1097results about "Nitro compound preparation" patented technology

The invention relates to a method for undergoing a chlorobenzene nitration reaction by using a micro-channel reactor, belonging to the technical field of application of organic synthesis. In the method, nitric acid, sulfuric acid, water and chlorobenzene are taken as initial reaction raw materials, and processes such as mixed acid preparation, mixed acid and chlorobenzene preheating, mixed acid and chlorobenzene reacting and the like are completed in a micro-channel reactor system. In the reaction, nitro-sulfuric mixed acid is taken as a nitrating agent, the effective concentration of sulfuric acid in the mixed acid is 50-90 percent, the molar ratio of the nitric acid to the sulfuric acid in the mixed acid is 1:1-1:10, the molar ratio of the chlorobenzene to the nitric acid is 1:1.0-1:2.0, the reaction temperature is 50-100 DEG C, and the reaction time is 30-120 seconds. The chlorobenzene transformation ratio is up to 97 percent, the selectivity of nitrochlorobenzene serving as a product is over 96.5 percent, and the ratio of ortho-para nitrochlorobenzene is over 0.6. A strengthened mixed micro-channel reactor adopted in the invention is particularly suitable for undergoing a continuous nitration reaction, and has the characteristics of stable temperature control and safe process.

The present invention relates to a process for working up or treating aqueous waste waters which are formed during the nitration of toluene to dinitrotoluene with nitrating acid. These aqueous waste waters containing acidic wash water and alkaline wash water from the dinitrotoluene washing step, and distillate from the sulfuric acid concentration step. The process comprises,

• • a) combining the acidic and alkaline waste waters from the washing step and the aqueous distillate from the sulfuric acid concentration step such that the resulting mixture has a pH below 5,
  • b) separating the aqueous and organic phases which are formed by phase separation,
  • c) subjecting the aqueous phase from b) to an extraction step, wherein
  • d) the organic components contained in the aqueous phase from c) are extracted with toluene, and
  • e) introducing the toluene phase enriched with the organic components into the toluene nitration.

The present invention generally relates to processes for the chemocatalytic conversion of a glucose source to an adipic acid product. The present invention includes processes for the conversion of glucose to an adipic acid product via glucaric acid or derivatives thereof. The present invention also includes processes comprising catalytic oxidation of glucose to glucaric acid or derivative thereof and processes comprising the catalytic hydrodeoxygenation of glucaric acid or derivatives thereof to an adipic acid product. The present invention also includes products produced from adipic acid product and processes for the production thereof from such adipic acid product.

The invention relates to a one-step method for synthesizing dinitrochlorobenzene from chlorobenzene, and a microchannel reactor. The method comprises the steps of taking chlorobenzene and mixed acid of nitric acid/sulfuric acid (n/s) as initial reaction materials, inputting material flow synchronously into a microreactor through a metering pump and finishing mixed mass transfer and reaction in a reaction channel. The substance ratio of n to s in the reactive mixed acid is 0.1 to 0.5, and the mass ratio of water is less than 10 percent. The microchannel reactor adopts a stainless steel flat-plate structure which comprises fixed pressing-sealing plates, a microchannel plate, a raw-material inlet, a product outlet, as well as a temperature-control pore channel and a thermal-couple measurement-control jack which are positioned on two sealing plates. The method is continuously operated under a technological condition with strong nitrating acid, and is safe in process. The selectivity of the dinitrochlorobenzene in the reactor at an operation temperature between normal temperature and 80 DEG C is more than 99.5 mol percent, wherein the selectivity of 2,4 dinitrochlorobenzene is more than 98 mol percent.

The invention relates to a combined nitrification method for synthesizing nitrobenzene and a combined device of a micro-reactor and a stirring reactor. During the synthesis, benzene and mixed acid of nitric acid and sulfuric acid are taken as initial materials, are conveyed to two inlets of the micro-reactor through a metering pump respectively, are premixed in micro-channels, and perform partialnitration reaction at the same time; and a first-stage nitration product with high dispersion state is produced at an outlet of the micro-reactor. The first-stage nitration product continuously flowsinto a stirred tank nitration reactor to continue to react. The method and the device perform continuous operation under the condition of the mixed acid with high water content and have safe process,the conversion rate of the benzene is 99.85 percent (mol), and the selectivity of a product, namely the nitrobenzene is 99.8 percent (mol).

