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Synthesis method of tetra (dimethylamino) zirconium

The technology of a dimethylamino group and a synthesis method, which is applied in the field of organic synthesis, can solve the problems of potential safety hazards, dangerous chemical reagents, large waste liquids and the like in the chemical industry, and achieve the effects of shortening the production cycle, improving the safety and reducing the cost.

Active Publication Date: 2021-10-29
苏州源展材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This preparation method requires the use of n-butyllithium, and n-butyllithium is an extremely dangerous chemical reagent that will spontaneously ignite when exposed to air, which is a major safety hazard for the chemical industry
In addition, industrial-grade n-butyl lithium products are generally diluted in alkane solvents, and a large amount of waste liquid will be generated during the production process

Method used

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  • Synthesis method of tetra (dimethylamino) zirconium
  • Synthesis method of tetra (dimethylamino) zirconium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Use a vacuum / nitrogen system to replace the gas in the 2 L reaction flask three times. Under a high-purity nitrogen atmosphere, add 1000 mL of n-hexane and 100 g of zirconium tetrachloride to the reaction flask to obtain the first reactant; control the reaction The temperature in the device is -10°C, and 78 g of dimethylamine gas is passed into the first reactant, and reacted at room temperature for 3 hours to obtain the second reactant; the temperature in the reaction device is controlled to be -10°C, and the 163 g of diethylamine was added to the second reactant, and then reacted at room temperature for 3 hours; after the reaction was completed, the reactant was distilled under reduced pressure, and the fraction at 80°C / 0.1 mmHg was collected to obtain 104 g of tetrakis(dimethylamino) ) zirconium, the yield is 91%.

[0030] figure 1 NMR spectrum of tetrakis(dimethylamino)zirconium prepared for this example. NMR: 1 H NMR (300 MHz, C 6 D. 6 ) : 2.98(s, 24H).

Embodiment 2

[0032] Use a vacuum / nitrogen system to replace the gas in the 2 L reaction flask three times. Under a high-purity nitrogen atmosphere, add 1000 mL of n-hexane and 110 g of zirconium tetrachloride to the reaction flask to obtain the first reactant; control the reaction The temperature in the device is -15°C, and 88 g of dimethylamine gas is passed into the first reactant, and reacted at room temperature for 5 hours to obtain the second reactant; the temperature in the reaction device is controlled to be -10°C, and the Add 262 g of di-n-propylamine to the second reactant, and then react at room temperature for 4 hours; after the reaction is completed, the reactant is distilled under reduced pressure, and the fraction at 80°C / 0.1 mmHg is collected to obtain 120 g of tetrakis(dimethylamino ) zirconium, the yield is 95%.

[0033] NMR: 1 H NMR (300 MHz, C 6 D. 6 ) : 2.98(s, 24H).

Embodiment 3

[0035] Use a vacuum / argon system to replace the gas in the 2 L reaction flask three times. Under the high-purity argon atmosphere, add 1000 mL of n-heptane and 100 g of zirconium tetrachloride to the reaction flask to obtain the first reactant ; Control the temperature in the reaction device to be-20°C, feed 81 g of dimethylamine gas into the first reactant, and react at room temperature for 6 hours to obtain the second reactant; control the temperature in the reaction device to be-10°C, Add 247 g of diisopropylamine to the second reactant in the device, and react at room temperature for 4 hours; after the reaction is completed, the reactant is distilled under reduced pressure, and the fraction at 80° C. / 0.1 mmHg is collected to obtain 107 g of tetra(diisopropylamine) Methylamino) zirconium, the yield is 93%.

[0036] NMR: 1 H NMR (300 MHz, C 6 D. 6 ) : 2.98(s, 24H).

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Abstract

The invention discloses a synthetic method of tetra (dimethylamino) zirconium, which comprises the following steps: (1) mixing zirconium tetrachloride with an alkane solvent in a protective atmosphere to obtain a mixed solution; (2) introducing dimethylamine into the mixed solution at -20 DEG C to -10 DEG C, and reacting to obtain a reaction solution; (3) adding dialkylamine into the reaction solution at the temperature of 120 DEG C to -10 DEG C, and reacting; wherein the dialkylamine is diethylamine, di-n-propylamine, diisopropylamine, di-n-butylamine or diisobutylamine; and (4) carrying out reduced pressure distillation and collecting fractions to obtain the tetra (dimethylamino) zirconium. According to the synthetic method of the tetra (dimethylamino) zirconium, provided by the invention, an organic metal compound which is spontaneously combusted in air and has an extremely high operation danger coefficient does not need to be used, so that the production safety is greatly improved; meanwhile, the raw material cost can be effectively reduced, the generation of waste liquid is reduced, the production period of the tetra (dimethylamino) zirconium is shortened, the yield is improved, and large-scale production is facilitated.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for synthesizing tetrakis(dimethylamino)zirconium. Background technique [0002] The feature size of semiconductor devices decreases with the development of integrated circuits, and the traditional gate material is mainly SiO 2 , when the thickness of the gate dielectric is less than 2 nm, direct electron tunneling and high leakage current seriously hinder the reliability of the device. These problems can be solved by increasing the physical thickness of the gate dielectric while maintaining the same gate capacitance. ZrO 2 compared to SiO 2 have a higher dielectric constant (ZrO 2 :25, SiO 2 :3.9), as a high-k material just meets the needs of the contemporary IC industry. [0003] Tetrakis(dimethylamino)zirconium is one of the common sources of zirconium. The current relatively mature preparation method is to first react dimethylamine and n-butyllithium...

Claims

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Application Information

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IPC IPC(8): C07C209/00C07C209/06C07C211/65
CPCC07C209/00C07C209/06C07C211/65
Inventor 周健
Owner 苏州源展材料科技有限公司