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
  • C07F7/0834—Compounds having one or more O-Si linkage
  • C07F7/0838—Compounds with one or more Si-O-Si sequences
  • C07F7/0872—Preparation and treatment thereof
  • C07F7/0874—Reactions involving a bond of the Si-O-Si linkage

Definitions

• the present invention relates to the production of tris- (trimethylsiloxy)-phenylsilane of the formula @sn-o-sqoum];
• the phenyltrichlorosilane can be converted to the extent of more than 90% into the desired tetrasiloxane, by a new combination of several process steps, without the simultaneously freshly formed amount of hexamethyldisiloxane exceeding a tol- Patented Sept. 17, 1974 erable level.
• tris-(trimethylsiloxy)-phenylsilane is produced by carrying out the hydrolytic reaction of trimethylchlorosilane, phenyltri chlorosilane and water in the presence of an amount of hexamethyldisiloxane which is 0.2 to 12 mols, preferably 2 to 6 mols, per mol of phenyltrichlorosilane, using a molar ratio of trimethylchlorosilane to phenyltrichlorosilane of between 3.3:1 and 4:1 and adding the water gradually, in excess, until the hydrolysis is complete.
• yields of up to 74% result.
• the amount of sulphuric acid can be kept low, for the same high yield, if initially the mixture of hexamethyldisiloxane and sulphuric acid is warmed to C. for about 30 minutes, the phenyltrichlorosilane is gradually added thereto, the trimethylchlorosilane is then added at 30 C. and the water is finally stirred in at room temperature, spread over a prolonged period of time.
• An elevated temperature during the hydrolysis reaction leads to a substantially reduced yield, for example, at 50 C., to 46% instead of 76%.
• hexamethyldisiloxane can also be produced in situ from excess trimethylchlorosilaue; and an appropriate amount of sulphuric acid can be mixed with the water used for the hydrolysis; While the yield then only remains moderate (for example 58%), it is nevertheless considerably higher than according to the known process mentioned initially.
• EXAMPLE 6 108 g. (6 mols) of water are added dropwise over the course of 3 hours to a mixture of 487 g. (3 mols) of hexamethyldisiloxane, 212 g. (1 mol) of phenyltrichlorosilane and 435 g. (4 mols) of trimethylchlorosilane at room temperature, while stirring, and the further procedure followed is as described in Example 1. The yield is 74%.
• EXAMPLE 7 A solution of 15 g. of concentrated sulphuric acid in 90 g. of water is added dropwise over the course of 6 hours to a mixture of 212 g. (1 mol) of phenyltrichlorosilane and 435 g. (4 mols) of trimethylchlorosilane at room temperature, while stirring, and the further procedure followed is as described in Example 1. The yield is 58%.

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• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Chemical Kinetics & Catalysis (AREA)

Applications Claiming Priority (1)

Publications (1)

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ID=5813947

Family Applications (1)

Country Status (7)

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• 0
  • BE BE786301D patent/BE786301A/fr not_active IP Right Cessation
• 1971
  • 1971-07-16 DE DE2135674A patent/DE2135674C3/de not_active Expired
• 1972
  • 1972-07-11 US US00270741A patent/US3836558A/en not_active Expired - Lifetime
  • 1972-07-13 FR FR7225394A patent/FR2146270B1/fr not_active Expired
  • 1972-07-13 NL NLAANVRAGE7209704,A patent/NL173526C/xx not_active IP Right Cessation
  • 1972-07-14 GB GB3309872A patent/GB1333035A/en not_active Expired
  • 1972-07-15 JP JP47070433A patent/JPS5810391B1/ja active Granted

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