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Synthesis and purification method of high-purity silicon tetrafluoride

A technology of high-purity silicon tetrafluoride and purification method, which is applied in the field of synthesis and purification of high-purity silicon tetrafluoride, can solve the problems of low reaction selectivity, many by-products, and no further inhibition of polymerization, and achieves improved conversion. efficiency and selectivity, increasing the effectiveness of complex rectification process systems

Active Publication Date: 2019-12-24
绿菱电子材料(天津)有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to reduce production costs and increase the production of silicon tetrafluoride, although a lot of work has been done in China, it has not been really realized.
In summary, there are still deficiencies: 1. The reaction conversion rate of silicon tetrafluoride is low; 2. The reaction selectivity is low and there are many by-products; Polymerization inhibition; 4. Impurities in the complex system of azeotrope cannot be effectively removed

Method used

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  • Synthesis and purification method of high-purity silicon tetrafluoride

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Embodiment 1

[0049] The present embodiment proposes a kind of synthetic and purification method of high-purity silicon tetrafluoride, and it comprises the following steps:

[0050] Step S1: 1000 kg of sodium fluorosilicate is pretreated; specifically, the sodium fluorosilicate is evacuated and heat-treated at 150° C. at the same time.

[0051] Step S2: The above-mentioned sodium fluorosilicate is subjected to cracking reaction in a reactor with a volume of 1000 L to prepare silicon tetrafluoride crude material; the specific cracking reaction conditions are: pressure 0.06MPa, temperature 400°C, reactor product outlet operation Flow control is 25 kg / h.

[0052] Step S3: removing trace moisture and acid gas in the first adsorption section;

[0053] Step S4: remove and inhibit polymerization of fluorosilicone in the second adsorption section; wherein, the removal and inhibition of fluorosilicone in the second adsorption section uses fluorinated resin, and the fluorinated resin is made of silv...

Embodiment 2

[0057] The present embodiment proposes a kind of synthetic and purification method of high-purity silicon tetrafluoride, and it comprises the following steps:

[0058] Step S1: 800 kg of barium fluorosilicate is pretreated; specifically, the barium fluorosilicate is evacuated and heat-treated at 100° C. at the same time.

[0059] Step S2: The above-mentioned barium fluorosilicate is subjected to cracking reaction in a reactor with a volume of 800L to prepare silicon tetrafluoride crude material; the specific cracking reaction conditions are: pressure 0.1MPa, temperature 300°C, reactor product outlet operating flow rate 20 kg / h, the reactor volume is 800 L.

[0060] Step S3: removing trace moisture and acid gas in the first adsorption section;

[0061] Step S4: remove and inhibit polymerization of fluorosilicone ether in the second adsorption section; wherein, fluorinated resin is used for removal and inhibition of fluorosilicone ether in the second adsorption section, and the...

Embodiment 3

[0065] The present embodiment proposes a kind of synthetic and purification method of high-purity silicon tetrafluoride, and it comprises the following steps:

[0066] Step S1: 400 kg of potassium fluorosilicate is pretreated; specifically, the potassium fluorosilicate is evacuated and heat-treated at 200° C. at the same time.

[0067]Step S2: The above-mentioned potassium fluorosilicate is subjected to cracking reaction in a reactor with a volume of 500 L to prepare silicon tetrafluoride crude material; the specific cracking reaction conditions are: pressure 0.02MPa, temperature 500°C, reactor product outlet operation Flow rate: 10kg / h, reactor volume: 500 L.

[0068] Step S3: removing trace moisture and acid gas in the first adsorption section;

[0069] Step S4: remove and inhibit polymerization of fluorosilicone ether in the second adsorption section; wherein, fluorinated resin is used for removal and inhibition of fluorosilicone ether in the second adsorption section, and...

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Abstract

The invention provides a synthesis and purification method of high-purity silicon tetrafluoride. The method for synthesizing and purifying high-purity silicon tetrafluoride comprises the following steps: pretreatment fluosilicate; carrying out cracking reaction on fluosilicate to prepare a silicon tetrafluoride coarse material; trace moisture and acid gas are removed in the first adsorption section; carrying out removal and polymerization inhibition control on fluorosilicone ether in a second adsorption section; separating the light components from the heavy components in the rectification section; and separating azeotrope impurities through a complex rectification section. According to the synthesis and purification method of high-purity silicon tetrafluoride provided by the invention, heating cracking, adsorption unit operation, rectification and complex rectification are scientifically combined, fluorosilicone ether is removed by adopting an adsorption unit, and a complex rectification process is added after conventional rectification unit operation to remove azeotrope.

Description

technical field [0001] The invention relates to the fields of chemical engineering, separation engineering and electronic special gases, and in particular to a method for synthesizing and purifying high-purity silicon tetrafluoride. Background technique [0002] Silicon tetrafluoride (SiF 4 ) has the highest proportion of silicon atoms (about 27%) among tetrahalosilane compounds, stable Si-F chemical bond energy (541.0 kJ / mol), and non-flammable and non-explosive characteristics. Silicon tetrafluoride exhibits unique physical and chemical properties in the high-depth and wide, large-capacity silicon / silicon oxide and metal interlayer insulating layer processing technology of the new generation of chip manufacturing. Silicon tetrafluoride and N 2 O, O 2 、SiH 4 and H 2 The chemical deposition rate of 300-500 nm / min can be achieved by using other gases together, and a wide and thick SiO can be obtained in a limited time 2 Insulation. In addition, silicon tetrafluoride ca...

Claims

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Application Information

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IPC IPC(8): C01B33/107
CPCC01B33/10705C01B33/10778C01P2006/80Y02P20/10
Inventor 马建修王新鹏杜文东张杰崔录芳
Owner 绿菱电子材料(天津)有限公司
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