CN109678114B - Method for removing arsenic impurity in electronic grade hydrochloric acid - Google Patents
Method for removing arsenic impurity in electronic grade hydrochloric acid Download PDFInfo
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- CN109678114B CN109678114B CN201910123200.9A CN201910123200A CN109678114B CN 109678114 B CN109678114 B CN 109678114B CN 201910123200 A CN201910123200 A CN 201910123200A CN 109678114 B CN109678114 B CN 109678114B
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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
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0718—Purification ; Separation of hydrogen chloride by adsorption
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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
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0712—Purification ; Separation of hydrogen chloride by distillation
Abstract
The invention discloses a method for removing arsenic impurity in electronic grade hydrochloric acid, which comprises the following steps: (1) putting the raw material concentrated hydrochloric acid into an oxidation device, adding an oxidant, and stirring at a constant speed; (2) sealing the stirred solution, and then standing; (3) adding an adsorbent to the solution; (4) taking out the adsorbent, filtering the solution, and feeding the filtered solution into an evaporation device; (5) distilling the solution at high temperature by using an evaporation device to obtain hydrogen chloride gas; (6) an absorption tank is arranged in a distillation pipeline of the evaporation device to absorb and filter the hydrogen chloride gas; (7) and (4) condensing the hydrogen chloride gas treated in the step (6) to obtain the electronic grade pure hydrochloric acid. The method can efficiently remove the arsenic impurity in the hydrochloric acid, does not bring other impurity ions in the removing process, and can produce the high-purity hydrochloric acid with the arsenic content reaching the standard on the premise of ensuring continuous and stable production.
Description
Technical Field
The invention relates to the technical field of preparation of ultrapure chemicals, and particularly relates to a method for removing arsenic impurity in electronic grade hydrochloric acid.
Background
Ultra-clean high-purity electronic chemicals are key integrated materials for manufacturing ultra-large scale integrated circuits, and the purity and cleanliness of the ultra-clean high-purity electronic chemicals have very important influences on the rate of finished products, the electrical performance, the reliability and the like. Currently, semiconductor-tip technology has reached the 7-22 nm level, and, correspondingly, the demand for purity of electronic chemicals is increasing.
The high-purity hydrochloric acid is one of electronic chemicals applied in the semiconductor manufacturing industry, is mainly applied to a standard RCA cleaning process of a silicon wafer, and is used for removing and cleaning metal and organic impurities on the surface of the silicon wafer. The purity of the hydrochloric acid determines the amount of surface metal residue remaining after cleaning, and thus determines the yield and performance of the semiconductor product.
At present, the industrial high-purity hydrochloric acid is prepared by burning high-purity hydrogen and high-purity chlorine, but in the burning process of the hydrogen and the chlorine and under the corrosivity of the chlorine, the hydrochloric acid is doped with a plurality of impurity ions in the production process, and the impurity ions must be removed to meet the requirements of the semiconductor industry.
The hydrochloric acid has low boiling point and is easy to distill, the boiling point of the hydrochloric acid is different from the salt boiling points of other impurity ions, and the impurity ions mixed in the hydrochloric acid can be removed only by distilling to meet the product requirement so as to reach the product standard. Distillation methods can remove most of the ions.
However, arsenic ions in the impurities are in a positive trivalent state in hydrochloric acid, trivalent arsenic and chloride ions form arsenic trichloride, the boiling point of the arsenic trichloride is 130.2 ℃, the temperature is very similar to that of hydrochloric acid distillation, therefore, the arsenic ions cannot be removed by a distillation method, and the product is unqualified if the impurity ions are removed by the distillation method only.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a simple and quick method for removing arsenic impurity from electronic grade hydrochloric acid, which can efficiently remove arsenic impurity from hydrochloric acid, does not bring other impurity ions in the removing process, and can produce high-purity hydrochloric acid with the arsenic content reaching the standard on the premise of ensuring continuous and stable production.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme: a method for removing arsenic impurity in electronic grade hydrochloric acid comprises the following steps:
(1) putting a raw material concentrated hydrochloric acid into an oxidation device, adding an oxidant, and stirring at a constant speed to oxidize arsenic in the hydrochloric acid;
(2) after stirring, covering a sealing cover on the oxidation device to seal the stirred solution, then standing, and adjusting the air pressure in the standing process to ensure stable air pressure;
(3) after standing, opening the cover of the oxidation device, and then adding an adsorbent into the solution to perform pressure adsorption;
(4) taking out the adsorbent, filtering the solution, and feeding the filtered solution into an evaporation device;
(5) distilling the solution at high temperature by using an evaporation device to obtain hydrogen chloride gas;
(6) an absorption tank is arranged in a distillation pipeline of the evaporation device to absorb and filter the hydrogen chloride gas;
(7) and (4) condensing the hydrogen chloride gas treated in the step (6) to obtain the electronic grade pure hydrochloric acid.
