Adsorbent, method of preparation and use thereof

The prepared adsorbent effectively solves the problem of removing organic impurities from trifluoromethanesulfonyl fluoride, achieving efficient and low-cost purification, and is suitable for the fields of large-scale integrated circuits and chip manufacturing.

CN122298343APending Publication Date: 2026-06-30QUANZHOU YUJI ADVANCED MATERIALS CO LTD +3

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
QUANZHOU YUJI ADVANCED MATERIALS CO LTD
Filing Date
2024-12-27
Publication Date
2026-06-30

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Abstract

This application discloses an adsorbent, its preparation method, and its application. The adsorbent comprises an active component and a support, wherein the mass ratio of the active component to the support is (1-20):100, preferably (10-20):100. The active component is selected from one or more oxides of alkali metals, oxides of alkaline earth metals, and oxides of Group III subgroup metals. The support is a porous material with an average pore size of 0.3 nm-1 nm, preferably 0.4 nm-0.7 nm, and a specific surface area of ​​20 m². 2 / g-1300m 2 / g, preferably 100m 2 / g-350m 2 / g.
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Description

Technical Field

[0001] This application relates to an adsorbent, and more particularly to a purification adsorbent for trifluoromethanesulfonyl fluoride, its preparation method, and its application. Background Technology

[0002] Trifluoromethanesulfonyl fluoride has an insulation strength 1.39 times that of sulfur hexafluoride. Studies have shown that trifluoromethanesulfonyl fluoride has a synergistic effect with nitrogen, and the breakdown voltage of its mixture is equal to or better than that of SF6. It also has good self-recovery properties and material compatibility, making it a potential SF6 substitute.

[0003] Numerous methods for synthesizing trifluoromethanesulfonyl fluoride have been reported. Patents CN 101842348B, EP2216325A1, CN 214654573U, and CN 109824551A all report processes for synthesizing trifluoromethanesulfonyl fluoride via liquid-phase fluorination, achieving a purity of up to 99.5% after purification. Patent 2022117262716 discloses a method for producing trifluoromethanesulfonyl fluoride based on a reaction-distillation coupling technology, achieving a purity exceeding 99.9%.

[0004] Currently, much research on trifluoromethanesulfonyl fluoride focuses on its synthesis and manufacturing, with limited reports on purification methods for high-purity products. Besides its use as an insulating gas, trifluoromethanesulfonyl fluoride may also be applied in large-scale integrated circuits and chip manufacturing. These industries have extremely stringent requirements for the impurities in their chemicals, often needing to control impurity levels at the ppm level. Therefore, it is necessary to develop an adsorbent for the purification of trifluoromethanesulfonyl fluoride to meet the requirements of high-end manufacturing. Summary of the Invention

[0005] The specific technical solution of this application is as follows:

[0006] This application provides an adsorbent for gas purification, wherein the adsorbent comprises an active component and a support, wherein the mass ratio of the active component to the support is (1-20):100, preferably (10-20):100.

[0007] The active component is selected from one or more of alkali metal oxides, alkaline earth metal oxides, and Group III subgroup metal oxides.

[0008] The carrier is a porous material with an average pore size of 0.3 nm to 1 nm, preferably 0.4 nm to 0.7 nm, and a specific surface area of ​​20 m². 2 / g-1300m 2 / g, preferably 100m 2 / g-350m 2 / g.

[0009] Furthermore, the alkali metal is selected from one or more of Li, Na, K, Rb, and Cs, or

[0010] The alkaline earth metal is selected from one or more of Be, Mg, Ca, Sr, and Ba, or

[0011] The group III subgroup metals are selected from one or more of La, Ce, Pr, Nd, Y, and Sc; or

[0012] Preferably, the alkali metal oxide is selected from one or more of Li₂O, Na₂O, K₂O, Rb₂O, and Cs₂O, or

[0013] The alkaline earth metal oxide is selected from one or more of BeO, MgO, CaO, SrO, and BaO, or

[0014] The oxides of the group III subgroup metals are selected from one or more of La2O3, Ce2O3, Pr2O3, Nd2O3, Y2O3, Sc2O3, and CeO2.

