Magnetic induction heating organic solvent dehydrating agent as well as preparation method and application thereof

By using magnetic induction heating technology, metal nanoparticles are heated within porous materials using an alternating magnetic field. This solves the problems of heat transfer lag and heat loss in traditional heating methods, and achieves efficient and low-energy organic solvent dehydration.

CN121016712APending Publication Date: 2025-11-28NANJING TECH UNIV
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Patent Information

Application Number
CN202511025321.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-07-24
Publication Date
2025-11-28

AI Technical Summary

Technical Problem

Traditional adsorbent regeneration processes rely on external hot air circulation for heating, which results in heat transfer lag and localized uncontrolled temperature rise, leading to crystal lattice collapse of the dehydrating agent and reduced dehydration efficiency.

Method used

The magnetic induction heating technology is used to mix metal or metal oxide nanoparticles with dehydrating agents and binders, and use an alternating magnetic field to make the nanoparticles heat up in the porous material, thereby achieving in-situ heat regeneration and avoiding heat loss.

Benefits of technology

It achieves low-energy consumption and high-efficiency dehydration, with fast thermal response rate, short heat transfer path, high energy conversion rate, and energy consumption reduction of more than 25%.

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Abstract

The invention relates to the technical field of dehydration treatment, and discloses a magnetic induction heating organic solvent dehydrating agent and a preparation method and application thereof.The preparation method comprises the steps that metal or metal oxide nanoparticles are mixed with hydrogen peroxide, surface modification is conducted on the metal or metal oxide nanoparticles, and modified metal or metal oxide nanoparticles are obtained; mixing the modified metal or metal oxide nanoparticles with a dehydrating agent and a binder to obtain slurry of the magnetic induction heating organic solvent dehydrating agent; and molding the slurry of the magnetic induction heating organic solvent dehydrating agent, and then roasting to obtain the magnetic induction heating organic solvent dehydrating agent. The magnetic induction heating organic solvent dehydrating agent prepared by the invention has the advantage of remarkable low energy consumption in the field of organic solvent dehydration, realizes in-situ regeneration of heat through an alternating magnetic field, is high in heating rate, short in heat transfer path and high in energy utilization rate, and reduces the energy consumption by more than 25% compared with a traditional high-temperature gas heating method.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of dehydration treatment, in particular to a magnetic induction heating organic solvent dehydrating agent and a preparation method and application thereof. BACKGROUND

[0002] Solvent dehydration is a basic process in industrial production. The presence of water in organic solvents not only causes microbial contamination, but also leads to product deterioration, pipeline blockage and other hazards, seriously affecting the safety and efficiency of the process. Adsorption separation technology selectively captures bound water and crystallization water in the material by active oxide dehydrating agent, which is the core means to achieve efficient and energy-saving dehydration.

[0003] Traditional adsorbent regeneration process relies on external hot air circulation heating, which has problems such as heat transfer lag, local temperature rise out of control leading to collapse of the dehydrating agent crystal lattice, and reduction of the dehydration efficiency of the dehydrating agent. Preparing new active oxide dehydrating agents and developing high-efficiency thermal desorption technology based on new materials are the key to solving the above problems.

[0004] Therefore, it is of great practical significance to provide a magnetic induction heating organic solvent dehydrating agent with high regeneration rate and a preparation method and application thereof. SUMMARY

[0005] In view of this, the present application provides a magnetic induction heating organic solvent dehydrating agent and a preparation method and application thereof, aiming to solve at least one of the above technical problems.

[0006] The present application provides a preparation method of a magnetic induction heating organic solvent dehydrating agent, comprising the following steps:

[0007] Mixing metal or metal oxide nanoparticles with hydrogen peroxide to modify the surface of the metal or metal oxide nanoparticles to obtain modified metal or metal oxide nanoparticles;

[0008] Mixing the modified metal or metal oxide nanoparticles with a dehydrating agent and a binder to obtain a slurry of the magnetic induction heating organic solvent dehydrating agent;

[0009] Forming the slurry of the magnetic induction heating organic solvent dehydrating agent, and then calcining to obtain the magnetic induction heating organic solvent dehydrating agent.