Preferably, the oxidant in step (1) is one or a mixture of more of chlorine, hypochlorous acid, hydrogen peroxide and ozone.
Preferably, in the step (1), the amount of the oxidant is 0.05-1.0% of the mass of the raw material concentrated hydrochloric acid solution, and the oxidant is an electronic grade ultrapure reagent.
Preferably, a pressure balancing device and an online pressure detection device are arranged on a sealing cover of the oxidation device so as to monitor the pressure in the oxidation device in real time.
Preferably, the stirring time in the step (1) is 30 minutes or more.
Preferably, the standing time in the step (2) is 3 hours or more.
Preferably, the adsorbent is one or a mixture of more of activated carbon, a carbon molecular sieve and a graphene nanotube.
Preferably, the dosage of the adsorbent in the step (3) is 2 to 5 percent of the mass of the raw material concentrated hydrochloric acid solution.
Preferably, the absorption tank in the step (6) is a cylindrical three-dimensional tank, and one or a mixture of more of high-purity alpha-alumina, tin ingot and titanium dioxide is added into the three-dimensional tank.
Preferably, step (7) condenses the hydrogen chloride gas using ultrapure water at 0 to 5 ℃.
The invention has the beneficial effects that: according to the invention, the oxidizing agent is added into the concentrated hydrochloric acid raw material to promote arsenic ions in the hydrochloric acid to be oxidized from trivalent to pentavalent high-boiling compounds, so that the content of arsenic ions in the hydrochloric acid gas after hydrochloric acid distillation is greatly reduced, and the arsenic impurities in the final ultrapure hydrochloric acid can be effectively removed. Meanwhile, the oxidant is selected from hydrogen peroxide, chlorine, hypochlorous acid and ozone, so that the injection of other impurity ions can be avoided, and the stability of the product quality can be ensured. The adsorbent can decompose and adsorb unreacted oxidant, and ensure the safety and stability of the production process. Meanwhile, chlorine generated in the reaction process can be absorbed by the adsorbent and the absorption tank, and the quality of the final product cannot be influenced.
Detailed Description
The following detailed description of the preferred embodiments of the present invention is provided to enable those skilled in the art to more readily understand the advantages and features of the present invention, and to clearly and unequivocally define the scope of the present invention.