[0015] Furthermore, the support is selected from one or more of type A molecular sieves, type X molecular sieves, activated carbon, and porous metal fluorides;

[0016] Preferably, the type A molecular sieve is selected from one or more of 3A molecular sieve, 4A molecular sieve, and 5A molecular sieve; or

[0017] The X-type molecular sieve is a 10X molecular sieve and / or a 13X molecular sieve; or

[0018] The porous metal fluoride is selected from one or more of aluminum fluoride, chromium fluoride, magnesium fluoride, and calcium fluoride.

[0019] Furthermore, the active component is composed of oxides of alkali metals, oxides of alkaline earth metals, and oxides of group III subgroup metals;

[0020] Preferably, the mass ratio of the oxides of the alkali metal, the oxides of the alkaline earth metal, and the oxides of the Group III subgroup metal is 1:(1-5):(1-5), more preferably 1:2:(1-3).

[0021] This application also provides a method for preparing an adsorbent for gas purification, comprising the following steps:

[0022] The ratio of active component to carrier in the adsorbent is calculated, and the soluble salt of the active component is prepared into a precursor salt solution of the active component. Then, the carrier is mixed and impregnated with the precursor salt solution of the active component. After standing for a certain period of time, the mixture is dried and calcined to obtain the adsorbent for gas purification.

[0023] The adsorbent comprises an active component and a carrier, wherein the mass ratio of the active component to the carrier is (1-20):100.

[0024] Furthermore, the precursor soluble salt of the active component is selected from nitrates, nitrites, carbonates, bicarbonates, and acetates.

[0025] Furthermore, the impregnation is an equal-volume impregnation method, wherein the volume ratio of the precursor salt solution of the active component to the saturated water absorption volume of the carrier is (1-1.2):1, and the standing time after impregnation is 12-36 hours.

[0026] Furthermore, the adsorbent prepared in this application is the aforementioned adsorbent.

[0027] This application also provides an adsorbent for gas purification, or the use of an adsorbent for gas purification prepared by the aforementioned method in adsorbing organic impurities in trifluoromethanesulfonyl fluoride.

[0028] Furthermore, the organic impurity is selected from one of trifluoromethanesulfonyl chloride, carbon tetrafluoride, trifluorochloromethane, and bis(trifluoromethyl)disulfide.

[0029] The adsorbent described in this application has a simple preparation process, good reproducibility, and low manufacturing cost.

[0030] The adsorption method described in this application has the characteristics of good adsorption effect, large adsorption capacity and long breakthrough time for a variety of organic impurities.

[0031] This application uses adsorption to remove organic impurities from trifluoromethanesulfonyl fluoride, which has advantages such as lower equipment investment, lower energy consumption, and simpler operation compared to traditional distillation. Attached Figure Description

[0032] The accompanying drawings are provided to better understand this application and do not constitute an undue limitation thereof. Wherein:

[0033] Figure 1 GC spectra of trifluoromethanesulfonyl fluoride before and after adsorption in Example 3 provided in this application. Detailed Implementation

[0034] The following description provides exemplary embodiments of this application, including various details to aid understanding, and should be considered merely exemplary. Therefore, those skilled in the art will recognize that various changes and modifications can be made to the embodiments described herein without departing from the scope and spirit of this application. Similarly, for clarity and brevity, descriptions of well-known functions and structures are omitted in the following description.

[0035] This application provides an adsorbent for gas purification, wherein the adsorbent comprises an active component and a carrier, wherein the mass ratio of the active component to the carrier is (1-20):100, preferably (10-20):100.

[0036] This application provides an adsorbent for gas purification, wherein the adsorbent is composed of an active component and a carrier, and the mass ratio of the active component to the carrier is (1-20):100, preferably (10-20):100.

[0037] In some embodiments, the mass ratio of the active component to the carrier is (10-15):100.

[0038] In some embodiments, the mass ratio of the active component to the carrier is (12-20):100.

