A fatty acid separation adsorbent and preparation method thereof

By modifying the carrier material to load Al3+ and Ag+ to form a bimetallic complex, the problem of low separation efficiency of existing fatty acid separation adsorbents is solved, and efficient graded separation of fatty acids and production of high-purity products are achieved.

CN117414799BActive Publication Date: 2025-09-19JIMEI UNIV
View PDF 3 Cites 0 Cited by

Patent Information

Application Number
CN202311450412.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-11-02
Publication Date
2025-09-19
Estimated Expiration
2043-11-02

AI Technical Summary

Technical Problem

Existing fatty acid separation adsorbents have low separation efficiency, easy loss of active centers, poor reusability, and cannot achieve efficient fractional separation of fatty acids.

Method used

Modified carrier materials are used to load Al3+ and Ag+, and bimetallic complexes are formed through π bond complexation to achieve differentiated adsorption of fatty acids with different saturations and prepare fatty acid separation adsorbents.

Benefits of technology

The efficient fractional separation of fatty acids was achieved, with a separation rate of over 92%. The process was simple, the product purity was high, and the separation cost was reduced.

✦ Generated by Eureka AI based on patent content.
Patent Text Reader

Abstract

The present invention relates to a fatty acid separation adsorbent and a preparation method thereof. The preparation method comprises the following steps: 1) mixing a carrier and a solvent, heating, adjusting the pH, and stirring evenly to obtain a carrier solution; dissolving an aminosilane coupling agent in the solvent, stirring evenly, and adding the mixture to the carrier solution; heating and refluxing, washing, filtering, and drying the mixture to obtain a modified carrier material; 2) dissolving the modified carrier material in dioxane, and then adding an AlCl3 ethanol solution containing carbon disulfide to the mixture, and reacting the mixture to obtain a single metal ion complex material Al2O3. 3+ / modified support material. 3) Take the Al 3+ The modified carrier material reacts with silver halide and is then vacuum dried. This fatty acid separation adsorbent has different adsorption and separation capabilities for saturated fatty acids, monounsaturated fatty acids, and polyunsaturated fatty acids, enabling efficient separation of fatty acids and promising industrial application prospects.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The present invention relates to a fatty acid separation technology, in particular to a fatty acid separation adsorbent and a preparation method thereof. Background Art

[0002] The main components of woody oils are saturated and unsaturated fatty acids. Unsaturated fatty acids, due to their varying degrees of saturation, are easily processed into high-value-added chemicals and are widely used in the pharmaceutical, food, and chemical industries. Therefore, further fractionation and separation of saturated and unsaturated fatty acids, especially those with varying degrees of saturation, is a key approach to increasing the economic value of woody oils.

[0003] Researchers have developed numerous fatty acid separation technologies, including urea inclusion complexation, low-temperature crystallization, solvent extraction, molecular distillation, supercritical extraction, and lipase concentration. While these technologies have achieved fatty acid separation, they are limited by their process and cannot achieve a single-stage fractionation of fatty acids. Furthermore, compared to these separation technologies, ion complex adsorbents based on π-bond complexation offer advantages such as simple operation, mild operating conditions, and differential adsorption capacity for fatty acids of varying degrees of saturation, making them promising adsorbents for fatty acid fractionation for industrial application.

[0004] However, the ion complexation technology currently used has a single active center, low separation efficiency, and a lack of strong chemical bonding, which leads to the easy loss of active centers, poor reusability, and high separation costs. Therefore, the development of separation materials with high separation efficiency and stable performance based on the structural and performance characteristics of fatty acids with different degrees of saturation in fatty acids has become the key to the industrial application of fatty acid separation.

