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A method for preparing ammonia by using ammonia synthesis-biomass conversion dual-functional photocatalytic reaction

A photocatalytic reaction and biomass technology, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, preparation/separation of ammonia, etc., can solve the problem of low photocatalyst photogenerated electron-hole separation and migration efficiency and low molecular reactivity , low reaction efficiency and other issues, to achieve high yield, high raw material utilization, and improved thermodynamics

Active Publication Date: 2020-11-06
HUAIBEI NORMAL UNIVERSITY
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  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0004] Photocatalytic N 2 Generate NH 3 The Gibbs free energy is much greater than zero (N 2 +3H 2 O→2NH 3 +3 / 2O 2 ,ΔG o =+681.1KJ / mol), so the photocatalytic N 2 Reduction is thermodynamically extremely difficult to occur; on the other hand, photocatalyst photogenerated electron-hole separation-migration efficiency is low and N 2 The low reactivity of the molecule leads to its inefficient reaction

Method used

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  • A method for preparing ammonia by using ammonia synthesis-biomass conversion dual-functional photocatalytic reaction
  • A method for preparing ammonia by using ammonia synthesis-biomass conversion dual-functional photocatalytic reaction
  • A method for preparing ammonia by using ammonia synthesis-biomass conversion dual-functional photocatalytic reaction

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Embodiment 1

[0030]This embodiment prepares Zn deficiency-Zn according to the following steps 3 In 2 S 6 nanomaterials:

[0031] Step 1, weigh 1.5mmol of zinc nitrate, 1mmol of indium nitrate hydrate and 3mmol of cysteine ​​in a beaker filled with 60mL of deionized water, and stir to dissolve them;

[0032] Step 2, transfer the mixture in step 1 to a 100ml polytetrafluoroethylene liner, seal it, heat it with water at 200°C, and after 20 hours, wash it with deionized water and dry it in vacuum to obtain the Zn defect-Zn 3 In 2 S 6 nanomaterials.

[0033] Other surface defect modified transition metal dichalcogenides (TMDs) such as Cd defect-CdIn 2 S 4 , Cd defect-CdLa 2 S 4 , Zn defect-Cd x Zn 1-x S(x=0-1) and Zn defects-Zn x In 2 S 3+x (x=1-5) and the like can be prepared by changing the raw materials and process conditions and adopting the above-mentioned preparation method. Among them, the raw materials of metal elements are their nitrates, and the ratio of raw materials i...

Embodiment 2

[0049] This example is the same as Example 1, except that the hydrothermal temperature in step 2 is 180°C, and Zn 3 In 2 S 6 nanomaterials.

[0050] For the Zn defect-Zn prepared by Example 1 of the present invention 3 In 2 S 6 And the Zn that embodiment 2 prepares 3 In 2 S 6 Nanomaterials were characterized, and the results were as follows figure 1 , figure 2 , image 3 and Figure 4 shown. in, figure 1 X-ray diffraction (XRD) pattern, Zn defect-Zn 3 In 2 S 6 and Zn 3 In 2 S 6 All the diffraction peaks in the diffraction pattern correspond well to the hexagonal phase Zn 3 In 2 S 6 . Illustrates the pure phase of Zn 3 In 2 S 6 was successfully prepared, and the Zn-defects did not cause the generation of new material phases.

[0051] figure 2 Zn defect-Zn 3 In 2 S 6 The transmission electron microscope (TEM) and high-resolution transmission electron microscope (HRTEM) images of the sample, it can be seen from the figure that the sample is an ultr...

Embodiment 3

[0055] This example is the construction of a bifunctional reaction system (benzyl alcohol is used in the mixed solution of biomass and water containing alcoholic hydroxyl groups), and the detailed steps are as follows:

[0056] Step 1, add 0.03g of Zn defect-Zn 3 In 2 S 6 Nanomaterials and 50mL of benzyl alcohol were added to a 100mL three-port polytetrafluoroethylene reactor;

[0057] Step 2, feed N into the reactor 2 After evacuating the air, keep the N in the reactor 2 The pressure is about 0.2Mpa;

[0058] Step 3: After stirring for about 0.5 h in the dark state to balance the adsorption and desorption, turn on the visible light source, extract 5 mL of the reaction solution every 1 hour, centrifuge, and analyze and detect the liquid phase products in the reaction solution such as ammonia and aldehydes.

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Abstract

The invention discloses a method for preparing ammonia by adopting ammonia synthesis-biomass conversion bifunctional photocatalytic reaction. The method comprises the following steps of: (1), adding asurface defect state modified nano material with selective oxidation and N2 reduction and a mixed solution of biomass containing alcohol hydroxyl and water into a three-port polytetrafluoroethylene reaction kettle; (2), introducing N2 into the reaction kettle to evacuate air; and (3), stirring a reaction solution in a dark state to reach adsorption desorption equilibrium, turning on a visible light source to irradiate the reaction solution, and extracting the reaction solution to centrifugally obtain a liquid-phase ammonia product. According to the method, photo-generated electrons-cavities is fully used, the photo-generated cavities are not wasted but are used for selectively converting biomass to produce chemicals with high added value; and high utilization rate of raw materials, high yield of the ammonia and environmental friendliness are achieved.

Description

technical field [0001] The invention relates to a method for preparing ammonia, in particular to a method for preparing ammonia by adopting ammonia synthesis-biomass conversion dual-functional photocatalytic reaction. Background technique [0002] Ammonia (NH 3 ), as a basic chemical with an annual output of more than 150 million tons, is an important cornerstone of modern social development and population growth. The current industrial ammonia synthesis technology is dominated by the Haber-Bosch process using iron-based catalysts, which converts nitrogen and hydrogen into ammonia under high temperature and pressure. However, this process requires harsh reaction conditions (high pressure 15-25Mpa, high temperature 400-550 ℃), and the high temperature and high pressure reaction conditions required for the reaction will cause huge consumption of global energy and environmental pollution every year. This process consumes 3-5% of the world's natural gas to produce hydrogen and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01C1/02C01G11/00C01G15/00B01J27/04
CPCY02P20/52
Inventor 孟苏刚郑秀珍吴惠惠付先亮陈士夫
Owner HUAIBEI NORMAL UNIVERSITY
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