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Preparation method of high-purity organosilicone monomer

A technology for organosilicon and monomers, which is applied in the field of preparation of high-purity organosilicon monomers, and can solve problems such as poor controllability of the processing process, inability to apply industrial production, and inability to guarantee

Inactive Publication Date: 2015-04-29
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method has a certain effect of removing metal ions, but requires a large amount of organic solvent as a carrier, the production yield is low, and the treatment process needs to be monitored in real time, repeated many times, the controllability of the treatment process is poor, and it cannot be applied to industrial production
[0007] Chinese patent CN102245618A discloses a method for purifying silicon compounds by adsorbing metal ions on an adsorbent. This method has a certain removal effect on specific types of metal ions, but simple physical adsorption filtration cannot guarantee the removal of all types of metal ions. , nor can it guarantee the introduction of other impurities due to the addition of adsorbent activated carbon or diatomaceous earth

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  • Preparation method of high-purity organosilicone monomer

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preparation example Construction

[0059] Preparation of High Purity Organosilicon Monomer

[0060] The present invention provides a kind of preparation method of high-purity organosilicon monomer, and described preparation method comprises the following steps:

[0061] (1) Pass the industrial organosilicon monomer through multiple rectification towers, so as to perform multiple rectification on it to obtain the first purified organosilicon monomer;

[0062] (2) Passing the first purified organosilicon monomer through the first membrane filter to perform coarse filtration to obtain the second purified organosilicon monomer;

[0063] (3) Entering the second purified organosilicon monomer into a multiple sub-boiling still, distilling it, and collecting fractions to obtain a third purified organosilicon monomer;

[0064] (4) Filtering the third purified organosilicon monomer through a second membrane filter to obtain a high-purity organosilicon monomer.

[0065] In another preferred embodiment, the organosilicon...

Embodiment 1

[0098] The preparation of embodiment 1 high-purity octamethylcyclotetrasiloxane

[0099] (1) Distillation

[0100] Under normal pressure, add industrial-grade octamethylcyclotetrasiloxane into the reaction kettle, and then conduct continuous rectification through four sets of rectification columns in series, control the split ratio and column temperature, and collect fractions at 173-175°C.

[0101] (2) Coarse filtration

[0102] Pass the collected fractions through a 0.5 μm membrane filter with a metering pump.

[0103] (3) sub-boiling distillation

[0104] Under the protection of nitrogen, continuously inject samples into the sub-boiling distiller through a metering pump, connect two groups of sub-boiling distillers in series, and raise the heating temperature to 150-155°C to collect fractions.

[0105] (4) Fine filtration

[0106] The collected fractions are passed through a 0.005 μm membrane filter by a metering pump, and then output to direct filling.

[0107] The pr...

Embodiment 2

[0108] The preparation of embodiment 2 high-purity octamethylcyclotetrasiloxane

[0109] (1) Distillation

[0110] Under normal pressure, add industrial-grade octamethylcyclotetrasiloxane into the reaction kettle, and then conduct continuous rectification through five sets of rectification columns in series, control the split ratio and column temperature, and collect fractions at 173-175°C.

[0111] (2) Coarse filtration

[0112] Pass the collected fractions through a 0.1 μm membrane filter with a metering pump.

[0113] (3) sub-boiling distillation

[0114] Under the protection of nitrogen, continuously inject samples into the sub-boiling stills through metering pumps, connect three groups of sub-boiling stills in series, and raise the heating temperature to 140-145°C to collect fractions.

[0115] (4) Fine filtration

[0116] The collected fractions are passed through a 0.005 μm membrane filter by a metering pump, and then output for direct filling.

[0117] The product...

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Abstract

The invention provides a preparation method of a high-purity organosilicone monomer and particularly relates to a method for preparing an electronic grade high-purity organosilicone monomer by carrying out the following steps on an industrial organosilicone monomer: multiple rectifying; membrane filtration; multiple sub-boiling distillation and the like. The method provided by the invention is simple in process operation and high in safety, the purity of the prepared organosilicone monomer is greater than 99.99%, the content of a single metal ion impurity is less than 0.1ppb and the density of solid particles which are greater than or equal to 0.5 micron is less than 5 / ml. Moreover, the product is stable in quality and can satisfy the preparation requirement of an ultra large scale integration circuit.

Description

technical field [0001] The invention provides a preparation method for producing high-purity organic silicon monomer, in particular to a purification method for organic silicon liquid source monomer used in the semiconductor industry. Background technique [0002] Because of its excellent dielectric properties, organosilane is an important raw material required in the VLSI manufacturing process and one of the indispensable microelectronic chemicals. The purity of organosilane products directly affects the performance of integrated circuits. The presence of impurities in products, especially metal ions, can easily lead to the generation of fault layers, thus increasing leakage current, causing breakdown and reducing the life of carriers. For nanoscale integration For electrical circuits, a few metal ions or dust particles are enough to destroy the entire circuit. Therefore, the development of VLSI requires an electronic-grade high-purity organic silicon liquid source. [00...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/21C07F7/20C07F7/18
Inventor 房强金凯凯
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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