[0039] Specifically, the mass ratio of the active component to the carrier can be 1:100, 2:100, 3:100, 4:100, 5:100, 6:100, 7:100, 8:100, 9:100, 10:100, 11:100, 12:100, 13:100, 14:100, 15:100, 16:100, 17:100, 18:100, 19:100, 20:100 or any range thereof.

[0040] In this application, the active component is selected from one or more of alkali metal oxides, alkaline earth metal oxides, and group III subgroup metal oxides, and the support is selected from one or more of type A molecular sieves, type X molecular sieves, activated carbon, and porous metal fluorides.

[0041] The alkali metal is selected from one or more of Li, Na, K, Rb, and Cs, with K being preferred.

[0042] The alkaline earth metal is selected from one or more of Be, Mg, Ca, Sr, and Ba, with Mg being preferred.

[0043] The group III subgroup metal is selected from one or more of La, Ce, Pr, Nd, Y, and Sc, with Ce being preferred.

[0044] Furthermore, the alkali metal oxide is selected from one or more of Li2O, Na2O, K2O, Rb2O, and Cs2O, preferably K2O.

[0045] The alkaline earth metal oxide is selected from one or more of BeO, MgO, CaO, SrO, and BaO, with MgO being preferred.

[0046] The oxide of the group III subgroup metal is selected from one or more of La2O3, Ce2O3, Pr2O3, Nd2O3, Y2O3, Sc2O3, and CeO2, preferably Ce2O3.

[0047] In some embodiments, the active component is an oxide of an alkali metal.

[0048] In some embodiments, the active component is an oxide of an alkaline earth metal.

[0049] In some embodiments, the active component is an oxide of a Group III subgroup metal.

[0050] In some embodiments, the active component consists of oxides of alkali metals and oxides of alkaline earth metals.

[0051] In some embodiments, the active component consists of oxides of alkali metals and oxides of Group III subgroup metals.

[0052] In some embodiments, the active component consists of oxides of alkaline earth metals and oxides of Group III subgroup metals.

[0053] In some embodiments, the active component consists of oxides of alkali metals, oxides of alkaline earth metals, and oxides of group III subgroup metals.

[0054] The mass ratio of the oxides of the alkali metal, the oxides of the alkaline earth metal, and the oxides of the Group III subgroup metal is 1:(1-5):(1-5).

[0055] In some embodiments, the mass ratio of the alkali metal oxide to the alkaline earth metal oxide is 1:(1-5).

[0056] In some embodiments, the mass ratio of the alkali metal oxide to the alkaline earth metal oxide is 1:(1-3).

[0057] Specifically, the mass ratio of the alkali metal oxide to the alkaline earth metal oxide is 1:1, 1:1.5, 1:2, 1:2.5, 1:3, 1:3.5, 1:4, 1:4.5, 1:5 or any range thereof.

[0058] In some embodiments, the mass ratio of the alkali metal oxide to the group III subgroup metal oxide is 1:(1-5).

[0059] In some embodiments, the mass ratio of the alkali metal oxide to the group III subgroup metal oxide is 1:(1-3).

[0060] Specifically, the mass ratio of the alkali metal oxide to the group III subgroup metal oxide is 1:1, 1:1.5, 1:2, 1:2.5, 1:3, 1:3.5, 1:4, 1:4.5, 1:5 or any range thereof.

[0061] In this application, the carrier is a porous material with an average pore size of 0.3 nm-1 nm, preferably 0.4 nm-0.7 nm, and a specific surface area of ​​20 m². 2 / g-1300m 2 / g, preferably 100m 2 / g-350m 2 / g.

[0062] In some embodiments, the average pore size of the porous material is 0.4 nm to 0.6 nm.

[0063] In some embodiments, the average pore size of the porous material is 0.5 nm to 0.7 nm.

[0064] Specifically, the average pore size of the porous material is 0.3nm, 0.4nm, 0.5nm, 0.6nm, 0.7nm, 0.8nm, 0.9nm, 1nm or any range thereof.

[0065] In some embodiments, the specific surface area of ​​the porous material is 100 m². 2 / g-500m 2 / g.

