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Purification method of electronic-grade methyl phenyl diethoxy silane

A technology of methylphenyldiethoxysilane and purification method, which is applied in chemical instruments and methods, silicon organic compounds, compounds of group 4/14 elements of the periodic table, etc., and can solve problems such as the influence of integrated circuit material manufacturing , to achieve the effect of simple method

Inactive Publication Date: 2012-04-25
SHANGHAI AIMO JINSHAN PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The organosilicon raw materials used in the manufacture of integrated circuits must reach electronic grade, that is, the purity is more than 99.8%, while the general commercialized methylphenyldiethoxysilane is only 99% after ordinary purification, and contains impurity metal ions. Can seriously affect the manufacture of integrated circuit materials

Method used

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  • Purification method of electronic-grade methyl phenyl diethoxy silane
  • Purification method of electronic-grade methyl phenyl diethoxy silane
  • Purification method of electronic-grade methyl phenyl diethoxy silane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1 ton of methylphenyldiethoxysilane with a content of 99% (weight) enters the desolventization tower of the electronic grade silane refining system through a silane compressor, and the number of theoretical plates is 60. The desolventization tower adopts normal pressure operation, and the temperature at the bottom of the tower is Heating by temperature programming, gradually heating from room temperature to 100 °C. The temperature of the distillate received at the top of the tower was 66°C, which was detected as the separated solvent tetrahydrofuran. When the amount of distillate is getting smaller and smaller until it does not come out, the temperature at the top of the tower begins to rise, and the bottom of the tower has no solvent.

[0019] The methylphenyldiethoxysilane that has been desolventized flows into the deheavy rectification tower from the bottom of the tower, and the desolventization tower restarts the next batch of rectification. The weight-removing rec...

Embodiment 2

[0022] The solvent removal tower and the weight removal rectification tower are the same as in Example 1.

[0023] The methylphenyldiethoxysilane with 99% content (weight) enters the desolventization tower of the electronic-grade silane refining system through a silane compressor. Heat to 100°C. The temperature of the distillate received at the top of the tower was 66°C, which was detected as the separated solvent tetrahydrofuran. When the amount of distillate is getting smaller and smaller until it does not come out, the temperature at the top of the tower begins to rise, and the bottom of the tower has no solvent.

[0024] The methylphenyldiethoxysilane that has been desolventized flows into the deheavy rectification tower from the bottom of the tower, and the desolventization tower restarts the next batch of rectification. The weight-removing rectification tower is operated under reduced pressure, and the vacuum degree is maintained at 31mmHg. The bottom of the tower is ...

Embodiment 3

[0027] The solvent removal tower and the weight removal rectification tower are the same as in Example 1.

[0028] The methylphenyldiethoxysilane with 99% content (weight) enters the desolventization tower of the electronic-grade silane refining system through a silane compressor. Heat to 100°C. The temperature of the distillate received at the top of the tower was 66°C, which was detected as the separated solvent tetrahydrofuran. When the amount of distillate is getting smaller and smaller until it does not come out, the temperature at the top of the tower begins to rise, and the bottom of the tower has no solvent.

[0029] The methylphenyldiethoxysilane that has been desolventized flows into the deheavy rectification tower from the bottom of the tower, and the desolventization tower restarts the next batch of rectification. The weight-removing rectification tower is operated under reduced pressure, and the vacuum degree is maintained at 31mmHg. The bottom of the tower is ...

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Abstract

The invention relates to a purification method of electronic-grade methyl phenyl diethoxy silane, which adopts a rectification mode for purification. The process comprises the following steps: 1) adding methyl phenyl diethoxy silane with a content of 99% into a solvent-removing tower, removing a few of residual solvents of tetrahydrofuran from the tower top at a normal pressure and a top temperature of 66 DEG C; 2) allowing the methyl phenyl diethoxy silane after solvent removal to flow out from the tower bottom and to enter a de-heavy rectification tower for reduced-pressure distillation, wherein the area where the de-heavy rectification tower is located is a super clean room; the vacuum degree of the tower top is maintained at 31 mmHg; the temperature of the top is 117 DEG C; methyl phenyl diethoxy silane with a content of more than 99.8% is received, and high-boiling point impurities are left and discharged from the tower bottom. Both the inner wall of the de-heavy rectification tower and a receiving container are wrapped with polytetrafluoroethylene, and the fillers of the rectification tower are wrapped with polytetrafluoroethylene.

Description

technical field [0001] The invention belongs to the technical field of chemistry and chemical engineering, and in particular relates to a method for purifying electronic-grade methylphenyldiethoxysilane. Background technique [0002] Methylphenyldiethoxysilane, a colorless, flammable, irritating liquid. It is mainly used to synthesize general silicone polymers, such as the polymerization of phenyl-containing high vacuum diffusion pump oil; it can also be used to prepare specific silicone compounds as various surface treatment agents, coupling agents, crosslinking agents, etc. . [0003] With the development of VLSI manufacturing, the density of interconnect lines in the chip continues to increase, and the width and spacing of interconnect lines continue to decrease, so the parasitic effects generated by interconnect resistance (R) and capacitance (C) become more and more more and more obvious. When the development of integrated circuits enters the technology era of 0.25 m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18C07F7/20
Inventor 姜标张黎明陈君陈旭敏徐志国
Owner SHANGHAI AIMO JINSHAN PHARM CO LTD
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