576 results about "Dinitrobenzene" patented technology

The invention discloses a polycyclic benzothiadiazole non-fullerene acceptor material, a preparation method thereof and an application of the material. The polycyclic benzothiadiazole non-fullerene acceptor material comprises a polycyclic benzothiadiazole center core and electrophilic end groups, the polycyclic benzothiadiazole center core is of a nitrogen bridge trapezoidal polycyclic structure,the electrophilic end groups are connected to two ends of the center core, 4, 7-dibromo-5, 6-binitro benzothiadiazole serves as a raw material in the preparation process, Stille coupling and Vilsmeier-Haack reaction are sequentially performed to obtain the polycyclic benzothiadiazole center core, and end-group structures are introduced by Knoevenagel reaction to obtain the polycyclic benzothiadiazole non-fullerene acceptor material. The acceptor material is good in solubility and easily processed into a film, has a good photoelectric conversion function and is used for preparing an organic solar battery device, and photoelectric conversion efficiency reaches nearly 16% of single battery conversion efficiency.

The invention relates to a compounded herbicide composition for rice fields, which contains the following two effective components: component (A): pyribenzoxim; component (B): a herbicide which is one of the following compounds: triazines compounds, heterocyclic compounds, phenoxy compounds, amide compounds, diphoenyl ether compounds, sulfonylurea compounds, phenoxyalkanoic acid compounds, botanical compounds, organic phosphorus compounds, urea compounds, dinitroaniline compounds, benzamide compounds and carbamate compounds; and wherein, the weight ratio of the component (A) to the component (B) is 1-50: 1-50.

The invention discloses a heptatomic condensed ring benzotriazole receptor micromolecule and a preparation method and application thereof. The compound takes heptatomic condensed ring benzotriazole (B) with an alkyl chain as intercalated nucleus, and cyan group as n-type fullerene receptor material (BIC) of an electrophilic unit. The preparation method comprises the following steps: by taking 4,7-dibromo-5,6-dinitro benzotriazole compound as a raw material, sequentially introducing thienothiophene with an alkyl chain by stille coupling reaction, then performing loop closing, introducing the alkyl chain to N by nucleophilic substitution, introducing aldehyde group via Vilsmeier-Haack, and then introducing a polar conjugation unit by Knoevenage reaction, so as to obtain a BIC compound; the micromolecule forms definite conformation and good solubility, has an electron receptor unit with universality, obtains a high efficiency (PCE of 13%) on a solar cell, and thus is a photovoltaic material full of potential.

A process for treating the waste water in oil field by electricity-multi-phase catalytic reaction features that under the existance of external electric field, the organic pollutants in the said waste water are catalytically oxidized by the surface of catalyst. The catalyst is composed of the active components chosen from one or several oxides of Fe, Co, NI, Mn, Cu, Ti, W and Pb and the carrier chosen from SiO2, Al2O3, zeolite molecular sieve and activated carbon. Among the mentioned catalyst, one or several oxides of rare earth metals as auxiliaries may be added. The said catalyst is made upthrough impregnating, oven-drying and sintering; and it can effectively treat oil-contained waste water as well as dinitrophenol waste water, fertilizer plant waste water, cutting liquid waste water,etc.. Its advantages are high effect and low cost.

The invention relates to a method for detecting eight volatile carbonyl compounds in a filter tip through liquid chromatography-tandem mass spectrometry. The eight volatile carbonyl compounds are formaldehyde, acetaldehyde, propanal, acetone, acraldehyde, crotonaldehyde, butanal and 2-butanone. The method comprises the following steps: performing ultrasonic extraction on the carbonyl compounds in a filter tip by using an acetonitrile / water mixed solution, performing 2,4-dinitrophenylhydrazine derivatization reaction, and analyzing through a liquid chromatography-tandem mass spectrometer (LC-MS / MS). Compared with the original gas chromatography, the LC-MS / MS method used in the method has the following advantages: (1) the LC-MS / MS method is higher in sensitivity, and the two-stage mass spectrometry can more effectively eliminate the false positive result, thus ensuring that the qualitative analysis accuracy is higher; (2) separation is performed through liquid chromatography, and 2,4-dinitrophenylhydrazone of the carbonyl compounds has favorable stability; (3) the sample does not need to be purified, and the pretreatment is simple and efficient; and (4) the method can realize the simultaneous detection of the eight volatile carbonyl compounds.

