Modified activated carbon and method for removing hydrogen fluoride in metal fluoride electron gas

Abstract

The invention discloses a method for removing hydrogen fluoride in metal fluoride electron gas by purifying modified activated carbon, which comprises the following steps: acidifying the activated carbon to remove oxides in the activated carbon; the acidified activated carbon is washed with water and then dried at a high temperature, finally, fluoride is loaded on the dried activated carbon, modified activated carbon is obtained, and hydrogen fluoride in the metal fluoride electronic gas is removed through the modified activated carbon. The method is easy to operate, compared with a traditional method for removing hydrogen fluoride, the efficiency is greatly improved, the technological process is simple, the raw material yield is high, and wide application prospects are achieved.

Description

Technical Field

[0001] The present invention belongs to the technical field of chemical engineering, and particularly relates to a modified activated carbon and a method for removing hydrogen fluoride from metal fluoride electronic gas. Background Art

[0002] As one of the widely used semiconductor materials, metal fluoride electronic gas mainly benefits from its excellent electrical properties. Semiconductor materials have electrical conductivity between conductors and insulators and can be used to manufacture various electronic devices. Metal fluoride electronic gas performs outstandingly in this regard and is widely used in the manufacture of key electronic components such as transistors and integrated circuits, playing an important role in promoting the development of modern electronics industry.

[0003] In materials science, metal fluoride electronic gas can be used as a coating material to provide surface protection and enhance the corrosion resistance of materials. In energy storage, metal fluoride electronic gas can be used as a battery material to provide higher energy density and longer cycle life. In the biomedical field, metal fluoride electronic gas is used as a drug carrier to stably deliver drugs to specific tissues or cells. In the paint industry, metal fluoride electronic gas can increase the weather resistance and chemical stability of paints.

[0004] Due to the special physical and chemical properties of metal fluoride electronic gas, it is quite difficult to purify it. Currently, there are very few reports on the purification of metal fluoride electronic gas at home and abroad. Therefore, it can be seen that there are still very big problems in the purification of metal fluoride electronic gas.

[0005] In the field of metal fluoride electronic gas, the removal of hydrogen fluoride has always been a concerned issue, especially the methods for removing hydrogen fluoride in metal fluoride electronic gas to a low content are very few. Summary of the Invention

[0006] The present invention adopts a method of modifying activated carbon to remove hydrogen fluoride from metal fluoride electronic gas, and provides a modified activated carbon and a method for removing hydrogen fluoride from metal fluoride electronic gas.

[0007] To solve the above technical problems, the technical solution adopted by the present invention is:

[0008] A modified activated carbon, the preparation method comprising the following steps:

[0009] S1. Acidify the activated carbon to remove oxides;

[0010] S2. Wash the acidified activated carbon with water, then dry it at high temperature, and finally load one or more of sodium fluoride, potassium fluoride and calcium fluoride on the dried activated carbon;

[0011] S3. Activating the loaded activated carbon at high temperature and under vacuum to obtain modified activated carbon.

[0012] A method for removing hydrogen fluoride from metal fluoride electronic gas by modified activated carbon comprises the following steps:

[0013] S4. The electronic gas of the metal fluoride is introduced into the activated modified activated carbon at a flow rate of 1000ml-3000ml / min, the temperature is controlled at 0°C-20°C, and the pressure is controlled at 0.5-0.8MPa to remove hydrogen fluoride in the electronic gas of the metal fluoride.

[0014] Preferably, the acidification time in S1 is 2 h to 10 h, and the mass concentration of the acid is 10% to 50%.

[0015] Preferably, the acid in S1 is hydrofluoric acid.

[0016] Preferably, the volume ratio of activated carbon to water in the water washing process in S2 is 1:20.

[0017] Preferably, the drying temperature in S2 is 100° C. to 150° C., and the drying time is 12 to 24 hours.

[0018] Preferably, the mass concentration of the sodium fluoride, potassium fluoride or calcium fluoride solution used in the loading process in S2 is 2% to 10%, and the immersion loading is performed for 1 hour to 5 hours.

[0019] Preferably, the activation temperature in S3 is controlled at 100-300° C., and the activation time is controlled at 1 h to 5 h.

[0020] Compared with the prior art, the present invention has the following advantages:

[0021] The invention has simple purification operation, low cost and high adsorption efficiency. The method is simple to operate and the hydrogen fluoride content can be reduced to below 10 ppm.