[0005] Patent application CN111944162A discloses a method for preparing a hyperbranched polyester modified silver ion-loaded diatomaceous earth, the preparation method comprising the following steps: (1) preparing silver ion-loaded diatomaceous earth: the diatomaceous earth is first completely wetted in an ascorbic acid solution, dried to constant weight, and then completely wetted in a silver nitrate solution, left to stand for 24 to 32 hours, and then dried to obtain a diatomaceous earth-loaded silver ion material; (2) preparing aminosilane-modified silver ion-loaded diatomaceous earth: the silver ion-loaded diatomaceous earth material prepared in step (1) is first activated in a NaOH solution, and then the activated diatomaceous earth powder is ultrasonically dispersed in an ethanol solution for 30 ~60min, a diatomite suspension with good dispersibility is prepared, aminosilane is added dropwise to the suspension, acetic acid is used to adjust the pH to 5.5~6, and the suspension is stirred in a water bath at 40~50℃ for 24~28h, washed, and dried to obtain aminosilane-modified silver ion-loaded diatomite; (3) Preparation of hyperbranched polyester-modified silver ion-loaded diatomite: the aminosilane-modified silver ion-loaded diatomite powder prepared in step (2) is dispersed in acetone, hyperbranched polyester CHBP and p-toluenesulfonic acid are gradually added, and the mixture is reacted for 40~60min, then taken out, filtered, washed, and dried to obtain hyperbranched polyester-modified silver ion-loaded diatomite material. This material has a strong adsorption capacity for heavy metal ions and organic pollutants in printing and dyeing wastewater, but does not have the ability to separate saturated fatty acids and unsaturated fatty acids, and cannot be used for the separation of fatty acids. Summary of the Invention

[0006] The purpose of the present invention is to overcome the problem of poor separation effect of existing fatty acid separation adsorbents and to provide a preparation method of the fatty acid separation adsorbent.

[0007] The specific plan is as follows:

[0008] A method for preparing a fatty acid separation adsorbent comprises the following steps:

[0009] 1) mixing a carrier and a solvent, heating, adjusting the pH, and stirring to obtain a carrier solution; dissolving an aminosilane coupling agent in the solvent, stirring to obtain a carrier solution, and then adding the mixture to the carrier solution. After heating under reflux, washing, filtering, and drying are performed to obtain a modified carrier material;

[0010] 2) Take the modified support material and dissolve it in dioxane, then add AlCl3 ethanol solution containing carbon disulfide, stir evenly and filter, wash with dioxane and deionized water and detect until there is no Cl - , vacuum drying was performed to obtain Al 3+ / modified support material, wherein Al 3+ Accounting for the Al 3+ / 1.1-14.3% of the total weight of the modified support material;

[0011] 3) Take the Al3+ / The modified carrier material is added to a solvent, and silver halide is added. The mixture is shielded from light and stirred evenly. The mixture is filtered, washed, and detected to be free of halide ions. The mixture is vacuum dried to obtain a fatty acid separation adsorbent.

[0012] Furthermore, the carrier in step 1) is at least one of activated clay, diatomaceous earth, MCM-41, ZSM-5, and MCM-49;

[0013] Optionally, the aminosilane coupling agent is one of: aminoethylaminopropyltriethoxysilane; 3-aminopropyldimethoxymethylsilane; N,N-dimethyl-3-aminopropyltrimethoxysilane; 3-aminopropyldiethoxymethylsilane;

[0014] Optionally, the mass ratio of the carrier to the aminosilane coupling agent is 1:(0.4-0.8), preferably 1:(0.5-0.7).

[0015] Furthermore, the solvent is any one of acetone, ethanol, butanol, and ether;

[0016] Preferably, in step 1), the carrier and the solvent are mixed and heated to 40-50° C., the pH is adjusted to 9-10.5, and stirred for 2-10 hours to obtain the carrier solution;

[0017] Preferably, the aminosilane coupling agent is dissolved in the solvent, stirred evenly, and then added to the carrier solution. After heating to 50-80° C. and reflux for 5-24 hours, the solution is washed with anhydrous ethanol until neutral, filtered, and dried at 50-100° C. for 5-24 hours to obtain the modified carrier material.