The invention discloses a core shell catalyst by taking hydrotalcite as a shell and a molecular sieve as a core as well as a preparation and an application thereof. According to the invention, divalent metal source and aluminum species in a core-shell molecular sieve are used for forming a hydrotalcite compound on the surface of the molecular sieve, and the core-shell structure molecular sieve by taking the molecular sieve as the core and the petal hydrotalcite as the shell is formed; after the molecular sieve is reduced, the nano-grade metal-modified molecular sieve catalyst having uniform size, high dispersibility, excellent heat stability and high universality is obtained, and can be used for a catalytic reaction for hydrogenation synthesis of m-dinitrobenzene to obtain m-phenylenediamine. compared with the prior art, the preparation process is simple, the metal atom utilization rate is high, applied metal source is almost completely reacted, no loss is generated, cost is reduced, and pollution on environment is reduced, industrial production is easy, and a series of different metal-modified molecular sieve catalysts can be prepared according to the modifiable character of the composition elements of the hydrotalcite and diversity of a topological structure of the molecular sieve.

The invention discloses a specific fluorescence probe for identifying thiophenol and application of the specific fluorescence probe and belongs to the field of fine chemical industry. The specific fluorescence probe is a derivative of 2-benzothiazole-6-naphthol and is prepared by the following steps: mixing the 2-benzothiazole-6-naphthol and 2, 4-dinitrobenzene into an N, N-dimethylformamide solution according to a proportion, heating, and finally, purifying by adopting silica gel chromatography to obtain the fluorescence probe. The fluorescence probe and a corresponding thiophenol content detecting process can not be interfered by matrixes and impurities in a biological system and can be used for quantitatively determining the thiophenol content in various biological systems. The specific fluorescence probe is high in specificity, can be hydrolyzed after being acted with the thiophenol, namely an ether bond is fractured; is cheap and is easy in acquisition, can be obtained by chemical synthesis, is simple and feasible in synthetic process; is high in sensitivity, is good in fluorescence attribute. A hydrolysate can be excited by a two-photon laser with 800nm as an excitation light source, a biological sample is weak in background fluorescence, and the specific fluorescence probe is suitable for detecting the thiophenol content in cells and is capable of quantitatively determining the thiophenol by drawing a standard curve.

The invention relates to a method for testing the content of formaldehyde in food by means of liquid chromatography, in particular to a method for testing the formaldehyde in import and export aquatic products, vegetables (including mushroom), cereal products, dairy products and beers, etc. The method for testing the content of the formaldehyde in the food by means of liquid chromatography comprises the steps of: (1) extracting; (2) purifying; (3) preparing formaldehyde standard work solution; (4) testing; (5) blank testing; and (6) computing and expressing a result. The method adopts acetonitrile / pH 5 ethylic acid buffer solution (1 / 1, v / v) of 2, 4-dinitrophenylhydrazine to directly derive and extract the formaldehyde in a sample and test by means of the liquid chromatography. The formaldehyde is extracted from the sample under water bath at the temperature of 60 DEG C and the derivatization reaction is performed. The 2, 4-dinitrophenylhydrazine and the group in protein compete for the formaldehyde in the reaction solution, thereby being capable of effectively preventing the formaldehyde from combining with the protein in the sample and having higher formaldehyde recovery ratio than that of by using an immersion method.

The invention discloses a synthetic method and application of a porphyrin type near-infrared sulfur ion fluorescence probe. The fluorescence probe is prepared by reaction of TPP-OH and 2,4-dinitrobenzene sulfonyl chloride as raw materials, N,N-DIEA as a catalyst and dichloromethane as a solvent at room temperature. The probe can carry out fluorescence detection of high sensitivity and selectivity on sulfur ions. Compared with an existing small organic molecule fluorescence probe, the obtained fluorescence probe has longer fluorescence emission wavelength (lambda em > 650 nm), can carry out detection of high sensitivity, selectivity and timeliness on the micro sulfur ions on a near infrared region, and has huge application prospects in the biological and environment detection field.

