Heterogeneous catalytic hydrodefluorination treatment method for efficient degradation of fluorinated phenols
A technology of fluorophenol and heterogeneous catalysis, applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of low treatment concentration, low degradation efficiency, and insufficient degradation, and achieve high treatment concentration, The effect of simple preparation, good production and practical value
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Embodiment 1
[0021] Embodiment 1, the preparation of supported Pd-Ni bimetallic catalyst:
[0022] Sedimentation and precipitation method: Take a three-necked flask and add an equimolar amount of NiCl 2 and PdCl 2 Dissolve in dilute hydrochloric acid respectively, mix the two solutions with activated carbon, add Na 2 CO 3 To pH = 10, continue to stir for 1 h; the precipitate was washed with deionized water until neutral, and AgNO 3 No Cl was detected in the filtrate - until; then, NaBH was added dropwise 4 solution, stirred for 1 h; the precipitate was washed with deionized water until neutral, and dried to obtain a supported Pd-Ni / C bimetallic catalyst; the bimetallic Pd-Ni / C catalysts with different contents are listed in Table 1; The preparation process, except that the carrier is different, the rest of the process is the same, the preparation can obtain the supported bimetallic catalyst of different supports, and the prepared supported Pd-Ni bimetallic catalyst is listed in Table ...
Embodiment 2
[0026] Example 2, the influence of different catalysts on the hydrodefluorination of 4-fluorophenol
[0027] Weigh 50 mg of the catalyst prepared in Example 1, add it to a 100 mL three-necked flask, add 4-fluorophenol (4-FP) with a concentration of 5 g / L, 40% isopropanol-water solution (V(isopropanol Alcohol) / V(water)=40 / 60) 80 mL, using hydrogen as hydrogen source (H 2 The flow rate is controlled at 20 mL / min), and the 4-FP in the liquid phase is subjected to catalytic hydrodefluorination in the presence of inorganic base NaOH. The ratio of the amount of inorganic base NaOH to the amount of fluorine element in the reaction substrate is 1.1:1, the reaction pressure was 0.1 MPa, and the reaction temperature was 40 °C. The specific hydrodefluorination results are shown in Table 2.
[0028]
Embodiment 3
[0029] Example 3, Effects of Different Temperatures and Pressures on 4-FP Hydrodefluorination Catalyzed by 2%Pd-2%Ni / C Bimetallic Catalyst
[0030] Weigh 50 mg of the 2%Pd-2%Ni / C bimetallic catalyst prepared by the electrostatic adsorption method in Example 1, add it to a 150 mL autoclave, and add 4-fluorophenol with a concentration of 5 g / L ( 4-FP) 40% isopropanol-water solution (V (isopropanol) / V (water) = 40 / 60) 80 mL, using hydrogen as the hydrogen source, in the presence of inorganic base NaOH, the 4- FP carries out catalytic hydrodefluorination treatment, the ratio of the amount of inorganic alkali NaOH to the amount of fluorine element in the reaction substrate is 1.1:1, the reaction pressure is 0.1 MPa, 0.5 MPa and 1.0 MPa, and the reaction temperature is controlled separately At 20 °C, 30 °C, 40 °C, 60 °C and 80 °C, the specific hydrodefluorination results are shown in Table 3.
[0031]
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