DD240897A1 - METHOD FOR THE PRODUCTION OF ODORLESS SILICONE OILS - Google Patents
METHOD FOR THE PRODUCTION OF ODORLESS SILICONE OILS Download PDFInfo
- Publication number
- DD240897A1 DD240897A1 DD28061485A DD28061485A DD240897A1 DD 240897 A1 DD240897 A1 DD 240897A1 DD 28061485 A DD28061485 A DD 28061485A DD 28061485 A DD28061485 A DD 28061485A DD 240897 A1 DD240897 A1 DD 240897A1
- Authority
- DD
- German Democratic Republic
- Prior art keywords
- silicone oils
- production
- equilibration
- odorless
- metal
- Prior art date
Links
- 229920002545 silicone oil Polymers 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 title claims abstract description 14
- 230000009965 odorless effect Effects 0.000 title claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 title abstract description 7
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- 239000002184 metal Substances 0.000 claims abstract description 12
- 238000011067 equilibration Methods 0.000 claims abstract description 9
- 239000000654 additive Substances 0.000 claims abstract description 5
- 230000000996 additive effect Effects 0.000 claims abstract description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- 230000002378 acidificating effect Effects 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 125000004122 cyclic group Chemical group 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000008187 granular material Substances 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 239000003377 acid catalyst Substances 0.000 abstract 1
- 235000019645 odor Nutrition 0.000 description 4
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 3
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- -1 siloxanes Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910006069 SO3H Inorganic materials 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- KTQYJQFGNYHXMB-UHFFFAOYSA-N dichloro(methyl)silicon Chemical compound C[Si](Cl)Cl KTQYJQFGNYHXMB-UHFFFAOYSA-N 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 239000005048 methyldichlorosilane Substances 0.000 description 1
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000005051 trimethylchlorosilane Substances 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
Landscapes
- Silicon Polymers (AREA)
Abstract
Bisher bekannte Verfahren zum Erhalt geruchsfreier Siliconoele beinhalten eine Nachbehandlung des Produktes in einer sich an den Herstellungsprozess anschliessenden Verfahrensstufe, die mit Produktionsverlust verbunden ist. Die erfindungsgemaesse Loesung umgeht diesen zusaetzlichen Aufwand, indem geruchsfreie Siliconoele durch Aequilibrierung von unterschiedlichen Polydiorganosiloxaenen in Gegenwart eines sauren Katalysators und eines Metallzusatzes hergestellt werden.Heretofore known methods for obtaining odor-free silicone oils involve aftertreatment of the product in a process stage subsequent to the production process, which is associated with a loss of production. The inventive solution avoids this additional expense by producing odorless silicone oils by equilibration of different polydiorganosiloxanes in the presence of an acid catalyst and a metal additive.
Description
Anwendungsgebiet der Erfindung ,Field of application of the invention,
Die Erfindung betrifft die Herstellung von Siliconölen, vorzugsweise Methylsiliconölen oder Methylhydrogensiliconöleri, die als wäßrige Emulsion, Paste, Lösung oder auch ohne weitere Verarbeitung in der Kosmetik-, Textil- und kunststoffverarbeitenden Industrie oder als Zwischenprodukt in der Silicon-Chemie angewendet werden.The invention relates to the preparation of silicone oils, preferably methylsilicone oils or Methylhydrogensiliconöleri, which are used as aqueous emulsion, paste, solution or even without further processing in the cosmetics, textile and plastics processing industry or as an intermediate in silicone chemistry.
