DE1048581B - - Google Patents
Info
- Publication number
- DE1048581B DE1048581B DENDAT1048581D DE1048581DA DE1048581B DE 1048581 B DE1048581 B DE 1048581B DE NDAT1048581 D DENDAT1048581 D DE NDAT1048581D DE 1048581D A DE1048581D A DE 1048581DA DE 1048581 B DE1048581 B DE 1048581B
- Authority
- DE
- Germany
- Prior art keywords
- mercury
- chloride
- aluminum
- reaction
- chlorides
- 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.)
- Pending
Links
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 11
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 229910052753 mercury Inorganic materials 0.000 claims description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- -1 aluminum alkyl chlorides Chemical class 0.000 claims description 7
- RCTYPNKXASFOBE-UHFFFAOYSA-M chloromercury Chemical compound [Hg]Cl RCTYPNKXASFOBE-UHFFFAOYSA-M 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 4
- 229910001514 alkali metal chloride Inorganic materials 0.000 claims description 2
- 239000011541 reaction mixture Substances 0.000 claims 1
- 229910052709 silver Inorganic materials 0.000 claims 1
- 239000004332 silver Substances 0.000 claims 1
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 9
- 235000002639 sodium chloride Nutrition 0.000 description 5
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000003085 diluting agent Substances 0.000 description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 3
- QPUYECUOLPXSFR-UHFFFAOYSA-N 1-methylnaphthalene Chemical compound C1=CC=C2C(C)=CC=CC2=C1 QPUYECUOLPXSFR-UHFFFAOYSA-N 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 230000009918 complex formation Effects 0.000 description 2
- 239000000375 suspending agent Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- BTZWIZOMVVQOAZ-UHFFFAOYSA-L dichlorosilver Chemical compound Cl[Ag]Cl BTZWIZOMVVQOAZ-UHFFFAOYSA-L 0.000 description 1
- 235000005911 diet Nutrition 0.000 description 1
- 230000000378 dietary effect Effects 0.000 description 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- QWUGXIXRFGEYBD-UHFFFAOYSA-M ethylmercuric chloride Chemical compound CC[Hg]Cl QWUGXIXRFGEYBD-UHFFFAOYSA-M 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- LWJROJCJINYWOX-UHFFFAOYSA-L mercury dichloride Chemical compound Cl[Hg]Cl LWJROJCJINYWOX-UHFFFAOYSA-L 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000010517 secondary reaction Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic Table
- C07F3/10—Mercury compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Es wurde gefunden, daß Alkyle des Quecksilbers in hohen Ausbeuten und von großem Reinheitsgrad hergestellt werden können durch Umsetzung von Quecksilberchloriden, mit Aluminiumtrialkylen., deren Ätheraten oder Aluminiiumalkylchloriden unter Zusatz von Alkalichloriden, insbesondere Na Cl.It has been found that alkyls of mercury are in high yields and of a high degree of purity can be produced by reacting mercury chlorides with aluminum trialkyls., whose Etherates or aluminum alkyl chlorides with the addition of alkali chlorides, in particular Na Cl.
Die Reaktionen verlaufen beispielsweise folgendermaßen :The reactions are as follows, for example:
3HgCl2+2AlR3-r-2NaCl -> 3 HgR2+2 NaAlCL3HgCl 2 + 2AlR 3 -r-2NaCl -> 3 HgR 2 +2 NaAlCl
Durch den erflnd<ungsgemäßen Zusatz von Alkalichlorid, vorzugsweise Natriumchlorid, wird bewinkt, daß das bei der Reaktion entstehende AlCl3, das die Umsetzung durch Nehenreaktionen, Verstopfung der Apparaturenteile u. dgl., erschweren, würde, durch Komplexbildung abgeschieden wird und mühelos aus dem Reaktionsgefäß entfernt werden, kanu· (z. B. durch HerausschmeLzen, Herauslösen oder Austragen). Es werden daher hohe Ausbeuten an sehr reinen Quecksilberarkylen erhalten, und. die an der Alkylierungskomponente vorhandenen Alkylgruppen werden/ vollständig ausgenutzt.The addition of alkali metal chloride, preferably sodium chloride, according to the invention, ensures that the AlCl 3 formed during the reaction, which would make the reaction more difficult due to secondary reactions, clogging of the apparatus parts and the like, is deposited through complex formation and is easily removed from the The reaction vessel can be removed (e.g. by melting out, dissolving or discharging). High yields of very pure mercury arkyls are therefore obtained, and. the alkyl groups present on the alkylation component are / are fully utilized.
