CN107486200A - A kind of preparation method of the compound wolframic acid Mn catalyst of carbon - Google Patents

Abstract

The invention discloses a preparation method of a carbon-composite manganese tungstate catalyst. The steps are as follows: adding 5-10 g of manganese dichloride into 50-100 mL of water to prepare a solution, and then adding 3-4 g of tungsten NaCl, stir in a water bath at 60-70°C for 10-50 minutes, then add 4-5 g of nonionic surfactant Triton X-100 (Triton X-100) and stir for 10-15 minutes, then add 1 ~5 g acetone, continue to stir for 5~10 minutes, transfer the solution to a hydrothermal reactor, react for 5~10 h at 180~260°C, filter to obtain a solid, wash with distilled water 3~5 times, and dry at 80°C Dry, place in a tube furnace, feed nitrogen, raise the temperature to 700-850°C at a rate of 10-15°C/min, keep it for 30-120 minutes, and cool down to room temperature under the condition of continuously feeding nitrogen to obtain A carbon composite manganese tungstate catalyst. The invention has the advantages of: utilizing the action of the non-ionic surfactant and acetone to form a carbon layer at high temperature, compound with manganese tungstate, promote the dispersion of manganese tungstate, and improve the degradation rate of pollutants.

Description

A kind of preparation method of carbon composite manganese tungstate catalyst

technical field

The invention relates to the field of new materials for environmental pollution control, in particular to a preparation method of a carbon-composite manganese tungstate catalyst.

Background technique

With the development of science and technology, toxic organic pollutants from industrial and agricultural production seriously threaten the environment and human health. It is of great significance to seek a new and efficient environmental governance technology. Photocatalytic technology has become an emerging environmental treatment technology with important application prospects due to its advantages of energy saving, high efficiency, complete pollutant degradation, and no secondary pollution. In recent years, the development of new and efficient visible light photocatalysts has become an important research content in photocatalytic technology. Among them, photocatalytic materials with surface plasmon resonance effect, because of their unique surface physical and chemical properties and efficient visible light photocatalytic performance, have become One of the hotspots of research.

Manganese tungstate is an important functional material with wolframite structure. It has broad application prospects in photoluminescence, optical fiber, multiferroic material, photocatalyst, scintillator, humidity sensor and magnetic material. However, the effect of using manganese tungstate alone as a photocatalyst is very poor, and the corresponding degradation rate cannot be obtained.

Contents of the invention

The object of the present invention is to provide a kind of preparation method of carbon composite manganese tungstate catalyst in order to overcome the deficiencies in the prior art.

The technical solution adopted by the present invention includes the following steps in turn: adding 5-10 g of manganese dichloride to 50-100 mL of water to prepare a solution, then adding 3-4 g of sodium tungstate to the solution, and placing it in a water bath at 60-70 ° C. Stir for 10 to 50 minutes, then add 4 to 5 g of nonionic surfactant Triton X-100 (Triton X-100) and stir for 10 to 15 minutes, then add 1 to 5 g of acetone while continuing to stir, and continue to stir for 5 After ~10 minutes, transfer the solution to a hydrothermal reactor, react at 180~260°C for 5~10 hours, filter to obtain a solid, wash with distilled water 3~5 times, dry at 80°C, and place in a tube furnace. Introduce nitrogen, raise the temperature to 700-850 ℃ at a rate of 10-15 ℃/min, keep it for 30-120 minutes, and cool down to room temperature under the condition of continuous nitrogen inflow to obtain a carbon composite manganese tungstate catalyst.

The invention has the advantages of: utilizing the action of the non-ionic surfactant and acetone to form a carbon layer at high temperature, compound with manganese tungstate, promote the dispersion of manganese tungstate, and improve the degradation rate of pollutants.

detailed description

Further provide 3 embodiments of the present invention below:

Example 1

Add 10 g of manganese dichloride to 100 mL of water to prepare a solution, then add 4 g of sodium tungstate to the solution, stir in a water bath at 60~70°C for 50 minutes, then add 5 g of nonionic surfactant triton X-100 (Triton X-100) was stirred for 15 minutes, and 1 g of acetone was added during continuous stirring. After stirring for 10 minutes, the solution was transferred to a hydrothermal reactor, reacted for 10 h at 260 ° C, and filtered to obtain a solid. Wash 5 times with distilled water, dry at 80°C, place in a tube furnace, feed nitrogen, raise the temperature to 850°C at a rate of 15°C/min, keep it for 120 minutes, and cool down to room temperature under the condition of continuously feeding nitrogen , that is, a carbon composite manganese tungstate catalyst is obtained.

