Method for removing metal impurities in organosilicon compounds

A technology of organosilicon compounds and metal impurities, which is applied in the direction of silicon organic compounds, etc., to achieve the effect of simplifying operations and reducing production costs

Active Publication Date: 2017-12-29
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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  • Abstract
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  • Application Information

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Problems solved by technology

[0009] In view of the above-mentioned shortcoming of the prior art, the purpose of the present invention is to provide a method for removing metal impurities in organosilicon compounds, which is used to solve the problem of trace metals in organosiloxanes, especially cyclopolysiloxanes, in the prior art. The problem of impurities

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  • Method for removing metal impurities in organosilicon compounds
  • Method for removing metal impurities in organosilicon compounds

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Embodiment 1

[0045]Provide industrial grade octamethylcyclotetrasiloxane (purity 98.0%), the main organosilicon impurities are hexamethylcyclotrisiloxane, etc., and the total metal ion content is 6.5ppm. 2000g of industrial grade octamethylcyclotetrasiloxane, 1000g of isopropanol and 10g of silica gel SiliaMets TAAcONa were added to the rectification kettle 12, and stirred at normal temperature and pressure for 3h. Vacuumize to a vacuum degree of 20KPa, raise the temperature of the magnetic stirring heater to 50°C, and collect the fraction at the top of the tower at 30-50°C in the receiving bottle 15 . After no fraction flows out, the temperature of the magnetic stirring heater is raised to 150° C., and the 80-105° C. fraction at the top of the tower is collected in the receiving bottle 16 . After the temperature of the overhead fraction is stabilized at 106° C., the fraction at the top of the tower at 106° C. is collected in the receiving bottle 17 . Sampling analysis shows that the puri...

Embodiment 2

[0047] Provide industrial grade trifluoropropylcyclotrisiloxane (purity 98.5%), the main organosilicon impurities are high boiling point organosiloxane, etc., and the total metal ion content is 3.2ppm. Add 1500g of technical grade trifluoropropylcyclotrisiloxane, 800g of acetone and 8g of activated carbon into the rectification kettle 12, raise the temperature of the magnetic stirring heater to 40°C under normal pressure and stir for 3h. The temperature of the magnetic stirring heater was raised to 70° C., and the 50-60° C. distillate at the top of the tower was collected in the receiving bottle 15 . After no fraction flows out, vacuumize to a vacuum degree of 4.5KPa, raise the temperature of the magnetic stirring heater to 160° C., and collect the fraction at 60-136° C. at the top of the tower in the receiving bottle 16 . After the temperature of the overhead fraction is stabilized at 137° C., the fraction at the top of the tower at 137° C. is collected in the receiving bottl...

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Abstract

The invention provides a method for removing metal impurities in organosilicon compounds, the method comprising the following steps: (1) mixing the organosilicon compound to be purified with a predetermined ratio of metal adsorbent and polar solvent to form a mixture; (2) Stir for a certain period of time at a certain temperature and normal pressure; (3) Increase the heating temperature in stages, under a certain degree of vacuum, vaporize and then condense the mixture, and collect the fractions of different stages in different receiving bottles. The invention solves the problem that organic impurities and metal impurities are difficult to remove in the preparation process of high-purity organosiloxane, especially the removal of trace metal ions in cyclopolysiloxane, so that the content of organic and metal impurities in organosiloxane reaches High-purity semiconductor grade. At the same time, the method combines dissolution, adsorption and rectification to complete the purification process of the organosiloxane in one step, thereby simplifying the operation and reducing the production cost.

Description

technical field [0001] The invention belongs to the field of preparation of high-purity semiconductor-grade organosilicon, and in particular relates to the purification of organosilicon compounds and a method for removing metal impurities in organosilicon compounds. Background technique [0002] As the size of integrated circuit chips decreases, deposited films with lower dielectric constants are key to advanced semiconductor manufacturing because they allow metal lines to be packed more closely on a chip without electrical gaps between adjacent layers. There is less risk of signal leakage. In the semiconductor manufacturing process, organosilicon compounds, such as tetramethylsilane, dimethyldimethoxysilane, octamethylcyclotetrasiloxane, trifluoropropylcyclotrisiloxane, etc., can be used as low dielectric Raw material of constant deposited film. [0003] However, the above commercially available silicone materials usually contain quite high concentrations of different met...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/21
Inventor 王万军袁京杜丽萍黄祚刚姜标
Owner SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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