DE2645792C2 - Verfahren zur Gewinnung von Hexamethyldisilazan - Google Patents
Verfahren zur Gewinnung von HexamethyldisilazanInfo
- Publication number
- DE2645792C2 DE2645792C2 DE19762645792 DE2645792A DE2645792C2 DE 2645792 C2 DE2645792 C2 DE 2645792C2 DE 19762645792 DE19762645792 DE 19762645792 DE 2645792 A DE2645792 A DE 2645792A DE 2645792 C2 DE2645792 C2 DE 2645792C2
- Authority
- DE
- Germany
- Prior art keywords
- hexamethyldisilazane
- ammonium chloride
- ammonia
- distillation
- mbar
- 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
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 title claims description 65
- 238000000034 method Methods 0.000 title claims description 20
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 58
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 45
- 235000019270 ammonium chloride Nutrition 0.000 claims description 29
- 229910021529 ammonia Inorganic materials 0.000 claims description 20
- 238000004821 distillation Methods 0.000 claims description 17
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 16
- 239000011541 reaction mixture Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 24
- 238000006243 chemical reaction Methods 0.000 description 12
- 238000003756 stirring Methods 0.000 description 7
- 239000005051 trimethylchlorosilane Substances 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- -1 monocyclic aryl radical Chemical class 0.000 description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 150000001367 organochlorosilanes Chemical class 0.000 description 6
- 238000000859 sublimation Methods 0.000 description 6
- 230000008022 sublimation Effects 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000001577 simple distillation Methods 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 230000003472 neutralizing effect Effects 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229920003043 Cellulose fiber Polymers 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 125000005263 alkylenediamine group Chemical group 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Chemical group BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002430 hydrocarbons Chemical group 0.000 description 2
- 239000012442 inert solvent Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical group [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- ZXZSEQFNAKXEAN-UHFFFAOYSA-N N.C[Si](C)(C)Cl Chemical compound N.C[Si](C)(C)Cl ZXZSEQFNAKXEAN-UHFFFAOYSA-N 0.000 description 1
- 229930182555 Penicillin Natural products 0.000 description 1
- JGSARLDLIJGVTE-MBNYWOFBSA-N Penicillin G Chemical compound N([C@H]1[C@H]2SC([C@@H](N2C1=O)C(O)=O)(C)C)C(=O)CC1=CC=CC=C1 JGSARLDLIJGVTE-MBNYWOFBSA-N 0.000 description 1
- 229910004028 SiCU Inorganic materials 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910001854 alkali hydroxide Inorganic materials 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000004508 fractional distillation Methods 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910000039 hydrogen halide Inorganic materials 0.000 description 1
- 239000012433 hydrogen halide Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052740 iodine Chemical group 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- AOZQTURTLIEFNQ-UHFFFAOYSA-N n,n'-bis(trimethylsilyl)ethane-1,2-diamine Chemical compound C[Si](C)(C)NCCN[Si](C)(C)C AOZQTURTLIEFNQ-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229940049954 penicillin Drugs 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000010626 work up procedure 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
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/10—Compounds having one or more C—Si linkages containing nitrogen having a Si-N linkage