Example 1
(1) Putting 1000kg of hydrochloric acid solution raw material with the concentration of 35% into an oxidation device, adding chlorine gas accounting for 0.05% of the mass of the hydrochloric acid solution raw material, and slowly and uniformly stirring by using a mechanical arm for 30min to oxidize arsenic in the hydrochloric acid; the oxidation device is a steel integrated container, the inner wall of the oxidation device is provided with a polymer lining, and the bottom of the oxidation device is provided with a substrate made of polytetrafluoroethylene;
(2) after stirring, covering a sealing cover on the oxidation device to seal the stirred solution, then standing for 3 hours, and adjusting the air pressure at any time according to the pressure value of the online pressure detection device in the standing process to ensure stable air pressure;
(3) after standing, opening a cover of the oxidation device, respectively adding an activated carbon adsorbent accounting for 2% of the mass of the raw material concentrated hydrochloric acid solution into the solution twice, filling high-purity nitrogen for pressure adsorption, and hermetically stirring for 2 hours after adding the adsorbent each time;
(4) taking out the adsorbent, filtering the solution to remove the residual adsorbent in the solution, and feeding the filtered solution into an evaporation device;
(5) distilling the solution at high temperature by using an evaporation device, wherein the distillation temperature is 130 ℃, and the pressure is controlled to be 0.25 +/-0.05 Mpa, so that hydrogen chloride gas is obtained after distillation, and arsenic ions are converted into pentavalent high-boiling compounds and cannot be distilled into gas to enter the hydrogen chloride gas;
(6) the method comprises the following steps that hydrogen chloride gas flows out along a distillation pipeline of an evaporation device at the flow rate of 450 +/-50L/h, an absorption tank is arranged in the distillation pipeline of the evaporation device to adsorb and filter the hydrogen chloride gas, wherein the absorption tank is a cylindrical three-dimensional tank, a mixture of high-purity alpha-alumina and tin ingots is added into the three-dimensional tank, and the absorption tank is made of a filtering material with the aperture of 0.1 mu m;
(7) and (4) condensing the hydrogen chloride gas treated in the step (6) by using ultrapure water at 0-5 ℃ to obtain electronic grade pure hydrochloric acid, and detecting the arsenic content of the obtained hydrochloric acid.
Example 2
(1) Putting 1000kg of hydrochloric acid solution raw material with the concentration of 35% into an oxidation device, adding hydrogen peroxide solution with the mass of 0.1% of that of the hydrochloric acid solution raw material, and slowly and uniformly stirring by using a mechanical arm for 40min to oxidize arsenic in the hydrochloric acid;
(2) after stirring, covering a sealing cover on the oxidation device to seal the stirred solution, then standing for 3 hours, and adjusting the air pressure at any time according to the pressure value of the online pressure detection device in the standing process to ensure stable air pressure;
(3) after standing, opening a cover of the oxidation device, respectively adding an activated carbon adsorbent accounting for 4% of the mass of the raw material concentrated hydrochloric acid solution into the solution twice, filling high-purity nitrogen for pressure adsorption, and hermetically stirring for 2 hours after adding the adsorbent each time;
(4) taking out the adsorbent, filtering the solution to remove the residual adsorbent in the solution, and feeding the filtered solution into an evaporation device;
(5) distilling the solution at high temperature by using an evaporation device, wherein the distillation temperature is 130 ℃, and the pressure is controlled to be 0.25 +/-0.05 Mpa, so that hydrogen chloride gas is obtained after distillation, and arsenic ions are converted into pentavalent high-boiling compounds and cannot be distilled into gas to enter the hydrogen chloride gas;
(6) the method comprises the following steps that hydrogen chloride gas flows out along a distillation pipeline of an evaporation device at the flow rate of 450 +/-50L/h, an absorption tank is arranged in the distillation pipeline of the evaporation device to adsorb and filter the hydrogen chloride gas, wherein the absorption tank is a cylindrical three-dimensional tank, a mixture of high-purity alpha-alumina and tin ingots is added into the three-dimensional tank, and the absorption tank is made of a filtering material with the aperture of 0.1 mu m;
(7) and (4) condensing the hydrogen chloride gas treated in the step (6) by using ultrapure water at 0-5 ℃ to obtain electronic grade pure hydrochloric acid, and detecting the arsenic content of the obtained hydrochloric acid.
