A kind of preparation method of high-purity silane
A silane and high-purity technology, applied in the field of high-purity silane preparation, can solve the problems of cumbersome silane production operations, low product purity, high energy consumption, etc., achieve significant economic and environmental benefits, high purity of by-products, and low energy consumption Effect
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Embodiment 1
[0033] The preparation method of the high-purity silane of the present embodiment comprises the following steps:
[0034] 1) Dissolve 500g sodium in 600g liquid ammonia to form a mixed solution;
[0035] 2) Put the mixed liquid obtained in step 1) in a closed reaction kettle with a stirring and cooling device, fill the reaction kettle with inert gas for gas replacement until the moisture in the gas in the reaction kettle is ≤10ppm, O 2 ≤20ppm;
[0036] 3) Under stirring conditions, the H 2 and 1000g of SiF 4 Continuously and evenly pass into the reactor, and react with the mixed solution for 4 hours to obtain crude silane;
[0037] 4) Adsorb and rectify the crude silane obtained in step 3) to obtain the high-purity silane.
[0038] Wherein, the pressure of the reactor in steps 2) and 3) is kept at 2.5MPa. The temperature in the reaction kettle in steps 2) and 3) was kept at 30°C.
[0039] The adsorption in step 4) is carried out through a packed tower, and the packing in...
Embodiment 2
[0042] The preparation method of the high-purity silane of the present embodiment comprises the following steps:
[0043] 1) Dissolve 500g sodium in 600g liquid ammonia to form a mixed solution;
[0044] 2) Put the mixed liquid obtained in step 1) in a closed reaction kettle with a stirring and cooling device, fill the reaction kettle with inert gas for gas replacement until the moisture in the gas in the reaction kettle is ≤10ppm, O 2 ≤20ppm;
[0045] 3) Under stirring conditions, the H 2 and 1000g of SiF 4 Continuously and evenly pass into the reactor, and react with the mixed solution for 3 hours to obtain crude silane;
[0046] 4) Adsorb and rectify the crude silane obtained in step 3) to obtain the high-purity silane.
[0047] Wherein, the pressure of the reactor in steps 2) and 3) is kept at 1.0 MPa. In steps 2) and 3), liquid nitrogen was used to keep the temperature inside the reactor at 100°C.
[0048] The adsorption in step 4) is carried out through a packed to...
experiment example 3
[0051] The preparation method of the high-purity silane of the present embodiment, as figure 1 shown, including the following steps:
[0052] 1) Dissolve 1100g sodium in 1200g liquid ammonia to form a mixed solution;
[0053] 2) Put 600g of the mixed solution obtained in step 1) into a closed reaction kettle 1 with a stirring and cooling device, and place the rest in a closed reaction kettle 2 with a stirring and cooling device, and fill the reaction with inert gas Carry out gas replacement in kettle 1 and reactor 2, until the moisture in the gas in reactor 1 and reactor 2≤10ppm, O 2 ≤20ppm;
[0054] 3) Under stirring conditions, the H 2 and 2000g of SiF 4 Continuously and evenly pass into the reactor 2, first SiF 4 React with the mixed liquid in Reactor 2; in Reactor 2, most of the SiF 4 converted to SiH 4 , almost all of the Na reacts completely; the remaining SiF 4 Use the pressure difference to enter the reactor 1 and continue to react with the mixed solution in th...
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