Preparation method of core-shell structure catalyst loaded with TiO2 and MoS2, reactor and application of core-shell structure catalyst loaded with TiO2 and MoS2
By supporting TiO2@MoS2 core-shell catalyst and combining photothermal dual-driven catalysis, the problems of high energy consumption, low efficiency and poor safety in traditional deuterated ammonia synthesis have been solved, realizing efficient and safe deuterated ammonia synthesis with high product purity.
Patent Information
- Application Number
- CN202511567607.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-10-30
- Publication Date
- 2026-03-06
AI Technical Summary
Traditional methods for synthesizing deuterated ammonia have high energy consumption, low deuterium source utilization, and insufficient product purity. Photocatalysis is inefficient and relies on precious metals, while thermal catalysis requires high temperature and pressure, posing high safety risks.
A core-shell structured TiO2@MoS2 catalyst was used, combined with photothermal dual-driven catalysis. MoS2 nanosheets were grown by hydrothermal method to form a core-shell heterojunction. Sulfur vacancy defects were introduced by acid etching to enhance the light absorption range and electron migration efficiency. Electron-hole pairs were excited by ultraviolet-infrared multi-band LED light source, and thermal catalysis was carried out by Fe-Co bimetallic catalyst to realize waste heat recycling.
It achieves a wide spectral response, increases quantum efficiency to 45%, reduces overall energy consumption by 40%, improves safety, produces deuterated ammonia with a purity of >99%, and exhibits good catalyst stability.
Abstract
Description
Technical Field
[0001] This invention belongs to the field of catalytic synthesis technology, specifically relating to a method for preparing a TiO2@MoS2 core-shell structure catalyst, a reactor, and its application. Background Technology
[0002] Traditional methods for synthesizing deuterated ammonia (such as the Haber process and calcium nitride hydrolysis) suffer from high energy consumption, low deuterium source utilization, and insufficient product purity. In recent years, photocatalysis has attracted attention due to its green and low-carbon characteristics; however, single-light-driven reactions are limited by narrow spectral absorption ranges (e.g., only ultraviolet response) and high carrier recombination rates, resulting in low efficiency. Furthermore, thermocatalytic pathways rely on noble metals (such as Ru and Pd) and require high-temperature and high-pressure conditions, posing significant cost and safety risks. Summary of the Invention
[0003] The purpose of this invention is to provide a method for preparing a TiO2@MoS2 core-shell structure catalyst, a reactor, and its application. This invention combines photothermal dual-drive catalysis with core-shell structure catalyst design, overcomes the limitations of a single energy source, achieves synergistic effects of broad-spectrum response and waste heat recycling, avoids high pressure and high temperature, and significantly improves safety.
[0004] The technical solution of this invention:
[0005] A method for preparing a TiO2@MoS2 core-shell structure catalyst includes the following steps: S1, synthesizing TiO2 nanorods by a hydrothermal method;
[0006] S2. Dissolve ammonium molybdate and thiourea in ethylene glycol, mix with the TiO2 nanorods prepared in step S1, and react to generate a core-shell structure of MoS2 coated with TiO2.
[0007] The TiO2 core-shell structure coated with S3 and MoS2 was etched with hydrofluoric acid to obtain the TiO2@MoS2 core-shell structure catalyst.
[0008] Preferably, the specific steps for hydrothermal synthesis of TiO2 nanorods in step S1 are as follows: using tetrabutyl titanate as the titanium source, it is mixed with concentrated hydrochloric acid (37wt%) and deionized water, and hydrothermally reacted at 160-180℃ for 12-24 hours. After the reaction, the mixture is centrifuged at 8000-12000 r / min for 5-10 minutes, washed until neutral, and dried at 100-150℃ for 4-6 hours to obtain TiO2 nanorods with a diameter of 40-60 nm and a length of 200-400 nm.
[0009] In step S1, the volume ratio of tetrabutyl titanate, concentrated hydrochloric acid, and deionized water is 1:10:10.
[0010] Preferably, in step S2, the mass ratio of ammonium molybdate: thiourea: ethylene glycol: TiO2 nanorods is 1:2:100:5;
[0011] In step S2, the reaction temperature is 190–210°C and the reaction time is 11–13 hours.
[0012] The hydrofluoric acid etching step in step S3 is as follows: using a hydrofluoric acid solution with a concentration of 2-5 wt%, the etching is carried out by stirring at room temperature for 2 hours, and the core-shell structure of MoS2 coated TiO2 is completely immersed in the 2-5 wt% hydrofluoric acid solution.