The invention belongs to a method for producing phenylene diamine, in particular to the method for producing the phenylene diamine by performing hydrogenation reduction on mixed dinitrobenzene with palladium catalyst. The prior art which produces the phenylene diamine by performing the hydrogenation reduction by adopting a Raney nickel or carrier nickel catalyst has the disadvantages of high energy consumption, low raw material conversion rate, and poor product quality. The method comprises the following steps of: adding 100 weight parts of dinitrobenzene, 100 to 200 weight parts of alcohols solvents and 0.5 to 1 weight part of the palladium catalyst into a reaction kettle, wherein the temperature in the reaction kettle is between 40 and 60 DEG C and the pressure is between 0.25 and 0.60 MPa; performing hydrogenation for 30 to 120 minutes; conveying a reaction product to a filter; dealcoholizing in a dealcoholization tower for recovering to obtain phenylene diamine solution; and obtaining m-phenylenediamine, o-phenylenediamine and p-phenylenediamine products by dewatering, rectifying and separating. The method has the advantages of improving product quality, reducing raw material consumption and reducing production cost.

The invention provides an excised mutagenesis tetraploid method of water melon and ploidy early stage certification technique, wherein dinitro toluene herbicide (DNH) is employed to substitute the conventional colchicines as inducer, whose function is to suppress the Mitosis in the metaphase of cell division through the mechanism of interfering spindle, so as to double the tissue cell chromosome. The method has the advantages of increased inducement success rate and substantially shortened time required for inducement.

The invention relates to an enzymatic test kit for glycosylated hemoglobin, which is composed of hemolysis buffer solution, reagent R1a, reagent R1b and reagent 2; wherein, the hemolysis buffer solution is 10 to 1000mmol / L N- cycloethyl-2-aminoethanesulfonic acid, 10 to 1000mmol / L MOPS and 1 to 100g / L polyethylene glycol oxide dodecyl ether; the reagent R1a is 100 to 10000 kU / L metalloproteinase, 0.1 to 10mmol / L 2-(iodophenyl)-3-(2, 4- dinitrobenzene)-5-(2, 4-disulfophenyl)-2H tetrazole sodium salt; the reagent R1b is 0.1 to 10mmol / L MES and 0.5 to 50mmol / L CaCl2; the reagent 2 is 1 to 100kU / L fructose valine oxidase with high activity, 30 to 600kU / L POD, 0.01 to 0.5mmol / L DA-64 and 10 to 1000mmol / L Tris-HCl. The test kit coincides with the characteristics of rapidness, large batch size and economy which are required by the glycosylated hemoglobin clinical tests.

The invention relates to a kit for quickly detecting toxicity of pesticide residue, in particular to a kit for quickly detecting the toxicity of pesticide residue containing a mixture of acetylcholinesterase and butyryl cholinesterase. The kit consists of choline esterase, a substrate, a color-developing agent 5,5'-dithio-2-2'-dinitrobenzoic acid (DTNB) and phosphate buffer solution, wherein the choline esterase is the mixture containing the acetylcholinesterase and the butyryl cholinesterase, and the substrate contains butyrylthiocholine iodide.

The invention discloses a method for continuously producing resorcin. According to the method, benzene serves as a starting raw material, resorcin is continuously produced through three steps, namely benzene nitration, dinitrobenzene hydrogenated reduction and m-phenylenediamine hydrolysis, devices for benzene nitration and m-phenylenediamine hydrolysis are microchannel reactors, and the reaction for preparing m-phenylenediamine through the catalytic hydrogenated reduction of dinitrobenzene adopts a loop reaction device. The method has the advantages that the phenomena of material backmixing and non-uniform material temperature distribution of the conventional reactors are thoroughly solved, the occurrence of side reactions is reduced, the yield of the product is increased, and the quality of the product is improved; the safety of production during nitration and hydrolysis is improved, meanwhile, the waste of reactants is avoided, and environmental pollution is reduced; and the unit volume production capacity of equipment is increased greatly and is increased by 8-10 times compared with that of kettle type equipment, the production process flow is simplified, and the equipment investment is reduced.

