Preparation method of catalyst for methyl chlorosilane disproportionation
A technology of methyl chlorosilane and catalyst, applied in the field of catalyst preparation, can solve problems such as unexplained stability and regeneration of catalyst, and achieve the effects of good immobilization effect, simple preparation method and good regeneration performance.
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Embodiment 1
[0032] 1) γ-Al 2 o 3 preprocessing
[0033] At room temperature, 10 g γ-Al 2 o 3 The granules are soaked in 1M sulfuric acid solution for 2 hours, dried in vacuum, calcined at 100°C for 2 hours, cooled and sealed for storage;
[0034] 2) AlCl 3 Immobilized γ-Al 2 o 3
[0035] In the fixed bed reactor, add 10 g of anhydrous AlCl 3 , and then add the pretreated γ-Al 2 o 3 , immobilized at 200°C for 1 hour, and then in N 2 Decrease to room temperature under protection or vacuum state, and finally seal and store.
[0036] Add 100 g of the prepared solid-supported catalyst into the fixed-bed reactor, and the reaction raw material is CH 3 SiCl 3 with (CH 3 ) 3 SiCl, the reaction temperature is 150-400°C, the reaction pressure is 0.1-1.0Mpa, the reactant CH 3 SiCl 3 with (CH 3 ) 3 The SiCl feed ratio is 1:10-1, and the product after the reaction is quantitatively analyzed by gas chromatography, (CH 3 ) 2 SiCl 2 The quality fraction is 60%.
Embodiment 2
[0038] 1) γ-Al 2 o 3 preprocessing
[0039] At room temperature, 200g γ-Al 2 o 3 The granules are soaked in 1M hydrochloric acid solution for 48 hours, dried in vacuum, calcined at 800°C for 24 hours, sealed and stored after cooling down;
[0040] 2) AlCl 3 Immobilized γ-Al 2 o 3
[0041] In the fixed bed reactor, add 50g of anhydrous AlCl 3 , and then add the pretreated γ-Al 2 o 3 , immobilized at 400°C for 12 hours, and then in N 2 Decrease to room temperature under protection or vacuum state, and finally seal and store.
[0042] Add 100 g of the prepared solid-supported catalyst into the fixed-bed reactor, and the reaction raw material is CH 3 SiCl 3 with (CH 3 ) 3 SiCl, the reaction temperature is 150-400°C, the reaction pressure is 0.1-1.0Mpa, the reactant CH 3 SiCl 3 with (CH 3 ) 3 The feed ratio of SiCl is 1:10-1, quantitative analysis is carried out by gas chromatography after the reaction, (CH 3 ) 2SiCl 2 The quality score is 66%.
Embodiment 3
[0044] 1) γ-Al 2 o 3 preprocessing
[0045] 100g γ-Al 2 o 3 Immerse in 1M hydrochloric acid solution for 8 hours, vacuum-dry and then calcinate at 500°C for 8 hours, then seal and store after cooling down;
[0046] 2) AlCl 3 Immobilized γ-Al 2 o 3
[0047] Add 15g of anhydrous aluminum trichloride at the bottom of the fixed bed reactor first, then add the pretreated γ-Al 2 o 3 The carrier was kept at 250° C. for 12 hours, and the catalyst was taken out and sealed for future use after cooling down to room temperature in a vacuum state.
[0048] Add 100 g of the prepared solid-supported catalyst into the fixed-bed reactor, and the reaction raw material is CH 3 SiCl 3 with (CH 3 ) 3 SiCl, the reaction temperature is 150-400°C, the reaction pressure is 0.1-1.0Mpa, the reactant CH 3 SiCl 3 with (CH 3 ) 3 The feed ratio of SiCl is 1:10-1, quantitative analysis is carried out by gas chromatography after the reaction, (CH 3 ) 2 SiCl 2 The quality score is 69%.
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