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A kind of method for removing impurity ions in liquid ammonia

A technology for impurity ions and liquid ammonia, which is used in the preparation/separation of ammonia, chemical instruments and methods, ammonia compounds, etc., and can solve problems such as the difficulty of removing boron and calcium elements.

Active Publication Date: 2022-06-17
ZHEJIANG KAISN FLUOROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Boron and calcium elements can form coordination bonds with ammonia, making it difficult to remove boron and calcium elements in liquid ammonia by conventional distillation

Method used

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  • A kind of method for removing impurity ions in liquid ammonia
  • A kind of method for removing impurity ions in liquid ammonia
  • A kind of method for removing impurity ions in liquid ammonia

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A method for removing impurity ions in liquid ammonia, the scheme of which is:

[0029] Step 1: Adsorption and complexation, add 0.5kg of modified MCM-41 molecular sieve to 50kg of liquid ammonia, stir and mix evenly, add 0.1kg of polyhydric alcohol, and mix and adsorb for 2h. The method for preparing the modified MCM-41 molecular sieve for:

[0030] After taking 100-120 parts of MCM-41 molecular sieves and refluxing 300-400 parts of nitric acid at 80-90 ° C for 4-6 hours, filtered, washed with water, and dried to obtain activated MCM-41 molecular sieves;

[0031] Place 100-120 parts of activated MCM-41 molecular sieves in 500-1000 parts of ethanol aqueous solution, add 2-5 parts of γ-mercaptopropyltrimethoxysilane (KH590), stir mechanically at room temperature for 2-4 hours, filter , washed with water, and dried to obtain MCM-41 molecular sieve chemically modified by thiol groups;

[0032] 100-120 parts of sulfhydryl chemically modified MCM-41 molecular sieves were p...

Embodiment 2

[0037] A method for removing impurity ions in liquid ammonia, the scheme of which is:

[0038] Step 1: Adsorption and complexation: Add 2.5kg of modified MCM-41 molecular sieve to 65kg of liquid ammonia, stir and mix evenly, add 0.3kg of polyhydric alcohol, and mix and absorb for 3.5h. The modified MCM-41 molecular sieve is prepared The method is:

[0039] After taking 100-120kg MCM-41 molecular sieve and refluxing 300-400kg nitric acid at 80-90°C for 4-6 hours, filter, wash with water and dry to obtain MCM-41 molecular sieve after active treatment;

[0040] Place 100-120kg of activated MCM-41 molecular sieves in 500-1000kg of ethanol aqueous solution, add 2-5kg of γ-mercaptopropyltrimethoxysilane (KH590), stir mechanically at room temperature for 2-4h, filter, wash with water, and dry , to obtain MCM-41 molecular sieve chemically modified by thiol groups;

[0041] 100-120kg of sulfhydryl chemically modified MCM-41 molecular sieves were placed in 20-30kg of methyl 2-acetamid...

Embodiment 3

[0047] A method for removing impurity ions in liquid ammonia, the scheme of which is:

[0048] Step 1, adsorption and complexation, add 5kg of modified MCM-41 molecular sieve to 80kg of liquid ammonia, stir and mix evenly, add 0.5kg of polyhydric alcohol, and mix and adsorb for 5h. The preparation method of the modified MCM-41 molecular sieve is as follows: :

[0049] After taking 100-120kg MCM-41 molecular sieve and refluxing 300-400kg nitric acid at 80-90°C for 4-6 hours, filter, wash with water and dry to obtain MCM-41 molecular sieve after active treatment;

[0050] Place 100-120kg of activated MCM-41 molecular sieves in 500-1000kg of ethanol aqueous solution, add 2-5kg of γ-mercaptopropyltrimethoxysilane (KH590), stir mechanically at room temperature for 2-4h, filter, wash with water, and dry , to obtain MCM-41 molecular sieve chemically modified by thiol groups;

[0051] 100-120kg of sulfhydryl chemically modified MCM-41 molecular sieves were placed in 20-30kg of methy...

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Abstract

The invention relates to the field of chemical industry. The invention discloses a method for removing impurity ions in liquid ammonia, which includes two steps of adsorption complexation and rectification to remove impurities; two different complexing agents are used, and the effect of removing impurities is better; This method first adds a kind of modified MCM-41 molecular sieve into liquid ammonia, utilizes the organic N-containing group on the modified MCM-41 molecular sieve to form a coordination organic compound with heteroelement calcium or boron, and further boron elements can be It complexes with polyhydroxy compounds to form boron polyhydroxy complexes, which increases the boiling point of heteroelements, and finally uses rectification to effectively separate them from ammonia to obtain ultra-pure ammonia water. The modified MCM-41 molecular sieve of the present invention has the characteristics of large specific surface area and many N-containing groups, and has high complexation efficiency for the complexation of liquid ammonia heteroelements, and the immobilized N-containing groups have no volatilization Hidden dangers will not affect the quality of ultra-pure ammonia water.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for removing impurity ions in liquid ammonia. Background technique [0002] Ultra-pure ammonia water is an important electronic chemical material, and its consumption ranks third in the IC industry. It is mainly used for wafer cleaning and etching. [0003] CN101143728A relates to a production process of ultra-high-purity ammonia water, comprising the following process steps: feeding liquid ammonia in a liquid ammonia tank into a buffer tank; passing ammonia gas in the buffer tank into a first cleaning tower; The ammonia gas enters the second cleaning tower and is absorbed by deionized water into ammonia water, and releases relatively pure ammonia gas; the ammonia gas in the second cleaning tower enters the third cleaning tower and is absorbed by deionized water into ammonia water , and release ammonia gas with extremely high purity; the ammonia gas with extremely high ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01C1/02
CPCC01C1/024
Inventor 王海周黎旸童继红陈刚贺辉龙张学良程文海周涛涛卢振成蒋梁疏赵晓亚
Owner ZHEJIANG KAISN FLUOROCHEM
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