CN110589770A - Preparation method of electronic-grade hydrofluoric acid - Google Patents
Preparation method of electronic-grade hydrofluoric acid Download PDFInfo
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- CN110589770A CN110589770A CN201911038160.4A CN201911038160A CN110589770A CN 110589770 A CN110589770 A CN 110589770A CN 201911038160 A CN201911038160 A CN 201911038160A CN 110589770 A CN110589770 A CN 110589770A
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- hydrofluoric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/19—Fluorine; Hydrogen fluoride
- C01B7/191—Hydrogen fluoride
- C01B7/195—Separation; Purification
- C01B7/196—Separation; Purification by distillation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/19—Fluorine; Hydrogen fluoride
- C01B7/191—Hydrogen fluoride
- C01B7/195—Separation; Purification
- C01B7/197—Separation; Purification by adsorption
Abstract
The invention discloses a preparation method of electronic grade hydrofluoric acid, which comprises the following preparation steps: (1) preparing high-purity hydrogen fluoride gas; (2) preparing high-purity water; (3) and (3) feeding the high-purity hydrogen fluoride gas prepared in the step (1) and the high-purity water prepared in the step (2) into an absorption tower, fully contacting and absorbing the hydrogen fluoride gas and the high-purity water in the absorption tower to prepare a high-purity hydrofluoric acid crude product, and carrying out ultra-clean filtration on the crude product to obtain electronic hydrofluoric acid. The preparation method has simple process, can effectively remove the arsenic impurity in the hydrogen fluoride raw material under the action of the strong oxidant, thereby improving the concentration and the yield of the hydrofluoric acid, and the strong oxidant can be used for distillation and purification alone or can be selected to be distilled and purified in sequence, thereby improving the purity of the hydrogen fluoride; the use of high purity water can improve the quality of hydrofluoric acid.
Description
Technical Field
The invention relates to the field of hydrofluoric acid, in particular to a preparation method of electronic-grade hydrofluoric acid.
Background
With the shift of semiconductor chip manufacturing industry and LCD manufacturing industry to China, the usage amount of domestic electronic hydrofluoric acid will increase dramatically, and the electronic hydrofluoric acid market will undoubtedly have a wide development prospect. The electronic grade hydrofluoric acid is a colorless transparent liquid, is weakly acidic, has strong pungent smell and has strong corrosivity. Electronic grade hydrofluoric acid has a wide range of applications for etching and cleaning in the manufacture of large scale integrated circuit chips, solar cells, LEDs and TET-LCD panels, atomic energy industrial chemicals. Electronic grade hydrofluoric acid is mainly used for cleaning and corroding Integrated Circuit (IC) and very large scale integrated circuit (VLSI) chips, is one of key basic chemical materials in the manufacturing process of the microelectronic industry, and can also be used as an analytical reagent and for preparing high-concentration fluorine-containing chemicals.
At present, electronic grade hydrofluoric acid can be prepared by processes such as rectification, sub-boiling distillation, gas absorption and the like, and distillation equipment used in the distillation process is generally made of precious metals such as platinum, gold, silver and the like or polytetrafluoroethylene materials due to the strong corrosivity of the hydrofluoric acid, so that the equipment is quite expensive and the production cost is very high. The most common domestic process route is rectification, and the process is approximately as follows: acid raw material → chemical treatment → continuous rectification → ultra-clean filtration → split charging of finished product → packaging.
However, the key impurity in hydrofluoric acid is arsenic, the impurity arsenic in the raw material generally exists in a trivalent state, and the boiling point of AsF3 is not greatly different from that of hydrofluoric acid, so that the separation effect of the arsenic is not ideal only by rectification.
Disclosure of Invention
The invention aims to provide a preparation method of electronic grade hydrofluoric acid, which solves the problems that arsenic impurities are difficult to separate and remove and the concentration of hydrofluoric acid is low through a distillation process in the prior art.