[0066] In some embodiments, the specific surface area of ​​the porous material is 100 m². 2 / g-400m 2 / g.

[0067] In some embodiments, the specific surface area of ​​the porous material is 100 m². 2 / g-350m 2 / g.

[0068] Specifically, the specific surface area of ​​the porous material is 20 m². 2 / g、30m 2 / g、40m 2 / g, 50m 2 / g、60m2 / g、70m 2 / g、80m 2 / g, 100m 2 / g、110m 2 / g、120m 2 / g、130m 2 / g, 140m 2 / g, 150m 2 / g、160m 2 / g、170m 2 / g、180m 2 / g、190m 2 / g、200m 2 / g、210m 2 / g、220m 2 / g、230m 2 / g、240m 2 / g、250m 2 / g、260m 2 / g、270m 2 / g、280m 2 / g、290m 2 / g、300m 2 / g、310m 2 / g、320m 2 / g、330m 2 / g、340m 2 / g, 350m 2 / g、360m 2 / g、370m 2 / g、380m 2 / g、390m 2 / g、400m 2 / g、450m 2 / g、500m 2 / g、550m 2 / g、600m 2 / g、650m 2 / g、700m 2 / g、750m 2 / g、800m 2 / g、850m 2 / g、900m 2 / g、950m 2 / g, 1000m 2 / g、1100m 2 / g、1200m 2 / g、1300m 2 / g or any range thereof.

[0069] In this paper, the average pore size and specific surface area of ​​the support were determined by low-temperature nitrogen adsorption method.

[0070] Furthermore, the carrier is selected from one or more of type A molecular sieves, type X molecular sieves, activated carbon, and porous metal fluorides.

[0071] Furthermore, the type A molecular sieve is selected from one or more of 3A molecular sieve, 4A molecular sieve and 5A molecular sieve.

[0072] The X-type molecular sieve is a 10X molecular sieve and / or a 13X molecular sieve.

[0073] The porous metal fluoride is selected from one or more of aluminum fluoride, chromium fluoride, magnesium fluoride, and calcium fluoride.

[0074] The activated carbon is selected from one of coal-based carbon, wood-based carbon, and coconut shell carbon.

[0075] In some embodiments, the active component is K2O-MgO-La2O3, and the molecular sieve is a type 3A molecular sieve.

[0076] In some embodiments, the active component is K2O-MgO-La2O3, and the molecular sieve is a type 4A molecular sieve.

[0077] In some embodiments, the active component is K2O-MgO-La2O3, and the molecular sieve is a 5A type molecular sieve.

[0078] In some embodiments, the active component is K2O-MgO-La2O3, and the molecular sieve is a 10X type molecular sieve.

[0079] In some embodiments, the active component is K2O-MgO-La2O3, and the molecular sieve is a 13X type molecular sieve.

[0080] In some embodiments, the active component is K2O-MgO-Y2O3, and the molecular sieve is a type 3A molecular sieve.

[0081] In some embodiments, the active component is K2O-MgO-Y2O3, and the molecular sieve is a type 4A molecular sieve.

[0082] In some embodiments, the active component is K2O-MgO-Y2O3, and the molecular sieve is a 5A type molecular sieve.

[0083] In some embodiments, the active component is K2O-MgO-Y2O3, and the molecular sieve is a 10X type molecular sieve.

[0084] In some embodiments, the active component is K2O-MgO-Y2O3, and the molecular sieve is a 13X type molecular sieve.

[0085] In some embodiments, the active component is K2O-MgO-Ce2O3, and the molecular sieve is a type 3A molecular sieve.

[0086] In some embodiments, the active component is K2O-MgO-Ce2O3, and the molecular sieve is a type 4A molecular sieve.

[0087] In some embodiments, the active component is K2O-MgO-Ce2O3, and the molecular sieve is a 5A type molecular sieve.

[0088] In some embodiments, the active component is K2O-MgO-Ce2O3, and the molecular sieve is a 10X type molecular sieve.

[0089] In some embodiments, the active component is K2O-MgO-Ce2O3, and the molecular sieve is a 13X type molecular sieve.