[0022] The technical solution of the present invention is further described in detail below through embodiments. DETAILED DESCRIPTION

[0023] Example 1

[0024] The method for removing hydrogen fluoride from metal fluoride electronic gas by purified modified activated carbon of this embodiment comprises the following steps:

[0025] S1. Acidify the activated carbon to remove the oxides inside. The acidification time is 2 hours and the mass concentration of hydrofluoric acid is 30%.

[0026] S2. The acidified activated carbon is washed with water, and the volume ratio of activated carbon to water is 1:20 during the washing process. It is then dried at a high temperature of 120°C for 20 hours. Finally, the dried activated carbon is loaded with sodium fluoride, and the concentration of the sodium fluoride solution is 5%, and the loading time is 3 hours.

[0027] S3. Activate the loaded activated carbon at high temperature and under vacuum, with the temperature controlled at 200° C. and the time controlled at 3 h.

[0028] S4. The electronic gas of metal fluoride is introduced into the activated modified activated carbon at a flow rate of 2000 ml / min, the temperature is controlled at 10° C., and the pressure is controlled at 0.6 MPa.

[0029] Table 1. Hydrogen fluoride content before and after adsorption

[0030] Hydrogen fluoride before adsorption / ppm Hydrogen fluoride after adsorption / ppm 800-1000 0-10

[0031] Example 2

[0032] The method for removing hydrogen fluoride from metal fluoride electronic gas by purified modified activated carbon of this embodiment comprises the following steps:

[0033] S1. Acidify the activated carbon to remove the oxides inside. The acidification time is 2 hours and the mass concentration of hydrofluoric acid is 30%.

[0034] S2. The acidified activated carbon is washed with water, and the volume ratio of activated carbon to water is 1:20 during the washing process. It is then dried at a high temperature of 120°C for 20 hours. Finally, the dried activated carbon is loaded with sodium fluoride, and the mass concentration of potassium fluoride is 5%, and the loading time is 3 hours.

[0035] S3. Activate the loaded activated carbon at high temperature and under vacuum, with the temperature controlled at 200° C. and the time controlled at 3 h.

[0036] S4. The electronic gas of metal fluoride is introduced into the activated modified activated carbon at a flow rate of 2000 ml / min, the temperature is controlled at 10° C., and the pressure is controlled at 0.6 MPa.

[0037] Table 2. Hydrogen fluoride content before and after adsorption

[0038] Hydrogen fluoride before adsorption / ppm Hydrogen fluoride after adsorption / ppm 800-1000 10-20

[0039] Example 3

[0040] The method for removing hydrogen fluoride from metal fluoride electronic gas by purified modified activated carbon of this embodiment comprises the following steps:

[0041] S1. Acidify the activated carbon to remove the oxides inside. The acidification time is 2 hours and the mass concentration of hydrofluoric acid is 30%.

[0042] S2. The acidified activated carbon is washed with water, and the volume ratio of activated carbon to water is 1:20 during the washing process. It is then dried at a high temperature of 120°C for 20 hours. Finally, sodium fluoride and potassium fluoride are loaded on the dried activated carbon, with a concentration of 5% and a loading time of 3 hours.

[0043] S3. Activate the loaded activated carbon at high temperature and under vacuum, with the temperature controlled at 200° C. and the time controlled at 3 h.

[0044] S4. The electronic gas of metal fluoride is introduced into the activated modified activated carbon at a flow rate of 2000 ml / min, the temperature is controlled at 10° C., and the pressure is controlled at 0.6 MPa.

[0045] Table 3. Hydrogen fluoride content before and after adsorption

[0046]

[0047] Example 4

[0048] The method for removing hydrogen fluoride from metal fluoride electronic gas by purified modified activated carbon of this embodiment comprises the following steps:

[0049] S1. Acidify the activated carbon to remove the oxides inside. The acidification time is 10 hours and the mass concentration of hydrofluoric acid is 50%.

[0050] S2. The acidified activated carbon is washed with water, and the volume ratio of activated carbon to water is 1:20 during the washing process. Then it is dried at high temperature, the drying temperature is 100°C, and the drying time is 24 hours. Finally, the dried activated carbon is loaded with sodium fluoride, the concentration of the sodium fluoride solution is 2%, and the loading time is 5 hours.

[0051] S3. Activate the loaded activated carbon at high temperature and under vacuum, with the temperature controlled at 300° C. and the time controlled at 1 h.

[0052] S4. The electronic gas of metal fluoride is introduced into the activated modified activated carbon at a flow rate of 3000 ml / min, the temperature is controlled at 0°C, and the pressure is controlled at 0.5 MPa.

