Preparation device and preparation method of high-purity electronic-grade diiodosilane

A preparation device and electronic-grade technology, which is applied in the direction of halosilane, chemical instruments and methods, silicon compounds, etc., can solve the problems of undiscovered industrial-scale continuous production, long reaction time, and low reaction controllability, and achieve the realization of The effect of large-scale continuous operation, improving the conversion rate of raw materials, and increasing the reaction rate

Active Publication Date: 2021-10-26
福建福豆新材料有限公司
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Problems solved by technology

[0004] The synthesis and purification of diiodosilane only existed in the gram-level experimental stage in the past. Due to the problem of low reaction controllability, no reports of industrial-scale continuous production have been found.
Therefore, the by-product SiH in the crude product 3 There is a lot of I, and the conversion rate of raw ma

Method used

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  • Preparation device and preparation method of high-purity electronic-grade diiodosilane

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preparation example Construction

[0045] The embodiment of the present invention proposes a preparation method of high-purity electronic grade diiodosilane, comprising the following steps:

[0046] Nitrogen replacement: Nitrogen purging replaces the preparation device of high-purity electronic-grade diiodosilane to completely remove water and air;

[0047] Initiate the first step reaction: make a mixture of phenylsilane and oxygen-containing compound catalyst with a volume ratio of 1: (0.01-0.03), and an aromatic organic solvent, and mix the mixture for 50-200h -1 The space velocity is passed into the first reactor through the feeding port for reaction, and generates a top-down phenylsilane layer, an iodophenylsilane layer and a hydrogen iodide layer;

[0048] Control the reaction stability: continuously feed phenylsilane into the first reactor, adjust the flow of phenylsilane at the same time with the flow of the two outlets, and control the interface between the iodophenylsilane layer and the hydrogen iodide...

Embodiment 1

[0053] This embodiment proposes a high-purity electronic-grade diiodosilane preparation device, which includes a first reactor 110 , a second reactor 120 and a vacuum distillation purifier 130 connected in sequence.

[0054] The upper end of the first reactor 110 is provided with a feeding port 111 . The first reactor 110 is divided into a fluidized bed section 112 , an oil phase section 113 and a hydrogen iodide section 114 from top to bottom. The above-mentioned fluidized bed section 112 is provided with a fixed fluidized bed of iodine. The iodine fixed fluidized bed is a catalyst support plate provided with iodine particles. Among them, the oil phase section 113 is used to place an iodophenylsilane layer, or part of the phenylsilane layer (including unreacted phenylsilane, a small amount of catalyst and aromatic organic solvent that initiates the reaction), and the hydrogen iodide section 114 is used to place Hydrogen iodide layer. Due to the first step reaction of Ph-Si...

Embodiment 2

[0066] The present embodiment also proposes a preparation method of high-purity electronic grade diiodosilane, which comprises the following steps:

[0067] Nitrogen replacement: Nitrogen purging replaces the preparation device of high-purity electronic-grade diiodosilane to completely remove water and air;

[0068] Initiate the first step reaction: 10L of phenylsilane, 0.1L of oxygen-containing compound catalyst (acetone), and 12L of aromatic organic solvent (benzene) are made into a mixed solution, and the mixed solution is heated for 50h -1 The space velocity is passed into the first reactor through the feed port for reaction, and generates a top-down phenylsilane layer, an iodophenylsilane layer and a hydrogen iodide layer; in the present embodiment, the oxygen-containing compound catalyst is acetone, In other embodiments, the above-mentioned oxygen-containing compound catalyst can also be ethanol or ethyl acetate, or a mixture of at least two of acetone, ethanol and ethyl...

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Abstract

The invention provides a preparation device and a preparation method of high-purity electronic-grade diiodosilane, and relates to the technical field of diiodosilane purification. The preparation device comprises a first reactor, a second reactor and a vacuum rectification purifier. The first reactor is divided into a fluidized bed section, an oil phase section and a hydrogen iodide section; the lower ends of the oil phase section and the hydrogen iodide section are connected to the second reactor. The preparation method of the high-purity electronic-grade diiodosilane comprises the following steps: nitrogen replacement; initiating reaction by adopting phenylsilane, an oxygen-containing compound catalyst and an aromatic organic solvent to generate a phenylsilane layer, a monoiodobenzene silane layer and a hydrogen iodide layer; continuously introducing phenylsilane, adjusting the flow of the discharge port and the flow of the phenylsilane, and controlling the interface of the monoiodobenzene silane layer and the hydrogen iodide layer to be on the interface of the oil phase section and the hydrogen iodide section; and rectifying under reduced pressure. According to the preparation device and the preparation method, side reactions are reduced by isolating the contact between phenylsilane and HI, and the purity of the product and the conversion rate of raw materials are improved.

Description

technical field [0001] The invention relates to the technical field of diiodosilane purification, and in particular to a high-purity electronic-grade diiodosilane preparation device and a preparation method thereof. Background technique [0002] Diiodosilane, molecular formula SiH 2 I 2 , CAS No. 13760-02-6, referred to as DIS, is widely used in the catalytic reaction process of silylation and halosilylbenzene. [0003] With the development of semiconductor manufacturing process, diiodosilane is used as an important silicon source for chemical vapor deposition (CVD). Due to the appropriate bond angle between Si-I, the diiodosilane molecules can be arranged side by side on the surface of silicon / silicon dioxide regularly, and when ammonia gas is introduced, it can evenly react to the thickness of the molecular layer of silicon nitride, that is formed by atomic layer deposition (ALD). Moreover, under plasma enhancement, diiodosilane can generate more active silicon radical...

Claims

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Application Information

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IPC IPC(8): C01B33/107
CPCC01B33/107C01B33/10778
Inventor 马建修靖宇杜文东
Owner 福建福豆新材料有限公司
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