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A kind of preparation method of copper borate with rod-shaped single crystal structure

A single crystal structure, copper borate technology, applied in borates, chemical instruments and methods, boron oxide compounds, etc., can solve the problems of high reaction temperature, unsuitable for industrial production, etc., achieve strong light degradation ability, and simple method Ease of operation and the effect of reducing production costs

Active Publication Date: 2015-10-07
杜丽红
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The problem to be solved in the present invention is: overcome the present solid phase sintering method and prepare single crystal Cu 3 B 2 o 6 , the reaction temperature is too high, not suitable for industrial production, creatively use the sol-gel method instead of the high temperature solid phase method to prepare single crystal Cu 3 B 2 o 6 , this method is simple, simple equipment, mild synthesis conditions, and has industrialization prospects

Method used

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  • A kind of preparation method of copper borate with rod-shaped single crystal structure
  • A kind of preparation method of copper borate with rod-shaped single crystal structure
  • A kind of preparation method of copper borate with rod-shaped single crystal structure

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Effect test

Embodiment 1

[0031] Weigh 2.5mmol (0.5g) of copper acetate (Cu(CH 3 COO) 2 ·H 2O), 7.5mmol glucose (1.35g) was dissolved in 20mL distilled water, and magnetically stirred for 2h. Dissolve 2.5mmol (1.55g) of boric acid in 30mL of deionized water, add the obtained aqueous solution of boric acid to the aforementioned reaction solution, and stir magnetically for 2h. Then dry the mixed solution in an oven at 150°C to obtain a brown xerogel, which is then roasted at 850°C for 6 hours to obtain a dark green powder, which is washed with 0.1mol / L hydrochloric acid and deionized water at 60°C respectively 3 to 4 times, centrifuge, and dry the powder at 60°C to obtain Cu 3 B 2 o 6 Single crystal 0.21g. Detected by XRD, as attached figure 1 As shown, the resulting Cu 3 B 2 o 6 It is a pure substance, the corresponding PDF card number: 28-398; tested by SEM, if attached figure 2 As shown, sample Cu 3 B 2 o 6 It is rod-shaped, with a diameter of about 300-600 nm and a length of about 6 μm...

Embodiment 2

[0034] Take by weighing 2.5mmol of copper nitrate (Cu(NO 3 ) 2 ·3H 2 O), 5.0mmol malic acid was dissolved in 20mL distilled water, and magnetically stirred for 3h. Dissolve 2.5 mmol of boric acid in 30 mL of deionized water, and then add this solution dropwise to the aforementioned reaction solution, and magnetically stir for 4 h. Then the mixed solution was dried in an oven at 140°C to obtain a brown gel, which was roasted at 900°C for 7 hours to obtain a dark green powder, which was washed with 0.21mol / L hydrochloric acid and deionized water at 80°C for 3-3 hours. 4 times, centrifuged, and the powder was dried at 80°C to obtain Cu 3 B 2 o 6 sample. After XRD detection, the results are attached figure 1 , the resulting Cu 3 B 2 o 6 It is a pure substance, corresponding PDF card number: 28-398; tested by HRTEM, as attached image 3 shown, indicating that the prepared Cu 3 B 2 o 6 a single crystal structure. After the UV-vis test, the UV-visible diffuse reflectan...

Embodiment 3

[0037] Take by weighing 2.5mmol of copper nitrate (Cu(NO 3 ) 2 ·3H 2 O), 7.5mmol glucose was dissolved in 20mL distilled water, and magnetically stirred for 3h. Dissolve 1.75 mmol of boric acid in 30 mL of deionized water, and then add this solution dropwise to the aforementioned reaction solution, and magnetically stir for 2 h. Then dry the mixture in an oven at 120°C to obtain a brown gel, which is then roasted at 850°C for 7 hours to obtain a dark green powder, which is washed with 0.4mol / L hydrochloric acid and deionized water at 80°C for 3-3 hours. 4 times, centrifuged, and the powder was dried at 60°C to obtain Cu 3 B 2 o 6 sample. As in Example 1, the resulting Cu 3 B 2 o 6 It is a pure substance and has a single crystal structure.

[0038] Take 40mg of Cu obtained above 3 B 2 o 6 Add 35mL methylene blue solution (35mg / L) to the powder, react under the conditions of 600nm visible light, 25°C, 1200rpm, take samples regularly and determine the concentration o...

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Abstract

The invention discloses a preparation method of rodlike single-crystal structure cupric borate, which adopts a sol-gel method and comprises the following steps: mixing water-soluble copper salt and a foaming agent according to an amount ratio of substances of 1:(0.1 to 6), adding water to prepare copper-containing aqueous solution and stirring for 1 to 4h at a room temperature; then dropwise adding 0.05 to 2.0mol / L boric acid or tributyl borate solution into the solution and stirring for 1 to 4h at room temperature; then drying at a temperature of 120 to 170 DEG C to obtain xerogel; calcining the xerogel for 2 to 10h at a temperature of 550 to 1,000 DEG C in the air atmosphere to obtain powder; carrying out washing and centrifugation on the powder and drying the powder at a temperature of 40 to 120 DEG C to prepare the rodlike single-crystal structure cupric borate Cu3B2O6. The method disclosed by the invention is simple and easy to operate, has low energy consumption, greatly reduces production cost and is easy to implement industrial production.

Description

(1) Technical field [0001] The invention relates to a method for preparing copper borate with a rod-shaped single crystal structure, in particular to preparing copper borate single crystal by a sol-gel method. (2) Background technology [0002] In the 21st century, with the improvement of industrialization, the problem of environmental pollution has become increasingly serious, and the treatment of dye wastewater is particularly difficult. Dye wastewater usually contains some highly toxic and refractory organic pollutants. Due to the high concentration of pollutants, complex components, and poor biodegradability, it is difficult to effectively treat them by conventional methods, thus causing harm to human health and biodiversity. huge threat. [0003] As a deep oxidation method, photocatalysis has been recognized as the most promising pollutant removal technology. However, after more than 30 years of extensive and in-depth research, it is still difficult for photocatalytic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/72C01B35/12B01J35/02C02F1/30C02F101/38C02F103/30B01J35/00
CPCY02W10/37Y02P20/133
Inventor 陈爱民薄盈盈邵晨熠胡军汪晶
Owner 杜丽红