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High-purity SiCl4 purification method

A purification method and high-purity technology, applied in the direction of silicon halide compounds, halosilanes, etc., can solve the problems such as difficult separation of azeotrope impurities, achieve the effect of eliminating particle dust, eliminating polluted products, and overcoming poor strength

Active Publication Date: 2013-08-14
杨恺
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is in order to solve the high-purity SiCl that existing method prepares 4 Azeotrope, boron-containing phosphorus and OH compound impurities are difficult to separate technical problems, providing a high-purity SiCl 4 Purification method

Method used

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specific Embodiment approach 1

[0035] Specific implementation mode one: the high-purity SiCl of this implementation mode 4 The purification method is as follows:

[0036] 1. The crude SiCl 4 , cuprous chloride or zinc chloride and inorganic salts are added to the reaction kettle, and the crude SiCl 4 The azeotrope reacts with the inorganic salt under the catalysis of cuprous chloride or zinc chloride for 20-60min, and the inorganic salt is Na 2 CO 3 or K 2 CO 3 , the dosage of cuprous chloride or zinc chloride is crude SiCl 4 0.01%-0.1% of the mass, the amount of inorganic salt added is based on the crude SiCl 4 The azeotrope content is determined to be 100.1%-102% of the azeotrope mass, and the reaction obtains a high boiling point mixture;

[0037] 2. The product of step 1 is pumped into the atmospheric rectification tower 1 through a canned pump, the heavy components are discharged from the bottom of the tower, and the light components are discharged from the top of the tower, SiCl 4 The crude re...

specific Embodiment approach 2

[0042] Specific embodiment two: the difference between this embodiment and specific embodiment one is that the adsorbent filled in the adsorption column described in step three is silica gel modified by silane coupling agent γ-chloropropyl-triethoxysilane , Silane coupling agent γ-chloropropyl-trimethoxysilane modified silica gel, silane coupling agent γ-chloropropyl-dimethoxyethoxysilane modified silica gel or silane coupling agent γ-chloro Propyl-methoxydiethoxysilane modified silica gel. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0043] Embodiment 3: This embodiment differs from Embodiment 1 or Embodiment 2 in that the degree of vacuum described in Step 5 is -0.03MPa. Others are different from the first or second specific embodiment.

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Abstract

The invention discloses a high-purity SiCl4 purification method, relates to a SiCl4 purification method, and is used for solving the technical problem that azeotrope and compound impurities containing boron, phosphorus and OH in high-purity SiCl4 prepared by the existing method are difficult to separate. The method disclosed by the invention comprises the following steps of: 1, chemical reaction; 2, rectification under normal pressure; 3, adsorption; 4, rectification under normal pressure; 5, treatment by a reduced pressure rectifying tower; and 6, storage of pure SiCl4 in a product tank under protection of high-purity nitrogen or argon, thus finishing purification of high-purity SiCl4, wherein in the step 3, an adsorbent filled in an adsorption column is an silica gel adsorbent modified by a silane coupling agent. SiCl4 purified by the method is low in production cost, the purity of ordinary-grade SiCl4 is up to 99.9999%, and the purity of fiber-grade SiCl4 is up to 99.99999999%. The method disclosed by the invention can perform continuous production, and is high in productivity. The high-purity SiCl4 purification method belongs to the field of crude product purification.

Description

technical field [0001] The present invention relates to a SiCl 4 Purification method. Background technique [0002] The electronic information industry is an important industry in the 21st century, and optical fiber communication has gradually become an important way of information transmission due to its large transmission capacity, long transmission distance, small attenuation, and strong anti-interference ability, and is one of the pillars of the future information industry. In recent years, China's optical fiber demand has surpassed that of the United Kingdom, and it is the third largest country after the United States and Japan. China has become the largest optical fiber manufacturing country. Optical fiber preform is the raw material of optical fiber, which plays a vital role in the performance and quality of optical fiber. In 2007, the domestic demand for optical fiber preform reached 20 million kilometers, in 2009 it reached 80 million kilometers, and in 2012 it re...

Claims

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Application Information

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IPC IPC(8): C01B33/107
Inventor 杨恺
Owner 杨恺
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