[0013] Preferably, the sulfur vacancy defect density of the TiO2@MoS2 core-shell structure catalyst is 1 to 3 × 10⁻⁶. 15 cm -2 The shell thickness of the TiO2@MoS2 core-shell structure catalyst is 5–100 nm.
[0014] A reactor supported on a TiO2@MoS2 core-shell catalyst is provided, comprising a photocatalytic zone, a thermal catalytic zone, and a gas-liquid separation module for separating deuterium, nitrogen, and liquid deuterated ammonia. The photocatalytic zone is supported on a TiO2@MoS2 core-shell catalyst, and the thermal catalytic zone is supported on an Fe-Co bimetallic catalyst.
[0015] Preferably, the Fe-Co bimetallic catalyst is prepared by co-precipitation, in which an aqueous solution of ferric nitrate and cobalt nitrate is mixed with an excess of sodium carbonate precipitant, aged at 58-63°C for 2 hours, filtered, washed to neutral, dried at 100-150°C for 4-6 hours, and then calcined at 400°C in a hydrogen atmosphere for 2 hours, wherein the molar ratio of ferric nitrate to cobalt nitrate is 1:1.
[0016] Preferably, the photocatalytic region is equipped with an ultraviolet-infrared multi-band LED light source.
[0017] Preferably, it is used for the synthesis of deuterated amines;
[0018] The specific steps for synthesizing deuterated ammonia are as follows: N2 and D2 are irradiated by a multi-band ultraviolet-infrared LED light source in the photocatalytic zone, with a reaction pressure of 1-5 MPa and a temperature of 4-100℃, and reacted in the photocatalytic zone for 0.5-4 hours under the catalysis of a TiO2@MoS2 core-shell structure catalyst.
[0019] Entering the thermocatalytic zone, the thermocatalytic reaction was carried out for 12 to 200 hours at 60–120°C using an Fe-Co bimetallic catalyst.
[0020] After the reaction is completed in the thermocatalytic zone, the gas enters the gas separation module to separate and obtain ND3 with a purity of >99%.
[0021] Preferably, the ultraviolet-infrared multi-band LED light source is a xenon lamp with a wavelength range of 300-800nm.
[0022] Preferably, the molar ratio of N2 to D2 is 1:3 to 3.2.
[0023] The beneficial effects of this invention are:
[0024] This invention presents a method for the efficient synthesis of deuterated ammonia from nitrogen and deuterium, applicable to the nuclear industry, pharmaceuticals, and high-purity materials. This invention proposes combining photothermal dual-drive catalysis with core-shell structured catalyst design, overcoming the limitations of a single energy source, achieving synergistic effects of broad-spectrum response and waste heat recycling, avoiding high pressure and high temperature, and significantly improving safety.
[0025] This invention grows MoS2 nanosheets on the surface of TiO2 nanorods using a hydrothermal method to form a core-shell heterojunction. Sulfur vacancy defects are introduced through acid etching, enhancing the light absorption range (UV-IR) and electron mobility. The surface defects of MoS2 act as active sites, promoting D2 dissociation, while TiO2 provides strong redox capabilities. The Z-shaped heterojunction design suppresses electron-hole recombination, resulting in a quantum efficiency of up to 45%.
[0026] Photocatalytic zone of reactor: Equipped with ultraviolet-infrared multi-band LED light source to excite TiO2@MoS2 to generate electron-hole pairs, driving N2 activation and D2 dissociation; Thermal catalytic zone: Utilizes the residual heat of photoreaction to maintain the hydrogenation reaction temperature at 60-120℃, combined with Fe-Co iron-based catalyst to promote ND bond formation; Energy synergy: Light energy drives the initial reaction, and residual heat supplies subsequent hydrogenation steps, reducing overall energy consumption by 40%. Detailed Implementation
[0027] Preparation Method Example 1
[0028] A method for preparing a TiO2@MoS2 core-shell structured catalyst includes the following steps:
[0029] S1. TiO2 nanorods were synthesized by hydrothermal method. The specific steps of the hydrothermal synthesis of TiO2 nanorods were as follows: tetrabutyl titanate was used as the titanium source, and mixed with concentrated hydrochloric acid and deionized water at a concentration of 37wt%. The mixture was subjected to hydrothermal reaction at 170℃ for 18 hours. After the reaction was completed, the nanorods were centrifuged, washed, and dried to obtain TiO2 nanorods with a diameter of 40nm and a length of 300nm. The volume ratio of tetrabutyl titanate:concentrated hydrochloric acid:deionized water was 1:10:10.
