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Synthesis method of tetra(dimethylamino)titanium

A technology of dimethylamino and synthetic methods, which is applied in the field of compound synthesis, can solve problems such as waste of raw materials, yield, easy escape and reduction of dimethylamine, and achieve the effect of improving conversion rate and process environmental protection

Active Publication Date: 2020-08-28
苏州欣溪源新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) Dimethylamine is directly introduced into the reaction kettle or the reaction solvent. Since dimethylamine is extremely volatile, it is easy to undergo a highly active gas-liquid interface reaction, and the uncontrollable and violent exotherm of the gas-liquid interface reaction will cause The pressure in the kettle increases sharply and there is a hidden danger of explosion. At the same time, dimethylamine is easy to escape out of the reactor, resulting in a reduction in the amount of dimethylamine actually reacted, resulting in a waste of raw materials and a reduction in yield;

Method used

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  • Synthesis method of tetra(dimethylamino)titanium

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preparation example Construction

[0030] The embodiment of the present invention provides a synthesis method of tetrakis(dimethylamino)titanium, comprising the following steps:

[0031] mixing an alkane solvent and an organometallic lithium compound to prepare a first reactant;

[0032] The dimethylamine gas is exported at a gas outflow pressure of 0.12~0.15MPa, the dimethylamine gas is condensed at a temperature of -10~-20°C, and the formed dimethylamine condensate is added to the first reactant for The first reaction prepares the second reactant;

[0033] Titanium tetrachloride is added to the second reactant to carry out the second reaction, and the tetrakis(dimethylamino)titanium is prepared through post-treatment.

[0034] The synthesis of tetrakis(dimethylamino)titanium mainly includes two steps: (1) the intermediate dimethylamide lithium is generated by the reaction of dimethylamine and organometallic lithium compound; (2) the reaction of dimethylamide lithium with titanium tetrachloride Tetrakis(dime...

Embodiment 1

[0070] In this embodiment, a synthetic method of tetrakis(dimethylamino)titanium, the specific steps are as follows:

[0071] Step 1, the reaction device is a 2L reaction flask, and the reaction device is replaced three times with a vacuum / nitrogen system. Under a nitrogen atmosphere, 500 mL of n-hexane and 500 mL of n-butyllithium (2.5M) are added; the first reaction is obtained thing;

[0072] Step 2, the high-pressure gas storage device is a steel cylinder of dimethylamine gas, and the gas outflow pressure of dimethylamine gas is controlled to be 0.12 MPa by adjusting the pressure reducing valve arranged on it; the dimethylamine gas flowing out through the pressure reducing valve Through the serpentine condenser with a condensation temperature of -15°C, condensate to form a dimethylamine condensate, and slowly drop it into the reaction device to mix with the first reactant, and control the temperature in the reaction device to -20 ℃, a total of 56g of dimethylamine was int...

Embodiment 2

[0076] In this embodiment, a synthetic method of tetrakis(dimethylamino)titanium, the specific steps are as follows:

[0077] Step 1, the reaction device is a 2L reaction flask, and the reaction device is replaced three times with a vacuum / nitrogen system. Under a nitrogen atmosphere, 600 mL of n-heptane and 550 mL of n-butyllithium (2.5M) are added; the first Reactant;

[0078] Step 2, the high-pressure gas storage device is a steel cylinder of dimethylamine gas, and by adjusting the pressure reducing valve on it, the gas outflow pressure of dimethylamine gas is controlled to be 0.13MPa; the dimethylamine gas flowing out through the pressure reducing valve Through the serpentine condenser with a condensation temperature of -15°C, condensate to form a dimethylamine condensate, and slowly drop it into the reaction device to mix with the first reactant, and control the temperature in the reaction device to -20 ℃, a total of 62g of dimethylamine was introduced; after the dimethy...

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Abstract

The invention relates to a synthesis method of tetra(dimethylamino)titanium. The synthesis method comprises the following steps: mixing an alkane solvent and an organic metal lithium compound to prepare a first reactant; introducing dimethylamine gas at a gas outflow pressure of 0.12-0.15 MPa, condensing the dimethylamine gas at a temperature of -10 to -20 DEG C, and adding the formed dimethylamine condensate into the first reactant to carry out a first reaction so as to prepare a second reactant; and adding titanium tetrachloride into the second reactant to carry out a second reaction, and carrying out post-treatment to prepare the tetra(dimethylamino)titanium. The synthesis method can avoid the hidden danger of explosion and dangerous factors, can greatly reduce the generation of solid waste and liquid waste, is safe and environment-friendly, and has the advantages of high yield of the tetra(dimethylamino)titanium and convenient operation of the process.

Description

technical field [0001] The invention relates to the technical field of compound synthesis, in particular to a synthesis method of tetrakis(dimethylamino)titanium. Background technique [0002] With the continuous development of the semiconductor manufacturing industry, ALD (atomic layer deposition) technology has become one of the most ideal deposition methods for semiconductor manufacturing due to its simple operation, highly controllable deposition parameters, and excellent deposition uniformity. Finding high-k and metal gate material precursors suitable for ALD and improving the purity of materials have become critical. Tetrakis(dimethylamino)titanium, formula C 8 h 24 N 4 Ti is a compound that is very sensitive to air and water vapor, and can be dissolved in organic solvents such as alcohols, benzene, and carbon tetrachloride. Tetrakis(dimethylamino)titanium not only has good stability and high vapor pressure, but also shows quite high reactivity, and is a hot materi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/28
CPCC07F7/003
Inventor 周健黄艺
Owner 苏州欣溪源新材料科技有限公司
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