Die Reaktion kann in Gegenwart oder Abwesenheit von Lösungs-, Suspensions- oder Verdünnungsmitteln durchgeführt werden. Mitunter ist es zweckmäßig, als Lösungsmittel das herzustellende Quecksilberalkyl selbst zu verwenden. Die Reaktion wird zweckmäßigerweise )>ei Atmosp'härendruck durchgeführt, doch kann Unter- oder Ül>erdruck ebenfalls angewendet werden.The reaction can be carried out in the presence or absence of solvents, suspending agents or diluents be performed. It is sometimes useful to use the alkyl mercury to be produced as the solvent to use yourself. The reaction is expediently carried out at atmospheric pressure, however, negative or excessive pressure can also be used.
Das Verfahren kann so durchgeführt werden, daß eine Lösung von alurn'rai umorganischen Verbindungenin einem geeigneten Lösungsmittel wie Methylenchlorid, Chlorbenizol, Methylnaphthalin und Mineralöl mit AIkalichIorid versetzt wird, worauf das Quecksilberchlorid eingetragen wird. Man kann auch umgekehrt in eine Lösung bzw. Suspension des Quecksilberchlorids in einem geeigneten Lösungs- bzw. Suspensionsmittel (auch in dem Quecksilber selbst) die aluminiumorganische Verbindung bzw. deren Lösung zugeben.The process can be carried out so that a solution of aluminum organic compounds in a suitable solvent such as methylene chloride, chlorobenzene, methylnaphthalene and mineral oil AlkalichIorid is added, whereupon the mercury chloride is entered. You can also do the other way around into a solution or suspension of the mercury chloride in a suitable solution or Suspending agent (also in the mercury itself) is the organoaluminum compound or its Add solution.
Zu 57 Alurriiniiumtriäthyl, in welches unter Rühren 23 g Natriumchlorid eingetragen worden waren, wurden sukzessive insgesamt 203,6 g Ouecksilber(II)-chlorid zugesetzt. Die Temperatur der exothermen Reaktion wurde anfangs zwischen 30 und 40° C, gegen Ende zwischen 70 und 80° C gehalten. Durch Vakuumdestillation konnten von dem NaAlCl4-Ritckstand 175 g reines, chloridfreies Ouecksilberdiäthyl erhalten werden, was einer Auslaute von mehr als 90% der Theorie entspricht.A total of 203.6 g of mercury (II) chloride were successively added to 57 aluminum triethyl into which 23 g of sodium chloride had been introduced with stirring. The temperature of the exothermic reaction was initially kept between 30 and 40 ° C, towards the end between 70 and 80 ° C. Vacuum distillation made it possible to obtain 175 g of pure, chloride-free mercury diethyl from the NaAlCl 4 residue, which corresponds to more than 90% of theory.