In order to solve the technical problems, the invention is realized by the following technical scheme:
a preparation method of electronic grade hydrofluoric acid comprises the following preparation steps:
(1) preparing high-purity hydrogen fluoride gas: pumping industrial anhydrous hydrogen fluoride into a degassing tower in a continuous mode, removing trace low-boiling-point substances, then feeding the industrial anhydrous hydrogen fluoride into a rectifying tower, adding a strong oxidant into the rectifying tower, rectifying and purifying to obtain high-purity hydrogen fluoride gas, and discharging tower bottom liquid to prepare industrial hydrofluoric acid;
(2) preparing high-purity water: removing most of anions and cations from tap water through an anion-cation exchange column, filtering the tap water through a microporous filter to obtain common deionized water, further purifying the deionized water by adopting multistage reverse osmosis and electrodialysis membrane treatment, and finally sterilizing and performing ultrafiltration to obtain high-purity water;
(3) and (3) feeding the high-purity hydrogen fluoride gas prepared in the step (1) and the high-purity water prepared in the step (2) into an absorption tower, fully contacting and absorbing the hydrogen fluoride gas and the high-purity water in the absorption tower to prepare a high-purity hydrofluoric acid crude product, and carrying out ultra-clean filtration on the crude product to obtain electronic hydrofluoric acid.
Preferably, the strong oxidant in the step (1) is potassium permanganate or hydrogen peroxide or a combination of the potassium permanganate and the hydrogen peroxide.
Preferably, the strong oxidant is a combination of potassium permanganate and hydrogen peroxide, and the weight ratio of the potassium permanganate to the hydrogen peroxide is 1: 1.
Preferably, in the step (3), the charged weight ratio of the high-purity hydrogen fluoride to the high-purity water is 1 to 1.2: 1.
Preferably, in the step (3), the charged weight ratio of the high-purity hydrogen fluoride to the high-purity water is 1.02 to 1.08: 1.
Preferably, the degassing column in the step (1) is lined with tetrafluoroethylene.
Preferably, the absorption column in the step (3) is lined with tetrafluoroethylene.
The invention has the beneficial effects that: the preparation method has simple process, can effectively remove the arsenic impurity in the hydrogen fluoride raw material under the action of the strong oxidant, thereby improving the concentration and the yield of the hydrofluoric acid, and the strong oxidant can be used for distillation and purification alone or can be selected to be distilled and purified in sequence, thereby improving the purity of the hydrogen fluoride; the use of high purity water can improve the quality of hydrofluoric acid.
Detailed Description
The following further describes the embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
A preparation method of electronic grade hydrofluoric acid comprises the following preparation steps:
(1) preparing high-purity hydrogen fluoride gas: pumping industrial anhydrous hydrogen fluoride into a degassing tower lined with tetrafluoroethylene in a continuous mode, removing trace low-boiling-point substances, then feeding the low-boiling-point substances into a rectifying tower, adding potassium permanganate into the rectifying tower, wherein the adding amount of the potassium permanganate is 0.005% of that of the industrial anhydrous hydrogen fluoride, performing rectification and purification to obtain high-purity hydrogen fluoride gas, and discharging tower bottom liquid to prepare industrial-grade hydrofluoric acid;
(2) preparing high-purity water: removing most of anions and cations from tap water through an anion-cation exchange column, filtering the tap water through a microporous filter to obtain common deionized water, further purifying the deionized water by adopting multistage reverse osmosis and electrodialysis membrane treatment, and finally sterilizing and performing ultrafiltration to obtain high-purity water;
(3) and (2) feeding the high-purity hydrogen fluoride gas prepared in the step (1) and the high-purity water prepared in the step (2) into an absorption tower lined with tetrafluoroethylene, wherein the input weight ratio of the high-purity hydrogen fluoride to the high-purity water is 1:1, fully contacting and absorbing the hydrogen fluoride gas and the high-purity water in the absorption tower to prepare a hydrofluoric acid crude product with the concentration of 52%, and carrying out ultra-clean filtration on the crude product to obtain electronic grade hydrofluoric acid with the concentration of 50%.
Example 2
A preparation method of electronic grade hydrofluoric acid comprises the following preparation steps:
(1) preparing high-purity hydrogen fluoride gas: pumping industrial anhydrous hydrogen fluoride into a degassing tower lined with tetrafluoroethylene in a continuous mode, removing trace low-boiling-point substances, then feeding the low-boiling-point substances into a rectifying tower, adding hydrogen peroxide into the rectifying tower, wherein the addition amount of the hydrogen peroxide is 0.005% of that of the industrial anhydrous hydrogen fluoride, performing rectification and purification to obtain high-purity hydrogen fluoride gas, and discharging tower bottom liquid to prepare industrial-grade hydrofluoric acid;
(2) preparing high-purity water: removing most of anions and cations from tap water through an anion-cation exchange column, filtering the tap water through a microporous filter to obtain common deionized water, further purifying the deionized water by adopting multistage reverse osmosis and electrodialysis membrane treatment, and finally sterilizing and performing ultrafiltration to obtain high-purity water;
(3) and (2) feeding the high-purity hydrogen fluoride gas prepared in the step (1) and the high-purity water prepared in the step (2) into an absorption tower lined with tetrafluoroethylene, wherein the input weight ratio of the high-purity hydrogen fluoride to the high-purity water is 1.2:1, fully contacting and absorbing the hydrogen fluoride gas and the high-purity water in the absorption tower to prepare a hydrofluoric acid crude product with the concentration of 51%, and carrying out ultra-clean filtration on the crude product to obtain electronic grade hydrofluoric acid with the concentration of 50.5%.
