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Tri(dimethylamine)cyclopentadiene hafnium production method

A technology for cyclopentadiene, a production method, applied in the directions of bulk chemical production, chemical instruments and methods, compounds of elements of Group 4/14 of the periodic table, etc., capable of solving tris(dimethylamine)cyclopentadiene hafnium The problem of low purity, etc., can avoid the formation of by-products, improve the purity, and improve the yield.

Pending Publication Date: 2020-12-11
芯越芯(南京)电子科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the deficiencies in the prior art, the invention provides a production method for tris(dimethylamine)cyclopentadiene hafnium, which mainly solves the problem that the purity of the tris(dimethylamine)cyclopentadiene hafnium synthesized by the existing method is not high and cannot The problem of meeting people's demands

Method used

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  • Tri(dimethylamine)cyclopentadiene hafnium production method

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Experimental program
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Effect test

Embodiment 1

[0031] refer to figure 1 , three (dimethylamine) cyclopentadiene hafnium production method, comprises the following steps:

[0032] S1: Add raw materials, under the protection of an inert atmosphere, add 20-60 parts of hafnium tetrachloride to the flask; 1000-1800 parts of ionic liquid buffer solvent to facilitate the reaction of objects, and 100-300 parts of lithium salt of dimethylammonia;

[0033] S2: heating and stirring, heating during reaction, and then intermittent stirring;

[0034] S3: Purification, adding activated carbon particles to the reacted solution, fully stirring with a glass rod after adding, then filtering after standing for 10-30 minutes, collecting the filtrate to obtain high-precision tetrakis (dimethylamino) hafnium;

[0035] S4: prepare bromocyclopentane, select cyclopentane, make it react with bromine under light to obtain bromocyclopentane;

[0036] S5: To prepare cyclopentadiene, take monobromocyclopentane and heat it in the alcohol solution of so...

Embodiment 2

[0041] refer to figure 1 , three (dimethylamine) cyclopentadiene hafnium production method, comprises the following steps:

[0042] S1: Add raw materials, under the protection of an inert atmosphere, add 20-60 parts of hafnium tetrachloride to the flask; 1000-1800 parts of ionic liquid buffer solvent to facilitate the reaction of objects, and 100-300 parts of lithium salt of dimethylammonia;

[0043] S2: heating and stirring, heating during reaction, and then intermittent stirring;

[0044] S3: Purification, adding activated carbon particles to the reacted solution, fully stirring with a glass rod after adding, then filtering after standing for 10-30 minutes, collecting the filtrate to obtain high-precision tetrakis (dimethylamino) hafnium;

[0045] S4: prepare bromocyclopentane, select cyclopentane, make it react with bromine under light to obtain bromocyclopentane;

[0046] S5: To prepare cyclopentadiene, take monobromocyclopentane and heat it in the alcohol solution of so...

Embodiment 3

[0051] refer to figure 1 , three (dimethylamine) cyclopentadiene hafnium production method, comprises the following steps:

[0052] S1: Add raw materials, under the protection of an inert atmosphere, add 20-60 parts of hafnium tetrachloride to the flask; 1000-1800 parts of ionic liquid buffer solvent to facilitate the reaction of objects, and 100-300 parts of lithium salt of dimethylammonia;

[0053] S2: heating and stirring, heating during reaction, and then intermittent stirring;

[0054] S3: Purify, distill the reacted solution under reduced pressure, and collect fractions at 76-79°C / 5-9mmHg;

[0055] S4: prepare bromocyclopentane, select cyclopentane, make it react with bromine under light to obtain bromocyclopentane;

[0056] S5: To prepare cyclopentadiene, take monobromocyclopentane and heat it in the alcohol solution of sodium hydroxide to obtain cyclopentene, then react with bromine carbon tetrachloride solution to obtain o-dibromocyclopentane, and finally reheat El...

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Abstract

The invention relates to the technical field of compound production, and discloses a tris(dimethylamine)cyclopentadiene hafnium production method, which comprises: S1, adding a raw material, wherein 20-60 parts of hafnium tetrachloride, 1000-1800 parts of an ionic liquid buffer solvent, and 100-300 parts of a lithium salt of dimethylamine are added to a flask under the protection of an inert atmosphere; S2, heating and stirring, wherein heating is conducted during reaction, and then intermittent stirring is conducted; and S3, purifying, wherein activated carbon particles are added into the reacted solution, full stirring is performed with a glass rod, standing is performed for 10-30 minutes, filtering is performed, and the filtrate is collected to obtain the high-precision tetra(dimethylamino) hafnium. According to the method, reaction heat release can be reduced, generation of by-products is avoided, the yield of hafnium tetra (dimethylamino) is increased, and distillation and purification are performed after hafnium tri(dimethylamino) cyclopentadienyl is generated through reaction, so that the purity of hafnium is improved.

Description

technical field [0001] The invention relates to the technical field of compound production, in particular to a production method of tris(dimethylamine)cyclopentadiene hafnium. Background technique [0002] Tris(dimethylamino)cyclopentadienyl hafnium is liquid at room temperature, and is a compound that is very sensitive to air and water vapor. It can be dissolved in organic solvents such as hydrocarbons and carbon tetrachloride, and not only has good stability. Therefore, the physicochemical properties of tris(dimethylamino)cyclopentadienyl hafnium can be used in CVD or ALD techniques to prepare hafnium oxide thin films. [0003] In many syntheses, it generally takes two steps to introduce cyclopentadienyl groups on intermediates. The first step is to synthesize cyclopentadienyl sodium first, and then react with intermediates in the second step to finally obtain the target product, but The tri(dimethylamino)cyclopentadienyl hafnium synthesized by this method is not high in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F17/00C07F7/00C07C17/10C07C23/08C07C1/30C07C13/12C07C13/15
CPCC07F17/00C07F7/003C07C17/10C07C1/30C07C2601/08C07C2601/10C07C23/08C07C13/12C07C13/15Y02P20/54
Inventor 曹季
Owner 芯越芯(南京)电子科技有限公司
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