Packing layer bed in chlorine trifluoride distillation column, preparation method therefor and use method thereof

Abstract

A packing layer bed in a chlorine trifluoride distillation column, a preparation method therefor and a use method thereof, comprising the following steps: S1, leveling nickel chloride, placing same in a tray, placing into an oven for initial baking, to remove moisture, and drying at a high temperature until brownish yellow, and crushing the baked nickel chloride powder; S2, mixing the nickel chloride with sodium chloride powder and sintering to obtain particles, to obtain a packing layer bed. By means of optimizing the distribution ratio of a packing section of a reaction chamber, the proportion of nickel used to adhere to the hydrogen fluoride in chlorine trifluoride is increased, thereby improving distillation yield.

Description

A packing layer bed in a chlorine trifluoride distillation tower and its preparation method and use method Technical Field

[0001] The present invention relates to the field of chlorine trifluoride purification, and in particular to a packing layer bed in a chlorine trifluoride distillation tower, and a preparation method and a use method thereof. Background Art

[0002] Chlorine trifluoride gas, with its strong oxidizing properties and high reactivity, is widely used in the semiconductor industry, particularly in the cleaning process of product manufacturing, where high purity is crucial. During its preparation, chlorine trifluoride gas can be contaminated with a large number of impurities, such as hydrogen fluoride and chlorine monofluoride, which can severely impact its cleaning effectiveness. Distillation is a crucial step in the purification process.

[0003] A packed tower refers to a distillation tower in which the packing is placed in the middle of the column. In a packed tower, gas enters the tower from the bottom, then flows upward, and the liquid refluxed from the top of the tower flows downward, with the gas and liquid phases undergoing mass transfer contact in the packing layer. The packing in the packed tower can absorb hydrogen fluoride doped with chlorine trifluoride. However, the applicant found that due to insufficient performance and the fact that the packing ratio was not optimized for the case of hydrogen fluoride doped with chlorine trifluoride, there was a certain interaction between chlorine trifluoride and hydrogen fluoride, making it difficult to further improve the packing's removal effect on hydrogen fluoride.

[0004] In view of the above problems in the prior art, the present invention aims to design a packing layer bed in a chlorine trifluoride distillation tower and a preparation method and a use method thereof. Summary of the Invention

[0005] In response to the problems existing in the above-mentioned prior art, the present invention provides a packed bed in a chlorine trifluoride distillation tower and a preparation method and a use method thereof, which can effectively solve at least one problem existing in the above-mentioned prior art.

[0006] The technical solution of the present invention is:

[0007] A method for preparing a packed bed in a chlorine trifluoride distillation tower comprises the following steps:

[0008] S1, smoothing the nickel chloride powder, placing it into a tray, placing it in an oven to initially dry out the moisture, then drying it at high temperature until it turns brownish yellow, and crushing the baked nickel chloride powder;

[0009] S2, mixing nickel chloride and sodium chloride powder, and sintering to obtain particles, that is, obtaining a filler layer bed.

[0010] Furthermore, in step S1, the product is placed in an oven and dried at 60-90°C to remove moisture, and then dried at above 200°C to a brownish yellow color.

[0011] Furthermore, in step S1, the baked nickel chloride powder is crushed by a small hammer crusher.

[0012] Furthermore, in step S2, nickel chloride and sodium chloride powders are mixed and sintered under an inert gas to obtain particles.

[0013] Furthermore, in step S2, the weight percentage of nickel chloride is higher than the weight percentage of sodium chloride.

[0014] A packed bed in a chlorine trifluoride distillation tower is prepared by the method for preparing a packed bed in a chlorine trifluoride distillation tower.

[0015] A method for using a packed bed in a chlorine trifluoride distillation tower comprises the steps of uniformly filling the packed bed into the second inverted tray of the distillation tower.

[0016] Therefore, the present invention provides the following effects and / or advantages:

[0017] The invention optimizes the component distribution ratio of the packing section of the reaction hall and increases the proportion of nickel, which is used to stick the hydrogen fluoride in the chlorine trifluoride, thereby achieving a high distillation yield.

[0018] It is to be understood that both the foregoing general description and the following detailed description of the present invention are exemplary and explanatory and are intended to provide further explanation of the invention as claimed. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] FIG1 is a schematic diagram of a preparation method according to one embodiment of the present invention. Implementation Method

[0020] In order to facilitate understanding by those skilled in the art, the present invention is now described in further detail with reference to the following examples:

[0021] Referring to FIG1 , a method for preparing a packed bed in a chlorine trifluoride distillation tower comprises the following steps:

[0022] S1, smoothing the nickel chloride powder, placing it into a tray, placing it in an oven to initially dry out the moisture, then drying it at high temperature until it turns brownish yellow, and crushing the baked nickel chloride powder;

[0023] In this embodiment, nickel chloride provides nickel ions, which can alter the interaction between chlorine trifluoride and hydrogen fluoride, weakening the interaction. Furthermore, one nickel chloride can bond two fluoride ions, thereby better "sticking" to the hydrogen fluoride in the chlorine trifluoride.

[0024] S2, mixing nickel chloride and sodium chloride powder, and sintering to obtain particles, that is, obtaining a filler layer bed.

