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Method for purifying tetraethyl orthosilicate

A technology of tetraethyl orthosilicate and its purification method, which is applied in the field of purification of tetraethyl orthosilicate, and can solve the problems such as the difficulty in removing metal ultrafine particles and water molecules in tetraethyl orthosilicate

Pending Publication Date: 2019-05-10
大连恒坤新材料有限公司
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Problems solved by technology

[0002] With the development of semiconductor and integrated circuit manufacturing technology, especially after the mainstream technology enters 10 nanometers, the requirements for materials are getting higher and higher. ) has higher requirements for purity, and the existing purification process has been difficult to meet the requirements of the existing 10 nanometer process for the removal of metal ultrafine particles and water molecules in tetraethyl orthosilicate

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  • Method for purifying tetraethyl orthosilicate
  • Method for purifying tetraethyl orthosilicate

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Embodiment

[0024] Choose the orthoethyl silicate (TEOS) raw material to be purified, wherein the content of TEOS is 99.87wt%, the content of metal ultrafine ions is 0.07wt%, and the content of water molecules is 0.05wt%, described by the above-mentioned purification method Sequence and device (the first adsorption resin and the second adsorption resin are both 300nm pore size and 30 mesh macroporous adsorption resins, the first adsorption resin is polymethacrylate with functional groups as hydrogen ions, the second adsorption resin It is a polymethacrylate whose functional group is a hydroxide ion, and the weight ratio of the first adsorption resin and the second adsorption resin to the TEOS raw material is 5:100), by setting different process conditions (specifically as shown in Table 1) Shown) implement and complete purification (protection nitrogen concentration 100ppb, atmospheric pressure 0.1MPa). The results are compared as shown in Table 1 below:

[0025] Table 1

[0026]

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Abstract

The invention belongs to the field of substance purification, and particularly discloses a method for purifying tetraethyl orthosilicate. The method includes carrying out heating distillation on to-be-purified tetraethyl orthosilicate raw materials under the conditions of the temperature of 160-170 DEG C and the normal pressure; carrying out reduced-pressure distillation on obtained liquid-state fraction under the conditions of the temperature of 70-80 DEG C and the vacuum degree lower than or equal to 95 kPa; further carrying out liquefaction treatment on obtained gas-state fraction; then sequentially carrying out first resin adsorption and second resin adsorption on liquefaction treatment products under the conditions of the temperature of 20-40 DEG C and the normal pressure. First adsorption resin for the first resin adsorption is methyl methacrylate with hydrogen ions which are functional groups, and second adsorption resin for the second resin adsorption is polymethacrylate with hydroxyl ions which are functional groups. The method for purifying the tetraethyl orthosilicate has the advantages that the tetraethyl orthosilicate can be purified by the aid of the method, the purity of finished products of the method can be improved to reach the 7N level (99.99999%) or even the higher levels from the 6N level (99.9999%), and accordingly the high requirements of semiconductor manufacturing processes on materials can be met.

Description

technical field [0001] The invention belongs to the field of substance purification, and in particular relates to a method for purifying ethyl orthosilicate. Background technique [0002] With the development of semiconductor and integrated circuit manufacturing technology, especially after the mainstream technology enters 10 nanometers, the requirements for materials are getting higher and higher. ) has higher requirements for purity, and the existing purification process has been difficult to meet the requirements of the existing 10 nanometer process for the removal of metal ultrafine particles and water molecules in tetraethyl orthosilicate. Contents of the invention [0003] The present invention aims to provide a new purification method of ethyl orthosilicate. [0004] Specifically, the present invention provides a method for purifying tetraethyl orthosilicate, which comprises heating and distilling the raw orthosilicate raw material to be purified at 160-170°C under...

Claims

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Application Information

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IPC IPC(8): C07F7/04
Inventor 赵明海
Owner 大连恒坤新材料有限公司
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