DE1150661B - Process for the production of hexachlorodisiloxane from its mixtures with titanium tetrachloride - Google Patents
Process for the production of hexachlorodisiloxane from its mixtures with titanium tetrachlorideInfo
- Publication number
- DE1150661B DE1150661B DED38867A DED0038867A DE1150661B DE 1150661 B DE1150661 B DE 1150661B DE D38867 A DED38867 A DE D38867A DE D0038867 A DED0038867 A DE D0038867A DE 1150661 B DE1150661 B DE 1150661B
- Authority
- DE
- Germany
- Prior art keywords
- hexachlorodisiloxane
- titanium tetrachloride
- mixtures
- production
- reducing agent
- 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
- QHAHOIWVGZZELU-UHFFFAOYSA-N trichloro(trichlorosilyloxy)silane Chemical compound Cl[Si](Cl)(Cl)O[Si](Cl)(Cl)Cl QHAHOIWVGZZELU-UHFFFAOYSA-N 0.000 title claims description 15
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 title claims description 11
- 239000000203 mixture Substances 0.000 title claims description 9
- 238000000034 method Methods 0.000 title claims description 8
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000003638 chemical reducing agent Substances 0.000 claims description 6
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 3
- -1 oxygen hexachlorodisiloxane Chemical compound 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000005049 silicon tetrachloride Substances 0.000 description 3
- 229910000519 Ferrosilicon Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 229910003074 TiCl4 Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 125000001153 fluoro group Chemical class F* 0.000 description 1
- 238000004508 fractional distillation Methods 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- CLXMTJZPFVPWAX-UHFFFAOYSA-N trichloro-[dichloro(trichlorosilyloxy)silyl]oxysilane Chemical compound Cl[Si](Cl)(Cl)O[Si](Cl)(Cl)O[Si](Cl)(Cl)Cl CLXMTJZPFVPWAX-UHFFFAOYSA-N 0.000 description 1
- 238000010626 work up procedure Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Description
Verfahren zur Gewinnung von Hexachlordisiloxan aus seinen Gemischen mit Titantetrachlorid Die Erfindung bezieht sich auf ein Verfahren, welches es gestattet, Titantetrachlorid von Hexachlordisiloxan abzutrennen und dabei das Hexachlordisiloxan in reiner Form zu gewinnen.Process for the production of hexachlorodisiloxane from its mixtures with titanium tetrachloride The invention relates to a method which allows Separate titanium tetrachloride from hexachlorodisiloxane and thereby the hexachlorodisiloxane to be won in pure form.
Bei der Herstellung von Siliciumtetrachlorid durch Chlorierung von Ferrosilicium entstehen neben Eisenchlorid und Titantetrachlorid als Folge des nicht immer zu vermeidenden Zutrittes von Luftsauerstoff Hexachlordisiloxan, Octachlortrisiloxan sowie entsprechende cyclische, d. h. trimere oder tetramere Chlorsiloxane. Bei der Aufarbeitung solcher Produkte bestehen insofern Schwierigkeiten, als das Titantetrachlorid und das Hexachlordisiloxan denselben Siedepunkt von 135,5`= C haben, so daß diese beiden Stoffe destillativ nicht zu trennen sind. Es ist bekanntgeworden, solche Gemische dadurch zu trennen, daß man die Siliciumverbindung in eines der möglichen Fluorderivate überführt und sodann diese Substanz destillativ abtrennt. Nach dieser Methode ist es jedoch nicht möglich, Hexachlordisiloxan in reiner Form zu gewinnen.In the production of silicon tetrachloride by chlorination of Ferrosilicon is not formed in addition to iron chloride and titanium tetrachloride as a result Always avoid access of atmospheric oxygen hexachlorodisiloxane, octachlorotrisiloxane as well as corresponding cyclic, d. H. trimeric or tetrameric chlorosiloxanes. In the Work-up of such products are difficult insofar as the titanium tetrachloride and the hexachlorodisiloxane have the same boiling point of 135.5` = C, so that this the two substances cannot be separated by distillation. It has become known such Separate mixtures by converting the silicon compound into one of the possible Transferred fluorine derivatives and then this substance is separated off by distillation. After this Method, however, it is not possible to obtain hexachlorodisiloxane in pure form.
Es wurde nun gefunden, daß man Hexachlordisiloxan aus seinen Gemischen mit Titantetrachlorid gewinnen kann, wenn man das Gemisch bei einer Temperatur zwischen 100 und 250° C und unter erhöhtem Druck mit einem an sich bekannten metallischen Reduktionsmittel behandelt. Hierbei wird das Titantetrachlorid zu Titantrichlorid reduziert, welches als Schlamm ausfällt. Das gebildete Titantrichlorid wird sodann abgetrennt und das Hexachlordisiloxan gegebenenfalls zur weiteren Reinigung destilliert.It has now been found that hexachlorodisiloxane can be obtained from its mixtures with titanium tetrachloride can be obtained if the mixture is at a temperature between 100 and 250 ° C and under increased pressure with a known metallic Treated reducing agent. Here, the titanium tetrachloride becomes titanium trichloride reduced, which precipitates as sludge. The titanium trichloride formed is then separated off and the hexachlorodisiloxane distilled, if necessary, for further purification.