[0018] Furthermore, the mass ratio of the modified support material to dioxane in step 2) is 1:(1-3);

[0019] Preferably, the concentration of AlCl3 in the AlCl3 ethanol solution is 5-20wt%, and the concentration of carbon disulfide is 0.5-5wt%.

[0020] Furthermore, the mass ratio of the modified support material to the AlCl3 ethanol solution in step 2) is 1:(0.5-7.5), preferably 1:(2-5).

[0021] Furthermore, in step 3), the silver halide is AgF, and the Al 3+ The mass ratio of the modified carrier material to AgF is 1:0.01-0.15, preferably 1:0.08-0.12.

[0022] The present invention also protects the fatty acid separation adsorbent prepared by the preparation method of the fatty acid separation adsorbent.

[0023] Furthermore, the separation rate of the fatty acid separation adsorbent for saturated fatty acids is above 92%.

[0024] Furthermore, the fatty acid separation adsorbent has a separation rate of more than 85% for monounsaturated fatty acids and a separation rate of more than 82% for polyunsaturated fatty acids.

[0025] The present invention also protects the use of the fatty acid separation adsorbent in fatty acid separation.

[0026] Beneficial effects: The preparation method of the fatty acid separation adsorbent of the present invention modifies the carrier material, which can improve the binding force of the carrier material. On this basis, the metal loading object can be combined more stably.

[0027] Furthermore, in the present invention, the modified carrier is first loaded with Al 3+ , through chemical reaction, Al 3+ The aluminum is bound to the active sites on the support, which is better than physical adsorption. However, since the intermediate products produced during the chemical reaction will cover the support, the adsorption separation effect is reduced. By controlling the reaction conditions, the aluminum loading is made to account for the Al 3+ / 1.1-14.3% of the total weight of the modified carrier material can avoid the adverse effects of aluminum-containing insoluble matter on the adsorption performance of the material.

[0028] Furthermore, the present invention is loaded with Al 3+ On this basis, Ag+ is complexed with the π bond in the material to form a bimetallic complex, which makes the material have a large difference in adsorption capacity for saturated fatty acids and unsaturated fatty acids, monounsaturated fatty acids and polyunsaturated fatty acids, thereby realizing the separation of fatty acids.

[0029] In summary, the fatty acid separation adsorbent prepared by the present invention has a significant effect on distinguishing fatty acids of different saturations, and the higher the unsaturation, the easier it is to be adsorbed. Therefore, the order of fatty acids eluting from a chromatography column equipped with the separation adsorbent prepared by the method of the present invention is: saturated fatty acids, monounsaturated fatty acids, and polyunsaturated fatty acids. Utilizing the bimetallic ion complex adsorbent prepared by the present invention, it is possible to achieve the fractional separation of saturated fatty acids, monounsaturated fatty acids, and polyunsaturated fatty acids in fatty acids. Compared to other methods that can only separate saturated fatty acids from unsaturated fatty acids, or require multiple separations to achieve the fractional separation of unsaturated fatty acids, the present invention has the advantages of achieving fractional separation of fatty acids in one step, a simple process, and high product purity. DETAILED DESCRIPTION

[0030] The preferred embodiments of the present invention will be described in more detail below. Although the preferred embodiments of the present invention are described below, it should be understood that the present invention can be implemented in various forms and should not be limited by the embodiments set forth herein. In the examples, if specific techniques or conditions are not specified, the techniques or conditions described in the literature in this area or the product specifications are used. Reagents or instruments used that do not specify the manufacturer are conventional products that can be obtained commercially. In the following examples, if not clearly stated, "%" refers to weight percentage.

[0031] The main reagents used include:

[0032] The fatty acid sample to be separated is a mixed fatty acid, and the main components and mass proportions are as follows: saturated fatty acids account for 30% by mass, unsaturated fatty acids account for 65.54%, of which monounsaturated fatty acids account for 37.21% and polyunsaturated fatty acids account for 28.33%.