The invention relates to one-step dinitrotoluene synthesis in a microchannel reactor. The method comprises the steps of taking toluene and mixed acid of nitric acid/sulfuric acid (n/s) as initial reaction materials, inputting material flow synchronously into a microreactor through a metering pump and finishing mixed mass transfer and reaction in a reaction channel. The substance ratio of n to s in the reactive mixed acid is 0.1 to 1.0, and the mass ratio of water is less than 15 percent. The liquid hourly space velocity in the reactor is 500 to 50,000 h<-1>. The microchannel reactor adopts a stainless steel flat-plate structure which comprises fixed pressing-sealing plates, a microchannel plate, a raw-material inlet, a product outlet, as well as a temperature-control pore channel and a thermal-couple measurement-control jack which are positioned on two sealing plates. The method is continuously operated under a technological condition with medium/strong nitrating acid, and is safe in process. The conversion rate of the toluene in the reactor at an operation temperature between normal temperature and 80 DEG C is higher than 98 percent, and the yield of dinitrotoluene is higher than 95 percent, wherein the ratio of two main isomer components, namely 2,4-dinitrotoluene and 2,6-dinitrotoluene, is more than 4 and can be nearly 5 under optimum conditions.

The invention relates to a method to continuously produce dinitrotoluene and the device that is suited to the method. The method adopts two steps to make dinitrotoluene and organic phase and spent acid phase are separated. The acid phase is cycling used in the first and the second stage; toluene, nitric acid and mixture acid are added into the center of draft tube of reactor synchronously, mixing fully, cycling in the center and outside of the draft tube; after fully reacting, the taking gravity settling separation in the separator where spent acid cycling device, stop cycling device, and disc type separating device are installed.

The invention relates to a production method for preparing 2,5-dichloronitrobenzene (DCNB) through continuous nitration, which particularly realizes the recycling of waste acids in the preparing process. The invention provides a technological program capable of recycling acids for preparing 2,5-dichloronitrobenzene (DCNB) through the continuous nitration, which is characterized in that sulfuric acid and nitric acid are prepared into a mixed acid, the mixed acid and paradichlorobenzene are simultaneously fed into a three-stages kettle (ring) type continuous reactor to carry out nitration reaction, a nitration reaction solution discharged form the third-stage kettle (ring) type continuous reactor is stood for layering so as to obtain a nitrifying oil layer and a nitrifying waste acid, and the nitrifying oil layer is subjected to alkali cleaning, water washing and light component removal so as to obtain a 2,5-DCNB finished product; paradichlorobenzene is added into the nitrifying waste acid to extract organic matters in the acid layer, residual HNO3 in the acid layer is consumed, after the extraction is completed, the obtained product is layered so as to obtain an extraction oil layer and an extracted residual waste acid, the extraction oil layer is used for next-batch nitrification, the extracted residual waste acid after being concentrated and nitric acid are prepared into the waste acid for next-batch nitrification, a small amount of emulsion layer is produced in the process of recycling, and the emulsion layer after being combined with the nitrifying oil layer is subjected to alkali cleaning and water washing.

The invention discloses a method for continuously preparing dinitrochlorobenzene. Multiple dinitration reactors are connected in series for reaction, and mononitrochlorobenzene is continuously added to the first dinitration reactor, and continuously flows through all the dinitration reactors and flows out; a mixed acid nitrating agent is prepared from 75-85% of sulfuric acid, 2-7% of nitric acid and 5-15% of water; the reaction temperature is 40-95 DEG C; and each dinitration reactor is provided with a separation device for separating an organic phase from an inorganic phase, and the inorganic phase is returned into the reactor, thereby keeping the inorganic phase and the organic phase in the required proportion. In the invention, the dinitrochlorobenzene is prepared by continuous reactions, and the reactions are continuously carried out and sequentially completed; chlorobenzene is used for extracting nitrates and nitric acid in an acid phase, thereby lowering the content of the nitric acid in the acid phase and recycling the nitrates in the acid phase; by the invention, the dinitrochlorobenzene can be continuously prepared from two raw materials (chlorobenzene and p-nitrochlorobenzene) by using one set of devices; and the invention has the advantages of low raw material consumption and high production capacity.

A process for preparing nitrophenylether, aminophenylether and amidophenylether between chlorobenzene and acid mixture removing water, liquid-liquid separation to obtain organic phase consisting of o-, p- and meta-nitro chlorobenzene compounds, etherifying said mixture, recovering etherifying agent, vacuum distilling, separating and refining meta-nitro chlorobenzene, removing chloride salt generated in etherification, crystallizing separation, recrystallizing p- and o-nitro phenylether compounds, catalytic hydrogenating reaction, nitrifying reaction to obtain 2,4-drinitro phenylether, catalytic hydroreducing reaction to obtain 2,4-diamino phenylether, and aceylating reaction to obtain 2-amino-4-acetylamino phenylether.