[0010] Preferably, the metal or metal oxide nanoparticles are Fe3O4, gamma-Fe2O3, CuFe2O4, Cu3Fe4O9, Mn x Zn 1-x Fe2O4(0≤x≤1), Ni x Zn 1-x Fe2O4(0≤x≤1), Zn 1-x Mo xFe2O4(0≤x≤1), CoFe2O4, Li 0.5 Fe 2.5 O4, Mg 1-x Ni x Fe2O4 (0≤x≤1), BaFe 12 O 19 FeB 23 C 0.05 FeB 16 C 1.0 FeCo 35 FeCo 50 Ni 70 Fe 30 Ni 50 Fe 50 Ni 30 Fe 70 FeCr 55 FeMn 78 C 8.0 FeMn 82 C 1.0 FeMo 65 The metal or metal oxide nanoparticles are one or more of FeSiAl or stainless steel, and the morphology of the nanoparticles is spherical, cubic or spindle-shaped, with a particle size of 3nm-300μm.

[0011] Preferably, the ratio of the metal or metal oxide nanoparticles to hydrogen peroxide is 1g:4-8mL; and the concentration of the hydrogen peroxide is 15%.

[0012] Preferably, the surface modification conditions are: temperature 40°C and time 3 hours.

[0013] Preferably, the dehydrating agent is one or more of SiO2, γ-Al2O3, ZnO, Fe2O3·nH2O, TiO2, or SnO2; the binder is one or more of bentonite, kaolin, attapulgite, clay mineral, silica sol, alumina sol, aluminum dihydrogen phosphate, aluminate cement, water glass, phosphate cement, or ceramic clay.

[0014] Preferably, the mass ratio of the modified metal or metal oxide nanoparticles to the dehydrating agent and binder is (2-4):(5-3):3.

[0015] Preferably, the molding method is extrusion molding or ball rolling molding, and the particle size of the slurry after molding is 3-5 mm; the calcination conditions are: temperature of 500℃ and time of 2h.

[0016] The present invention also provides a magnetic induction heating organic solvent dehydrating agent, which is obtained by the preparation method described in the above technical solution.

[0017] The present invention also provides the application of the magnetic induction heating organic solvent dehydrating agent described in the above technical solution, wherein the application is in the dehydration of organic solvents.

[0018] The present invention also provides a method for regenerating the magnetic induction heating organic solvent dehydrating agent described in the above technical solution. The regeneration method specifically involves: placing the dehydrating agent in an induction coil, generating an alternating magnetic field by applying electricity, and causing the metal / metal oxide nanoparticles to desorb water molecules through magnetic induction heating; the frequency of the alternating magnetic field is 50Hz-10MHz, the power is 100-5000W, and the regeneration temperature is 100-550℃.

[0019] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0020] The magnetic induction heating organic solvent dehydrating agent prepared by this invention exhibits significant low-energy consumption advantages in the field of organic solvent dehydration. It achieves in-situ efficient heat regeneration using an alternating magnetic field, possessing advantages such as fast thermal response rate, short heat conduction path, and high energy conversion rate, reducing energy consumption by more than 25% compared to traditional high-temperature gas heating methods. This is attributed to the synergistic effect of raw material selection and preparation process: dehydrating agents such as SiO2 and γ-Al2O3 have high specific surface area and abundant porous structures, providing ample sites for water adsorption; metal or metal oxide nanoparticles are dispersed within the porous material, directly converting electromagnetic energy into heat energy through hysteresis loss and eddy current effect in the alternating magnetic field. Furthermore, the particle size of 3nm-300μm and spherical and cubic morphologies increase the contact area, ensuring rapid heat transfer. During regeneration, heat diffuses from the metal or metal oxide nanoparticles inside the dehydrating agent to the surface, resulting in a short heat transfer path and avoiding heat loss associated with traditional high-temperature gas heating methods. Detailed Implementation

[0021] Various exemplary embodiments of the present invention will now be described in detail. This detailed description should not be considered as a limitation of the present invention, but rather as a more detailed description of certain aspects, features, and embodiments of the present invention. It should be understood that the terminology used in this invention is merely for describing particular embodiments and is not intended to limit the present invention.