[0033] Example 1

[0034] A method for preparing a fatty acid separation adsorbent, the main steps are as follows:

[0035] 1) At 40°C, 20 g of activated clay (AC) was added to 60 g of acetone. The pH was adjusted to 10 and stirred thoroughly for 4 hours. 8 g of aminoethylaminopropyltriethoxysilane (aminosilane coupling agent, SCA) was dissolved in an appropriate amount of ethanol, stirred thoroughly, and slowly added dropwise to the mixture. The mixture was refluxed at 60°C for 12 hours, then washed with anhydrous ethanol until neutral and filtered. Drying was performed at 80°C for 12 hours to produce the SCA-AC modified support material.

[0036] 2) Weigh 20 g of SCA-AC and dissolve it in 40 g of dioxane. Then add 10 g of anhydrous AlCl3 ethanol solution containing 2 wt% carbon disulfide (concentration is 11 wt%, the same below), stir thoroughly for 3 hours, filter, wash with dioxane and deionized water, and detect until there is no Cl3. - After vacuum drying at 105℃ for 10 hours, the single metal ion complex material Al 3+ / SCA-AC, where Al 3+ It accounts for 1.1% of the total weight of the single metal ion complex material.

[0037] 3) Weigh 20g of Al 3+ / SCA-AC was dissolved in 40 g of acetone and stirred evenly, then 0.2 g of AgF4 was added, stirred for 10 h in a dark place, filtered, and washed with acetone and deionized water until no F was found. - , vacuum dried at 100℃ for 6 hours to obtain fatty acid separation adsorbent, bimetallic ion complex material Ag + -Al3+ / SCA-AC.

[0038] The fatty acid sample to be separated was taken and separated by a chromatography column (chromatographic column size: outer diameter 20 mm, length 300 mm, wet column packing, column height 220 mm, eluent: n-hexane) containing the above-mentioned separation adsorbent. The separation rate of fatty acids was: saturated fatty acids 92.1%; monounsaturated fatty acids 87.2%; polyunsaturated fatty acids 83.6%.

[0039] Example 2

[0040] A method for preparing a fatty acid separation adsorbent, the main steps are as follows:

[0041] 1) 20 g of DE (diatomaceous earth) was added to 60 g of acetone at 50°C, the pH adjusted to 10, and stirred thoroughly for 4 hours. 16 g of 3-aminopropyldimethoxymethylsilane was dissolved in an appropriate amount of ethanol, stirred thoroughly, and slowly added dropwise to the mixture. The mixture was refluxed at 60°C for 12 hours, then washed with anhydrous ethanol until neutral, and filtered. Drying was performed at 80°C for 12 hours to obtain an SCA-DE modified support material.

[0042] 2) Weigh 20 g of SCA-DE and dissolve it in 40 g of dioxane. Then add 150 g of anhydrous AlCl3 ethanol solution containing 2 wt% carbon disulfide, stir thoroughly for 3 hours, filter, and wash with dioxane and deionized water until there is no Cl3. - After vacuum drying at 105℃ for 10 hours, the single metal ion complex material Al 3+ / SCA-DE, where Al 3+ It accounts for 14.3% of the total weight of the single metal ion complex material.

[0043] 3) Weigh 20g of Al 3+ / SCA-DE was dissolved in 40 g of acetone, stirred evenly, and then 3 g of AgF4 was added. The mixture was stirred for 16 hours in a dark place, filtered, and washed with acetone and deionized water until no F was found. - , vacuum dried at 100℃ for 6 hours to obtain fatty acid separation adsorbent, bimetallic ion complex material Ag + -Al 3+ / SCA-DE.

[0044] Fatty acid separation test Referring to Example 1, after separation using a chromatography column loaded with the separation adsorbent prepared in this example, the separation rates of fatty acids were: 94.5% for saturated fatty acids; 93.5% for monounsaturated fatty acids; and 89.3% for polyunsaturated fatty acids.

