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Method for preparing electronic grade hydrazine hydrate by purifying hydrazine hydrate

A technology of hydrazine hydrate and electronic grade, which is applied in the field of purifying commercial hydrazine hydrate to prepare electronic grade hydrazine hydrate, which can solve the problems of not being able to use integrated circuits and not reaching such a high level

Inactive Publication Date: 2019-03-12
YIBIN HAIFENG HERUI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] According to the existing industrial hydrazine hydrate product standard HG / T 3259-2012, metal ions such as iron and heavy metals (calculated as Pb) in hydrazine hydrate products are only required to be no more than 0.0005%, that is, 5000ppb, and the existing industrial hydrazine hydrate Most of the metal content in the hydrazine hydrate is 3000-5000ppb. Such hydrazine hydrate will not affect its many uses, but it cannot be used in integrated circuits, because if it is used in integrated circuits, hydrazine hydrate is required to be an electronic grade chemical reagent, and electronic High-grade chemical reagents usually require metal impurities to be at the ppb level. Obviously, the existing industrial-grade hydrazine hydrate cannot meet such high requirements, so it must be purified again
[0013] At present, there is no case involving the preparation of electronic-grade hydrazine hydrate in the prior art, so it is necessary to conduct in-depth research on electronic-grade hydrazine hydrate

Method used

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  • Method for preparing electronic grade hydrazine hydrate by purifying hydrazine hydrate

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Embodiment 1

[0032] A method for purifying hydrazine hydrate to prepare electronic grade hydrazine hydrate, comprising the steps of: first reserve commercial hydrazine hydrate, the concentration of hydrazine hydrate in the commercial hydrazine hydrate is 80%, and its metal ion content is 3500ppb after determination, and then the commercial hydrazine hydrate is hydrated Hydrazine continuously passes through a chelating resin column made of plexiglass, and the temperature of the control system is 40°C. The chelating resin used is a styrene resin as a skeleton and connected with -CH 2 N(CH 2 COOH) 2 The structure is made of special functional groups, the diameter of the chelating resin column is 5cm, the height is 80cm, and the volume of a single resin column is 0.00157m 3 , the average flow rate of commercial hydrazine hydrate is 245ml per minute, and the total flow rate is 430L. After the hydrazine hydrate passes through the chelating resin column, it is filtered through a ceramic micropor...

Embodiment 2

[0036] A method for purifying hydrazine hydrate to prepare electronic grade hydrazine hydrate, comprising the steps of: first reserve commercial hydrazine hydrate, the concentration of hydrazine hydrate in the commercial hydrazine hydrate is 80%, and its metal ion content is 4550ppb after determination, and then the commercial hydrazine hydrate is hydrated Hydrazine continuously passes through a chelating resin column made of plexiglass, and the temperature of the system is controlled at 60 ° C. The chelating resin used is a styrene resin as a skeleton and connected with -CH 2 N(CH 2 COOH) 2 The structure is made of special functional groups, the diameter of the chelating resin column is 5cm, the height is 80cm, and the volume of a single resin column is 0.00157m 3 , the average flow rate of commercial hydrazine hydrate is 245ml per minute, and the total flow rate is 200L. After the hydrazine hydrate passes through the chelating resin column, it is filtered through a ceramic ...

Embodiment 3

[0040] A method for purifying hydrazine hydrate to prepare electronic grade hydrazine hydrate, comprising the steps of: first reserve commercial hydrazine hydrate, the concentration of hydrazine hydrate in the commercial hydrazine hydrate is 80%, and its metal ion content is 4550ppb after determination, and then the commercial hydrazine hydrate is hydrated Hydrazine continuously passes through a chelating resin column made of plexiglass, and the temperature of the control system is 45°C. The chelating resin used is a divinylbenzene resin as a skeleton and is connected with -CH 2 N(CH 2 COOH) 2 The structure is made of special functional groups, the diameter of the chelating resin column is 5cm, the height is 80cm, and the volume of a single resin column is 0.00157m 3 , the average flow rate of commercial hydrazine hydrate is 245ml per minute, and the total flow rate is 430L. After the hydrazine hydrate passes through the chelating resin column, it is filtered through a cerami...

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Abstract

The invention discloses a method for preparing electronic grade hydrazine hydrate by purifying hydrazine hydrate, relating to the technical field of chemical purification. The method comprises the following steps: enabling a commodity hydrazine hydrate to pass through chelate resin firstly with a system controlled to be 40-60 DEG C and then pass through a filter with a pore size of 0.05 mu m to obtain qualified electronic grade hydrazine hydrate; the chelate resin is formed by taking a crosslinked polymer as a skeleton and connecting with a special functional group with a -CH2N(CH2COOH)2 structure. The electronic grade hydrazine hydrate product prepared by the invention is extremely low in metal ion content, has appropriate particle sizes, does not have a color, has very good quality, andthus is fully applicable to the field of integrated circuits.

Description

technical field [0001] The invention relates to the technical field of chemical purification, in particular to a method for preparing electronic-grade hydrazine hydrate by purifying commercial hydrazine hydrate. Background technique [0002] Hydrazine hydrate, also known as: hydrazine hydrate, chemical formula is N 2 h 4 ·H 2 O, a strong reducing agent, is an important chemical raw material, and is also a raw material for medicine, pesticides, dyes, foaming agents, developers, antioxidants, etc.; it is mainly used for boiler water deoxidation, high-purity metal production, and organic compound synthesis. And reduction, separation of rare elements, and also used in the manufacture of rocket fuel and explosives. With the advancement of technology and the development of society, the application fields of hydrazine hydrate are also expanding in recent years. [0003] Hydrazine hydrate is very suitable for production and use on integrated circuits (ICs) because of its strong r...

Claims

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Application Information

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IPC IPC(8): C01B21/16
CPCC01B21/16
Inventor 陈尚思柴进祥杨郭金永奎舒帮会刘志明罗浩
Owner YIBIN HAIFENG HERUI
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