[0022] Furthermore, regarding the numerical ranges in this invention, it should be understood that each intermediate value between the upper and lower limits of the range is also specifically disclosed. Every smaller range between any stated value or intermediate value within a stated range, and any other stated value or intermediate value within said range, is also included within this invention. The upper and lower limits of these smaller ranges may be independently included or excluded from the range.

[0023] Unless otherwise stated, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. While only preferred methods and materials have been described herein, any methods and materials similar or equivalent to those described herein may be used in the implementation or testing of this invention. All references to this specification are incorporated by way of citation to disclose and describe methods and / or materials associated with those references. In the event of any conflict with any incorporated reference, the content of this specification shall prevail.

[0024] Various modifications and variations can be made to the specific embodiments described in this specification without departing from the scope or spirit of the invention, as will be apparent to those skilled in the art. Other embodiments derived from this specification will also be apparent to those skilled in the art. This specification and embodiments are merely exemplary.

[0025] The terms “include,” “including,” “have,” “contain,” etc., used in this article are all open-ended terms, meaning that they include but are not limited to.

[0026] This invention proposes a method for preparing a magnetic induction heating organic solvent dehydrating agent, comprising the following steps:

[0027] Metal or metal oxide nanoparticles are mixed with hydrogen peroxide to modify the surface of the metal or metal oxide nanoparticles, thereby obtaining modified metal or metal oxide nanoparticles.

[0028] The modified metal or metal oxide nanoparticles are mixed with a dehydrating agent and a binder to obtain a slurry of a magnetic induction heating organic solvent dehydrating agent.

[0029] The slurry of the magnetic induction heating organic solvent dehydrating agent is shaped and then calcined to obtain the magnetic induction heating organic solvent dehydrating agent.

[0030] This invention modifies metal or metal oxide nanoparticles with hydrogen peroxide, filters them, washes them three times with anhydrous ethanol, and finally dries them to obtain the modified metal or metal oxide nanoparticles.

[0031] In this invention, the metal or metal oxide nanoparticles are preferably Fe3O4, γ-Fe2O3, CuFe2O4, Cu3Fe4O9, or Mn. x Zn 1-x Fe2O4 (0≤x≤1), Ni x Zn 1-x Fe2O4 (0≤x≤1), Zn 1-x Mo x Fe2O4(0≤x≤1), CoFe2O4, Li 0.5 Fe2.5 O4, Mg1-xNi x Fe2O4 (0≤x≤1), BaFe 12 O 19 FeB 23 C 0.05 FeB 16 C 1.0 FeCo 35 FeCo 50 Ni 70 Fe 30 Ni 50 Fe 50 Ni 30 Fe 70 FeCr 55 FeMn 78 C 8.0 FeMn 82 C 1.0 FeMo 65 The metal or metal oxide nanoparticles are one or more of FeSiAl or stainless steel, and the morphology of the nanoparticles is spherical, cubic or spindle-shaped, with a particle size of 3nm-300μm.

[0032] The stainless steel used in this invention is preferably 316 stainless steel or 304 stainless steel.

[0033] In this invention, the preferred ratio of the metal or metal oxide nanoparticles to hydrogen peroxide is 1g:4-8mL, more preferably 1g:4-6mL; the concentration of the hydrogen peroxide is 15%.

[0034] In this invention, the preferred conditions for surface modification are: a temperature of 40°C and a time of 3 hours.

[0035] In this invention, the dehydrating agent is preferably one or more of SiO2, γ-Al2O3, ZnO, Fe2O3·nH2O, TiO2, or SnO2; the binder is preferably one or more of bentonite, kaolin, attapulgite, clay mineral, silica sol, alumina sol, aluminum dihydrogen phosphate, aluminate cement, water glass, phosphate cement, or ceramic clay.

[0036] In this invention, the preferred mass ratio of the modified metal or metal oxide nanoparticles to the dehydrating agent and binder is (2-4):(5-3):3.