[0045] Example 3

[0046] A method for preparing a fatty acid separation adsorbent, the main steps are as follows:

[0047] 1) At 40°C, 20 g of MCM-41 (nanostructured material) was added to 60 g of acetone. The pH was adjusted to 10 and stirred thoroughly for 4 hours. Then, 12 g of N,N-dimethyl-3-aminopropyltrimethoxysilane was dissolved in an appropriate amount of ethanol, stirred thoroughly, and slowly added dropwise to the mixture. The mixture was refluxed at 60°C for 12 hours, then washed with anhydrous ethanol until neutral and filtered. Drying was performed at 80°C for 12 hours to obtain the SCA-MCM-41 modified support material.

[0048] 2) Weigh 20 g of SCA-MCM-41 and dissolve it in 40 g of dioxane. Then add 50 g of anhydrous AlCl3 ethanol solution containing 2 wt% carbon disulfide, stir thoroughly for 3 hours, filter, and wash with dioxane and deionized water until there is no Cl3. - After vacuum drying at 105℃ for 10 hours, the single metal ion complex material Al 3+ / SCA-MCM-41.

[0049] 3) Weigh 20g of Al 3+ / SCA-MCM-41 was dissolved in 40 g of acetone and stirred evenly, then 1.6 g of AgF4 was added, stirred for 12 hours in a dark place, filtered, and washed with acetone and deionized water until no F was found. - , vacuum dried at 100℃ for 6 hours to obtain fatty acid separation adsorbent, bimetallic ion complex material Ag + -Al 3+ / SCA-MCM-41.

[0050] Fatty acid separation test Referring to Example 1, after separation using a chromatography column loaded with the separation adsorbent prepared in this example, the separation rates of fatty acids were: 98.8% for saturated fatty acids; 85.1% for monounsaturated fatty acids; and 85.7% for polyunsaturated fatty acids.

[0051] Example 4

[0052] A method for preparing a fatty acid separation adsorbent, the main steps are as follows:

[0053] 1) At 45°C, 20 g of ZSM-5 (zeolite molecular sieve) was added to 60 g of acetone, the pH was adjusted to 10, and the mixture was stirred thoroughly for 4 hours. Then, 10 g of 3-aminopropyldiethoxymethylsilane was dissolved in an appropriate amount of ethanol, stirred evenly, and slowly added dropwise to the mixture. The mixture was refluxed at 60°C for 12 hours, then washed with anhydrous ethanol until neutral, and filtered. Drying was performed at 80°C for 12 hours to obtain an SCA-ZSM-5 modified support material.

[0054] 2) Weigh 20 g of SCA-ZSM-5 and dissolve it in 40 g of dioxane. Then add 80 g of anhydrous AlCl3 ethanol solution containing 2 wt% carbon disulfide, stir thoroughly for 3 hours, filter, and wash with dioxane and deionized water until there is no Cl - After vacuum drying at 105℃ for 10 hours, the single metal ion complex material Al 3+ / SCA-ZSM-5.

[0055] 3) Weigh 20g of Al 3+ / SCA-ZSM-5 was dissolved in 40 g of acetone and stirred evenly, then 2.0 g of AgF4 was added, stirred for 14 hours in a dark place, filtered, and washed with acetone and deionized water until no F was found. - , vacuum dried at 100℃ for 6 hours to obtain fatty acid separation adsorbent, bimetallic ion complex material Ag + -Al 3+ / SCA-ZSM-5.

[0056] Fatty acid separation test Referring to Example 1, after separation using a chromatography column loaded with the separation adsorbent prepared in this example, the separation rates of fatty acids were: 96.4% for saturated fatty acids; 86.7% for monounsaturated fatty acids; and 90.3% for polyunsaturated fatty acids.

[0057] Example 5

[0058] A method for preparing a fatty acid separation adsorbent, the main steps are as follows:

[0059] 1) At 45°C, 20 g of MCM-49 (molecular sieve) was added to 60 g of acetone, the pH was adjusted to 10, and the mixture was stirred thoroughly for 4 hours. 8 g of 3-aminopropyldiethoxymethylsilane was dissolved in an appropriate amount of ethanol, stirred thoroughly, and slowly added dropwise to the mixture. The mixture was refluxed at 60°C for 12 hours, then washed with anhydrous ethanol until neutral, and filtered. Drying was performed at 80°C for 12 hours to obtain the SCA-MCM-49 modified support material.