Example 3
(1) Putting 1000kg of hydrochloric acid solution raw material with the concentration of 35% into an oxidation device, adding hypochlorous acid solution with the mass of 0.3% of that of the hydrochloric acid solution raw material, and slowly and uniformly stirring by using a mechanical arm for 50min to oxidize arsenic in the hydrochloric acid;
(2) after stirring, covering a sealing cover on the oxidation device to seal the stirred solution, then standing for 3 hours, and adjusting the air pressure at any time according to the pressure value of the online pressure detection device in the standing process to ensure stable air pressure;
(3) after standing, opening the cover of the oxidation device, respectively adding a carbon molecular sieve adsorbent accounting for 5% of the mass of the raw material concentrated hydrochloric acid solution into the solution twice, filling high-purity nitrogen for pressure adsorption, and hermetically stirring for 3 hours after adding the adsorbent each time;
(4) taking out the adsorbent, filtering the solution to remove the residual adsorbent in the solution, and feeding the filtered solution into an evaporation device;
(5) distilling the solution at high temperature by using an evaporation device, wherein the distillation temperature is 130 ℃, and the pressure is controlled to be 0.25 +/-0.05 Mpa, so that hydrogen chloride gas is obtained after distillation, and arsenic ions are converted into pentavalent high-boiling compounds and cannot be distilled into gas to enter the hydrogen chloride gas;
(6) the method comprises the following steps that (1) hydrogen chloride gas flows out along a distillation pipeline of an evaporation device at the flow rate of 450 +/-50L/h, an absorption tank is arranged in the distillation pipeline of the evaporation device to adsorb and filter the hydrogen chloride gas, wherein the absorption tank is a cylindrical three-dimensional tank, high-purity alpha-alumina is added into the three-dimensional tank, and the absorption tank is made of a filtering material with the aperture of 0.1 mu m;
(7) and (4) condensing the hydrogen chloride gas treated in the step (6) by using ultrapure water at 0-5 ℃ to obtain electronic grade pure hydrochloric acid, and detecting the arsenic content of the obtained hydrochloric acid.
Example 4
(1) Putting 1000kg of hydrochloric acid solution raw materials with the concentration of 35% into an oxidation device, adding chlorine with the mass of 0.03% of that of the hydrochloric acid solution and hypochlorous acid with the mass of 0.02% of that of the hydrochloric acid solution, and slowly and uniformly stirring by using a mechanical arm for 30min to oxidize arsenic in the hydrochloric acid;
(2) after stirring, covering a sealing cover on the oxidation device to seal the stirred solution, then standing for 3 hours, and adjusting the air pressure at any time according to the pressure value of the online pressure detection device in the standing process to ensure stable air pressure;
(3) after standing, opening the cover of the oxidation device, respectively adding a carbon molecular sieve adsorbent accounting for 5% of the mass of the raw material concentrated hydrochloric acid solution into the solution twice, filling high-purity nitrogen for pressure adsorption, and hermetically stirring for 3 hours after adding the adsorbent each time;
(4) taking out the adsorbent, filtering the solution to remove the residual adsorbent in the solution, and feeding the filtered solution into an evaporation device;
(5) distilling the solution at high temperature by using an evaporation device, wherein the distillation temperature is 130 ℃, and the pressure is controlled to be 0.25 +/-0.05 Mpa, so that hydrogen chloride gas is obtained after distillation, and arsenic ions are converted into pentavalent high-boiling compounds and cannot be distilled into gas to enter the hydrogen chloride gas;
(6) the method comprises the following steps that hydrogen chloride gas flows out along a distillation pipeline of an evaporation device at the flow rate of 450 +/-50L/h, an absorption tank is arranged in the distillation pipeline of the evaporation device to adsorb and filter the hydrogen chloride gas, wherein the absorption tank is a cylindrical three-dimensional tank, a mixture of tin ingots and titanium dioxide is added into the three-dimensional tank, and the absorption tank is made of a filtering material with the aperture of 0.1 mu m;
(7) and (4) condensing the hydrogen chloride gas treated in the step (6) by using ultrapure water at 0-5 ℃ to obtain electronic grade pure hydrochloric acid, and detecting the arsenic content of the obtained hydrochloric acid.