The invention provides a method for separating and measuring acetylcysteine enantiomers. In the method, before acetylcysteine is added in a chromatographic column, a derivatization reagent is used to perform derivatization, wherein the derivatization reagent is N(alpha)-(5-fluoro-2,4-dinitrophenyl)-L-amino acid compound. The method for separation and measurement combines the high performance liquid chromatography (HPLC) or high performance liquid chromatography-mass spectrum (HPLC-MS), and the used chromatographic column uses octadecylsilane chemically bonded silica as filler. The method for separation and measurement comprises the following steps: (1) taking acetylcysteine or a preparation with acetylcysteine, dissolving in low-concentration acid solution, adjusting the pH value of the mixed solution to 6.0-8.0 with alkaline solution to obtain a sample solution for testing; (2) mixing the acetylcysteine solution with 1mol / L of carbonate solution, adding N(alpha)-(5-fluoro-2,4-dinitrophenyl)-L-amino acid compound to mix evenly; (3) reacting the solution obtained by the step (2) at 40-60 DEG C in a dark place, adding hydrochloric acid solution after the reaction; (4) adding the solution obtained by the step (3) in a drying solution with the prestored phosphorus pentoxide and potassium hydroxide, adding phosphate buffer solution-acetonitrile, dissolving residues through ultrasonic treatment, filtering to obtain filtrate which is used as a testing solution; and (5) adopting HPLC or HPLC-MS to separate and measure the testing solution prepared by the step (4).

The invention discloses a production method of flumioxazin. The production method comprises the following steps: by using 2,4-difluoronitrobenzene as an initial raw material, sequentially carrying out nitrification to obtain 1,5-difluoro-2,4-dinitrobenzene, and carrying out etherification reaction on the 1,5-difluoro-2,4-dinitrobenzene and butyl hydroxyacetate to obtain butyl 3-fluoro-4,6-dinitrophenoxyacetate; carrying out reduction cyclization with hydrogen to obtain 7-fluoro-6-amino-2H-1,4-benzoxazinyl-3(4H)-one; under alkaline conditions, carrying out alkynylation reaction with propargyl chloride to obtain an intermediate product; and finally, carrying out amidation reaction with 3,4,5,6-tetrahydrophthalic anhydride to obtain the flumioxazin. The production technique of the method has the advantages of short process, mild reaction conditions and cheap and accessible raw materials, and is convenient to operate; and the solvent used in the preparation process is recyclable. The method also has the advantages of high total reaction yield, high product purity, low production cost and low environmental pollution.

The invention provides a preparation method of 6-amino-7-fluoro-1,4-benzoxazine-3(4H)-ketone, which comprises the following steps: taking 2-(5-fluoro-2,4-dinitrobenzene oxygen) acetic acid as an initial raw material; carrying out hydrogenation reaction to generate 2-(5-fluoro-2,4-diaminobenzene oxygen) acetic acid; and then, carrying out cyclization reaction to obtain the 6-amino-7-fluoro-1,4-benzoxazine-3(4H)-ketone.

The invention discloses a high performance selection coloration compound, the fluorinion detection method and fluorinion reagent paper based on the compound, the compound being coordinated complex characterized by single (2,4-dinitro phenyl hydrazone,10-orthophenanthrolene-5,6-diketone ligand coordination, the compound can be used for the detection of fluorinion within the concentration range of 10-5M, wherein absorption spectrophotometry or naked eye visual colorimetry detections can be employed. The color change reagent paper made through impregnating the compound can appreciably detect fluorine ions whose concentration is below 10mg / L.

The invention relates to a method for preparing m-phenylenediamine. The method comprises the following steps of: (1) preparing m-phthalamide by taking m-xylene as an initial raw material; and (2) reacting isophthalamide with hypohalite or halogen in an alkaline solvent to prepare m-phenylenediamine. Compared with the prior art, the method for preparing m-phenylenediamine completely avoids a mixedacid nitration process, does not generate waste acid, does not generate a strong explosive compound dinitrobenzene, and is safe, clean and efficient.

