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JOURNAL OF CHEMICAL TECHNOLOGY AND BIOTECHNOLOGY · 2022 ·Vol. 97 ·期 5 ·1293-1304 · IF 3.709

Production of NMSBA catalyzed by Co/Mn/Br together with the porous carbon made from coconut shell with ZnCl2 as activator

Le-Yao Wang,Zhen Yang,Feng Guo,Xiang-Li Long

BACKGROUND 2-nitro-4-methylsulfonylbenzoic acid (NMSBA) is commercially produced from the oxidation of 2-nitro-4-methylsulfonyltoluene (NMST) with nitric acid as oxidant and V 2 O 5 as catalyst in a strong acid solution; this process suffers from the following shortcomings: the discharge of large amounts of wastewater and waste gas, as along with the generation of polynitro compounds. It is necessary to develop a technology to avoid the pollution caused by oxidizing NMST with nitric acid. NMSBA can be synthesized by oxidizing NMST with air under the catalysis of the porous carbon made from coconut shell with ZnCl 2 as an activator together with Co/Mn/Br. RESULTS The optimum conditions for the preparation of the porous carbon are as follows: impregnation temperature 60 °C, ZnCl 2 concentration 0.50 mol L −1 , impregnation duration 6 h, carbonization temperature 600 °C, and carbonization time 4 h. The surface characterization suggests that the carbon made in this study holds smaller surface area, acidic groups, and basic groups than the commercial carbon but owns more carboxyl. CONCLUSION The Co/Mn/Br/AC (AC,the porous carbon made in this study) catalytic system is superior to the Co/Mn/Br/H 3 PMo 12 O 40 @CAC(CAC,commercial activated carbon) catalytic system in the production of NMSBA from the oxidation of NMST. The NMSBA selectivity gained by the former is 93.40%, while that gained by the latter is 87.14%. The former can cut down the consumption of NMST and the expenditure of catalysts. The catalytic ability of the AC catalyst relies on its surface chemical characteristics and physical properties. More carboxyl on AC is the reason for the upgrade of NMSBA selectivity. © 2022 Society of Chemical Industry (SCI).

CAS / MDL: 6147-53-1 6156-78-1

研究领域: 化学工程 · 环境科学

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International Journal of Chemical Reactor Engineering · 2022 ·Vol. 21 ·期 5 ·663-678 · IF 1.636

Oxidation of NMST to NMSBA catalyzed by Co/Mn/Br together with porous carbon made from coconut shell with acetic acid as an activator

Feng Guo,Hua-jie Liu,Xin-zhi Zhou,Xiang-li Long

In this paper, a heterogeneous catalytic system consisting of Co/Mn/Br/activated carbon is used to catalyze 2-nitro-4-methylsulfonyl benzoic acid (NMSBA) production from the oxidation of 2-nitro-4-methylsulfonyltoluene (NMST) by oxygen. The activated carbon (AC) is made from coconut shell with acetic acid as an activator. The experiments indicate that the best AC is made by immersing coconut shell in 12 mol L −1 HAc solution at 50 °C for 32 h with a liquid/solid ratio (mL/g) of 5:1 and then being heated in nitrogen at 800 °C for 6 h. Compared with the Co/Mn/Br/H 3 PMo 12 O 40 @CAC (CAC, commercial activated carbon originated from coconut shell) catalytic system, the Co/Mn/Br/AC catalytic system is able to gain much higher NMSBA selectivity. In spite of holding smaller surface and less acidic groups, the AC owns much more carboxyl than CAC, which is the main reason for its better performance in the preparation of NMSBA.

CAS / MDL: 6147-53-1 6156-78-1

研究领域: 化学工程 · 催化材料

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JOURNAL OF CHEMICAL TECHNOLOGY AND BIOTECHNOLOGY · 2025 · IF 2.4

Production of NMSBA from the oxidation of NMST by air under the catalysis of sandwich-type polyoxometalate

Yu-cheng Jiang,Jun-qi Hai,Xiang-li Long

BACKGROUND Mesotrione, a key herbicide for weed management and yield improvement in broad-leaved crops including corn, is synthesized with 2-nitro-4-methylsulfonylbenzoic acid (NMSBA) as an important intermediate. The commercial synthesis of NMSBA typically begins with the nitration of 4-methylsulfonyltoluene to form 2-nitro-4-methanesulfonyltoluene (NMST), followed by oxidation with nitric acid. However, the utilization of nitric acid gives rise to severe environmental and ecological concerns due to its corrosive nature and inherent hazards. Consequently, there is an imperative need to develop a sustainable and green oxidation process for the conversion of NMST to NMSBA in order to mitigate the reliance on chemical oxidants and their associated environmental impacts. RESULTS The synthesis of NMSBA, a catalytic system composed of Co, Mn, Br and sandwich-type polyoxometalate, has been developed to aid the oxidation of NMST to NMSBA by air. The sandwich-type polyoxometalate (POM) {K 10 Co x Mn 4− x (H 2 O) 2 P 2 W 18 O 68 } was synthesized and the best Co/Mn atomic ratio was determined to be 1.5:2.5. The doping of Ce in the POM as a counter-cationic metal improved the selectivity to NMSBA, and the best Ce/K atomic ratio was determined to be 1:7. The immobilization of {CeK 7 Co 1.5 Mn 2.5 (H 2 O) 2 P 2 W 18 O 68 } on activated carbon (AC) not only enhanced the reaction rate and the production of NMSBA but also reduced the amount of POM used. The optimal loading amount of the POM on AC was 20%. CONCLUSION Experiments revealed that the catalytic system composed of Co, Mn, Br and {K 10 Co 1.5 Mn 2.5 (H 2 O) 2 P 2 W 18 O 68 } was superior to the catalytic system consisting of Co, Mn, Br and heteropoly acids H 3 PW 12 O 40 /H 3 PMo 12 O 40 . The catalytic performance of {CeK 7 Co 1.5 Mn 2.5 (H 2 O) 2 P 2 W 18 O 68 }/AC exceeded that of H 3 PMo 3 W 9 O 40 /AC in the production of NMSBA by oxidizing NMST with oxygen. © 2025 Society of Chemical Industry (SCI).

CAS / MDL: 6147-53-1 6156-78-1

研究领域: 催化化学 · 绿色化学 · 有机合成 · 环境科学 · 多金属氧酸盐化学 · 工业化学

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Production of NMSBA catalyzed by Co/Mn/Br together with the porous carbon made from coconut shell with ZnCl2 as activator

Oxidation of NMST to NMSBA catalyzed by Co/Mn/Br together with porous carbon made from coconut shell with acetic acid as an activator

Production of NMSBA from the oxidation of NMST by air under the catalysis of sandwich-type polyoxometalate