[0060] 2) Weigh 20 g of SCA-MCM-49 and dissolve it in 40 g of dioxane. Then add 100 g of anhydrous AlCl3 ethanol solution containing 2 wt% carbon disulfide, stir thoroughly for 3 hours, filter, wash with dioxane and deionized water, and detect until there is no Cl - After vacuum drying at 105℃ for 10 hours, the single metal ion complex material Al 3+ / SCA-MCM-49.

[0061] 3) Weigh 20g of Al 3+ / SCA-MCM-49 was dissolved in 40 g of acetone and stirred evenly. Then 1.0 g of AgF4 was added. The mixture was stirred for 10 hours in a dark place. The mixture was filtered and washed with acetone and deionized water until no AgF4 was found. - , vacuum dried at 100℃ for 6 hours to obtain fatty acid separation adsorbent, bimetallic ion complex material Ag + -Al 3+ / SCA-MCM-49.

[0062] Fatty acid separation test Referring to Example 1, after separation using a chromatography column loaded with the separation adsorbent prepared in this example, the separation rates of fatty acids were: 93.2% for saturated fatty acids; 90.6% for monounsaturated fatty acids; and 89.5% for polyunsaturated fatty acids.

[0063] Example 6

[0064] A method for preparing a fatty acid separation adsorbent, the main steps are as follows:

[0065] 1) At 50°C, 20 g of ZSM-5 was added to 60 g of acetone, the pH was adjusted to 10, and the mixture was stirred thoroughly for 4 hours. 8 g of N,N-dimethyl-3-aminopropyltrimethoxysilane was dissolved in an appropriate amount of ethanol, stirred thoroughly, and slowly added dropwise to the mixture. The mixture was refluxed at 60°C for 12 hours, then washed with anhydrous ethanol until neutral, and filtered. Drying was performed at 80°C for 12 hours to obtain the SCA-ZSM-5 modified support material.

[0066] 2) Weigh 20 g of SCA-ZSM-5 and dissolve it in 40 g of dioxane. Then add 20 g of anhydrous AlCl3 ethanol solution containing 2 wt% carbon disulfide, stir thoroughly for 3 hours, filter, and wash with dioxane and deionized water until there is no Cl - After vacuum drying at 105℃ for 10 hours, the single metal ion complex material Al 3+ / SCA-ZSM-5.

[0067] 3) Weigh 20g of Al 3+ / SCA-ZSM-5 was dissolved in 40 g of acetone and stirred evenly, then 3.0 g of AgF4 was added, stirred for 16 hours in a dark place, filtered, and washed with acetone and deionized water until no F was found. - , vacuum dried at 100℃ for 6 hours to obtain fatty acid separation adsorbent, bimetallic ion complex material Ag + -Al 3+ / SCA-ZSM-5.

[0068] Fatty acid separation test Referring to Example 1, after separation using a chromatography column loaded with the separation adsorbent prepared in this example, the separation rates of fatty acids were: 91.7% for saturated fatty acids; 92.7% for monounsaturated fatty acids; and 82.5% for polyunsaturated fatty acids.

[0069] Comparative Example 1

[0070] Refer to Example 2, the difference is that the loaded Al 3+ Too high, the main steps are as follows:

[0071] 1) 20 g of DE (diatomaceous earth) was added to 60 g of acetone at 50°C, the pH adjusted to 10, and stirred thoroughly for 4 hours. 16 g of 3-aminopropyldimethoxymethylsilane was dissolved in an appropriate amount of ethanol, stirred thoroughly, and slowly added dropwise to the mixture. The mixture was refluxed at 60°C for 12 hours, then washed with anhydrous ethanol until neutral, and filtered. Drying was performed at 80°C for 12 hours to obtain an SCA-DE modified support material.