[0030] S2. Ammonium molybdate and thiourea are dissolved in ethylene glycol and mixed with the TiO2 nanorods prepared in step S1 to react and generate a core-shell structure of MoS2 coated with TiO2; the mass ratio of ammonium molybdate:thiourea:ethylene glycol:TiO2 nanorods is 1:2:100:5; the reaction temperature is 200℃ and the reaction time is 12 hours.
[0031] The TiO2@MoS2 core-shell structure was etched with hydrofluoric acid to obtain a TiO2@MoS2 core-shell catalyst. The specific steps of the hydrofluoric acid etching were as follows: a 4 wt% hydrofluoric acid solution was used, and the etching was carried out with stirring at room temperature for 2 hours, during which the MoS2-coated TiO2 core-shell structure was completely immersed in a 3 wt% hydrofluoric acid solution.
[0032] The obtained TiO2@MoS2 core-shell catalyst has a sulfur vacancy defect density of 2×10⁻⁶. 15 cm -2 The TiO2@MoS2 core-shell catalyst has a shell thickness of 50 nm. XPS confirmed that Mo... 3+ / Mo 4+ The ratio was increased to 1:1.3 to enhance D2 adsorption.
[0033] Preparation Method Example 2
[0034] A method for preparing a TiO2@MoS2 core-shell structured catalyst includes the following steps:
[0035] S1. TiO2 nanorods were synthesized by hydrothermal method. The specific steps of the hydrothermal synthesis of TiO2 nanorods were as follows: tetrabutyl titanate was used as the titanium source, mixed with concentrated hydrochloric acid (37wt%) and deionized water, and the mixture was subjected to hydrothermal reaction at 160℃ for 24 hours. After the reaction, the mixture was centrifuged, washed, and dried to obtain TiO2 nanorods with a diameter of 60nm and a length of 400nm. The volume ratio of tetrabutyl titanate:concentrated hydrochloric acid:deionized water was 1:10:10.
[0036] S2. Ammonium molybdate and thiourea are dissolved in ethylene glycol and mixed with the TiO2 nanorods prepared in step S1 to react and generate a core-shell structure of MoS2 coated with TiO2; the mass ratio of ammonium molybdate:thiourea:ethylene glycol:TiO2 nanorods is 1:2:100:5; the reaction temperature is 190℃ and the reaction time is 13 hours.
[0037] The TiO2@MoS2 core-shell structure was etched with hydrofluoric acid to obtain a TiO2@MoS2 core-shell catalyst. The specific steps of the hydrofluoric acid etching were as follows: a 5 wt% hydrofluoric acid solution was used, and the etching was carried out with stirring at room temperature for 2 hours, completely immersing the MoS2-coated TiO2 core-shell structure in the 5 wt% hydrofluoric acid solution.
[0038] The obtained TiO2@MoS2 core-shell catalyst has a sulfur vacancy defect density of 1×10⁻⁶. 15 cm -2 The shell thickness of the TiO2@MoS2 core-shell catalyst is 20 nm. XPS confirmed that Mo... 3+ / Mo 4+ The ratio was increased to 1:1.25 to enhance D2 adsorption.
[0039] Preparation Method Example 3
[0040] A method for preparing a TiO2@MoS2 core-shell structured catalyst includes the following steps:
[0041] S1. TiO2 nanorods were synthesized by hydrothermal method. The specific steps of the hydrothermal synthesis of TiO2 nanorods were as follows: tetrabutyl titanate was used as the titanium source, mixed with concentrated hydrochloric acid (37wt%) and deionized water, and the mixture was subjected to hydrothermal reaction at 180℃ for 12 hours. After the reaction, the mixture was centrifuged, washed, and dried to obtain TiO2 nanorods with a diameter of 50nm and a length of 200nm. The volume ratio of tetrabutyl titanate:concentrated hydrochloric acid:deionized water was 1:10:10.
[0042] S2. Ammonium molybdate and thiourea are dissolved in ethylene glycol and mixed with the TiO2 nanorods prepared in step S1 to react and generate a core-shell structure of MoS2 coated with TiO2; the mass ratio of ammonium molybdate:thiourea:ethylene glycol:TiO2 nanorods is 1:2:100:5; the reaction temperature is 210℃ and the reaction time is 11 hours.