[0025] In this step, a chloride salt reacts with hydrofluoric acid. Sodium chloride reacts with anhydrous hydrogen fluoride to produce sodium fluoride, which dissolves in hydrofluoric acid to form sodium bifluoride. Sodium bifluoride, a colorless or white quicksand-like crystal or powder, removes hydrogen fluoride from chlorine trifluoride. Furthermore, the nickel chloride powder provides nickel chloride, which "sticks" more hydrogen fluoride while preventing chlorine trifluoride from sticking. Therefore, the nickel chloride further improves the removal rate.

[0026] Furthermore, in step S1, the product is placed in an oven and dried at 60-90°C to remove moisture, and then dried at above 200°C to a brownish yellow color.

[0027] This step can further improve the dehydration of nickel chloride. Water reacts with chlorine trifluoride to generate a large amount of heat, so complete dehydration is required.

[0028] Furthermore, in step S1, the baked nickel chloride powder is crushed by a small hammer crusher.

[0029] Furthermore, in step S2, nickel chloride and sodium chloride powders are mixed and sintered under an inert gas to obtain particles.

[0030] Furthermore, in step S2, the weight percentage of nickel chloride is higher than the weight percentage of sodium chloride.

[0031] The weight fraction of nickel chloride in this embodiment is higher than that of sodium chloride, which provides a large amount of nickel ions and sodium ions. In addition, the nickel ions are more abundant, and the prepared packing bed improves the adsorption capacity of hydrogen fluoride impurities from chlorine trifluoride.

[0032] A packed bed in a chlorine trifluoride distillation tower is prepared by the method for preparing a packed bed in a chlorine trifluoride distillation tower.

[0033] A method for using a packed bed in a chlorine trifluoride distillation tower comprises the steps of uniformly filling the packed bed into the second inverted tray of the distillation tower.

[0034] The packed bed provided in the present application is used in a distillation tower to purify chlorine trifluoride through the distillation tower. The purity of the chlorine trifluoride finally obtained is higher than that of the traditional packed bed that only uses chloride salt for purification. The packed bed provided in the present application improves the purity of the chlorine trifluoride.

[0035] It should be noted that in the claims, any reference signs placed between parentheses shall not be construed as limiting the claims. The word "comprising" does not exclude the presence of components or steps not listed in the claim. The word "a" or "an" preceding a component does not exclude the presence of a plurality of such components. The invention can be implemented by means of hardware comprising several different components and by means of a suitably programmed computer. In a unit claim enumerating several means, several of these means may be embodied by one and the same item of hardware. The use of the words first, second, third etc. does not indicate any order. These words may be interpreted as names.

[0036] Although the preferred embodiments of the present invention have been described, those skilled in the art may make additional changes and modifications to these embodiments once they have learned the basic creative concept. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments and all changes and modifications that fall within the scope of the present invention.

[0037] In the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," "connect," "fixed," etc. should be understood broadly. For example, they may refer to fixed connection, detachable connection, or integration; mechanical connection or electrical connection; direct connection or indirect connection through an intermediate medium; internal communication between two components or interaction between two components. Those skilled in the art will understand the specific meanings of the above terms in the present invention based on specific circumstances.

[0038] In the description of this specification, the reference terms "one embodiment", "some embodiments", "example", "specific example", or "some examples" mean that the specific features, structures, materials, or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic expressions of the above terms should not be understood as necessarily referring to the same embodiment or example. Moreover, the specific features, structures, materials, or characteristics described can be combined in any one or more embodiments or examples in a suitable manner. In addition, those skilled in the art can combine and combine different embodiments or examples described in this specification and features of different embodiments or examples without contradiction.

Claims

1. A method for preparing a packed bed in a chlorine trifluoride distillation tower, characterized in that: The following steps are involved: S1, smoothing the nickel chloride powder, putting it into a plate, putting it into an oven to initially dry out the moisture, and then drying it at high temperature until it turns brownish yellow, and breaking the baked nickel chloride powder; S2, mixing nickel chloride and sodium chloride powder, and sintering to obtain particles, that is, obtaining a packing layer bed.

2. The method for preparing a packed bed in a chlorine trifluoride distillation tower according to claim 1, characterized in that: In step S1, the mixture is placed in an oven at 60-90°C to remove moisture, and then dried at above 200°C to brownish yellow.

3. The method for preparing a packed bed in a chlorine trifluoride distillation tower according to claim 1, characterized in that: In step S1, the baked nickel chloride powder is crushed by a small hammer crusher.

4. The method for preparing a packed bed in a chlorine trifluoride distillation tower according to claim 1, characterized in that: In step S2, nickel chloride and sodium chloride powders are mixed and sintered under an inert gas to obtain particles.

5. The method for preparing a packed bed in a chlorine trifluoride distillation tower according to claim 1, characterized in that: In step S2, the weight percentage of nickel chloride is higher than the weight percentage of sodium chloride.

6. A packed bed in a chlorine trifluoride distillation tower, characterized in that: The invention is prepared by the method for preparing a packed bed in a chlorine trifluoride distillation tower according to any one of claims 1 to 5.

7. A method for using a packed bed in a chlorine trifluoride distillation tower, comprising the packed bed in a chlorine trifluoride distillation tower according to claim 6, characterized in that: The packing layer bed is uniformly filled into the second inverted tray of the distillation tower.

Images