Preparation method of monosilane

A technology of monosilane and silicon tetrachloride, applied in the field of inorganic synthesis, can solve the problems of low conversion rate, loss of resin active groups, low-boiling carbon impurities, etc., and achieves the effects of high conversion rate, no catalyst, and improved utilization rate

Inactive Publication Date: 2015-01-14
NINGBO UNIV
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Problems solved by technology

Chinese patent 201010563176.X reports the method of preparing monosilane by reacting citric acid with magnesium silicide, which is only suitable for small-scale production, and produces 9 tons of magnesium citrate by-product per ton of silane
[0007] Each of the above-mentioned reactions is restricted by the reaction balance, so the conversion rate of trichlorosilane into monosilane is low. According to the public documents of NASA, in the above reactions, trichlorosilane is converted into dichlorodihydro The conversion rate of silicon is about 10%, and the conversion rate of dichlorodihydrosilane to monochlorotrihydrosilane is about 10%. The document does not mention the yield of monosilane but it can be speculated that trichlorosilane undergoes a three-step reaction The equilibrium conversion to monosilane must be less than 1%
And because the reaction is carried out on a resin-supported catalyst, it is easy to cause the loss of resin active groups and the introduction of low-boiling carbon impurities

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[0032] The preparation method of monosilane of the present invention, step is as follows:

[0033] A, hydride and silicon tetrachloride are carried out metathesis reaction and make monosilane and chloride;

[0034] B, the chloride electrolysis that step a obtains obtains elemental chlorine and metallic element;

[0035] c, the elemental chlorine obtained in step b reacts with metal silicon to obtain silicon tetrachloride, the metal element reacts with hydrogen to obtain a hydride, and the obtained silicon tetrachloride and hydride return to step a;

[0036] Wherein, the hydride is sodium hydride or lithium hydride.

[0037] The metathesis reaction of silicon tetrachloride and hydride is expressed by reaction formula (1), monosilane is produced in gaseous form, chloride is precipitated in the form of solid particles, and XH is used to represent the chemical formula of hydride, and the reaction formula is:

[0038] SiCl 4 +4XH→4XCl+SiH 4 (1)

[0039] After the chloride...

Embodiment 1

[0054] Embodiment 1 adopts the inventive method to prepare monosilane

[0055] 96kg (4000mol) of sodium hydride below 100 microns was put into the reactor at one time, and then 1700kg (10000mol) of silicon tetrachloride was injected into the reactor, the temperature was raised to 50°C, and the system pressure was maintained at 0.1MPa. In the reaction, silicon tetrachloride and sodium hydride are liquid-solid reaction, and silicon tetrachloride is in liquid state. The reaction is carried out in a gap mode, and the reaction ends after about 100 hours, and the conversion rate of sodium hydride is 99.92%. A total of 22.4Nm of monosilane gas was obtained after metering 3 , Sodium chloride 234kg. Repeat above-mentioned steps 5 times, obtain the sodium chloride that is enough to be used in next step and total 1170kg. The above-mentioned sodium chloride is used for electrolysis to prepare metallic sodium and chlorine gas, and a total of 460 kg of metallic sodium and 224 Nm of chlor...

Embodiment 2

[0056] Embodiment 2 adopts the inventive method to prepare monosilane

[0057] Put 48kg (2000mol) of sodium hydride below 100 microns into the reactor at one time, then inject 255kg (1500mol) of silicon tetrachloride into the reactor, raise the temperature to 200°C, and maintain the system pressure at 3.0MPa. In the reaction, silicon tetrachloride and sodium hydride are liquid-solid reaction, and silicon tetrachloride is in liquid state. The reaction was carried out in a gap mode, and the reaction was completed after about 2 hours, and the conversion rate of sodium hydride was 99.99%. A total of 11.2Nm of monosilane gas was obtained after metering 3 , Sodium chloride 117kg. Repeat above-mentioned steps 5 times, obtain the sodium chloride that is enough to be used in next step and total 585kg. The above-mentioned sodium chloride is used for electrolysis to prepare metallic sodium and chlorine gas, and a total of 230 kg of metallic sodium and 112 Nm of chlorine gas are obtain...

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Abstract

The invention relates to a preparation method of monosilane and belongs to the technical field of inorganic synthesis. The preparation method of the monosilane comprises the following preparation steps of: a, carrying out decomposition reaction on hydride and silicon tetrachloride to obtain monosilane and chloride; b, electrolyzing the chloride obtained in step a to obtain elemental chlorine and metallic simple substance; and c, enabling the elemental chlorine obtained in step b to react with metal silicon to obtain silicon tetrachloride, enabling the metallic simple substance to react with hydrogen gas to obtain hydride, and returning the obtained tetrachloride and the hydride to step a, wherein the hydride is sodium hydride or lithium hydride. According to the preparation method of the monosilane disclosed by the invention, the by-products generated in the process flow are returned to the system while the closed-loop use of the materials is achieved, so that the utilization rate of the materials is improved, and the preparation method can be used for the large-scale production. Meanwhile, the preparation method has the advantages of being free of catalyst, high in conversion rate and the like.

Description

technical field [0001] The invention relates to a preparation method of monosilane, which belongs to the technical field of inorganic synthesis. Background technique [0002] Silane Molecular Formula SiH 4 , plays an important role in the manufacture of large-scale integrated circuits. In recent years, with the development of polysilicon industry technology, the fluidized bed polysilicon production process using monosilane as raw material has attracted much attention, which further enhances the importance of monosilane in the industrial field. sex. Therefore, the development of monosilane production process has also attracted much attention. The classic small-scale production of monosilane is the Japanese Komatsu method using magnesium silicide and ammonium chloride as raw materials. The production of 1 ton of monosilane will produce 2.1 tons of ammonia and 5.9 tons of magnesium chloride by-product. Chinese patent 201010563176.X reports the method of preparing monosilane...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/04
Inventor 赵燕
Owner NINGBO UNIV
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