3-Glycidoxypropyltrimethoxysilane synthesis

Yield:2530-83-8 89%

Reaction Conditions:

with platinum⁽⁰⁾-1,3-divinyl-1,1,3,3-tetramethyldisiloxane complex in methanol at 70 - 80; under 760.051 Torr;Reagent/catalyst;

Steps:

1.2-1.3; 2.2-2.3; 3.2-3.3; 4.2-4.3; 5.2-5.3; 6.2-6.3; 7.2-7.3; 1.2-1.3 S2: Addition section

20kg of methanol, 600kg of allyl glycidyl ether (AKGE) and 550kg of metered trimethoxysilane were transported to the respective metering tanks through the material pump, and the quantitative AKGE and solvent methanol were added to the synthesis reactor through a flowmeter, and 100×10 -5 catalyst, 15kg co-catalyst, turn on stirring, heat and raise temperature at the same time, raise the temperature to 80°C under normal pressure, close the heating valve, slowly add trimethoxysilane dropwise, the trimethoxysilane pipeline is provided with a flow meter and a flow control valve, The dropwise addition is realized by adjusting the valve; the reaction temperature is controlled below 70°C, and the temperature is kept for about 5 hours after the dropwise addition, and the synthetic liquid is taken for gas chromatography analysis. , carry out distillation after producing two batches of synthetic liquids; Finished product distillation includes two sets of distillation system, low boiling distillation system and finished product distillation system. Each set of distillation system includes distillation still and distillation column, column top condenser, gas-liquid separator, receiving tank, tail gas condenser and tail gas condensation receiving tank. ;First, turn on the vacuum pump of the box, and pass the two batches of synthetic liquid to the low-boiling distillation kettle. After the feeding is completed, open the steam heating valve to heat the material and receive the distilled solvent methanol. When the vacuum degree of the low-boiling distillation still is lower than -0.098MPa and the temperature is 160°C, the low-boiling distillation is stopped, the methanol recovered in the solvent receiving tank is directly pumped into the recovery methanol metering tank for reuse, and the methanol in the tail gas condensation receiving is transported to the solvent Temporary storage tank, then through the solvent distillation still to recover methanol under reduced pressure for reuse;After the distillation of the low-boiling material is completed, close the steam heating and vacuum of the low-boiling distillation system and the valve of the material receiving pipeline, pass nitrogen to balance the negative pressure, and turn on the Roots vacuum pump of the finished distillation system at the same time. The middle material is pumped into the finished product distillation kettle while hot to start the finished product distillation; after the crude product is passed through, the heat-conducting oil is turned on to heat the crude product while the hot product is still hot. After the distillation is completed, the sample is taken for analysis and the content is qualified, and the qualified finished product is transported to the finished product storage tank by the finished product pump.

References:

CN114773377,2022,A Location in patent:Paragraph 0008; 0012-0027