Example 3
A preparation method of electronic grade hydrofluoric acid comprises the following preparation steps:
(1) preparing high-purity hydrogen fluoride gas: pumping industrial anhydrous hydrogen fluoride into a degassing tower lined with tetrafluoroethylene in a continuous mode, removing trace low-boiling-point substances, then feeding the low-boiling-point substances into a rectifying tower, adding potassium permanganate into the rectifying tower, wherein the adding amount of the potassium permanganate is 0.005 percent of the adding amount of the industrial anhydrous hydrogen fluoride, performing primary rectification purification, adding hydrogen peroxide, the adding amount of the hydrogen peroxide is also 0.005 percent of the adding amount of the industrial anhydrous hydrogen fluoride, performing secondary rectification purification to obtain high-purity hydrogen fluoride gas, and discharging tower bottom liquid to prepare industrial-grade hydrofluoric acid;
(2) preparing high-purity water: removing most of anions and cations from tap water through an anion-cation exchange column, filtering the tap water through a microporous filter to obtain common deionized water, further purifying the deionized water by adopting multistage reverse osmosis and electrodialysis membrane treatment, and finally sterilizing and performing ultrafiltration to obtain high-purity water;
(3) and (2) feeding the high-purity hydrogen fluoride gas prepared in the step (1) and the high-purity water prepared in the step (2) into an absorption tower lined with tetrafluoroethylene, wherein the input weight ratio of the high-purity hydrogen fluoride to the high-purity water is 1.04:1, fully contacting and absorbing the hydrogen fluoride gas and the high-purity water in the absorption tower to prepare a hydrofluoric acid crude product with the concentration of 55%, and carrying out ultra-clean filtration on the crude product to obtain electronic grade hydrofluoric acid with the concentration of 51%.
Example 4
A preparation method of electronic grade hydrofluoric acid comprises the following preparation steps:
(1) preparing high-purity hydrogen fluoride gas: pumping industrial anhydrous hydrogen fluoride into a degassing tower lined with tetrafluoroethylene in a continuous mode, removing trace low-boiling-point substances, then feeding the low-boiling-point substances into a rectifying tower, adding potassium permanganate into the rectifying tower, wherein the adding amount of the potassium permanganate is 0.005 percent of the adding amount of the industrial anhydrous hydrogen fluoride, performing primary rectification purification, adding hydrogen peroxide, the adding amount of the hydrogen peroxide is also 0.005 percent of the adding amount of the industrial anhydrous hydrogen fluoride, performing secondary rectification purification to obtain high-purity hydrogen fluoride gas, and discharging tower bottom liquid to prepare industrial-grade hydrofluoric acid;
(2) preparing high-purity water: removing most of anions and cations from tap water through an anion-cation exchange column, filtering the tap water through a microporous filter to obtain common deionized water, further purifying the deionized water by adopting multistage reverse osmosis and electrodialysis membrane treatment, and finally sterilizing and performing ultrafiltration to obtain high-purity water;
(3) and (2) feeding the high-purity hydrogen fluoride gas prepared in the step (1) and the high-purity water prepared in the step (2) into an absorption tower lined with tetrafluoroethylene, wherein the input weight ratio of the high-purity hydrogen fluoride to the high-purity water is 1.02:1, fully contacting and absorbing the hydrogen fluoride gas and the high-purity water in the absorption tower to prepare a hydrofluoric acid crude product with the concentration of 53%, and carrying out ultra-clean filtration on the crude product to obtain electronic grade hydrofluoric acid with the concentration of 51.5%.