Example 5
(1) Putting 1000kg of hydrochloric acid solution raw material with the concentration of 35% into an oxidation device, adding ozone accounting for 0.5% of the mass of the hydrochloric acid solution and hydrogen peroxide accounting for 0.5% of the mass of the hydrochloric acid solution, and slowly and uniformly stirring by using a mechanical arm for 50min to oxidize arsenic in hydrochloric acid;
(2) after stirring, covering a sealing cover on the oxidation device to seal the stirred solution, then standing for 3 hours, and adjusting the air pressure at any time according to the pressure value of the online pressure detection device in the standing process to ensure stable air pressure;
(3) after standing, opening a cover of the oxidation device, respectively adding a graphene nanotube adsorbent accounting for 5% of the mass of the raw material concentrated hydrochloric acid solution into the solution twice, filling high-purity nitrogen for pressure adsorption, and hermetically stirring for 3 hours after adding the adsorbent each time;
(4) taking out the adsorbent, filtering the solution to remove the residual adsorbent in the solution, and feeding the filtered solution into an evaporation device;
(5) distilling the solution at high temperature by using an evaporation device, wherein the distillation temperature is 130 ℃, and the pressure is controlled to be 0.25 +/-0.05 Mpa, so that hydrogen chloride gas is obtained after distillation, and arsenic ions are converted into pentavalent high-boiling compounds and cannot be distilled into gas to enter the hydrogen chloride gas;
(6) the method comprises the following steps that hydrogen chloride gas flows out along a distillation pipeline of an evaporation device at the flow rate of 450 +/-50L/h, an absorption tank is arranged in the distillation pipeline of the evaporation device to adsorb and filter the hydrogen chloride gas, wherein the absorption tank is a cylindrical three-dimensional tank, a mixture of tin ingots and titanium dioxide is added into the three-dimensional tank, and the absorption tank is made of a filtering material with the aperture of 0.1 mu m;
(7) and (4) condensing the hydrogen chloride gas treated in the step (6) by using ultrapure water at 0-5 ℃ to obtain electronic grade pure hydrochloric acid, and detecting the arsenic content of the obtained hydrochloric acid.
Example 6
(1) Putting 1000kg of hydrochloric acid solution raw materials with the concentration of 35% into an oxidation device, adding hydrogen peroxide solution with the mass of 0.04% of that of the hydrochloric acid solution, ozone with the mass of 0.02% of that of the hydrochloric acid solution, chlorine with the mass of 0.03% of that of the hydrochloric acid solution and hypochlorous acid solution with the mass of 0.03% of that of the hydrochloric acid solution, and slowly and uniformly stirring by using a mechanical arm for 30min to oxidize arsenic in the hydrochloric acid;
(2) after stirring, covering a sealing cover on the oxidation device to seal the stirred solution, then standing for 3 hours, and adjusting the air pressure at any time according to the pressure value of the online pressure detection device in the standing process to ensure stable air pressure;
(3) after standing, opening a cover of the oxidation device, respectively adding a carbon molecular sieve adsorbent accounting for 3% of the mass of the raw material concentrated hydrochloric acid solution into the solution twice, filling high-purity nitrogen for pressure adsorption, and hermetically stirring for 3 hours after adding the adsorbent each time;
(4) taking out the adsorbent, filtering the solution to remove the residual adsorbent in the solution, and feeding the filtered solution into an evaporation device;
(5) distilling the solution at high temperature by using an evaporation device, wherein the distillation temperature is 130 ℃, and the pressure is controlled to be 0.25 +/-0.05 Mpa, so that hydrogen chloride gas is obtained after distillation, and arsenic ions are converted into pentavalent high-boiling compounds and cannot be distilled into gas to enter the hydrogen chloride gas;
(6) the method comprises the following steps that hydrogen chloride gas flows out along a distillation pipeline of an evaporation device at the flow rate of 450 +/-50L/h, an absorption tank is arranged in the distillation pipeline of the evaporation device to adsorb and filter the hydrogen chloride gas, wherein the absorption tank is a cylindrical three-dimensional tank, a mixture of tin ingots and titanium dioxide is added into the three-dimensional tank, and the absorption tank is made of a filtering material with the aperture of 0.1 mu m;
(7) and (4) condensing the hydrogen chloride gas treated in the step (6) by using ultrapure water at 0-5 ℃ to obtain electronic grade pure hydrochloric acid, and detecting the arsenic content of the obtained hydrochloric acid.
Comparative example
Adding 1000kg of 35% hydrochloric acid solution into a high temperature distillation device, preheating, and distilling at 130 deg.C under 0.25 + -0.05 MPa. The hydrogen chloride gas generated by distillation passes through a filter with the filter diameter of 0.1 μm, and is cooled and absorbed by ultrapure water at 0-5 ℃ to obtain high-purity hydrochloric acid, and the arsenic content of the obtained hydrochloric acid is detected.