[0053] Table 1. Hydrogen fluoride content before and after adsorption

[0054]

[0055] Example 5

[0056] The method for removing hydrogen fluoride from metal fluoride electronic gas by purified modified activated carbon of this embodiment comprises the following steps:

[0057] S1. Acidify the activated carbon to remove the oxides inside. The acidification time is 5 hours and the mass concentration of hydrofluoric acid is 10%.

[0058] S2. The acidified activated carbon is washed with water, and the volume ratio of activated carbon to water is 1:20 during the washing process. Then it is dried at high temperature, the drying temperature is 150°C, and the drying time is 12 hours. Finally, the dried activated carbon is loaded with sodium fluoride, the concentration of the sodium fluoride solution is 10%, and the loading time is 1 hour.

[0059] S3. Activate the loaded activated carbon at high temperature and under vacuum, with the temperature controlled at 100° C. and the time controlled at 5 h.

[0060] S4. The electronic gas of metal fluoride is introduced into the activated modified activated carbon at a flow rate of 1000 ml / min, the temperature is controlled at 20° C., and the pressure is controlled at 0.8 MPa.

[0061] Table 1. Hydrogen fluoride content before and after adsorption

[0062] Hydrogen fluoride before adsorption / ppm Hydrogen fluoride after adsorption / ppm 800-1000 0-10

[0063] Comparative Example 1

[0064] The method for removing hydrogen fluoride from metal fluoride electronic gas by purified modified activated carbon in this comparative example comprises the following steps:

[0065] S1. Acidify the activated carbon to remove the oxides inside. The acidification time is 2 hours and the mass concentration of hydrofluoric acid is 30%.

[0066] S2. The acidified activated carbon is washed with water, and the volume ratio of activated carbon to water is 1:20 during the washing process. It is then dried at a high temperature of 120°C for 20 hours. Finally, the dried activated carbon is loaded with sodium fluoride, and the concentration of the sodium fluoride solution is 5%, and the loading time is 3 hours.

[0067] S3. Activate the loaded activated carbon at high temperature and under vacuum, with the temperature controlled at 200° C. and the time controlled at 3 h.

[0068] S4. The electronic gas of metal fluoride is introduced into the activated modified activated carbon at a flow rate of 2000 ml / min, the temperature is controlled at 30° C., and the pressure is controlled at 0.6 MPa.

[0069] Table 3. Hydrogen fluoride content before and after adsorption

[0070] Hydrogen fluoride before adsorption / ppm Hydrogen fluoride after adsorption / ppm 800-1000 5-15

[0071] Comparative Example 2

[0072] The method for removing hydrogen fluoride from metal fluoride electronic gas by purified modified activated carbon in this comparative example comprises the following steps:

[0073] S1. Acidify the activated carbon to remove the oxides inside. The acidification time is 2 hours and the mass concentration of hydrofluoric acid is 30%.

[0074] S2. The acidified activated carbon is washed with water, and the volume ratio of activated carbon to water is 1:20 during the washing process. It is then dried at a high temperature of 120°C for 20 hours. Finally, the dried activated carbon is loaded with sodium fluoride, and the concentration of the sodium fluoride solution is 5%, and the loading time is 3 hours.

[0075] S3. Activate the loaded activated carbon at high temperature and under vacuum, with the temperature controlled at 200° C. and the time controlled at 3 h.

[0076] S4. The electronic gas of metal fluoride is introduced into the activated modified activated carbon at a flow rate of 2000 ml / min, the temperature is controlled at 40° C., and the pressure is controlled at 0.6 MPa.

[0077] Table 3. Hydrogen fluoride content before and after adsorption

[0078] Hydrogen fluoride before adsorption / ppm Hydrogen fluoride after adsorption / ppm 800-1000 10-25

[0079] Comparative Example 3

[0080] The method for removing hydrogen fluoride from metal fluoride electronic gas by purified modified activated carbon in this comparative example comprises the following steps:

[0081] S1. Acidify the activated carbon to remove the oxides inside. The acidification time is 2 hours and the mass concentration of hydrofluoric acid is 30%.

[0082] S2. The acidified activated carbon is washed with water, and the volume ratio of activated carbon to water is 1:20 during the washing process. It is then dried at a high temperature of 120°C for 20 hours. Finally, the dried activated carbon is loaded with sodium fluoride, and the concentration of the sodium fluoride solution is 5%, and the loading time is 3 hours.

[0083] S3. Activate the loaded activated carbon at high temperature and under vacuum, with the temperature controlled at 150°C and the time controlled at 3 hours.

[0084] S4. The electronic gas of metal fluoride is introduced into the activated modified activated carbon at a flow rate of 2000 ml / min, the temperature is controlled at 50° C., and the pressure is controlled at 0.6 MPa.