[0072] 2) Weigh 20 g of SCA-DE and dissolve it in 40 g of dioxane. Then add 200 g of anhydrous AlCl3 ethanol solution containing 2 wt% carbon disulfide, stir thoroughly for 3 hours, filter, wash with dioxane and deionized water, and detect until there is no Cl3. - After vacuum drying at 105℃ for 10 hours, the single metal ion complex material Al 3+ / SCA-DE, where Al 3+ It accounts for 18.2% of the total weight of the single metal ion complex material.

[0073] 3) Weigh 20g of Al 3+ / SCA-DE was dissolved in 40 g of acetone, stirred evenly, and then 3 g of AgF4 was added. The mixture was stirred for 16 hours in a dark place, filtered, and washed with acetone and deionized water until no F was found. - , vacuum dried at 100℃ for 6 hours to obtain fatty acid separation adsorbent, bimetallic ion complex material Ag + -Al 3+ / SCA-DE.

[0074] Fatty acid separation test Referring to Example 1, after separation using a chromatography column loaded with the separation adsorbent prepared in this example, the separation rates of fatty acids were: 82.7% for saturated fatty acids; 88.5% for monounsaturated fatty acids; and 75.2% for polyunsaturated fatty acids.

[0075] Comparative Example 2

[0076] Refer to Example 2, except that Al is not loaded 3+ The main steps are as follows:

[0077] 1) 20 g of DE (diatomaceous earth) was added to 60 g of acetone at 50°C, the pH adjusted to 10, and stirred thoroughly for 4 hours. 16 g of 3-aminopropyldimethoxymethylsilane was dissolved in an appropriate amount of ethanol, stirred thoroughly, and slowly added dropwise to the mixture. The mixture was refluxed at 60°C for 12 hours, then washed with anhydrous ethanol until neutral, and filtered. Drying was performed at 80°C for 12 hours to obtain an SCA-DE modified support material.

[0078] 2) Weigh 20g of SCA-DE in 40g of acetone, stir evenly, add 3g of AgF4, shield from light and stir for 16 hours, filter, wash with acetone and deionized water, and detect until there is no F4. - , and vacuum dried at 100°C for 6 hours to obtain a fatty acid separation adsorbent.

[0079] Fatty acid separation test Referring to Example 2, after separation using a chromatography column loaded with the separation adsorbent prepared in this example, the separation rates of fatty acids were: saturated fatty acids 70.1%; monounsaturated fatty acids 82.5%; and polyunsaturated fatty acids 66.5%.

[0080] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the scope of protection of the present invention.

[0081] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any appropriate manner without contradiction. To avoid unnecessary repetition, the present invention will not further describe various possible combinations.

[0082] In addition, the various embodiments of the present invention may be arbitrarily combined, and as long as they do not violate the concept of the present invention, they should also be regarded as the contents disclosed by the present invention.

Claims

1. A method for preparing a fatty acid separation adsorbent, characterized in that: The following steps are involved: 1) mixing a carrier and a solvent, heating them, adjusting the pH, and stirring them uniformly to obtain a carrier solution; dissolving an aminosilane coupling agent in the solvent, stirring them uniformly, and adding them to the carrier solution; heating them under reflux, washing them, filtering them, and drying them to obtain a modified carrier material; 2) Take the modified support material and dissolve it in dioxane, then add AlCl3 ethanol solution containing carbon disulfide, stir evenly and filter, wash with dioxane and deionized water and detect until there is no Cl - , vacuum drying was performed to obtain Al 3+ / modified support material, wherein Al 3+ Accounting for the Al 3+ / 1.1-14.3% of the total weight of the modified carrier material; 3) Take the Al 3+ / The modified carrier material is added to a solvent, and silver halide is added. The mixture is shielded from light and stirred evenly. The mixture is filtered, washed, and detected to be free of halide ions. The mixture is vacuum dried to obtain a fatty acid separation adsorbent.