The arsenic content of the hydrochloric acid obtained in examples 1 to 6 and comparative example 1 is shown in table 1 below.
Table 1 examples and comparative examples the arsenic content of hydrochloric acid
| Experimental sequences | Arsenic content (ppb) |
| Comparative example | ＞100 |
| Example 1 | ＜0.5 |
| Example 2 | ＜0.6 |
| Example 3 | ＜0.6 |
| Example 4 | ＜0.6 |
| Example 5 | ＜0.5 |
| Example 6 | ＜0.5 |
As can be seen from Table 1, the removal method of the invention can effectively remove arsenic impurities in the final ultrapure hydrochloric acid, and the whole process is simple and rapid, low in production cost, high in production efficiency and relatively environment-friendly.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (7)
1. A method for removing arsenic impurity in electronic grade hydrochloric acid is characterized by comprising the following steps:
(1) putting a raw material concentrated hydrochloric acid into an oxidation device, adding an oxidant, and stirring at a constant speed to oxidize arsenic in the hydrochloric acid; the oxidant is one or a mixture of more of chlorine, hypochlorous acid, hydrogen peroxide and ozone;
(2) after stirring, covering a sealing cover on the oxidation device to seal the stirred solution, then standing, and adjusting the air pressure in the standing process to ensure stable air pressure;
(3) after standing, opening a cover of the oxidation device, and then adding an adsorbent into the solution to perform pressure adsorption so as to remove unreacted oxidant and part of chlorine generated by oxidation; the adsorbent is one or a mixture of activated carbon and a carbon molecular sieve;
(4) taking out the adsorbent, filtering the solution, and feeding the filtered solution into an evaporation device;
(5) distilling the solution at high temperature by using an evaporation device to obtain hydrogen chloride gas;
(6) arranging an absorption tank in a distillation pipeline of the evaporation device to absorb and filter the hydrogen chloride gas so as to further remove chlorine generated in the oxidation reaction process; the absorption tank is a cylindrical three-dimensional tank, and one or a mixture of more of high-purity alpha-alumina, tin ingot and titanium dioxide is added into the three-dimensional tank;
(7) and (4) condensing the hydrogen chloride gas treated in the step (6) to obtain the electronic grade pure hydrochloric acid.
2. The method for removing arsenic impurity from electronic grade hydrochloric acid as claimed in claim 1, wherein: in the step (1), the dosage of the oxidant is 0.05-1.0% of the mass of the concentrated hydrochloric acid solution as the raw material, and the oxidant is an electronic grade ultra-pure reagent.
3. The method for removing arsenic impurity from electronic grade hydrochloric acid as claimed in claim 1, wherein: the sealing cover of the oxidation device is provided with a pressure balancing device and an online pressure detection device so as to monitor the pressure in the oxidation device in real time.
4. The method for removing arsenic impurity from electronic grade hydrochloric acid as claimed in claim 1, wherein: the stirring time in the step (1) is more than 30 minutes.
5. The method for removing arsenic impurity from electronic grade hydrochloric acid as claimed in claim 1, wherein: the standing time in the step (2) is more than 3 hours.
6. The method for removing arsenic impurity from electronic grade hydrochloric acid as claimed in claim 1, wherein: the dosage of the adsorbent in the step (3) is 2 to 5 percent of the mass of the raw material concentrated hydrochloric acid solution.
7. The method for removing arsenic impurity from electronic grade hydrochloric acid as claimed in claim 1, wherein: and (7) condensing the hydrogen chloride gas by using ultrapure water at 0-5 ℃.
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| CN111960384B (en) * | 2020-08-26 | 2022-04-12 | 浙江凯圣氟化学有限公司 | Method for removing free chlorine in hydrochloric acid |
| CN114560442A (en) * | 2022-03-28 | 2022-05-31 | 联仕(昆山)化学材料有限公司 | Purification process of electronic grade hydrochloric acid |
| CN115010091B (en) * | 2022-06-17 | 2023-10-31 | 多氟多新材料股份有限公司 | Impurity removal method for hydrogen fluoride, purification method for hydrogen fluoride and purification device for hydrogen fluoride |
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