Verfahren zur Herstellung
von QuecksilberalkylenMethod of manufacture
of mercury alkyls
Anmelder:
Kali-Chemie Aktiengesellschaft,
Hannover, Hans-Böckler-Allee 20Applicant:
Kali-Chemie Aktiengesellschaft,
Hanover, Hans-Böckler-Allee 20
Dr. Herbert Jenkner, Hannover-Wülfel,
ist als Erfinder genannt wordenDr. Herbert Jenkner, Hanover-Wülfel,
has been named as the inventor
Gemäß Beispiel 1 wurden die gleichen Mengen Aluminiumtriäthyl, Natriumchlorid und OuecksiIber(II)-chlorid zur Reaktion gebracht. Als Lösungsmittel bzw. Verdünnungsmittel für Al R3 wurden 90 ecm Methylenchlorid zusätzlich eingesetzt. Erhalten- wurden 168 g Quecksi lberdiäthyl, Kp. 26° C/0,5 mm.According to Example 1, the same amounts of aluminum triethyl, sodium chloride and OuecksiIber (II) chloride were reacted. 90 ecm of methylene chloride were also used as a solvent or diluent for Al R 3. 168 g of mercury diethyl, boiling point 26 ° C./0.5 mm, were obtained.
Wird an Stelle von Methylenchlorid Ouecksilberdiäthyl selbst als Lösungsmittel bzw. Verdünnungsmittel für AlR3 verwendet, so betragen die Ausbeuten ebenfalls mehr als 90% der Theorie. Ebenso kann man ein Gemisch von Ouecksilberdiäthyl und Ouecksilber(II)-Chlorid (Bildung von Äthylquecksilberchlorid) gemäß Beispiel 1 und 2 mit Aluminiumtriäthyl umsetzen. Die Ausbeuten l>etragen ebenfalls mehr als 90%.If, instead of methylene chloride, diethyl sucrose itself is used as a solvent or diluent for AlR 3 , the yields are likewise more than 90% of theory. It is also possible to convert a mixture of diethyl and silver (II) chloride (formation of ethylmercury chloride) according to Examples 1 and 2 with aluminum triethyl. The yields are also more than 90%.
Wird an. Stelle von Aluminiumtriäthyl Aluminiumtrimethyl bzw. Aluminiumtripropyl oder aber Diathylaluminiumchlorid gemäß Beispiel 1 und 2 mit Quecksilberchlorid bzw. Alkylquedksilberchlorid umgesetzt, so erhält man- in- jedem Falle die entsprechenden Ouecksilberalkyle in über 85%iger Ausbeute.We then. Place of aluminum triethyl aluminum trimethyl or aluminum tripropyl or dietary aluminum chloride reacted according to example 1 and 2 with mercury chloride or alkyl mercury chloride, in any case, the corresponding mercury alkyls are obtained in a yield of over 85%.
Zum Vergleich wurde gemäß Beispiel 1 gearbeitet, doch mit dem Unterschied, daß kein Kochsalz zur Komplexbildung des entstandenen Aluminiumchlorids eingesetzt wurde. Es wurden bei der Destillation nur 16 g eines 31% Chlor enthaltenden Reaktionsproduktes erhalten.For comparison, the procedure was as in Example 1, but with the difference that no table salt was used Complex formation of the resulting aluminum chloride was used. There were only distillation 16 g of a reaction product containing 31% chlorine were obtained.
100Gewichtsteile Benzol werden mit 12,9Gewichtsteilen NaCl versetzt, worauf 22,8 Gewichtsteile Aluminiumtriäthyl zugegeben werden.100 parts by weight of benzene are mixed with 12.9 parts by weight of NaCl, whereupon 22.8 parts by weight of aluminum triethyl be admitted.
809 729/284809 729/284
Claims (1)
Verfahren zur Herstellung von Quecksilberalkylen, gekennzeichnet durch die Umsetzung von Ouecksilberchloriden mit Aluminiurntrialkylen, deren Ätheraten oder Aluminiumalkylchloriden unter Zusatz von Alkalic'hloriden, insbesondere Natriumchlorid. Claim:
Process for the preparation of mercury alkyls, characterized by the reaction of mercury chlorides with aluminum trialkyls, their etherates or aluminum alkyl chlorides with the addition of alkali metal chlorides, in particular sodium chloride.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE1048581B true DE1048581B (en) | 1959-01-15 |
Family
ID=589739
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DENDAT1048581D Pending DE1048581B (en) |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE1048581B (en) |
-
0
- DE DENDAT1048581D patent/DE1048581B/de active Pending
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