[0043] The TiO2@MoS2 core-shell structure was etched with hydrofluoric acid to obtain a TiO2@MoS2 core-shell catalyst. The specific steps of the hydrofluoric acid etching were as follows: a 2 wt% hydrofluoric acid solution was used, and the etching was carried out with stirring at room temperature for 2 hours, completely immersing the MoS2-coated TiO2 core-shell structure in the 2 wt% hydrofluoric acid solution.
[0044] The obtained TiO2@MoS2 core-shell catalyst has a sulfur vacancy defect density of 3 × 10⁻⁶. 15 cm -2 The shell thickness of the TiO2@MoS2 core-shell catalyst is 80 nm. XPS confirmed that Mo... 3+ / Mo 4+ The ratio was increased to 1:1.2 to enhance D2 adsorption.
[0045] Reactor Examples
[0046] A reactor supported on a TiO2@MoS2 core-shell catalyst comprises a layered reactor with a photocatalytic zone, a thermal catalytic zone, and a gas-liquid separation module for separating deuterium, nitrogen, and liquid deuterated ammonia. The photocatalytic zone is supported on the TiO2@MoS2 core-shell catalyst and is equipped with a UV-IR multi-band LED light source. The thermal catalytic zone is supported on an Fe-Co bimetallic catalyst. The Fe-Co bimetallic catalyst is prepared by a co-precipitation method, in which an aqueous solution of ferric nitrate and cobalt nitrate is mixed with an excess of sodium carbonate precipitant, aged at 58–63°C for 2 hours, filtered, washed, dried, and then calcined at 400°C in a hydrogen atmosphere for 2 hours. The molar ratio of ferric nitrate to cobalt nitrate is 1:1.
[0047] Application Example 1
[0048] Application Examples: The TiO2@MoS2 core-shell structured catalyst prepared in Example 1 was applied using the reactor from the reactor example.
[0049] The specific steps for synthesizing deuterated ammonia are as follows: N2 at a flow rate of 280 g / h and D2 at a flow rate of 120 g / h are reacted in the photocatalytic zone with a UV-IR multi-band LED light source under a reaction pressure of 2 MPa and a temperature of 20 °C. The reaction is carried out in the photocatalytic zone for 1 hour under the catalysis of TiO2@MoS2 core-shell structure catalyst, and the catalyst addition amount is 100 g.
[0050] Entering the thermocatalytic zone, the Fe-Co bimetallic catalyst was used for a thermocatalytic reaction for 24 hours at 80°C, with a catalyst addition of 800g.
[0051] After the reaction is completed in the thermocatalytic zone, the gas enters the gas separation module to separate and obtain ND3.
[0052] The ultraviolet-infrared multi-band LED light source is a xenon lamp with a wavelength range of 300-800nm.
[0053] The molar ratio of N2 to D2 is 1:3.
[0054] Results: ND3 yield: 12.8 mmol / g·h; purity >99%;
[0055] Catalyst stability: Activity decreases by <5% after 200 hours of continuous operation.
[0056] Application Example 2
[0057] Application Examples: The TiO2@MoS2 core-shell structured catalyst prepared in Example 1 was applied using the reactor from the reactor example.
[0058] The specific steps for synthesizing deuterated ammonia are as follows: N2 at a flow rate of 280 g / h and D2 at a flow rate of 120 g / h are reacted in the photocatalytic zone with a UV-IR multi-band LED light source under a reaction pressure of 2 MPa and a temperature of 20 °C, and the reaction is carried out in the photocatalytic zone for 1 hour under the catalysis of TiO2@MoS2 core-shell structure catalyst, with a catalyst addition amount of 200 g.
[0059] Entering the thermocatalytic zone, the Fe-Co bimetallic catalyst was used for a thermocatalytic reaction for 24 hours at 80°C, with a catalyst addition of 700g.
[0060] After the reaction is completed in the thermocatalytic zone, the gas enters the gas separation module to separate and obtain ND3.
[0061] The ultraviolet-infrared multi-band LED light source is an ultraviolet lamp with a wavelength range of 280–400 nm.
[0062] The molar ratio of N2 to D2 is 1:3.
[0063] Results: ND3 yield: 10.5 mmol / g·h; purity >99%;
[0064] Catalyst stability: Activity decreases by <5% after 200 hours of continuous operation.
[0065] A comparison of Application Example 1 and Application Example 2 shows that xenon lamps are more effective.
