Method for producing dialkylaminosilane

A technology of alkylaminosilane and its manufacturing method, which is applied in chemical instruments and methods, compounds of group 4/14 elements of the periodic table, organic chemistry, etc., can solve problems such as volume efficiency reduction, and prevent runaway reactions and reduce halogen content Less, good yield effect

Inactive Publication Date: 2019-10-11
JNC CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in addition to the target dialkylaminosilane, a large amount of dialkylamine hydrochloride is by-produced. Therefore, in order to obtain the dialkylaminosilane, volume efficiency decreases due to a large amount of solvent, or filtration or decantation is required. Solid-liquid separation operation

Method used

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  • Method for producing dialkylaminosilane
  • Method for producing dialkylaminosilane
  • Method for producing dialkylaminosilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068]

[0069]

[0070] 7.66 g (0.32 mol) of magnesium and 90 g of n-heptane were placed in a 300 mL four-necked flask. While stirring, the oil bath was heated to 115° C., kept in a reflux state for 1 hour, and the solvent and moisture in the apparatus were reacted with magnesium to perform dehydration. After that, the oil bath was left to cool with ice water. 40.8 g (30 mL, 0.30 mol) of trichlorosilane (TCS) was charged in a 50 mL supply tank, and when the internal temperature dropped to 5° C., 3 mL of TCS was charged into a 300 mL four-necked flask. Dimethylamine (DMA) was supplied from the gas phase portion of the flask at a rate of 16 mL per minute while maintaining 10° C. or lower for 1 hour.

[0071]

[0072] The cooling with ice water was stopped, and the 300 mL 4-necked flask was immersed in the oil bath again, the oil temperature was set to 90° C., and the temperature of the reaction solution was heated to 80° C. or higher. During the heating, the reaction be...

Embodiment 2

[0078]

[0079]

[0080] 7.64 g (0.31 mol) of magnesium, 60 g of n-heptane, and 30 g of 1,2-dimethoxyethane (DME) were placed in a 300 mL four-necked flask. While stirring, the oil bath was heated to 115° C. and kept under reflux for 1 hour to dehydrate the solvent and moisture in the apparatus by reacting with magnesium, and then cooled with ice water. 45.0 g (32 mL, 0.33 mol) of TCS was charged into a 50 mL supply tank, and when the internal temperature dropped to 5° C., 3 mL of TCS was charged into a 300 mL four-necked flask. DMA was supplied from the gas phase portion of the flask at a rate of 37 mL per minute while maintaining 10° C. or lower for 1 hour.

[0081]

[0082]The oil bath was set at 90°C, and the temperature of the reaction solution was heated to above 80°C. During the heating, the reaction between the hydrochloride salt of DMA and magnesium occurred, but a significant rapid rise in temperature was not observed. When the internal temperature exceeded ...

Embodiment 3

[0088]

[0089]

[0090] 5.10 g (0.21 mol) of magnesium, 60 g of n-heptane, and 15 g of THF were placed in a 300 mL four-necked flask. While stirring, the oil bath was heated to 115° C. and kept under reflux for 1 hour to dehydrate the solvent and moisture in the apparatus by reacting with magnesium, and then cooled with ice water. 28.0 g (20 mL, 0.21 mol) of TCS was charged into a 50 mL supply tank, and when the internal temperature dropped to 5° C., 3 mL of TCS was charged into a 300 mL four-necked flask. While maintaining 10° C. or lower, DMA was supplied from the gas phase portion of the flask at a rate of 16 mL per minute for 1 hour.

[0091]

[0092] The oil bath was set at 90°C, and the temperature of the reaction solution was heated to above 80°C. During the heating, the reaction between the hydrochloride salt of DMA and magnesium occurred, but a significant rapid rise in temperature was not observed. When the internal temperature exceeded 80° C., TCS was adde...

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Abstract

Provided is a method for safely and efficiently producing a high-purity dialkylaminosilane. In the method, chlorosilane is fed in the presence of a metal and a dialkylamine is simultaneously fed and reacted therewith. For example, chlorosilane and a portion of a dialkylamine are fed and thereafter another portion of the dialkylamine only is fed and reacted, thereby producing a dialkylaminosilane.

Description

technical field [0001] The invention relates to a method for producing high-purity dialkylaminosilane. More specifically, it relates to a method for safely and efficiently producing dialkylaminosilane by supplying dialkylamine while supplying chlorosilane in the presence of a metal. Background technique [0002] Dialkylaminosilane is a compound having a silicon atom and a nitrogen atom in the molecule. In recent years, especially in the field of electronic information materials such as semiconductor insulating film materials and super water-repellent agents on the surface of silicon wafers, corrosion caused by chlorine is expected. High-purity products with high properties and low halogen content require a method for producing them inexpensively and efficiently. [0003] As a method for producing dialkylaminosilane, a method of synthesizing by reaction of chlorosilane and dialkylamine is known (Non-Patent Document 1). However, in addition to the target dialkylaminosilane, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/10
CPCC07F7/10C07F7/025
Inventor 田中亨
Owner JNC CORP
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