HCID 21872162, compound → Tetraethoxysilane

HRID 636262Notes

Reaction equation

C(O)C.[CH2:4]([O:6][Si:7]([O:14][CH2:15][CH3:16])([O:11][CH2:12][CH3:13])[O:8][CH2:9][CH3:10])[CH3:5]>C(O)C>[CH2:9]([O:8][Si:7]([O:11][CH2:12][CH3:13])([O:6][CH2:4][CH3:5])[O:14][CH2:15][CH3:16])[CH3:10]

Participants

Conditions

Temperature: 195 °C

Procedure

Reactor B was a bubble column with stirrers and a reaction volume of 10 liter. A 7 kg amount of catalyst (stream 4), and 3 kg comminuted silicon (stream 5) with a mean particle size d50%=27 micron were charged to the reactor. At 170° C. the reaction began. Thereafter the dosing of 3.5 mol/hr silicon (stream 6) and 34 mol/hr ethanol (stream 9) began. A 20 mol/hr amount of the ethanol was provided by recycle ethanol (stream 9). The temperature was increased to 190-200° C. and kept constant. High-boiling components (stream 7) were retained by means of the overhead column C, and the ethanol/tetraethoxysilane mixture (stream 8) was fractionated in column E, yielding tetraethoxysilane product in the amount of 3.5 mol/hr (stream 10). The ethanol (stream 9) was sent in dose amounts to reactor B, as excess ethanol. The impurities in the silicon powder (stream 12) were drawn off at the bottom of the reactor with other residual reactor contents and were collected in filter F, wherewith the liquid components (stream 13) were returned to the reactor.

Workup

customReactor B was
customA 7 kg amount of catalyst (stream 4), and 3 kg comminuted silicon (stream 5) with a mean particle size d50%=27 micron
additionwere charged to the reactor
customAt 170° C.

Sources & evidence

ORD record: ord-e6c05d48cd9848b289f861b5a1ff19d7
Source dataset: uspto-grants-2001_02
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US06191296B1

Reaction notes

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