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR7635495A FR2334687A1 (fr) | 1975-12-10 | 1976-11-25 | Procede de preparation d'hexamethyldisilazane avec emploi de cette substance comme solvant et separation par distillation de l'hexamethyldisilazane forme |
| IT5250676A IT1069982B (it) | 1975-12-10 | 1976-12-07 | Procedimento per la produzione di e sametil disilazano |
| NL7613725A NL162655C (nl) | 1975-12-10 | 1976-12-09 | Werkwijze voor het bereiden van hexamethyldisilazan. |
| GB5176976A GB1516900A (en) | 1976-10-09 | 1976-12-10 | Process for the manufacture of hexamethyldisilazane |
| ES456309A ES456309A1 (es) | 1976-10-09 | 1977-02-25 | Procedimiento para la preparacion de hexametildisilazano. |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB5068075A GB1516899A (en) | 1975-12-10 | 1975-12-10 | Process for the manufacture of hexamethyldisilazane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| DE2645792A1 DE2645792A1 (de) | 1977-06-16 |
| DE2645792C2 true DE2645792C2 (de) | 1982-12-23 |
Family
ID=10456916
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE19762645792 Expired DE2645792C2 (de) | 1975-12-10 | 1976-10-09 | Verfahren zur Gewinnung von Hexamethyldisilazan |
| DE19762645703 Expired DE2645703C3 (de) | 1975-12-10 | 1976-10-09 | Verfahren zur Herstellung von Hexamethyldisilazan |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE19762645703 Expired DE2645703C3 (de) | 1975-12-10 | 1976-10-09 | Verfahren zur Herstellung von Hexamethyldisilazan |
Country Status (6)
| Country | Link |
|---|---|
| BE (1) | BE849293A (nl) |
| DE (2) | DE2645792C2 (nl) |
| ES (1) | ES454033A1 (nl) |
| FR (1) | FR2334688A1 (nl) |
| GB (1) | GB1516899A (nl) |
| NL (1) | NL159987B (nl) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19753480C1 (de) * | 1997-12-02 | 1999-01-07 | Wacker Chemie Gmbh | Verfahren zur Herstellung von Organosilazanen und Ammonchlorid |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1516899A (en) * | 1975-12-10 | 1978-07-05 | Goldschmidt Ag Th | Process for the manufacture of hexamethyldisilazane |
| NL7812080A (nl) * | 1978-02-03 | 1979-08-07 | Goldschmidt Ag Th | Werkwijze voor het bereiden van hexamethyldisilazan. |
| JP6176175B2 (ja) * | 2014-04-03 | 2017-08-09 | 信越化学工業株式会社 | シラザン化合物の製造方法 |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5112608B2 (nl) * | 1973-05-29 | 1976-04-21 | ||
| GB1516899A (en) * | 1975-12-10 | 1978-07-05 | Goldschmidt Ag Th | Process for the manufacture of hexamethyldisilazane |
-
1975
- 1975-12-10 GB GB5068075A patent/GB1516899A/en not_active Expired
-
1976
- 1976-10-09 DE DE19762645792 patent/DE2645792C2/de not_active Expired
- 1976-10-09 DE DE19762645703 patent/DE2645703C3/de not_active Expired
- 1976-11-25 FR FR7635496A patent/FR2334688A1/fr active Granted
- 1976-12-07 ES ES454033A patent/ES454033A1/es not_active Expired
- 1976-12-09 NL NL7613726A patent/NL159987B/nl not_active Application Discontinuation
- 1976-12-10 BE BE173163A patent/BE849293A/xx not_active IP Right Cessation
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19753480C1 (de) * | 1997-12-02 | 1999-01-07 | Wacker Chemie Gmbh | Verfahren zur Herstellung von Organosilazanen und Ammonchlorid |
| US6051729A (en) * | 1997-12-02 | 2000-04-18 | Wacker-Chemie Gmbh | Process for preparing organosilazanes |
Also Published As
| Publication number | Publication date |
|---|---|
| DE2645703B2 (de) | 1979-01-04 |
| GB1516899A (en) | 1978-07-05 |
| DE2645703A1 (de) | 1977-06-16 |
| FR2334688A1 (fr) | 1977-07-08 |
| DE2645703C3 (de) | 1979-08-30 |
| BE849293A (fr) | 1977-04-01 |
| DE2645792A1 (de) | 1977-06-16 |
| NL7613726A (nl) | 1977-06-14 |
| NL159987B (nl) | 1979-04-17 |
| ES454033A1 (es) | 1977-11-16 |
| FR2334688B1 (nl) | 1979-03-09 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| D2 | Grant after examination | ||
| 8339 | Ceased/non-payment of the annual fee |