Example 5
A preparation method of electronic grade hydrofluoric acid comprises the following preparation steps:
(1) preparing high-purity hydrogen fluoride gas: pumping industrial anhydrous hydrogen fluoride into a degassing tower lined with tetrafluoroethylene in a continuous mode, removing trace low-boiling-point substances, then feeding the low-boiling-point substances into a rectifying tower, adding potassium permanganate into the rectifying tower, wherein the adding amount of the potassium permanganate is 0.005 percent of the adding amount of the industrial anhydrous hydrogen fluoride, performing primary rectification purification, adding hydrogen peroxide, the adding amount of the hydrogen peroxide is also 0.005 percent of the adding amount of the industrial anhydrous hydrogen fluoride, performing secondary rectification purification to obtain high-purity hydrogen fluoride gas, and discharging tower bottom liquid to prepare industrial-grade hydrofluoric acid;
(2) preparing high-purity water: removing most of anions and cations from tap water through an anion-cation exchange column, filtering the tap water through a microporous filter to obtain common deionized water, further purifying the deionized water by adopting multistage reverse osmosis and electrodialysis membrane treatment, and finally sterilizing and performing ultrafiltration to obtain high-purity water;
(3) and (2) feeding the high-purity hydrogen fluoride gas prepared in the step (1) and the high-purity water prepared in the step (2) into an absorption tower lined with tetrafluoroethylene, wherein the input weight ratio of the high-purity hydrogen fluoride to the high-purity water is 1.08:1, fully contacting and absorbing the hydrogen fluoride gas and the high-purity water in the absorption tower to prepare a hydrofluoric acid crude product with the concentration of 53%, and carrying out ultra-clean filtration on the crude product to obtain electronic grade hydrofluoric acid with the concentration of 50%.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (7)
1. A preparation method of electronic-grade hydrofluoric acid is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
(1) preparing high-purity hydrogen fluoride gas: pumping industrial anhydrous hydrogen fluoride into a degassing tower in a continuous mode, removing trace low-boiling-point substances, then feeding the industrial anhydrous hydrogen fluoride into a rectifying tower, adding a strong oxidant into the rectifying tower, rectifying and purifying to obtain high-purity hydrogen fluoride gas, and discharging tower bottom liquid to prepare industrial hydrofluoric acid;
(2) preparing high-purity water: removing most of anions and cations from tap water through an anion-cation exchange column, filtering the tap water through a microporous filter to obtain common deionized water, further purifying the deionized water by adopting multistage reverse osmosis and electrodialysis membrane treatment, and finally sterilizing and performing ultrafiltration to obtain high-purity water;
(3) and (3) feeding the high-purity hydrogen fluoride gas prepared in the step (1) and the high-purity water prepared in the step (2) into an absorption tower, fully contacting and absorbing the hydrogen fluoride gas and the high-purity water in the absorption tower to prepare a high-purity hydrofluoric acid crude product, and carrying out ultra-clean filtration on the crude product to obtain electronic hydrofluoric acid.
2. The method for preparing electronic grade hydrofluoric acid according to claim 1, wherein: the strong oxidant in the step (1) is potassium permanganate or hydrogen peroxide or the combination of the potassium permanganate and the hydrogen peroxide.
3. The method for preparing electronic grade hydrofluoric acid according to claim 2, wherein: the strong oxidant is a combination of potassium permanganate and hydrogen peroxide, and the weight ratio of the potassium permanganate to the hydrogen peroxide is 1: 1.
4. The method for preparing electronic grade hydrofluoric acid according to claim 1, wherein: the input weight ratio of the high-purity hydrogen fluoride to the high-purity water in the step (3) is 1-1.2: 1.
5. The method for preparing electronic grade hydrofluoric acid according to claim 4, wherein: the input weight ratio of the high-purity hydrogen fluoride to the high-purity water in the step (3) is 1.02-1.08: 1.
6. The method for preparing electronic grade hydrofluoric acid according to claim 1, wherein: tetrafluoroethylene is lined in the degassing tower in the step (1).
7. The method for preparing electronic grade hydrofluoric acid according to claim 1, wherein: and (4) lining tetrafluoroethylene in the absorption tower in the step (3).
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111994874A (en) * | 2020-09-03 | 2020-11-27 | 福建天甫电子材料有限公司 | Preparation method of electronic-grade hydrofluoric acid |
| CN112897467A (en) * | 2021-03-18 | 2021-06-04 | 福建省建阳金石氟业有限公司 | Production method of electronic-grade hydrofluoric acid |
| CN114712877A (en) * | 2022-04-15 | 2022-07-08 | 南京佳华工程技术有限公司 | Method and equipment for preparing electronic grade gas by adopting thermal coupling technology |
| CN116425124A (en) * | 2023-04-19 | 2023-07-14 | 天津中科拓新科技有限公司 | Preparation method of electronic grade ultra-clean high-purity acid |
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