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Slag slurry recycling method in cold hydrogenation process and recycling system used in slag slurry recycling method

A technology of cold hydrogenation and slag slurry, applied in chemical instruments and methods, zirconium halides, aluminum halides, etc., can solve the problems of not considering silicon powder, catalyst recycling, reducing the recycling rate of chlorosilanes, increasing production costs, etc., to achieve The effect of improving comprehensive utilization rate, eliminating environmental pollution and reducing labor intensity

Inactive Publication Date: 2020-12-29
XINTE ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This treatment method not only reduces the recycling rate of chlorosilane, increases the production cost, but also produces a large amount of industrial waste, which causes a lot of environmental protection costs for enterprises.
In the prior art, for the slurry produced by cold hydrogenation, the chlorosilane liquid in the slurry is mainly recovered, and the recycling of silicon powder and catalyst in the slurry is not considered, resulting in a great waste of resources

Method used

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  • Slag slurry recycling method in cold hydrogenation process and recycling system used in slag slurry recycling method

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Effect test

Embodiment 1

[0043] This embodiment provides a method for recycling slag in a cold hydrogenation process, comprising the following steps:

[0044] Separating the slurry in the cold hydrogenation process from solid to liquid to obtain separated solids and separated liquids, the solids include silicon and catalyst cuprous chloride and / or nickel chloride, and the liquids include chlorosilanes;

[0045] Heating the separated solid with zircon sand, carbonaceous reducing agent, and chlorine gas, the zircon sand, carbonaceous reducing agent, and chlorine gas react under the catalysis of cuprous chloride in the solid to form zirconium tetrachloride and silicon tetrachloride , Carbon monoxide, silicon in the solid reacts with chlorine to form silicon tetrachloride.

[0046] This embodiment also provides a recycling system used in the above-mentioned slurry recycling method in the cold hydrogenation process, including:

[0047]The solid-liquid separation device is used for solid-liquid separation ...

Embodiment 2

[0051] Such as figure 1 As shown, this embodiment provides a recycling system used in the slurry recycling method in the cold hydrogenation process, including:

[0052] The solid-liquid separation device is used for solid-liquid separation of the slurry in the cold hydrogenation process to obtain separated solids and separated liquids. The solids include: silicon and metal chlorides, and the metal chlorides include catalyst cuprous chloride And / or nickel chloride, liquid comprises chlorosilane; Wherein, solid comprises the silicon of 30~60mas%, the metal chloride of 35~55mas%, wherein metal chloride comprises catalyst cuprous chloride and / or nickel chloride, catalyst Cuprous chloride and / or nickel chloride account for 15-25mas% of the total solid mass.

[0053] It should be noted that the solid-liquid separation device in this embodiment includes:

[0054] Suspension separator 1, used for suspension separation of the slurry in the cold hydrogenation process, to obtain separa...

Embodiment 3

[0082] This embodiment provides a method for recycling slurry in the cold hydrogenation process using the system in Embodiment 2, the difference from the system in Embodiment 2 is:

[0083] The heating temperature is 1100~1200℃

[0084] The mass ratio of zircon sand, carbonaceous reducing agent and separated solid is 26:8.4:7. The mass ratio of heat supplement to separated solid is 0.2:1

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Abstract

The invention discloses a slag slurry recycling method in a cold hydrogenation process and a slag slurry recycling system used in the method. The slag slurry recycling method in the cold hydrogenationprocess comprises the following steps: carrying out solid-liquid separation on slag slurry in the cold hydrogenation process to respectively obtain separated solid and separated liquid, wherein the solid comprises silicon and a catalyst cuprous chloride, and the liquid comprises chlorosilane; heating the separated solid with zircon sand, a carbonaceous reducing agent and chlorine, reacting the zircon sand, the carbonaceous reducing agent and the chlorine under the catalysis of cuprous chloride in the solid to generate zirconium tetrachloride, silicon tetrachloride and carbon monoxide, and reacting silicon in the solid with the chlorine to generate silicon tetrachloride. The slag slurry in the cold hydrogenation process is applied to the zirconium tetrachloride production process, on one hand, chlorosilane, silicon and the catalyst in the slag slurry are completely recycled and reused, the comprehensive utilization rate of the slag slurry is increased, on the other hand, heat supplementing of the zirconium tetrachloride chlorination reaction is achieved, and energy consumption is reduced.

Description

technical field [0001] The invention belongs to the technical field of polysilicon production, and in particular relates to a method for recycling slag in a cold hydrogenation process and a used recycling system. Background technique [0002] Cold hydrogenation technology has become the mainstream process of trichlorosilane production due to its low energy consumption and large production capacity. In the cold hydrogenation reaction process, in order to increase the conversion rate of silicon tetrachloride, a transition metal catalyst such as a copper-based or nickel-based catalyst is also added in the reaction process. During the reaction process, the catalyst and silicon powder are taken out of the reactor along with the chlorosilane. In addition, in the cold hydrogenation reaction, a certain amount of chlorosilane high boilers will inevitably be generated. This kind of high boiling matter enters the cooling system at the back end together with silicon powder and catalyst...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/107C01G25/04C01B32/40C01G3/05C01G53/09C01G49/10C01F7/56
CPCC01B33/1071C01B33/10726C01G25/04C01B32/40C01G3/05C01G53/09C01G49/10C01F7/56
Inventor 武珠峰刘兴平银波范协诚宋高杰
Owner XINTE ENERGY