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Bimetallic PD‑NI/CEO for nitrosodimethylamine reduction 2 ‑tio 2 Catalyst and its preparation method

A nitrosodimethylamine and catalyst technology, which is applied in the field of liquid-phase catalytic hydrogenation reduction of nitrosodimethylamine, can solve the problems of few reports and achieve the effects of low loading, good application prospects, and improved degradation efficiency

Inactive Publication Date: 2017-10-31
NANJING UNIV OF SCI & TECH
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  • Summary
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, about CeO 2 -TiO 2 There are few reports on composite oxides and their application in catalytic hydrogenation reduction reactions

Method used

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  • Bimetallic PD‑NI/CEO for nitrosodimethylamine reduction <sub>2</sub> ‑tio <sub>2</sub> Catalyst and its preparation method
  • Bimetallic PD‑NI/CEO for nitrosodimethylamine reduction <sub>2</sub> ‑tio <sub>2</sub> Catalyst and its preparation method
  • Bimetallic PD‑NI/CEO for nitrosodimethylamine reduction <sub>2</sub> ‑tio <sub>2</sub> Catalyst and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0024] Example 1: Preparation and application of Pd-Ni / Ce:Ti=4:1

[0025] (1) Take cerium nitrate hexahydrate solution and titanium sulfate as cerium salt and titanium salt respectively, prepare Ce:Ti=4:1 (molar ratio) solution and mix well.

[0026] (2) Titrate the precipitant ammonia water into the beaker of the above mixed solution until the pH=10, stir to make the precipitate uniform, age for 12 hours, centrifuge, wash, dry, and then bake in a muffle furnace at 600°C for 4 hours.

[0027] (3) Add the powder obtained in (2) to PdCl 2 and Ni(NO 3 ) 2 solution with 1M Na 2 CO 3 Adjust the pH value of the solution to 10.5, stir magnetically for 3 hours at this pH value, and then add NaBH dropwise to the solution under vigorous stirring conditions 4 solution, after 1 hour, the hydrogen bubbles generated in the solution gradually disappeared, the solution was centrifugally washed to neutrality, and the material was dried at 70°C. The mass of Pd and Ni is respectively 2.5% an...

example 2

[0037] Example 2: Preparation and application of Pd-Ni / Ce:Ti=9:1

[0038] (1) Take cerium nitrate hexahydrate solution and titanium sulfate as cerium salt and titanium salt respectively, prepare Ce:Ti=9:1 (molar ratio) solution and mix well.

[0039] Other steps follow (2), (3) and (4) in Example 1 to synthesize Pd-Ni / Ce:Ti=9:1.

[0040] Using Pd-Ni / Ce:Ti=9:1 as a catalyst, catalytic hydrogenation reduces NDMA. Under the same reaction conditions as example 1, Pd-Ni / Ce:Ti=9:1 NDMA degradation efficiency reached 94.1% in the time of 30min (see Figure 4 ). It can be seen that under the same conditions, Pd-Ni / Ce:Ti=9:1 ratio Pd-Ni / CeO 2 It has higher catalytic activity, but it is not as active as Pd-Ni / Ce:Ti=4:1.

example 3

[0041] Example 3: Preparation and application of Pd-Ni / Ce:Ti=2:1

[0042] (1) Take cerium nitrate hexahydrate solution and titanium sulfate as cerium salt and titanium salt respectively, prepare Ce:Ti=2:1 (molar ratio) solution and mix well.

[0043] Other steps follow (2), (3) and (4) in Example 1 to synthesize Pd-Ni / Ce:Ti=2:1.

[0044] Using Pd-Ni / Ce:Ti=2:1 as a catalyst, catalytic hydrogenation reduces NDMA. Under the same reaction conditions as example 1, Pd-Ni / Ce:Ti=2:1 NDMA degradation efficiency reached 86.7% in the time of 30min (see Figure 4 ). It can be seen that under the same conditions, Pd-Ni / Ce:Ti=2:1 ratio Pd-Ni / CeO 2 The catalytic activity of Pd-Ni / Ce:Ti=4:1 is not as high as that of Pd-Ni / Ce:Ti=4:1, indicating that further Ti doping will inhibit the Pd-Ni / CeO 2 -TiO 2 catalytic activity of the catalyst.

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Abstract

The present invention discloses a preparation method of a Pd-Ni / CeO2-TiO2 bimetallic composite oxide catalyst and an application thereof in nitrosodimethylamine reduction by liquid phase catalytic hydrogenation. The catalyst uses CeO2-TiO2 as a carrier, and supports active ingredients Pd and Ni, wherein the molar ratio of Ce to Ti is x to 1, x is greater than or equal to 1 but less than or equal to 9. The preparation method for the catalyst is a co-deposition precipitation method which specifically comprises the following steps of: (1) using cerium nitrate hexahydrate and titanium sulfate as raw materials, dropwise adding ammonia water into a mixed solution to precipitate and age, then performing centrifugalization, washing and drying and finally roasting the precipitate to obtain CeO2-TiO2; and (2) using PdCl2 and Ni(NO3)2 as an active ingredient, supporting the active ingredient on the CeO2-TiO2 carrier by using the co-deposition precipitation method, adding sodium borohydride for reduction, and obtaining the Pd-Ni / CeO2-TiO2 after washing and drying. An effect of using the catalyst for the nitrosodimethylamine reduction by catalytic hydrogenation, which is good, is better than that by using a conventional oxide as a carrier. The catalyst and the preparation method provided by present invention have great significance on development of catalysts, and have a wide application prospect in governance of a typical disinfection byproduct nitrosodimethylamine.

Description

technical field [0001] The present invention relates to a bimetallic Pd-Ni / CeO for the reduction of nitrosodimethylamine 2 -TiO 2 Catalyst, preparation method thereof, and application in liquid-phase catalytic hydrogenation reduction of nitrosodimethylamine. Background technique [0002] Nitrosodimethylamine (NDMA) is a typical representative of nitrosamines. Recently, as a new type of disinfection by-product, it is often detected in water disinfected with chlorine or chloramine. Due to its strong carcinogenic potential, it has been attracted extensive attention of researchers. The results of toxicity tests show that NDMA can cause liver cancer, lung cancer and nervous system damage. Therefore, the U.S. Environmental Protection Agency has listed it as a B2 chemical pollutant, and the European Union has also listed it as a genotoxic carcinogen. The tolerable limit for NDMA in drinking water established by the California Department of Health Services is 10 ng / L. [0003] T...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/89C02F1/70C02F101/38
CPCB01J23/002B01J23/894B01J2523/00C02F1/70C02F2101/38B01J2523/824B01J2523/847B01J2523/3712B01J2523/47
Inventor 陈欢李婷谭玲江芳
Owner NANJING UNIV OF SCI & TECH
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