[0090] In some embodiments, the active component is K2O-CaO-Ce2O3, and the molecular sieve is a type 3A molecular sieve.

[0091] In some embodiments, the active component is K2O-CaO-Ce2O3, and the molecular sieve is a type 4A molecular sieve.

[0092] In some embodiments, the active component is K2O-CaO-Ce2O3, and the molecular sieve is a 5A type molecular sieve.

[0093] In some embodiments, the active component is K2O-CaO-Ce2O3, and the molecular sieve is a 10X type molecular sieve.

[0094] In some embodiments, the active component is K2O-CaO-Ce2O3, and the molecular sieve is a 13X type molecular sieve.

[0095] In some embodiments, the active component is K2O-BaO-Ce2O3, and the molecular sieve is a type 3A molecular sieve.

[0096] In some embodiments, the active component is K2O-BaO-Ce2O3, and the molecular sieve is a type 4A molecular sieve.

[0097] In some embodiments, the active component is K2O-BaO-Ce2O3, and the molecular sieve is a type 5A molecular sieve.

[0098] In some embodiments, the active component is K2O-BaO-Ce2O3, and the molecular sieve is a 10X type molecular sieve.

[0099] In some embodiments, the active component is K2O-BaO-Ce2O3, and the molecular sieve is a 13X type molecular sieve.

[0100] In some embodiments, the active component is Na2O-MgO-Ce2O3, and the molecular sieve is a type 3A molecular sieve.

[0101] In some embodiments, the active component is Na2O-MgO-Ce2O3, and the molecular sieve is a type 4A molecular sieve.

[0102] In some embodiments, the active component is Na2O-MgO-Ce2O3, and the molecular sieve is a type 5A molecular sieve.

[0103] In some embodiments, the active component is Na2O-MgO-Ce2O3, and the molecular sieve is a 10X type molecular sieve.

[0104] In some embodiments, the active component is Na2O-MgO-Ce2O3, and the molecular sieve is a 13X type molecular sieve.

[0105] In some embodiments, the active component is Rb2O-MgO-Ce2O3, and the molecular sieve is a type 3A molecular sieve.

[0106] In some embodiments, the active component is Rb2O-MgO-Ce2O3, and the molecular sieve is a type 4A molecular sieve.

[0107] In some embodiments, the active component is Rb2O-MgO-Ce2O3, and the molecular sieve is a type 5A molecular sieve.

[0108] In some embodiments, the active component is Rb2O-MgO-Ce2O3, and the molecular sieve is a 10X type molecular sieve.

[0109] In some embodiments, the active component is Rb2O-MgO-Ce2O3, and the molecular sieve is a 13X type molecular sieve.

[0110] This application provides a method for preparing an adsorbent for gas purification, comprising the following steps:

[0111] The ratio of active component to carrier in the adsorbent is calculated, and the soluble salt of the active component is prepared into a precursor salt solution of the active component. Then, the carrier is mixed and impregnated with the precursor salt solution of the active component. After standing for a certain period of time, the mixture is dried and calcined to obtain the adsorbent for gas purification.

[0112] The adsorbent comprises an active component and a carrier, wherein the mass ratio of the active component to the carrier is (1-20):100.

[0113] Specifically, the precursor soluble salt of the active component is selected from nitrate, nitrite, carbonate, bicarbonate, and acetate.

[0114] Furthermore, the impregnation is an equal-volume impregnation method, wherein the volume ratio of the precursor salt solution of the active component to the saturated water absorption volume of the carrier is (1-1.2):1, and the standing time after impregnation is 12-36 hours. For example, the volume ratio of the precursor salt solution of the active component to the saturated water absorption volume of the carrier can be 1:1, 1.1:1, 1.2:1, or any range thereof; the standing time after impregnation can be 12h, 13h, 14h, 15h, 16h, 17h, 18h, 19h, 20h, 21h, 22h, 23h, 24h, 25h, 26h, 27h, 28h, 29h, 30h, 31h, 32h, 33h, 34h, 35h, 36h, or any range thereof.