[0085] Table 3. Hydrogen fluoride content before and after adsorption

[0086] Hydrogen fluoride before adsorption / ppm Hydrogen fluoride after adsorption / ppm 800-1000 15-30

[0087] Comparative Example 4

[0088] The method for removing hydrogen fluoride from metal fluoride electronic gas by purified modified activated carbon of this embodiment comprises the following steps:

[0089] S1. Acidify the activated carbon to remove the oxides inside. The acidification time is 2 hours and the mass concentration of hydrofluoric acid is 30%.

[0090] S2. The acidified activated carbon is washed with water, and the volume ratio of activated carbon to water is 1:20 during the washing process. It is then dried at a high temperature of 120°C for 20 hours. Finally, the dried activated carbon is loaded with sodium fluoride, and the concentration of the sodium fluoride solution is 5%, and the loading time is 3 hours.

[0091] S3. Activate the loaded activated carbon at high temperature and under vacuum, with the temperature controlled at 200° C. and the time controlled at 3 h.

[0092] S4. The electronic gas of metal fluoride is introduced into the activated modified activated carbon at a flow rate of 4500 ml / min, the temperature is controlled at 10° C., and the pressure is controlled at 0.6 MPa.

[0093] Table 3. Hydrogen fluoride content before and after adsorption

[0094] Hydrogen fluoride before adsorption / ppm Hydrogen fluoride after adsorption / ppm 800-1000 30-40

[0095] It can be seen from Examples 1-3 that the effect of loading sodium fluoride is the best; it can be seen from Comparative Examples 1-3 that the adsorption effect becomes worse with the increase of the adsorption temperature; it can be seen from Comparative Example 4 that the greater the electron gas flow rate of the metal fluoride, the worse the adsorption effect.

[0096] The technical solutions disclosed and proposed by the present invention can be realized by those skilled in the art by referring to the contents of this article and appropriately changing the conditions, routes and other links. Although the methods and preparation techniques of the present invention have been described through preferred embodiments, relevant technicians can obviously modify or re-combine the methods and technical routes described herein without departing from the content, spirit and scope of the present invention to realize the final preparation technology. It should be particularly noted that all similar substitutions and modifications are obvious to those skilled in the art, and they are all considered to be included in the spirit, scope and content of the present invention.

Claims

1. A modified activated carbon, characterized in that: The preparation method comprises the following steps: S1. Acidifying the activated carbon to remove oxides; S2, washing the acidified activated carbon with water, then drying it, and finally loading one or more of sodium fluoride, potassium fluoride and calcium fluoride on the dried activated carbon; S3. Activating the loaded activated carbon at high temperature and under vacuum to obtain modified activated carbon.

2. A method for removing hydrogen fluoride from metal fluoride electronic gas by using modified activated carbon as claimed in claim 1, characterized in that: The following steps are involved: S4. The electronic gas of the metal fluoride is introduced into the activated modified activated carbon at a flow rate of 1000ml-3000ml / min, the temperature is controlled at 0°C-20°C, and the pressure is controlled at 0.5-0.8MPa to remove hydrogen fluoride in the electronic gas of the metal fluoride.

3. The method for removing hydrogen fluoride from metal fluoride electronic gas by using modified activated carbon according to claim 1, characterized in that: The acidification time in S1 is 2 hours to 10 hours, and the mass concentration of the acid is 10% to 50%.

4. The method for removing hydrogen fluoride from metal fluoride electronic gas by using modified activated carbon according to claim 3, characterized in that: The acid in S1 is hydrofluoric acid.

5. The method for removing hydrogen fluoride from metal fluoride electronic gas by using modified activated carbon according to claim 1, characterized in that: The volume ratio of activated carbon to water in the water washing process in S2 is 1:

20.

6. The method for removing hydrogen fluoride from metal fluoride electronic gas by using modified activated carbon according to claim 1, characterized in that: The drying temperature in S2 is 100° C. to 150° C., and the drying time is 12 to 24 hours.

7. The method for removing hydrogen fluoride from metal fluoride electronic gas by using modified activated carbon according to claim 1, characterized in that: The mass concentration of the sodium fluoride, potassium fluoride or calcium fluoride solution used in the loading process in S2 is 2% to 10%, and the immersion loading is performed for 1 hour to 5 hours.

8. The method for removing hydrogen fluoride from metal fluoride electronic gas by using modified activated carbon according to claim 1, characterized in that: The activation temperature in S3 is controlled at 100-300° C., and the activation time is controlled at 1 h-5 h.

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