The invention discloses N-(2,4-dinitrophenyl)-rhodamine B hydrazide and a preparation method and an application of the N-(2,4-dinitrophenyl)-rhodamine B hydrazide. The rhodamine B derivative provided by the invention is N-(2,4-dinitrophenyl)-rhodamine B hydrazide, the structural formula of which is I. The N-(2,4-dinitrophenyl)-rhodamine B hydrazide, is colorless and free from fluorescence, but can selectively react with Cu<2+> ions in chromogenic and fluorescent opening reaction. The colorless substance generates a system with excellent optical performance, so that the detection sensitivity and selectivity of Cu<2+> ions are greatly improved. Therefore, the N-(2,4-dinitrophenyl)-rhodamine B hydrazide is appropriate for high selectivity and high sensitivity detection for the Cu<2+> ions. Detection can be carried out by a light absorption spectrum and a fluorescence spectrum. (FORMULA I).

The invention discloses a method for preparing 2-(5-fluoro-2,4-dinitrophenoxy) acetic acid and ester thereof, which comprises two steps of reactions: performing nitration reaction on 2,4-difluoronitrobenzene serving as a starting material to generate 1,5-difluoro-2,4-dinitrobenzene; and performing etherification with glycollic acid or ester thereof to obtain the 2-(5-fluoro-2,4-dinitrophenoxy) acetic acid and the ester thereof, wherein the condensation reaction is completed at the temperature of between -10 and 50 DEG C for 1 to 12 hours under the action of an acid binding agent in an organic solvent.

The invention discloses a fluorescent probe used for detecting hydrogen sulfide based on a protection-deprotection mechanism. The fluorescent probe provided by the invention has a highly-sensitive highly-selective recognition capacity for detection of hydrogen sulfide. The fluorescent probe provided by the invention is simple to synthesize and high in yield. According to the invention, due to presence of 2,4-dinitro benzenesulfonyl in the probe, the probe itself is free of fluorescence, and fluorescence rapidly increases when a protective group of hydroxy is deprotected after reaction with sulfur ions. The probe can detect hydrogen sulfide in chemical samples, biological samples or medical samples based on fluorescence enhancement or color enhancement, and is suitable for fluorescence imaging.

The invention relates to a catalyst used for coupling reaction of carbon dioxide and an epoxy compound. The catalyst is a Salen-metal complex (I) which has a structural formula shown in the specifications, wherein R1 is 1,2-disubstituted diamine; when R2 is a substituent group with a formula shown in the specifications or nitrogen substituted heterocyclic compound, R3 is tertiary butyl, hydrogen, alkyl or alkoxy; or when R2 is the tertiary butyl, hydrogen, alkyl or alkoxy, R3 is the substituent group with the formula shown in the specifications or nitrogen substituted heterocyclic compound; M is chlorine or bromine, Z is nitrogen or phosphorus, and Y1, Y2 and Y3 are alkane with 1 to 16 carbon atoms respectively; and X is nitrate, boron tetrafluoride, trichloroacetic acid, azide or 2,4-dinitrophenol. For the Salen-metal complex, preparation steps are simple and convenient to operate, cost is low and heavy metal pollution is avoided; 1 mol of catalyst catalyzes 3750mol of cyclic carbonate ester; a cocatalyst and a solvent are not needed; and the cyclic carbonate ester content of a product is over 99 percent.

The invention relates to a synthetic method of dinitrobenzene in a micro-channel reactor. The method comprises the following steps: (1) preparing a mixed acid solution of nitric acid and sulfuric acidat a molar ratio of 0.2-1.0; (2) respectively and simultaneously conveying initial reactants benzene and the mixed acid solution into two inlets of the micro-reactor by a metering pump; (3) mixing reactant benzene and the mixed acid solution in the micro-channel reactor and reacting, wherein the reaction residence time is 8-500 seconds; (4) outputting an obtained reaction material to a collectorfrom a channel of the micro-reactor, and continuously carrying out heat-preservation stirring reaction for 0-1 hour; and separating, washing and drying on the basis of a conventional method to obtaina target product. According to the method, dinitrobenzene synthesis is achieved through the efficient mass and heat transfer capacity of the micro-channel reactor, the process is safe and efficient, the conversion rate is close to 100% under the optimized condition, the yield of the obtained dinitrobenzene is higher than 99%, and the yield of the main product 1, 3-dinitrobenzene reaches 84%.

