Trimethyliodosilane preparation method
A technology for trimethyl iodide silane and trimethyl chlorosilane is applied in the field of preparing trimethyl iodide silane, which can solve the problems of many by-products and low yield, and achieve the effects of less impurities, high yield and simple purification.
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Embodiment 1
[0022] A method for preparing iodotrimethylsilane, the method comprising the following steps:
[0023] 1) A 250ml three-necked flask, equipped with a feeding funnel, a nitrogen conduit and a reflux condenser, opened the nitrogen purge, and mixed 17.4g of anion exchange resin (201×4(711) strong basic styrene type I anion exchange resin) and 26ml of water (1.4mol) into a three-necked flask, start stirring, heat up to 45°C, add 43.4g (400mmol) of trimethylchlorosilane, add trimethylchlorosilane, heat up to 75°C, stir for 2.5 hours, distill at atmospheric pressure, Collect fractions at 99-100°C, dry with anhydrous sodium sulfate, and filter to obtain 30.5 g of hexamethyldisiloxane with a purity of 99.5% and a yield of 93.8%;
[0024] 2) A 250ml three-neck flask, equipped with a feeding funnel, a nitrogen conduit and a reflux condenser, opened the nitrogen purge, and added step 1) 16.2g (100mmol) of hexamethyldisiloxane and 4.9g (180mmol) of aluminum powder, with an average particl...
Embodiment 2
[0026] A method for preparing iodotrimethylsilane, the method comprising the following steps:
[0027] 1) A 250ml three-neck flask, equipped with a feeding funnel, a nitrogen conduit and a reflux condenser, turned on the nitrogen purge, and added 19.4g of anion exchange resin (D201 macroporous strongly basic styrene-based anion exchange resin) and 23ml (1.2mol) of water Put it into a three-necked flask, start stirring, heat up to 45°C, add 43.4g (400mmol) of trimethylchlorosilane, add trimethylchlorosilane, heat up to 70°C and stir for 1.5 hours, distill at normal pressure, collect 99-100°C The fraction was dried with anhydrous sodium sulfate and filtered to obtain 29.8 g of hexamethyldisiloxane with a purity of 99.6% and a yield of 91.7%;
[0028] 2) A 250ml three-neck flask, equipped with an addition funnel, a nitrogen conduit and a reflux condenser, opened the nitrogen purge, added 16.2g (100mmol) of hexamethyldisiloxane and 4g (150mmol, average particle size: 30μm) of alum...
Embodiment 3
[0030] A method for preparing iodotrimethylsilane, the method comprising the following steps:
[0031] 1) A 250ml three-necked flask, equipped with a feeding funnel, a nitrogen conduit and a reflux condenser, turned on the nitrogen purge, and added 15.2g of anion exchange resin (303 weakly basic epoxy anion exchange resin) and 30ml (1.6mol) of water into the three-necked flask In the flask, start stirring, heat up to 45°C, add 43.4g (400mmol) of trimethylchlorosilane, add trimethylchlorosilane, heat up to 65°C and stir for 2 hours, distill at normal pressure, collect 99-100°C fractions, Dry with anhydrous sodium sulfate and filter to obtain 29.5 g of hexamethyldisiloxane with a purity of 99.8% and a yield of 90.9%;
[0032] 2) A 250ml three-neck flask, equipped with an addition funnel, a nitrogen conduit and a reflux condenser, turned on the nitrogen purge, added 16.2g (100mmol) of hexamethyldisiloxane and 4.3g (160mmol, average particle size of 50μm) of aluminum powder, Star...
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