Die Herstellung von Siliconölen ist bekannt. Zum Beispiel wird ein Dimethyl-dichlorsilan-Hydrolysat, enthaltend cyclische und OH-endgruppenhaltige Dimethylpolysiloxane, mit einem Kettenabbrecher, z. B. Hexamethyldisiloxan, in Gegenwart eines Katalysators umgesetzt. Bei dieser als Äquilibrierung bezeichneten Verfahrensstufe, bei der von einem Gemisch von mono-und difunktionellen Siloxanen ausgegangen wird, bilden sich mit Trimethylsiloxygruppen blockierte Ketten bestimmter Molmassenverteilung. Die so gewonnenen Siliconöle enthalten noch niedermolekulare Anteile, die durch Destillation im Unterdruck entfernt werden. Der Destillationsrückstand weist alle Merkmale eines Siliconöles auf. Herstellungsbedingt hat dieses Siliconöl einen deutlich wahrnehmbaren, unangenehmen Geruch, der jedoch analytisch nicht nachgewiesen werden kann. Dies bedingt eine Nachbehandlung. Diese zusätzliche Verfahrensstufe kann z. B. mit Aktivkohle ausgeführt werden, wodurch zwar der Geruch weitgehend beseitigt wird, jedoch Produktverluste unvermeidbar sind.The production of silicone oils is known. For example, a dimethyl-dichlorosilane hydrolyzate containing cyclic and OH-endblocked dimethylpolysiloxanes is reacted with a chain terminator, e.g. As hexamethyldisiloxane, reacted in the presence of a catalyst. In this process step, referred to as equilibration, in which a mixture of monofunctional and difunctional siloxanes is used, chains having a molecular weight distribution which have been blocked with trimethylsiloxy groups are formed. The silicone oils thus obtained still contain low molecular weight fractions, which are removed by distillation under reduced pressure. The distillation residue has all the characteristics of a silicone oil. Due to its production, this silicone oil has a distinct, unpleasant odor, which, however, can not be detected analytically. This requires a treatment. This additional process stage can, for. B. be carried out with activated carbon, whereby the odor is largely eliminated, however, product losses are unavoidable.
Ziel der Erfindung ist die Herstellung von geruchsfreien Siliconölen mit einfachen Mitteln ohne zusätzliche Verfahrensstufe und ohne Produktverlust. Die physikalischen und chemischen Parameter des Siliconöls sollen erhalten bleiben.The aim of the invention is the production of odorless silicone oils with simple means without additional process stage and without product loss. The physical and chemical parameters of the silicone oil should be preserved.
Darlegung des Wesens der Erfindung -Explanation of the essence of the invention
Es wurde überraschenderweise gefunden, daß die geruchsverursachenden Spuren in Siliconölen, die in so geringer Menge verhanden sind, daß sie sich dem chemischen Nachweis entziehen, durch einen Metallzusatz bei der Äquilibrierung völlig beseitigt werden.It has surprisingly been found that the odor-causing traces in silicone oils, which are present in such a small amount that they escape the chemical detection, are completely eliminated by a metal addition during the equilibration.
Der Metallzusatz bei der Äquilibrierung von linearen und/oder cyclischen Hydrolysaten bzw. Cohydrolysaten von Diorganodichlorsilanen, Monoorganodichlorsilanen und/oder Triorganochlorsilanen in Anwesenheit eines sauren Äpuilibrierungskatalysators beträgt 0,3 bis 0,7%, bezogen auf die Gesamtmasse. Als Metalle haben sich Aluminium, Zink, Eisen und/oder Kupfer in Form von Pulver, Grieß oder Granulat besonders bewährt. Es ist vorteilhaft, den Metallzusatz vor dem Einsatz bei der Äquilibrierung mit dem sauren Äquilibrierungskatalysator innig zu vermischen. Der Metallzusatz beseitigt alle den Siliconölen anhaftenden, störenden Gerüche ohne eine zusätzliche Verfahrensstufe und ohne Produktverlust. Das Verfahren findet Anwendung bei der Herstellung von geruchsfreien Siliconölen.The addition of metal during the equilibration of linear and / or cyclic hydrolysates or co-hydrolysates of diorganodichlorosilanes, monoorganodichlorosilanes and / or triorganochlorosilanes in the presence of an acidic equilibration catalyst amounts to 0.3 to 0.7%, based on the total mass. As metals, aluminum, zinc, iron and / or copper in the form of powder, semolina or granules have proven particularly useful. It is advantageous to intimately mix the metal additive with the acidic equilibration catalyst prior to use in the equilibration. The addition of metal eliminates any interfering odors adhering to the silicone oils without an additional process step and product loss. The process finds application in the production of odorless silicone oils.