2. The method for preparing a fatty acid separation adsorbent according to claim 1, wherein: The carrier in step 1) is at least one of activated clay, diatomaceous earth, MCM-41, ZSM-5, and MCM-49.

3. The method for preparing the fatty acid separation adsorbent according to claim 2, wherein: The aminosilane coupling agent is one of aminoethylaminopropyltriethoxysilane, 3-aminopropyldimethoxymethylsilane, N,N-dimethyl-3-aminopropyltrimethoxysilane and 3-aminopropyldiethoxymethylsilane.

4. The method for preparing the fatty acid separation adsorbent according to claim 2, wherein: The mass ratio of the carrier to the aminosilane coupling agent is 1:(0.4-0.8).

5. The method for preparing the fatty acid separation adsorbent according to claim 4, wherein: The mass ratio of the carrier to the aminosilane coupling agent is 1:(0.5-0.7).

6. The method for preparing the fatty acid separation adsorbent according to claim 1, wherein: The solvent is any one of acetone, ethanol, butanol and ether.

7. The method for preparing the fatty acid separation adsorbent according to claim 6, wherein: In step 1), the carrier and the solvent are mixed and heated to 40-50° C., the pH is adjusted to 9-10.5, and stirred for 2-10 hours to obtain the carrier solution.

8. The method for preparing the fatty acid separation adsorbent according to claim 6, wherein: The aminosilane coupling agent is dissolved in the solvent, stirred evenly, and then added to the carrier solution. The solution is heated to 50-80° C. and refluxed for 5-24 hours. The solution is then washed with anhydrous ethanol until neutral, filtered, and dried at 50-100° C. for 5-24 hours to obtain the modified carrier material.

9. The method for preparing the fatty acid separation adsorbent according to claim 1, wherein: The mass ratio of the modified support material to dioxane in step 2) is 1:(1-3).

10. The method for preparing the fatty acid separation adsorbent according to claim 9, wherein: The concentration of AlCl 3 in the AlCl 3 ethanol solution is 5-20 wt %, and the concentration of carbon disulfide is 0.5-5 wt %.

11. The method for preparing the fatty acid separation adsorbent according to claim 9, wherein: The mass ratio of the modified support material to the AlCl3 ethanol solution in step 2) is 1: (0.5-7.5).

12. The method for preparing the fatty acid separation adsorbent according to claim 11, characterized in that: The mass ratio of the modified support material to the AlCl3 ethanol solution in step 2) is 1:(2-5).

13. The method for preparing the fatty acid separation adsorbent according to claim 1, wherein: In step 3), the silver halide is AgF, and the Al 3+ / The mass ratio of modified carrier material to AgF is 1:0.01-0.

15.

14. The method for preparing the fatty acid separation adsorbent according to claim 13, wherein: In step 3), the silver halide is AgF, and the Al 3+ / The mass ratio of modified carrier material to AgF is 1:0.08-0.

12.

15. The fatty acid separation adsorbent prepared by the method for preparing the fatty acid separation adsorbent according to any one of claims 1 to 14.

16. Use of the fatty acid separation adsorbent according to claim 15 in fatty acid separation.

17. Use of the fatty acid separation adsorbent according to claim 16 in fatty acid separation, characterized in that: The separation rate of the fatty acid separation adsorbent for saturated fatty acids is above 92%.

18. Use of the fatty acid separation adsorbent according to claim 16 or 17 in fatty acid separation, characterized in that: The fatty acid separation adsorbent has a separation rate of more than 85% for monounsaturated fatty acids and a separation rate of more than 82% for polyunsaturated fatty acids.

Citation Information

Patent Citations

  • Preparation method of hyperbranched polyester modified silver ion-loaded diatomite

    CN111944162A

  • Method for separating EPA (eicosapentaenoic acid) and DHA (docosahexaenoic acid) by using silver ion modified amino silica gel

    CN103962091A

  • Immobilized bimetallic catalyst as well as preparation method and application thereof

    CN112898555A