[0115] In this article, the precursor salt solution of the active component refers to the solution of the oxide precursor, such as the nitrate, nitrite, or carbonate of the oxide active component.

[0116] The saturated water absorption volume of a carrier refers to the mass difference of the carrier before and after water absorption, divided by the density of water, which gives the water absorption volume.

[0117] The adsorbent prepared by the preparation method described in this application is the aforementioned adsorbent.

[0118] This application provides the use of the aforementioned adsorbent for gas purification in the adsorption of organic impurities in trifluoromethanesulfonyl fluoride. The adsorbent of this application can adsorb organic impurities from trifluoromethanesulfonyl fluoride, thereby achieving the purpose of gas purification.

[0119] The organic impurity is selected from one of trifluoromethanesulfonyl chloride, carbon tetrafluoride, trifluorochloromethane, and bis(trifluoromethyl)disulfide.

[0120] This application provides the application of the above-mentioned adsorbent in the adsorption of trifluoromethanesulfonyl fluoride, with an adsorption temperature of -20℃ to 100℃, an adsorption pressure of 0 to 1 MPa, and a feed volume hourly space velocity of 1 to 1000 h⁻¹ for trifluoromethanesulfonyl fluoride. -1 .

[0121] Specifically, the adsorption temperature can be -20℃, -15℃, -10℃, -5℃, 0℃, 5℃, 10℃, 15℃, 20℃, 25℃, 30℃, 35℃, 40℃, 45℃, 50℃, 55℃, 60℃, 65℃, 70℃, 75℃, 80℃, 85℃, 90℃, 95℃, 100℃, etc.

[0122] Specifically, the adsorption pressure can be 0 MPa, 0.2 MPa, 0.4 MPa, 0.6 MPa, 0.8 MPa, 1 MPa, etc.

[0123] Specifically, the feed volume hourly space velocity of the trifluoromethanesulfonyl fluoride is 1 h⁻¹. -1 100h -1 200h -1 300h -1 400h -1 500h -1 600h -1 700h -1 800h -1 900h -1 1000h -1 wait.

[0124] Example

[0125] Unless otherwise specified, the experimental methods used in the following examples are conventional methods.

[0126] Unless otherwise specified, all materials and reagents used in the following examples are commercially available.

[0127] Example 1

[0128] Weigh out 4.3g KNO3, 14.8g Mg(NO3)2, and 15.9g La(NO3)3·6H2O, dissolve them in 250g deionized water, add 100g 5A molecular sieve, and let stand for 24h to impregnate. Dry the impregnated mixture in an oven at 80℃ for 12h, and then calcine it in a muffle furnace at 350℃ for 24h to obtain sample 1# adsorbent, 2% K2O-4% MgO-6% La2O3 / 5A.

[0129] 2%K₂O-4%MgO-6%La₂O₃ / 5A means: relative to 100 parts by weight of 5A molecular sieve, K₂O is 2 parts by weight, MgO is 4 parts by weight, and La₂O₃ is 6 parts by weight. The average pore size of the 5A molecular sieve is 0.5 nm, and the specific surface area is 178 m². 2 / g.

[0130] The difference between Examples 2-3, 30-32 and Example 1 is that the types of oxides of Group III transition metals in the active components are different, while other parameters are the same. Specific parameters are shown in Table 1 and Table 2.

[0131] The difference between Examples 4-6 and Example 1 is that the active components contain only alkali metal oxides, while all other parameters are the same. Specific parameters are shown in Table 1 and Table 2.

[0132] The difference between Examples 7 and 8 and Example 3 is that the active components contain only oxides of Group III subgroup metals and oxides of alkaline earth metals. All other parameters are the same. Specific parameters are shown in Table 1 and Table 2.

[0133] The difference between Examples 9-10, Examples 15-16, Comparative Examples 1 and 2 and Example 3 is that the mass ratio of active component to carrier is different, while other parameters are the same. Specific parameters are shown in Table 1 and Table 2.