Provided is a process for making nitrated hydrocarbons by reacting aqueous nitric acid with a hydrocarbon feedstock and a carboxylic acid under specific reaction conditions.

Provided is a process for the formation of 2-nitropropane and/or 2,2-dinitropropane by the nitration of propane with dilute nitric acid.

The invention discloses a method for treating waste residue for producing 1-aminoanthraquinone into a raw material for producing 1,5(1, 8)-dinitroanthraquinone. The method treats and removes isomer containing beta-nitroanthraquinone in the waste residue for producing the 1-aminoanthraquinone to obtain mixed nitroanthraquinone (mixed niter for short), and the mixed niter mainly contains the 1,5(1, 8)-dinitroanthraquinone and the 1-aminoanthraquinone and can be used as the raw material for producing the 1,5(1, 8)-dinitroanthraquinone. The method comprises the following steps: crushing 100 portions by mass of dry waste residue for producing the 1-aminoanthraquinone into powder, adding 400 to 500 portions by mass of sulfuric acid or nitric acid into the powder, heating the mixture to between 50 and 65 DEG C, stirring the mixture for 1 to 2 hours, and filtering, washing and drying the mixture to obtain the mixed niter which can be directly used as the raw material for producing the 1,5(1, 8)-dinitroanthraquinone, wherein the 1,5(1, 8)-dinitroanthraquinone can be produced through dinitration reaction of anthraquinone according to the method of CN101423477A, and bulk commodity dye disperse blue 2BLN (C.I. disperse blue 56) is further produced. The method has simple process; and the obtained product has stable quality and obvious economic benefit.

The invention relates to the nitration of aromatic or heteroaromatic compounds, wherein an activated aromatic or heteroaromatic compound and a nitrating agent, in the presence, if desired, of a solvent, are mixed intensely in a microreactor, and wherein the proportion of the nitrating agent to the activated aromatic or heteroaromatic compound, the concentration of nitrating agent in the reaction mixture, and the temperature are selected at levels such that the nitration begins autocatalytically, and wherein the nitration product is obtained after leaving the microreactor and, if desired, after an after-reaction time outside the microreactor.

The invention provides a process for producing a variety renewable aromatic compounds such as benzene, toluene, xylenes, and cumene, as well as compounds derived from these including, for example, aniline, benzoic acid, cresol, cyclohexane, cyclohexanone, phenol and bisphenol A, toluene di-isocyanate, isophthalic acid, phthalic anhydride, terephthalic acid and dimethyl terephthalate. The invention also provides for renewable forms of these aromatic compounds.

The invention relates to the field of pharmaceutical synthesis, and in particular relates to a preparation method for a medicament Ivacaftor for treating cystic fibrosis. The method is characterized by comprising the following steps of: protecting phenolic hydroxyl by using alkoxycarbonyl by using 2,4-ditertiary butyl phenol as an initial raw material; nitrifying and reducing phenolic hydroxyl; condensing the phenolic hydroxyl with 4-oxo-1,4-dihydroquinolines-3-formyl chloride to obtain carbonic acid (2,4-ditertiary butyl-5-(1,4-dihydro-4-oxoquinoline-3-formamide) phenylester ethyl ester; and finally removing alkoxycarbonyl under an alkali condition to obtain the Ivacaftor. The method can be used for overcoming multiple defects of the existing synthetic method, is simple and easily available in raw materials, convenient to experimentally operate and postprocess, high in yiled, good in product quality and suitable for scale production.

A catalyst of the invention includes a cyclic acylurea compound having a cyclic acylurea skeleton represented by following Formula (I):

wherein R is a hydrogen atom or a hydroxyl-protecting group; n is 1 or 2; G is a carbon atom or a nitrogen atom, where two Gs are the same or different when n is 2. The catalyst may include the cyclic acylurea compound and a metallic compound in combination. In the presence of the catalyst, (A) a compound capable of forming a radical is allowed to react with (B) a radical scavenging compound and thereby yields an addition or substitution reaction product of the compound (A) and the compound (B) or a derivative thereof. This catalyst can produce an organic compound with a high selectivity in a high yield as a result of, for example, an addition or substitution reaction under mild conditions.