[0037] In this invention, the molding method is preferably extrusion molding or ball rolling molding, and the particle size of the slurry after molding is 3-5 mm; the calcination conditions are preferably: temperature of 500℃ and time of 2h.

[0038] The present invention also provides a magnetic induction heating organic solvent dehydrating agent, which is obtained by the preparation method described in the above technical solution.

[0039] The present invention also provides the application of the magnetic induction heating organic solvent dehydrating agent described in the above technical solution, wherein the application is in the dehydration of organic solvents.

[0040] The present invention also provides a method for regenerating the magnetic induction heating organic solvent dehydrating agent described in the above technical solution. The regeneration method specifically involves: placing the dehydrating agent in an induction coil, generating an alternating magnetic field by applying electricity, and causing the metal / metal oxide nanoparticles to desorb water molecules through magnetic induction heating; the frequency of the alternating magnetic field is 50Hz-10MHz, the power is 100-5000W, and the regeneration temperature is 100-550℃.

[0041] Example 1

[0042] (1) Fe3O4 nanoparticles were mixed with 15% hydrogen peroxide at a ratio of 1g:4mL, stirred at a constant speed of 40℃ for 3h, filtered after the reaction was completed, washed three times with anhydrous ethanol, and dried to obtain modified Fe3O4 nanoparticles.

[0043] (2) The modified Fe3O4 nanoparticles obtained in step (1) are mixed with γ-Al2O3 and kaolin in a mass ratio of 2:5:3, stirred in 20mL of deionized water for 2h, filtered, and a slurry of magnetic induction heating organic solvent dehydrating agent is obtained.

[0044] (3) The slurry obtained in step (2) is extruded to form a particle size of 3.0 mm, and then calcined at 500°C for 2 h in a nitrogen atmosphere to obtain a granular magnetic induction heating organic solvent dehydrating agent.

[0045] Examples 2-9

[0046] The other steps are the same as in Example 1. The differences between Examples 2 to 9 and Example 1 are shown in Table 1.

[0047] Table 1 Raw material data for Examples 1-9

[0048]

[0049] Performance tests

[0050] The dehydrating agents prepared in Examples 1-9 were used to dehydrate n-pentanol, toluene, and n-butyl propionate containing trace amounts of water. 20g of the prepared dehydrating agent was loaded into the bed, and after the solution passed through the bed for 2 hours, desorption experiments were conducted using different heating methods. The desorption time was obtained by liquid chromatography. The conditions and results are shown in Tables 2-4. The dehydrating agents obtained in Examples 1, 6, and 9 were regenerated, and their dehydration rates were tested. The results are shown in Table 5.

[0051] Table 2. Desorption parameters and results of the dehydrating agent on aqueous n-pentanol.

[0052]

[0053]

[0054] Table 3. Desorption parameters and results of dehydrating agent on aqueous toluene.

[0055]

[0056] Table 4. Desorption parameters and results of the dehydrating agent on aqueous n-butyl propionate.

[0057]

[0058] Table 5 Comparison of dehydration efficiency of dehydrating agents after the same regeneration time (100 min)

[0059]

[0060]

[0061] As shown in Tables 2-5, under the same conditions, the desorption time of the dehydrating agent regenerated using magnetic induction heating is shorter than that of the traditional hot nitrogen heating method, indicating that magnetic induction heating has a higher regeneration efficiency. The desorption efficiency of magnetic induction heating is closely related to parameters such as the power and frequency of the magnetic field. Higher power and better frequency adaptability result in shorter desorption time. Optimizing the magnetic field parameters can further improve the regeneration effect. Meanwhile, the raw material ratio of the dehydrating agent affects the desorption effect. A reasonable ratio and particle size design can enhance the regeneration performance of the dehydrating agent. Furthermore, this dehydrating agent has strong adaptability to dehydration of different organic solvents and can maintain stable and efficient desorption capacity in different systems. This fully demonstrates the advantages of magnetic induction heating in the regeneration of organic solvent dehydrating agents: high efficiency, low energy consumption, and strong adaptability, significantly superior to the traditional hot nitrogen heating process.