[0134] The difference between Examples 11-12 and Example 3 is that the types of alkaline earth metal oxides in the active components are different, while other parameters are the same. Specific parameters are shown in Table 1 and Table 2.

[0135] The difference between Examples 13 and 14 and Example 3 is that the types of alkali metal oxides in the active components are different, while the other parameters are the same. The specific parameters are shown in Table 1 and Table 2.

[0136] The difference between Examples 17-20 and Example 3 is that the mass ratios of the components in the active ingredient are different, while all other parameters are the same. Specific parameters are shown in Table 1 and Table 2.

[0137] The difference between Examples 21-25 and Example 3 is that the average pore size of the carrier is different, while other parameters are the same. Specific parameters are shown in Table 1 and Table 2.

[0138] The difference between Examples 26-29 and Example 3 is that the specific surface area of ​​the carrier is different, while other parameters are the same. Specific parameters are shown in Table 1 and Table 2.

[0139] Table 1. Parameters of the adsorbents in each embodiment

[0140]

[0141] Application examples

[0142] Application Example 1

[0143] A fixed-bed adsorption column with an inner diameter of 25 mm and a length of 600 mm was used, with an adsorbent loading of 100 g. The adsorption temperature was 20℃, the adsorption pressure was 0.1 MPa, and the space velocity was 200 h⁻¹. -1 The adsorption effect of each adsorbent on organic impurities in trifluoromethylsulfonyl fluoride was investigated, and quantitative analysis was performed using gas chromatography. See Table 2 for details.

[0144] The yield after adsorption is calculated using the following formula:

[0145] Yield = Mass of product after adsorption / Mass of raw material before adsorption × 100%.

[0146] Table 2. Adsorption efficiency of each adsorbent for organic impurities in trifluoromethylsulfonyl fluoride.

[0147]

[0148] Summary: As shown in Table 2, the adsorbents of this application, obtained by loading specific active components onto a support with specific pore size and specific surface area, exhibit significant adsorption effects on various organic impurities in trifluoromethanesulfonyl fluoride. Adsorbent #3 shows the best adsorption effect, with a total impurity content of only 0.006%. Binary active component adsorbents (adsorbents 7-8#) are more effective than single-active-component adsorbents, but less effective than ternary active component adsorbents. The loading amount of the active component significantly affects the adsorption effect; as the loading amount increases, the removal degree of organic impurities gradually improves. Alkali metals, alkaline earth metals, and Group III transition metal oxides exhibit a certain degree of synergistic enhancement, altering the physicochemical properties of the surface of a single active component, thus giving it a special adsorption effect on the aforementioned organic impurities. Excessively large molecular sieve pore sizes result in significantly poor adsorption of impurities and also reduce the yield of the target product. Insufficient specific surface area leads to low dispersion of the active component and poor adsorption effect, while excessively large specific surface areas also affect the product yield.

[0149] Application Example 2

[0150] Using 2% K₂O-4% MgO-6% Ce₂O₃ / 5A from Example 3 as the adsorbent, the adsorption effects on organic impurities in trifluoromethanesulfonyl fluoride under different temperatures, pressures, and space velocities were compared. The results are shown in Table 3. The GC spectra of trifluoromethanesulfonyl fluoride before and after adsorption in Examples 3-2 are shown below. Figure 1 ,in Figure 1 (A) is the GC spectrum before adsorption. Figure 1 (B) is the GC spectrum after adsorption.

[0151] Table 3. Adsorption effect of the adsorbent in Example 3 on organic impurities in trifluoromethylsulfonyl fluoride.

[0152]

[0153] Summary: Table 3 data shows that lowering the temperature is beneficial for the adsorption of organic impurities, while raising the temperature causes these impurities to desorb from the adsorbent, affecting the adsorption efficiency. Increasing the adsorption pressure also benefits the adsorption of organic impurities; however, considering equipment and operating costs, adsorption can be carried out at a lower pressure. Increasing the space velocity is detrimental to the complete adsorption of organic impurities; a space velocity of 1000 h⁻¹ is particularly problematic. -1 At that time, the total content of organic impurities in the product was 0.054%, and only 23% of the impurities were adsorbed.

