Ethanol → Tetraethoxysilane

HRID 1750719Notes

Reaction equation

HRID 1750719 reaction equation
[CH2:1]([O:3][SiH:4]([O:8][CH2:9][CH3:10])[O:5][CH2:6][CH3:7])[CH3:2].[CH2:11]([OH:13])[CH3:12]>Cl[Cu].COCCOC>[CH2:1]([O:3][SiH:4]([O:8][CH2:9][CH3:10])[O:5][CH2:6][CH3:7])[CH3:2].[CH2:1]([O:3][Si:4]([O:13][CH2:11][CH3:12])([O:8][CH2:9][CH3:10])[O:5][CH2:6][CH3:7])[CH3:2]

Participants

6

Reactant 2

HCID 702EthanolHCID 13830Triethoxysilane2×

Product 2

HCID 6517TetraethoxysilaneHCID 13830Triethoxysilane

Reagents, catalysts & solvents 2

HCID 62652Cuprous chlorideCatalystHCID 80711,2-DimethoxyethaneSolvent

Procedure

The preparation of triethoxysilane was carried out in a reactor having working capacity of 9 L, which was equipped with an electric heating control device of reaction capacity, and an impeller stirrer having 4 wings to control rotational speed to 300-1500 rpm. 3.3 kg of metal silicon was ground in a solvent environment of 6.6 kg of THERMINOL® 66 using Planetary Mill until the particle size is 30-100 μm. In the pulverizing process, 0.2 kg of CuCl catalyst was put into the suspension. In the state of continuous operation of the stirrer at 850 rpm, contact mass was heated to temperature of 242+2° C., the feed of ethanol as anhydrous alcohol to the reactor was started at 600 ml/hr using dosing pump (Digital dosing pump), GRUNDFOS® DME 60-10 AR. Samples were taken when liquid product was generated in the reactor, then every 30 minutes. As a result of analysis of the samples in Gas chromathograph, Agilent® GC7890A, synthesis reaction was started 10 minutes after alcohol was poured, and reaction rate increased for initial 60 minutes. The synthesis reaction rate of triethoxysilane decreased after 180 minutes, and completely slowed down 260 minutes after alcohol was fed. Herein, 1635 g of triethoxysilane and 105 g of tetraethoxysilane were obtained. The selectivity of triethoxysilane was 94%.

Workup

  1. customwas carried out in a reactor
  2. customwas equipped with an electric heating control device of reaction capacity, and an impeller stirrer
  3. customevery 30 minutes
  4. customAs a result of analysis of the samples in Gas chromathograph, Agilent® GC7890A, synthesis reaction
  5. customreaction rate
  6. temperatureincreased for initial 60 minutes
  7. waitdecreased after 180 minutes
  8. waitcompletely slowed down 260 minutes

Sources & evidence

ORD record
ord-2f71214019e542dca7e4911895b06efe
Source dataset
uspto-grants-2015_10
Patent number
US09156861B2

Reaction notes

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