99-51-4Relevant articles and documents
Self-powered continuous nitration method and device
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Paragraph 0057-0060, (2021/07/17)
The invention belongs to the technical field of organic synthesis application, and particularly relates to a self-powered continuous nitration method and device. According to the method, a raw material (or a raw material solution) and mixed acid (or nitric acid) are added into a self-powered continuous reactor at the same time, reaction feed liquid continuously and circularly flows, is mixed and reacts in a tube pass through self-propelling force generated by stirring of an impeller, the mass and heat transfer process is completed, and the target requirement is met. According to the invention, the mass transfer and heat transfer efficiency can be improved, the heat exchange and heat transfer capabilities are improved, the reaction time is shortened, the risk degree of art is reduced, the thermal runaway risk is avoided, the reaction safety is improved, and the realization of chemical industry intrinsic safety large scale production is facilitated.
Cyhalofop-containing pesticide composition and application thereof
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Paragraph 0016; 0035; 0040-0041; 0046; 0051-0052; 0057; ...., (2021/11/26)
The invention discloses a pesticide composition containing cyhalofop-butyl and application thereof, belongs to the technical field of pesticide preparation and comprises 10 - 20 parts of cyhalofop-butyl. Tetramethyl chloride 3-5 parts, synergistic microcapsule 8-13 parts, wetting agent 1.5 - 4.5 parts, dispersing agent 1-3 parts, defoaming agent 0.5 - 1.5 parts and water 40 - 50 parts. When the water in the soil is less, the weed is absorbed by the chitosan so as to accelerate the absorption of A the synergic microcapsule and the cyhalofop-butyl ester, so that the pesticide composition is greatly reduced per mu.
Photoinduced Iron-Catalyzed ipso-Nitration of Aryl Halides via Single-Electron Transfer
Wu, Cunluo,Bian, Qilong,Ding, Tao,Tang, Mingming,Zhang, Wenkai,Xu, Yuanqing,Liu, Baoying,Xu, Hao,Li, Hai-Bei,Fu, Hua
, p. 9561 - 9568 (2021/08/06)
A photoinduced iron-catalyzed ipso-nitration of aryl halides with KNO2 has been developed, in which aryl iodides, bromides, and some of aryl chlorides are feasible. The mechanism investigations show that the in situ formed iron complex by FeSO4, KNO2, and 1,10-phenanthroline acts as the light-harvesting photocatalyst with a longer lifetime of the excited state, and the reaction undergoes a photoinduced single-electron transfer (SET) process. This work represents an example for the photoinduced iron-catalyzed Ullmann-type couplings.
Method and device for preparing methylnitro-benzene by channelization
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Paragraph 0047; 0048; 0049, (2019/02/04)
The invention discloses a method and a device for preparing methylnitro-benzene by channelization. The device comprises a storage tank, a nitrogen dioxide cylinder, an ozone generator, a flow pump, agas flowmeter, a reaction pipeline filled with a catalyst, a mixing pipeline, two T-shaped mixed joints, a cooling system, a heating system, a back pressure valve and a receiving tank. The method specifically comprises the following steps: opening the cooling system and the heating system; opening the ozone generator; arranging the flow pump and the gas flowmeter; and mixing raw materials liquid methyl benzene and nitrogen dioxide through the first T-shaped mixing joint and feeding the mixture into the mixing pipeline, then mixing the mixture with ozone in the second T-shaped mixing joint, feeding the mixture into the reaction pipeline filled with the catalyst for a nitrifying reaction, and post-treating a reaction liquid to obtain methylnitro-benzene. The method is controlled precisely and automatically, and is simple to operate, mild in reaction condition, simple in post treatment, quick to transfer mass and heat, high in safety and good in economical benefit.
Hydrophobic WO3/SiO2 catalyst for the nitration of aromatics in liquid phase
Kulal,Kasabe,Jadhav,Dongare,Umbarkar
, p. 105 - 113 (2019/02/15)
WO3/SiO2 solid acid catalyst synthesized using sol gel method has shown promising activity (up to 65% conversion) for aromatic nitration in liquid phase using commercial nitric acid (70%) as nitrating agent without using any sulfuric acid. The water formed during the reaction as well as water from dilute nitric acid (70%) was removed azeotropically, however due to the hydrophilic nature of the catalyst, some water gets strongly adsorbed on catalyst surface forming a barrier layer between catalyst and organics. This prevents effective adsorption of substrate on catalyst surface for its subsequent reaction. To improve the activity further, the hydrophilic/hydrophobic nature of the catalyst was altered by post modification by grafting with commercial short chain organosilane (Dynasylan 9896). The modified 20% WO3/SiO2 catalyst when used for o-xylene nitration in liquid phase, showed significant increase in the conversion from 65% to 80% under identical reaction conditions. Catalyst characterization revealed decrease in the surface area of 20% WO3/SiO2 from 356 m2/g to 302 m2/g after grafting with Dynasylan 9896. The fine dispersion of WO3 particles (2–5 nm) on silica support was not affected due to modification. NMR and FTIR study revealed the decrease in surface hydroxyl groups imparting hydrophobicity to the catalyst. Interestingly the total acidic sites of the catalyst remained almost unaltered (0.54 mmol NH3/g) even after modification. Even though, the acidity and other characteristics of the catalyst did not change appreciably, there was a considerable increase in the o-xylene conversion which can be ascribed to the hydrophobic nature of the catalyst.