[0154] Although the embodiments of this application have been described above in conjunction with the accompanying drawings, this application is not limited to the specific embodiments and application fields described above. The specific embodiments described above are merely illustrative and instructive, not restrictive. Those skilled in the art can make many other forms based on the guidance of this specification and without departing from the scope of protection of the claims of this application, and these are all within the scope of protection of this application.

Claims

1. A sorbent for gas purification, wherein, The adsorbent comprises an active component and a carrier, wherein the mass ratio of the active component to the carrier is (1-20):100, preferably (10-20):

100. The active component is selected from one or more of alkali metal oxides, alkaline earth metal oxides, and Group III subgroup metal oxides. The carrier is a porous material having an average pore diameter of 0.3 nm to 1 nm, preferably 0.4 nm to 0.7 nm, and a specific surface area of 20 m 2 / g to 1300 m 2 / g, preferably 100 m 2 / g to 350 m 2 / g.

2. The adsorbent of claim 1, wherein, The alkali metal is selected from one or more of Li, Na, K, Rb, and Cs, or The alkaline earth metal is selected from one or more of Be, Mg, Ca, Sr, and Ba, or The group III subgroup metals are selected from one or more of La, Ce, Pr, Nd, Y, and Sc; or Preferably, the alkali metal oxide is selected from one or more of Li₂O, Na₂O, K₂O, Rb₂O, and Cs₂O, or The alkaline earth metal oxide is selected from one or more of BeO, MgO, CaO, SrO, and BaO, or The oxides of the group III subgroup metals are selected from one or more of La2O3, Ce2O3, Pr2O3, Nd2O3, Y2O3, Sc2O3, and CeO2.

3. The adsorbent of claim 1, wherein, The carrier is selected from one or more of type A molecular sieves, type X molecular sieves, activated carbon, and porous metal fluorides; Preferably, the type A molecular sieve is selected from one or more of 3A molecular sieve, 4A molecular sieve, and 5A molecular sieve; or The X-type molecular sieve is a 10X molecular sieve and / or a 13X molecular sieve; or The porous metal fluoride is selected from one or more of aluminum fluoride, chromium fluoride, magnesium fluoride, and calcium fluoride.

4. The adsorbent of claim 1, wherein, The active component is composed of oxides of alkali metals, oxides of alkaline earth metals, and oxides of group III subgroup metals. Preferably, the mass ratio of the oxides of the alkali metal, the oxides of the alkaline earth metal, and the oxides of the Group III subgroup metal is 1:(1-5):(1-5), more preferably 1:2:(1-3).

5. A method for the preparation of an adsorbent for gas purification, wherein, Includes the following steps: The ratio of active component to carrier in the adsorbent is calculated, and the soluble salt of the active component is prepared into a precursor salt solution of the active component. Then, the carrier is mixed and impregnated with the precursor salt solution of the active component. After standing for a certain period of time, the mixture is dried and calcined to obtain the adsorbent for gas purification. The adsorbent comprises an active component and a carrier, wherein the mass ratio of the active component to the carrier is (1-20):

100.

6. The production method according to claim 5, wherein The precursor soluble salt of the active component is selected from nitrate, nitrite, carbonate, bicarbonate, and acetate.

7. The preparation method according to claim 5, wherein, The impregnation is performed using an equal-volume impregnation method, wherein the volume ratio of the precursor salt solution of the active component to the saturated water absorption volume of the carrier is (1-1.2):1, and the standing time after impregnation is 12-36 hours.

8. The preparation method according to any one of claims 5-7, wherein, The prepared adsorbent is the adsorbent according to any one of claims 1-4.

9. The use of the adsorbent for gas purification according to any one of claims 1-4, or the adsorbent for gas purification prepared by the method according to any one of claims 5-8, in the adsorption of organic impurities in trifluoromethanesulfonyl fluoride.

10. The application according to claim 9, wherein, The organic impurity is selected from one of trifluoromethanesulfonyl chloride, carbon tetrafluoride, trifluorochloromethane, and bis(trifluoromethyl)disulfide.