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The synthetic method of tetrakis(dimethylamino)titanium

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

Active Publication Date: 2020-11-20
苏州欣溪源新材料科技有限公司
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  • Abstract
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  • Claims
  • Application Information

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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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  • The synthetic method of tetrakis(dimethylamino)titanium

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preparation example Construction

[0030] The embodiment of the invention provides a synthesis method of tetra (dimethylamino) titanium, which comprises the following steps:

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

[0032] Leading out dimethylamine gas at a gas outflow pressure of 0.12~0.15MPa, condensing the dimethylamine gas at a temperature of-10--20 DEG C, and adding the formed dimethylamine condensate into the first reactant for a first reaction to prepare a second reactant;

[0033] Adding titanium tetrachloride into the second reactant for a second reaction, and preparing the tetra (dimethylamino) titanium through post-treatment.

[0034] The synthesis of tetra (dimethylamino) titanium mainly includes two steps: (1) Dimethylamine reacts with organometallic lithium compounds to produce intermediate lithium dimethylamino; (2) lithium dimethylamino reacts with titanium tetrachloride to obtain tetra (dimethylamino) titanium.

[0035] In step (1), specif...

Embodiment 1

[0070] In this embodiment, a method for synthesizing tetra (dimethylamino) titanium comprises the following specific steps:

[0071] 1, the reaction device is a 2L reaction bottle, which is replaced by a vacuum / nitrogen system for three times, and 500mL of n-hexane and 500mL of n-butyl lithium (2.5m) are added in the nitrogen atmosphere; Obtaining a first reactant;

[0072] Secondly, the high-pressure gas storage device is a dimethylamine gas steel cylinder, and the gas outflow pressure of dimethylamine gas is controlled to be 0.12MPa； by adjusting a pressure reducing valve arranged on the high-pressure gas storage device; The dimethylamine gas flowing out of the pressure reducing valve passes through a serpentine condenser with a condensation temperature of -15℃, condenses to form dimethylamine condensate, and slowly drops into the reaction device to mix with the first reactant, controlling the temperature in the reaction device to -20℃, and introducing 56g； of dimethylamine in t...

Embodiment 2

[0076] In this embodiment, a method for synthesizing tetra (dimethylamino) titanium comprises the following specific steps:

[0077] 1, the reaction device is a 2L reaction bottle, which is replaced by a vacuum / nitrogen system for three times, and 600mL of n-heptane and 550mL of n-butyl lithium (2.5m) are added in the nitrogen atmosphere; Obtaining a first reactant;

[0078] Secondly, the high-pressure gas storage device is a dimethylamine gas steel cylinder, and the gas outflow pressure of dimethylamine gas is controlled to be 0.13MPa； by adjusting a pressure reducing valve arranged on the high-pressure gas storage device; The dimethylamine gas flowing out of the pressure reducing valve passes through a serpentine condenser with a condensation temperature of -15℃, condenses to form dimethylamine condensate, and slowly drops into the reaction device to mix with the first reactant, controlling the temperature in the reaction device to -20℃, and introducing 62g； dimethylamine in tot...

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Abstract

The invention relates to a synthesis method of tetrakis(dimethylamino)titanium. The synthesis method comprises the following steps: mixing an alkane solvent and an organometallic lithium compound to prepare a first reactant; deriving dimethylamine gas at a gas outflow pressure of 0.12-0.15 MPa, and dissolving the dimethylamine gas at -10-20 Condensation at a temperature of °C, adding the formed dimethylamine condensate to the first reactant for the first reaction to prepare the second reactant; adding titanium tetrachloride to the second reactant for the second reaction , preparing the tetrakis(dimethylamino)titanium after post-treatment. The synthesis method can avoid the above-mentioned hidden dangers of explosion and risk factors, and may greatly reduce the generation of solid waste and liquid waste, which is safe and environmentally friendly. At the same time, the yield of tetrakis(dimethylamino)titanium is high, and the process is easy to operate.

Description

Technical field [0001] The invention relates to the technical field of compound synthesis, in particular to a synthesis method of tetra (dimethylamino) titanium. technical background [0002] With the continuous development of semiconductor manufacturing, ALD (atomic layer deposition) technology has become one of the most ideal deposition methods for semiconductor manufacturing because of its simple operation, highly controllable deposition parameters and excellent deposition uniformity. It is very important to find precursors of high-k and metal gate materials suitable for ALD, and to improve the purity of materials. Tetra (dimethylamino) titanium, molecular formula c 8 H 24 N 4 Ti, a compound that is very sensitive to air and water vapor, can be dissolved in organic solvents such as alcohols, benzene and carbon tetrachloride. Tetra (dimethylamino) titanium not only has good stability, high vapor pressure, but also shows high reactivity, which is a hot material in the research f...

Claims

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Application Information

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Patent Type & Authority Patents(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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