Base promoted peroxide systems for the efficient synthesis of nitroarenes and benzamides
Gupta, Sampa,Ansari, Alisha,Sashidhara, Koneni V.
supporting information, (2019/09/07)
A useful and efficient approach for the synthesis of nitroarenes from several aromatic amines (including heterocycles) using peroxide and base has been developed. This oxidative reaction is very easy to handle and afforded the products in good yields. Formation of benzamides from benzylamine was also successfully carried out with this metal-free catalytic system in good to excellent yields.
Highly efficient protocol for the aromatic compounds nitration catalyzed by magnetically recyclable core/shell nanocomposite
Maleki, Ali,Aghaei, Morteza,Paydar, Reza
, p. 485 - 490 (2017/01/10)
An efficient protocol for the nitration of aromatic compounds in the presence of a catalytic amount of sulfuric acid-functionalized silica-based magnetic core/shell nanocomposite was reported. The designed products were obtained in high yields in relatively short reaction times at room temperature under solvent-free conditions. The nanocatalyst was simply recovered from the reaction mixture by using an external magnet and efficiently reused for several times. The characterization of particle size, morphology and elemental analysis of the nanocatalyst were provided by scanning electron microscopy, transmission electron microscopy and energy-dispersive X-ray spectroscopy analyses, respectively.
4-nitro-o-xylene continuous synthesis system and synthesis method
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Paragraph 0069; 0070; 0071; 0072, (2016/11/09)
The invention discloses a 4-nitro-o-xylene continuous synthesis system and synthesis method. The synthesis method is characterized in that after being mixed, o-xylene and nitric-sulfuric acid are pressed in a nitration system to undergo nitration reaction; a reaction liquid enters a first split phase tank to be layered and the upper oil phase enters a washing system to undergo labyrinth washing; a washing liquid is layered in a second split phase tank, the upper liquid enters a distillation system to undergo distillation treatment and 4-nitro-o-xylene is collected. Compared with existing vertical tubular nitration reactors, dual ring shaped nitration reactors provided by the invention have the advantages that material flow splitting is carried out more uniformly, backward flow of a reaction liquid can be effectively avoided, the probability of contact between o-xylene and nitric-sulfuric acid is increased, and the raw material conversion rate is increased; the heat exchange area is fuller, and the side reaction can be effectively reduced. The production system provided by the invention has the beneficial effects that all the materials are recycled, thus reducing the production cost; the raw material conversion rate of single batch production is effectively increased, thus reducing the amount of waste acid and wastewater.
N-(1-ethyl propyl)-3,4-dimethylaniline continuous production system and method
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Paragraph 0085; 0086; 0087; 0096; 0097, (2016/11/17)
The invention discloses an N-(1-ethyl propyl)-3,4-dimethylaniline continuous synthesis system and method. The method is characterized in that o-xylene and nitric-sulfuric acid carry out nitration reaction in a nitration system; a reaction liquid passes through a first split phase tank, a labyrinth washing system and a distillation system in sequence to undergo distillation treatment; collected 4-nitro-o-xylene and 3-pentanone carry out catalytic hydrogenation reaction in a hydrogenation reactor; then N-(1-ethyl propyl)-3,4-dimethylaniline is prepared through treatment carried out by a falling film evaporation system. The production system provided by the invention has the beneficial effects that all the materials are recycled, thus reducing the production cost; the raw material conversion rate of single batch production is effectively increased, thus reducing the amount of waste acid and wastewater.
Method for synthesis of 2-aldehyde-4-aminobenzoic acid
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Paragraph 0006, (2017/04/03)
The invention relates to a method for synthesis of 2-aldehyde-4-aminobenzoic acid. The method for synthesis of 2-aldehyde-4-aminobenzoic acid, which is provided by the invention, is simple and cheap, gentle in reaction condition in the preparation process, and high in yield.