In einen 2,5-l-Sulfierkolben mit Thermometer, Rückflußküler und Probenahmestelle gibt man das Äqulibriergemisch, bestehend aus 492g eines Hydrolysates von Dimethyldichlorsilan, 8g Hexamethyldisiloxan und 25g eines Styrendivinylenbenzen-Copolymerisates mit SO3H~-Ankergruppen, das mit 2,5g Aluminiumgranulat innig vermischt worden ist, und äquilibriert bei 350K bis zur Viskositätskonstanz. Nach Abtrennen des Katalysators mit dem Metallzusatz werden dieOligomeren aus dem System mittels Vakuumdestillation entfernt. Als Rückstand verbleibt geruchsfreies Methylsiliconöl.In a 2.5-liter sulfonating flask with thermometer, Rückflußküler and sampling are given the Äqulibriergemisch consisting of 492g of a hydrolyzate of dimethyldichlorosilane, 8g hexamethyldisiloxane and 25g of a Styrenedivinylenbenzen copolymer with SO3H ~ Ankergruppen intimately mixed with 2.5g aluminum granules and equilibrated at 350K until the viscosity is constant. After separating the catalyst with the metal additive, the oligomers are removed from the system by vacuum distillation. Odorless methylsilicone oil remains as residue.
Ein gleiches Ergebnis wird erhalten, wenn z. B. anstelle des Aluminiumgranulates Kupferpulver, Zinkstaub, Eisenspäne, Aluminiumgrieß bzw. -pulver oder ein Gemisch von Kupfer- und Aluminiumpulver eingesetzt werden.An identical result is obtained when z. B. instead of the aluminum granules copper powder, zinc dust, iron filings, aluminum grit or powder or a mixture of copper and aluminum powder can be used.
Verfährt man wie beschrieben, jedoch ohne Zusatz von Metall, so erhält man ein Methylsiliconöl mit störendem Geruch.If the procedure is as described, but without the addition of metal, we obtain a methyl silicone oil with a disturbing odor.
Verfährt man.wie im Beispiel 1 beschrieben, setzt jedoch alsÄquilibriergemisch 400g eines Cohydrolysates aus Dimethyldichlorsilan, Methyldichlorsilan undTrimethylchlorsilan, 590g Octamethylcyclotetrasiloxan, 8g Hexamethyldisiloxan und 30g Styrendivinylenbenzen-Copolymerisat mit SO3H"-Ankergruppen, das mit 6g Aluminiumgrieß vermischt wurde, ein und äquilibriert bei 340 K, so erhält man ein geruchsfreies Siliconöl.The procedure is repeated as described in Example 1 except that 400g of a co-hydrolyzate of dimethyldichlorosilane, methyldichlorosilane and trimethylchlorosilane, 590g of octamethylcyclotetrasiloxane, 8g of hexamethyldisiloxane and 30g of styrene-divinylenebenzene copolymer are mixed with SO 3 H "anchor groups mixed with 6g of aluminum grit and allowed to equilibrate 340 K, we obtain an odorless silicone oil.
Claims (4)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DD28061485A DD240897A1 (en) | 1985-09-16 | 1985-09-16 | METHOD FOR THE PRODUCTION OF ODORLESS SILICONE OILS |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DD28061485A DD240897A1 (en) | 1985-09-16 | 1985-09-16 | METHOD FOR THE PRODUCTION OF ODORLESS SILICONE OILS |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DD240897A1 true DD240897A1 (en) | 1986-11-19 |
Family
ID=5571258
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DD28061485A DD240897A1 (en) | 1985-09-16 | 1985-09-16 | METHOD FOR THE PRODUCTION OF ODORLESS SILICONE OILS |
Country Status (1)
| Country | Link |
|---|---|
| DD (1) | DD240897A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0522443A1 (en) * | 1991-07-04 | 1993-01-13 | Wacker-Chemie Gmbh | Process for purifying organopolysiloxanes |
| DE10392191B4 (en) * | 2002-11-18 | 2015-07-23 | Dow Corning Toray Co., Ltd. | A process for producing a deodorized polyether-modified polysiloxane and use thereof in a cosmetic product |
-
1985
- 1985-09-16 DD DD28061485A patent/DD240897A1/en not_active IP Right Cessation
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0522443A1 (en) * | 1991-07-04 | 1993-01-13 | Wacker-Chemie Gmbh | Process for purifying organopolysiloxanes |
| DE10392191B4 (en) * | 2002-11-18 | 2015-07-23 | Dow Corning Toray Co., Ltd. | A process for producing a deodorized polyether-modified polysiloxane and use thereof in a cosmetic product |
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