N 3-MCPD Chemical compound OCC(O)CCl SSZWWUDQMAHNAQ-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N Carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- XENVCRGQTABGKY-ZHACJKMWSA-N Chlorohydrin Chemical compound CC#CC#CC#CC#C\C=C\C(Cl)CO XENVCRGQTABGKY-ZHACJKMWSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C31/00—Saturated compounds having hydroxy or O-metal groups bound to acyclic carbon atoms
- C07C31/34—Halogenated alcohols
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
KAISERLICHESIMPERIAL
PATENTAMT.PATENT OFFICE.
£/■£ / ■
Bei der Darstellung des Dichlorhydrins C3H5Cl2OH aus Monochlorhydrin und Salzsäure tritt durch die Zunahme des bei der Esterifikation gebildeten Wassers sehr bald Reaktionsverzögerung bzw. -stillstand ein.When the dichlorohydrin C 3 H 5 Cl 2 OH is prepared from monochlorohydrin and hydrochloric acid, the increase in the water formed during the esterification very soon results in a reaction delay or standstill.
Es wurde gefunden, daß ein glatterer "Verlauf der Reaktion erfolgt, wenn man während des Einleitens gasförmiger Salzsäure in Monochlorhydrin das durch die Reaktion gebildete Wasser aus der Reaktionsmasse durch Abdestillieren unter vermindertem Druck oder mittels eines durchgeleiteten indifferenten Gasstroms entfernt.It has been found that a smoother course of the reaction occurs if one during introducing gaseous hydrochloric acid into monochlorohydrin that formed by the reaction Water from the reaction mass by distilling off under reduced pressure or removed by means of a passed through inert gas stream.
Beispiel. Man leitet im Vakuum bei etwa ioo° C. in Monochlorhydrin einen kräftigen Strom gasförmige Salzsäure ein, worauf sehr bald ein Gemisch von wässeriger Salzsäure mit gebildetem Dichlorhydrin abdestilliert. Das Gemisch wird in der Weise getrennt, daß man die wässerige Salzsäure mit Wasser oder Soda verdünnt, worauf sich das Dichlorhydrin als öl abscheidet.Example. One passes in a vacuum at about 100 ° C. in monochlorohydrin a strong Stream of gaseous hydrochloric acid, whereupon very soon a mixture of aqueous hydrochloric acid distilled off with dichlorohydrin formed. The mixture is separated in such a way that the aqueous hydrochloric acid is diluted with water or soda, whereupon the dichlorohydrin separates as oil.
Der durch dieses neue Verfahren erreichte Fortschritt ergibt sich aus folgenden Vergleichsversuchen: The progress achieved by this new process results from the following comparative tests:
In einem emaillierten Rührkessel wurden in drei aufeinanderfolgenden Versuchen gleiche Mengen Monochlorhydrin bei ungefähr gleichen Temperaturen mit Salzsäuregas behandelt, und zwar wurde beim ersten Versuch das Mono-35 In an enamelled stirred tank equal amounts monochlorohydrin were treated at about the same temperatures with hydrochloric acid gas in three consecutive trials, namely, the mono- was the first try 35
chlorhydrin mit Salzsäuregas gesättigt und dann erst im Vakuum das gebildete Dichlorhydrin abdestilliert — der Versuch bewegte sich also im Rahmen des bisher Bekannten ■—; beim zweiten und dritten Versuch wurde dagegen das gebildete Dichlorhydrin kontinuierlich im Gasstrom bzw. im Vakuum abdestilliert, wie im Beispiel beschrieben ist. Es ergab sich hierbei, daß bei Versuch 2 und 3 etwa doppelt so viel Dichlorhydrin in der gleichen Zeit gebildet wurde, wie beim Versuch im Rahmen des bisher bekannten Verfahrens. Das lästige Schäumen der Masse, das bei Versuch 1 beobachtet wurde, fällt beim Arbeiten nach dem vorliegenden Verfahren weg, und außerdem ist die Arbeitsweise viel einfacher, da der Prozeß ohne jede Unterbrechung unter einfachem Ersatz des verbrauchten Monochlorhydrins zu einem kontinuierlichen gestaltet werden kann.chlorohydrin is saturated with hydrochloric acid gas and only then is the dichlorohydrin formed in vacuo distilled off - the experiment was therefore within the framework of what was previously known ■ -; in the second and third attempts, however, the dichlorohydrin formed was continuous distilled off in a gas stream or in vacuo, as described in the example. It resulted It turns out that in experiments 2 and 3 about twice as much dichlorohydrin was formed in the same time as in the experiment as part of the previously known procedure. The troublesome foaming of the mass, which was observed in Experiment 1, falls in Working away according to the present method, and besides, the way of working is a lot Easier, since the process is used without any interruption with simple replacement of the consumed Monochlorhydrins can be made into a continuous.
Claims (1)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE263106C true DE263106C (en) |
Family
ID=520526
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DENDAT263106D Active DE263106C (en) |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE263106C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009104961A2 (en) * | 2008-02-21 | 2009-08-27 | Bouwe De Jong | Process for the preparation of a dichloropropanol product |
-
0
- DE DENDAT263106D patent/DE263106C/de active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009104961A2 (en) * | 2008-02-21 | 2009-08-27 | Bouwe De Jong | Process for the preparation of a dichloropropanol product |
| WO2009104961A3 (en) * | 2008-02-21 | 2009-10-15 | Bouwe De Jong | Process for the preparation of a dichloropropanol product |
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