[0066] Application Example 3
[0067] Application Examples: The TiO2@MoS2 core-shell structured catalyst prepared in Example 2 was applied using the reactor from the reactor example.
[0068] The specific steps for synthesizing deuterated ammonia are as follows: N2 at a flow rate of 280 g / h and D2 at a flow rate of 120 g / h are reacted in the photocatalytic zone with a UV-IR multi-band LED light source under a reaction pressure of 1 MPa and a temperature of 60 °C, and the reaction is carried out in the photocatalytic zone for 4 hours under the catalysis of TiO2@MoS2 core-shell structure catalyst, with a catalyst addition amount of 300 g.
[0069] Entering the thermocatalytic zone, the Fe-Co bimetallic catalyst was used for a thermocatalytic reaction for 12 hours at 60°C, with a catalyst addition of 600g.
[0070] After the reaction is completed in the thermocatalytic zone, the gas enters the gas separation module to separate and obtain ND3.
[0071] The ultraviolet-infrared multi-band LED light source is a xenon lamp with a wavelength range of 300-800nm.
[0072] The molar ratio of N2 to D2 is 1:3.2.
[0073] Results: ND3 yield: 12.3 mmol / g·h; purity >99%;
[0074] Catalyst stability: Activity decreases by <5% after 200 hours of continuous operation.
[0075] Application Example 4
[0076] Application Examples: The TiO2@MoS2 core-shell structured catalyst prepared in Example 3 was applied using the reactor from the reactor example.
[0077] The specific steps for synthesizing deuterated ammonia are as follows: N2 at a flow rate of 280 g / h and D2 at a flow rate of 120 g / h are reacted in the photocatalytic zone with a UV-IR multi-band LED light source, under a reaction pressure of 5 MPa and a temperature of 100 °C, and the reaction is carried out in the photocatalytic zone for 0.5 hours under the catalysis of TiO2@MoS2 core-shell structure catalyst, with a catalyst addition amount of 150 g.
[0078] Entering the thermocatalytic zone, the thermocatalytic reaction was carried out at 120℃ with Fe-Co bimetallic catalyst for 200 hours, with a catalyst addition of 400g.
[0079] After the reaction is completed in the thermocatalytic zone, the gas enters the gas separation module to separate and obtain ND3.
[0080] The ultraviolet-infrared multi-band LED light source is a xenon lamp with a wavelength range of 300-800nm.
[0081] The molar ratio of N2 to D2 is 1:3.1.
[0082] Results: ND3 yield: 11.5 mmol / g·h; purity >99%;
[0083] Catalyst stability: Activity decreases by <5% after 200 hours of continuous operation.
[0084] Application Example 5
[0085] Application Examples: The TiO2@MoS2 core-shell structured catalyst prepared in Example 1 was applied using the reactor from the reactor example.
[0086] The specific steps for synthesizing deuterated ammonia are as follows: N2 at a flow rate of 280 g / h and D2 at a flow rate of 120 g / h are reacted in the photocatalytic zone with a UV-IR multi-band LED light source under a reaction pressure of 3 MPa and a temperature of 300℃, and the reaction is carried out in the photocatalytic zone for 2 hours under the catalysis of TiO2@MoS2 core-shell structure catalyst, with a catalyst addition amount of 250 g.
[0087] Entering the thermocatalytic zone, the reaction was carried out at 100°C for 24 hours with the Fe-Co bimetallic catalyst, and the catalyst addition amount was 500g.
[0088] After the reaction is completed in the thermocatalytic zone, the gas enters the gas separation module to separate and obtain ND3.
[0089] The ultraviolet-infrared multi-band LED light source is a xenon lamp with a wavelength range of 300-800nm.
[0090] Preferably, the molar ratio of N2 to D2 is 1:3.
[0091] Results: ND3 yield: 12.7 mmol / g·h; purity >99%;
[0092] Catalyst stability: Activity decreases by <5% after 200 hours of continuous operation.
[0093] The technical solutions of this invention are not limited to the specific embodiments described above. Any technical modifications made to the technical solutions of this invention without departing from the scope of the claims are within the scope of protection of this invention.
Claims
1. A preparation method of a TiO2@MoS2 core-shell structure catalyst, characterized in that, It comprises the following steps: S1, synthesizing TiO2 nanorods by hydrothermal method; S2, dissolving ammonium molybdate and thiourea in ethylene glycol, mixing with TiO2 nanorods prepared in step S1, and then reacting to form MoS2-coated TiO2 core-shell structure; S3, etching the MoS2-coated TiO2 core-shell structure with hydrofluoric acid to obtain TiO2@MoS2 core-shell structure catalyst.