Es war hierbei überraschend, daß das Hexachlordisiloxan durch das Reduktionsmittel nicht angegriffen wird, und zwar auch dann nicht, wenn es in größeren Mengen oder gar als wesentlicher Bestandteil des Gemisches vorhanden ist.It was surprising that the hexachlorodisiloxane by the Reducing agent is not attacked, even if it is in larger ones Quantities or even as an essential part of the mixture is present.
Als Reduktionsmittel können Metalle, wie Eisen, Zink usw., verwendet werden. Bevorzugt wird jedoch das Aluminium eingesetzt. Vorteilhaft verwendet man das Reduktionsmittel in Mengen von etwa 10 bis 20 Gewichtsprozent, bezogen auf TiCl4.Metals such as iron, zinc, etc. can be used as the reducing agent will. However, aluminum is preferably used. It is advantageous to use the reducing agent in amounts of about 10 to 20 percent by weight, based on TiCl4.
Um thermische Zersetzungen zu vermeiden, soll die Reduktion unterhalb von 250° C durchgeführt werden. Bevorzugt wird eine Temperatur von etwa 200- C bis etwa 220° C eingehalten.In order to avoid thermal decomposition, the reduction should be below of 250 ° C. A temperature of about 200.degree. C. is preferred about 220 ° C maintained.
Wenn nach der Abtrennung des gebildeten Titantrichlorids nochmals eine Destillation des Hexachlordisiloxans erfolgt, wird ein außerordentlich reines Produkt erhalten, welches unmittelbar als Ausgangsmaterial für die Herstellung von Estern der Kieselsäure verwendet werden kann. Beispiel Bei der Chlorierung von Ferrosilicium entsteht ein Produkt, welches sieh nach dem Abdekantieren vom unlöslichen Eisenchlorid aus etwa 45 % Siliciumtetraehlorid, 45 0/OHexachlordisiloxan, etwa 5 % Titantetrachlorid und kleinen Mengen Hexachlordisiloxan und Polymeren des Dichlorsiloxans zusammensetzt. Aus diesem Gemisch wird zunächst das Siliciumtetrachlorid durch fraktionierte Destillation abgetrennt. Der flüssige Destillationsrückstand wird sodann in einer Destillationsapparatur mit Säule und Dephlegmator einer Fraktionierung unterworfen. Die bei 134 bis 136° C übergehende Fraktion enthält etwa 90 bis 9211/o Hexachlordisiloxan und 5 bis 81/o Titantetrachlorid. Diese Fraktion wird in einem eisernen Autoklav bei einem Druck von 4,5 atü in Gegenwart von 1,5% Aluminiumpulver etwa 1 Stunde lang unter Rühren auf 200° C erwärmt. Das Titantrichlorid fällt als Sehlamm aus und wird abgetrennt. Die flüssige Phase wird erneut destilliert. Man erhält ein reines Hexachlordisiloxan.If again after the separation of the titanium trichloride formed If the hexachlorodisiloxane is distilled, it becomes extremely pure Product obtained, which can be used directly as a starting material for the production of Esters of silica can be used. Example In the chlorination of ferro-silicon the result is a product that can be seen after decanting from the insoluble ferric chloride from about 45% silicon tetra chloride, 450 / OHexachlorodisiloxane, about 5% titanium tetrachloride and small amounts of hexachlorodisiloxane and polymers of dichlorosiloxane. The silicon tetrachloride is first produced from this mixture by fractional distillation severed. The liquid distillation residue is then in a distillation apparatus subjected to fractionation with column and dephlegmator. The one at 134 to 136 ° C passing fraction contains about 90 to 9211 / o hexachlorodisiloxane and 5 to 81 / o Titanium tetrachloride. This fraction is in an iron autoclave at one pressure of 4.5 atmospheres in the presence of 1.5% aluminum powder for about 1 hour with stirring heated to 200 ° C. The titanium trichloride precipitates in the form of sludge and is separated off. The liquid phase is distilled again. A pure hexachlorodisiloxane is obtained.
Claims (4)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DED38867A DE1150661B (en) | 1962-05-09 | 1962-05-09 | Process for the production of hexachlorodisiloxane from its mixtures with titanium tetrachloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DED38867A DE1150661B (en) | 1962-05-09 | 1962-05-09 | Process for the production of hexachlorodisiloxane from its mixtures with titanium tetrachloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE1150661B true DE1150661B (en) | 1963-06-27 |
Family
ID=7044382
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DED38867A Pending DE1150661B (en) | 1962-05-09 | 1962-05-09 | Process for the production of hexachlorodisiloxane from its mixtures with titanium tetrachloride |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE1150661B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3475139A (en) * | 1966-12-02 | 1969-10-28 | Degussa | Process for the separation of aluminum chloride and titanium tetrachloride from gaseous reaction gases containing chlorosilanes |
-
1962
- 1962-05-09 DE DED38867A patent/DE1150661B/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3475139A (en) * | 1966-12-02 | 1969-10-28 | Degussa | Process for the separation of aluminum chloride and titanium tetrachloride from gaseous reaction gases containing chlorosilanes |
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