0.5 g of carbon-composite manganese tungstate catalyst was added to 200 mL of methylene blue wastewater with a concentration of 25 mg/L, and reacted for 100 min under the irradiation of a 120 W LED lamp. The decolorization rate was 96.8%. After the catalyst was separated and reused 5 times, Under the same conditions, the reaction time was 100 min, and the decolorization rate was 92.8%.

Example 2

Add 5 g of manganese dichloride to 50 mL of water to prepare a solution, then add 3 g of sodium tungstate to the solution, stir in a water bath at 60°C for 10 minutes, then add 4 g of nonionic surfactant Triton X- 100 (Triton X-100) and stirred for 10 minutes, then added 5 g of acetone while continuing to stir, and continued to stir for 5 minutes, then transferred the solution to a hydrothermal reactor, reacted for 5 hours at 180°C, filtered to obtain a solid, and washed with distilled water 3 times, dry at 80°C, place in a tube furnace, feed nitrogen, raise the temperature to 700°C at a rate of 10°C/min, keep it for 30 minutes, and cool down to room temperature under the condition of continuously feeding nitrogen to obtain A carbon composite manganese tungstate catalyst.

0.5 g of carbon-composite manganese tungstate catalyst was added to 300 mL of acid scarlet wastewater with a concentration of 25 mg/L, and reacted for 100 min under the irradiation of 120 W LED lamp, the decolorization rate was 97.1%, and the catalyst was separated and reused 5 times , under the same conditions, the reaction time was 100 min, and the decolorization rate was 91.5%.

Example 3

Add 8 g of manganese dichloride to 90 mL of water to prepare a solution, then add 4 g of sodium tungstate to the solution, stir in a water bath at 70°C for 30 minutes, then add 5 g of nonionic surfactant Triton X- 100 (Triton X-100) and stirred for 15 minutes, then added 4 g of acetone while continuing to stir, and continued to stir for 10 minutes, then transferred the solution to a hydrothermal reactor, reacted for 10 h at 260°C, filtered to obtain a solid, and washed with distilled water Wash 5 times, dry at 80°C, place in a tube furnace, feed nitrogen, raise the temperature to 800°C at a rate of 15°C/min, keep it for 120 minutes, and cool down to room temperature under the condition of continuously feeding nitrogen, that is A carbon composite manganese tungstate catalyst is obtained.

0.5 g of carbon-composite manganese tungstate catalyst was added to 300 mL of Rhodamine B wastewater with a concentration of 25 mg/L, and reacted for 100 min under the irradiation of a 120 W LED lamp, the decolorization rate was 94.2%, and the catalyst was separated and reused 5 times Finally, under the same conditions, the reaction time was 100 min, and the decolorization rate was 91.5%.

Claims (1)

1. A kind of 1. preparation method of the compound wolframic acid Mn catalyst of carbon, it is characterized in that in turn including the following steps：By 5 ~ 10 g dichloros Change manganese, which is added in 50 ~ 100 mL water, is configured to solution, then 3 ~ 4 g sodium tungstates are added into the solution, is stirred in 60 ~ 70 DEG C of water-baths Mix 10~50 minutes, add 4 ~ 5 g nonionic surfactant triton x-100s（Triton X-100）10 ~ 15 points of stirring Clock, 1 ~ 5 g acetone is added in lasting stirring, after continuing stirring 5 ~ 10 minutes, solution is transferred in hydrothermal reactor, 180 ~ At 260 DEG C, 5 ~ 10 h are reacted, are filtrated to get solid, with water washing is distilled 3 ~ 5 times, 80 DEG C of drying, be placed in tube furnace, be passed through Nitrogen, 700 ~ 850 DEG C are warming up to 10 ~ 15 DEG C/min speed, is kept for 30 ~ 120 minutes, is being continually fed into the condition of nitrogen Under, room temperature is cooled to, that is, obtains a kind of compound wolframic acid Mn catalyst of carbon.