2. The method for preparing a TiO2@MoS2 core-shell structure catalyst according to claim 1, characterized in that, The specific steps of synthesizing TiO2 nanorods by hydrothermal method in step S1 are as follows: mixing tetrabutyl titanate as titanium source with concentrated hydrochloric acid with a concentration of 37wt% and deionized water, and then hydrothermal reaction at 160-180℃ for 12-24 hours; after the reaction is completed, centrifugation, washing to neutral, and drying are performed to obtain TiO2 nanorods with a diameter of 40-60nm and a length of 200-400nm; The volume ratio of tetrabutyl titanate, concentrated hydrochloric acid, and deionized water in step S1 is 1:10:
10.
3. The method for preparing a TiO2@MoS2 core-shell structure catalyst according to claim 1, characterized in that, The mass ratio of ammonium molybdate, thiourea, ethylene glycol, and TiO2 nanorods in step S2 is 1:2:100:5; The reaction temperature in step S2 is 190-210℃, and the reaction time is 11-13 hours; The specific steps of etching with hydrofluoric acid in step S3 are as follows: using a hydrofluoric acid solution with a concentration of 2-5wt%, stirring and etching at room temperature for 2 hours, and completely immersing the MoS2-coated TiO2 core-shell structure in the 2-5wt% hydrofluoric acid solution.
4. The method for preparing a TiO2@MoS2 core-shell structure catalyst according to claim 1, characterized in that, The sulfur vacancy defect density of the TiO2@MoS2 core-shell structure catalyst is 1-3 x 10 15 cm -2 -3, and the shell thickness of the TiO2@MoS2 core-shell structure catalyst is 5-100 nm.
5. A reactor loaded with TiO2@MoS2 core-shell structure catalyst, the reactor is loaded with the TiO2@MoS2 core-shell structure catalyst prepared by the preparation method of the TiO2@MoS2 core-shell structure catalyst according to any one of claims 1-4, characterized in that, A layered reactor comprising a photocatalytic zone and a thermal catalytic zone and a gas-liquid separation module are used to separate deuterium gas, nitrogen gas, and liquid deuterated ammonia, the photocatalytic zone is loaded with TiO2@MoS2 core-shell structure catalyst, and the thermal catalytic zone is loaded with Fe-Co bimetallic catalyst. 6.The reactor loaded with the TiO2@MoS2 core-shell structure catalyst according to claim 5, characterized in that, The preparation method of the Fe-Co bimetallic catalyst is to mix an aqueous solution of iron nitrate and cobalt nitrate with an excess of sodium carbonate precipitant by co-precipitation method, age at 58-63℃ for 2 hours, filter, wash to neutral, dry, and then calcine at 400℃ in a hydrogen atmosphere for 2 hours to obtain the catalyst, wherein the molar ratio of iron nitrate to cobalt nitrate is 1:
1. 7.The reactor loaded with the TiO2@MoS2 core-shell structure catalyst according to claim 5, characterized in that, The photocatalytic zone is equipped with a UV-IR multi-band LED light source.
8. Use of a reactor loaded with a TiO2@MoS2 core-shell structure catalyst, characterized in that, For synthesizing deuterated ammonia; The specific steps for synthesizing deuterated ammonia are as follows: under the irradiation of the UV-IR multi-band LED light source equipped in the photocatalytic zone, N2 and D2 are catalyzed by TiO2@MoS2 core-shell structure catalyst, the reaction pressure is 1-5MPa, the temperature is 4-100℃, and the reaction time in the photocatalytic zone is 0.5-4 hours; Then, it enters the thermal catalytic zone, and the thermal catalytic reaction is carried out at 60-120℃ for 12-200 hours under the catalysis of the Fe-Co bimetallic catalyst; After the reaction in the thermal catalytic zone is completed, it enters the gas separation module, and ND3 is separated and obtained, with a purity of >99%.
9. The use of a reactor loaded with a TiO2@MoS2 core-shell structure catalyst according to claim 8, characterized in that, The UV-IR multi-band LED light source is a xenon lamp with a wavelength range of 300-800nm.
10. The use of a reactor loaded with a TiO2@MoS2 core-shell structure catalyst according to claim 8, characterized in that, The mass ratio of N2 to D2 is 1:3-3.2.