[0062] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit it. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art should understand that modifications or equivalent substitutions can still be made to the specific implementation of the present invention. Any modifications or equivalent substitutions that do not depart from the spirit and scope of the present invention should be covered within the scope of protection of the claims of the present invention.

Claims

1. A method for preparing a magnetic induction heating organic solvent dehydrating agent, characterized in that, Includes the following steps: Metal or metal oxide nanoparticles are mixed with hydrogen peroxide to modify the surface of the metal or metal oxide nanoparticles, thereby obtaining modified metal or metal oxide nanoparticles. The modified metal or metal oxide nanoparticles are mixed with a dehydrating agent and a binder to obtain a slurry of a magnetic induction heating organic solvent dehydrating agent. The slurry of the magnetic induction heating organic solvent dehydrating agent is shaped and then calcined to obtain the magnetic induction heating organic solvent dehydrating agent.

2. The preparation method of the magnetic induction heating organic solvent dehydrating agent according to claim 1, characterized in that, The metal or metal oxide nanoparticles are Fe3O4, γ-Fe2O3, CuFe2O4, Cu3Fe4O9, Mn x Zn 1-x Fe2O4 (0≤x≤1), Ni x Zn 1-x Fe2O4 (0≤x≤1), Zn 1-x Mo x Fe2O4(0≤x≤1), CoFe2O4, Li 0.5 Fe 2.5 O4, Mg 1-x Ni x Fe2O4 (0≤x≤1), BaFe 12 O 19 FeB 23 C 0.05 FeB 16 C 1.0 FeCo 35 FeCo 50 Ni 70 Fe 30 Ni 50 Fe 50 Ni 30 Fe 70 FeCr 55 FeMn 78 C 8.0 FeMn 82 C 1.0 FeMo 65 The metal or metal oxide nanoparticles are one or more of FeSiAl or stainless steel, and the morphology of the nanoparticles is spherical, cubic or spindle-shaped, with a particle size of 3nm-300μm.

3. The preparation method of the magnetic induction heating organic solvent dehydrating agent according to claim 1, characterized in that, The ratio of the metal or metal oxide nanoparticles to hydrogen peroxide is 1g:4-8mL; the concentration of the hydrogen peroxide is 15%.

4. The preparation method of the magnetic induction heating organic solvent dehydrating agent according to claim 1, characterized in that, The surface modification conditions are: temperature 40℃ and time 3h.

5. The preparation method of the magnetic induction heating organic solvent dehydrating agent according to claim 1, characterized in that, The dehydrating agent is one or more of SiO2, γ-Al2O3, ZnO, Fe2O3·nH2O, TiO2, or SnO2; the binder is one or more of bentonite, kaolin, attapulgite, clay mineral, silica sol, alumina sol, aluminum dihydrogen phosphate, aluminate cement, water glass, phosphate cement, or ceramic clay.

6. The preparation method of the magnetic induction heating organic solvent dehydrating agent according to claim 1, characterized in that, The mass ratio of the modified metal or metal oxide nanoparticles to the dehydrating agent and binder is (2-4):(5-3):

3.

7. The preparation method of the magnetic induction heating organic solvent dehydrating agent according to claim 1, characterized in that, The molding method is extrusion molding or ball rolling molding, and the particle size of the slurry after molding is 3-5 mm; the calcination conditions are: temperature of 500℃ and time of 2h.

8. A magnetic induction heating organic solvent dehydrating agent, characterized in that, It is obtained by the preparation method according to any one of claims 1 to 7.

9. The application of the magnetic induction heating organic solvent dehydrating agent according to claim 8, characterized in that, The application is in the dehydration of organic solvents.

10. A method for regenerating the magnetic induction heating organic solvent dehydrating agent according to claim 8, characterized in that, The regeneration method specifically involves placing a dehydrating agent into an induction coil and generating an alternating magnetic field by applying electricity. The metal / metal oxide nanoparticles are heated by magnetic induction and desorb water molecules. The frequency of the alternating magnetic field is 50Hz-10MHz, the power is 100-5000W, and the regeneration temperature is 100-550℃.