The invention discloses a reparation method of a hexanitrohexaazaisowurtzitane (CL-20) and 2,5-dinitrotoluene (DNT) eutectic explosive and belongs to the field of energetic materials. Based on the mechanism of eutectic formation, a novel high-energy and low-sensitivity eutectic explosive is formed by high-energy and high-sensitivity CL-20 and low-sensitivity DNT through intermolecular hydrogen bonds. The preparation method is of significance on search of the energetic materials and is an effective modification means for a high-energy explosive. The preparation method specifically comprises the following steps: adding the CL-20 and DNT in a molar ratio of 1: 2 at normal temperature into a proper amount of a crystallizing agent; carrying out ultrasonic oscillation and uniformly mixing to obtain a saturated crystallizing solution; and slowly evaporating a solvent at room temperature; and washing and drying to obtain the light yellow CL-20 and DNT eutectic explosive. According to the CL-20 / 2,5-DNT eutectic explosive prepared by the preparation method, the density and smelting point are remarkably improved compared with those of DNT. The eutectic explosive as a novel insensitive explosive has a relatively broad application prospect and is simple in process flow and mild in experimental condition. The product is good in safety and relatively high in quality.

The invention provides a fluorescent probe with the advantages of reduced background interference, high sample penetration performance, good selectivity, high sensitivity and good imaging resolution for fluorescence open-close type near infrared detection of cysteine as well as a preparation method and application of the fluorescent probe. The fluorescent probe is subjected to fluorescence quenching by taking near infrared fluorescent parent nucleus containing a plurality of double bonds as a fluorophore and taking 2,4-dinitrobenzene sulfonamide as a quenching unit; in actual detection, in thepresence of the cysteine, sulfydryl of the cysteine carries out nucleophilic substitution reaction on electron deficient aromatic ring, a sulfonamide bond cracks and a fluorescence quencher is dissociated, so that the fluorescent probe without fluorescence or with weak fluorescence based on intramolecular charge transfer (ICT) process releases the fluorescent parent nucleus, fluorescence is enhanced or opened to generate a fluorescent signal for selectively recognizing the cysteine, and further the aims of selective recognition and analysis and detection of the cysteine (Cys) are achieved.

The invention discloses a preparation method of m-phenylenediamine. M-dinitrobenzene is subjected to continuous catalytic hydrogenation, settlement and membrane filtration, and m-phenylenediamine is obtained. The method is simple to operate and high in safety, can be used for continuous production, can achieve the effects of high production efficiency, high product quality, low labor intensity, environmental friendliness and high utilization rate of a catalyst, and is beneficial to the effect of industrialization.

The invention discloses a naphthyl two-photon fluorescent probe as well as a preparation method and application thereof. The preparation method of the probe comprises the steps of firstly, heating 1-methyl-4-[2-(6-hydroxyl-2-naphthalene)-vinyl]-pyridium and sodium methylate for 4 hours, then heating the heated materials together with 2,4-dinitrobenzene chlorine sulfonate and triethylamine in acetonitrile for 2 hours, and carrying out silica gel column separation to obtain the pure product. The probe takes a naphthalene ring as a two-photon parent structure, has both a pyridium mitochondrion targeted group and a fluorophore, and uses 2,4-dinitrobenzene sulfonyl as a Cys selective recognition group. The hydroxyl is produced by using sulfydryl to break the 2,4-dinitrobenzene sulfonyl, and fluorescence spectrum redshift occurs, so that the ratio test (F583nm / F485nm) of Cys is realized; during the detection, a maximum value is rapidly obtained within 2min, and the detection line is as low as 29 nm. The probe can be used for selective detection of the Cys in cellular mitochondria.