Method for producing electronic-grade ammonium fluoride water solution

A technology of ammonium fluoride and aqueous solution, which is applied in the direction of ammonium fluoride, chemical instruments and methods, ammonium halide, etc., which can solve problems such as unstable product quality, high impurity content, and large fluctuations in purity, and reduce reaction by-products , Improve the quality and high purity effect

Active Publication Date: 2012-07-11
SHANGAI HUAYI MICROELECTRONICS MATERIAL +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the disadvantages of high energy consumption, complex operation, unstable product quality and large fluctuations in purity in the prior art for producing electronic-grade ammonium fluoride aqueous solution, the invention provides a method for producing electronic-grade ammonium fluoride aqueous solution, which comprises ammonia gas After pretreatment, high-purity ammonia gas is produced, and then absorbed by hydrofluoric acid cycle to obtain the target product
Because the pretreatment removes the impurities in the raw materials, and the reaction is carried out in a cyclic absorption mode to quickly discharge the heat released in the reaction process and reduce the generation of by-products, so the method is simple to operate and the product quality is stable, which overcomes the problem of the existing method. Defects with high impurity content and unstable quality

Method used

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  • Method for producing electronic-grade ammonium fluoride water solution
  • Method for producing electronic-grade ammonium fluoride water solution
  • Method for producing electronic-grade ammonium fluoride water solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The industrial-grade liquid ammonia with a concentration of 75% is transported from the industrial-grade liquid ammonia raw material tank 1 to the heating filter 2, the industrial-grade liquid ammonia is heated to 40°C to generate ammonia gas, and the ammonia gas is passed through the The adsorber 3 of woody raw material powdered activated carbon removes organic gas impurities, and then deoxidizes through the deoxygenating adsorber 4 to produce high-purity ammonia gas.

[0034] The high-purity ammonia gas that makes passes into above reactor 5 with the flow rate of 10kg / h, with the high-purity hydrofluoric acid circulation absorption reaction of concentration 40% that passes into from reactor below high-purity hydrofluoric acid inlet 6, condensed water Cool down. After passing the test, the target product ammonium fluoride aqueous solution is collected and stored in the finished product tank 7.

[0035] The concentration of the obtained ammonium fluoride aqueous soluti...

Embodiment 2

[0037] Referring to the method described in Example 1.

[0038] Heating industrial-grade liquid ammonia with a concentration of 80% to 50°C produces ammonia gas, and removes organic gas impurities through an adsorber equipped with sawdust raw material powder activated carbon at 0.12MPa, and then passes through a deoxygenation adsorber to produce high-purity ammonia gas .

[0039] The generated high-purity ammonia gas is passed into the reaction vessel at a flow rate of 13kg / h, and the 50% concentration of high-purity hydrofluoric acid is used to circulate and absorb the reaction, and the condensed water is cooled to lower the temperature. After passing the test, collect the target product ammonium fluoride aqueous solution.

[0040] The concentration of the ammonium fluoride aqueous solution obtained was 50%, the detected metal ion impurity content was 0.1 ppm, and the dust particles larger than 0.5 μm were 3 / ml. The specific inspection results are shown in Table 1.

Embodiment 3

[0042] Referring to the method described in Example 1.

[0043] Heating industrial-grade liquid ammonia with a concentration of 90% to 55°C produces ammonia gas, and removes organic gas impurities through an adsorber equipped with powdered activated carbon of high-quality coal raw materials at 0.15 MPa, and then passes through a deoxygenation adsorber to obtain high-purity Ammonia.

[0044] The generated high-purity ammonia gas is passed into the reaction vessel at a flow rate of 510kg / h, and the high-purity hydrofluoric acid with a concentration of 55% is used to circulate and absorb the reaction, and the condensed water is cooled to lower the temperature. After passing the test, collect the target product ammonium fluoride aqueous solution.

[0045] The obtained ammonium fluoride aqueous solution has a concentration of 55%, the detected metal ion impurity content is less than 0.1 ppm, and the dust particles larger than 0.5 μm are 3 / ml. The specific inspection results are s...

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Abstract

The invention relates to a method for producing electronic-grade ammonium fluoride water solution. The method comprises the steps of taking industrial liquid ammonia as a raw material, heating the raw material to release ammonia; adsorbing and removing organic gas impurity in the ammonia by using active carbon; obtaining high-purity ammonia by deoxidizing adsorption; absorbing the high-purity ammonia by high-purity hydrofluoric acid, and then obtaining the electronic product grade ammonium fluoride water solution. The obtained electronic-grade ammonium fluoride water solution has high purity and stable quality, and can be directly used for producing electronic products. The method of the invention for producing electronic-grade ammonium fluoride water solution has a simple operation, and is suitable for continuously large-scale production.

Description

technical field [0001] The invention relates to a method for producing an aqueous ammonium fluoride solution, in particular to a method for producing an electronic-grade ammonium fluoride aqueous solution with simple operation. Background technique [0002] Ammonium fluoride has good etching ability, so it is widely used in the production process of electronic products. With the rapid development of the electronics industry, the demand for electronic grade ammonium fluoride is increasing, and the requirements for the purity of ammonium fluoride are also increasing. high. [0003] The traditional production process of electronic grade ammonium fluoride is the liquid phase method, that is, the reaction of hydrogen fluoride (or hydrofluoric acid) and ammonia water (or liquid ammonia), then cooling and crystallization, centrifugal dehydration, and drying to obtain the finished product. The method has long production cycle, high labor intensity, serious pollution, high energy co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01C1/16
CPCC01C1/162C01C1/024C01P2004/62C01P2006/80
Inventor 詹家荣周励
Owner SHANGAI HUAYI MICROELECTRONICS MATERIAL
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