27 results about "Dichloroaniline" patented technology

The invention relates to the technical field of preparation of organic compounds, in particular to 2-chlorophenylhydrazine hydrochloride and a preparation process thereof. The 2-chlorophenylhydrazine hydrochloride is prepared from 500-600 parts of ethyl alcohol, 500-600 parts of stannous chloride solution, 300-350 parts of hydrochloric acid solution, 100-120 parts of 2, 4-dichloronitrobenzene and 10-12 parts of reduced iron powder. According to the preparation method, 2, 4-dichloroaniline hydrochloride is firstly prepared by adopting 2, 4-dichloronitrobenzene as an initial raw material, and due to the relatively stable structure, the chemical property of an intermediate product can be better kept unchanged in the storage, transportation and subsequent reaction waiting links in the whole preparation process; due to the stability, unnecessary chemical reaction or degradation caused by external environment factors can be effectively avoided, so that the subsequent 2-chloroaniline hydrochloride extraction step can be carried out on the basis of a stable starting material, and the stability basis of final product extraction is improved.

The invention relates to a mutant based on cytochrome P450BM3 and application of the mutant in chloroaniline biodegradation, and belongs to the field of enzymology. The mutant is obtained by mutating threonine at the 268 site of an amino acid sequence shown in SEQ ID NO.1 into aspartic acid or glutamic acid, mutating alanine at the 328 site into phenylalanine, and mutating alanine at the 328 site into phenylalanine. According to the present invention, the amino acid at the 87 site is mutated into alanine, and the valine at the 78 site is mutated into alanine, such that a variety of mutants such as T268D / A328F, T268E / A328F, T268D / A328F / F87A, T268E / A328F / F87A, T268D / A328F / F87A / V78A and T268E / A328F / F87A / V78A are obtained; according to the present invention, the degradation rate of the mutant on 4-chloroaniline, 2-chloroaniline, 2, 4-dichloroaniline, 3, 4-dichloroaniline and 3, 5-dichloroaniline is achieved; the method has important significance and application value for promoting rapid degradation of chloroaniline pollutants in a water environment and maintaining ecological balance.

The application relates to the preparation field of quinoline compounds and discloses a method for preparing a quinoline compound shown in formula (I), which comprises the following steps: in the presence of inert high-boiling-point polyether solvents, substituting a compound shown in formula (III) with 3,5-dichloroaniline to obtain a compound shown in formula (II), and then performing ring closure reaction to obtain the compound shown in formula (I), wherein X1, X3, X4, X5 and X6 are each independently -CN or -COOR'; R' is C1-C4 alkyl; wherein X1 is same as at least one of X3, X4, X5 and X6; X3 and X4 are same or different, X5 and X6 are same or different; X2 is a hydroxyl group or an amino group; R1 and R2 are each independently hydrogen or C1-C4 alkyl; and R1 and R2 are same or different. The method has the advantages of low reaction temperature, low cost and high yield, and is beneficial to industrialization.

The invention discloses a synthesis method of 2, 4-dichlorobenzaldehyde, and belongs to the technical field of unsaturated halogenated hydrocarbons, the method comprises the following steps: diazotization, formylation, quenching and purification; the diazotization method comprises the following steps: dissolving 2, 4-dichloroaniline in an HCl solution, placing the solution in an ice salt bath, cooling to 0 DEG C, dropwise adding a NaNO2 solution through a constant-pressure funnel, controlling the dripping speed to be 1-2 drops per second, controlling the system temperature to be 0-2 DEG C, adding urea after dropwise adding is finished, and carrying out heat preservation and stirring for 25-35 minutes to form a diazonium salt suspension; the method for preparing the 2, 4-dichlorobenzaldehyde has the advantages of high yield, high purity and few byproducts, the total yield can reach 82.7-84.9%, the purity is 98.72-99.03%, and the content of the byproduct 3, 5-dichlorobenzaldehyde in a crude product is 1t; and 2%.

The invention discloses a detection kit and a detection method for chlorate in dairy products and water, chlorate is converted into 2, 4-dichloroaniline, the chlorate detection kit is prepared by constructing a 2, 4-dichloroaniline antigen-antibody expression system and utilizing an immunodetection technology, and further, colloidal gold test paper is prepared. The detection time of the kit is only 5-10 minutes, the sensitivity can reach 50-100 mu g / kg (0.05-0.1 ppm), on this basis, a method for detecting chlorate in dairy products and water is further provided, the method is simple in operation step, high in detection speed, high in sensitivity and small in relative error, and compared with the national standard, the method has the advantages that a detection instrument is simple and easy to operate, the detection cost is low, and the like. The method is suitable for rapid detection of large-batch samples.

The invention discloses a method for preparing 3, 5-dichloroaniline through continuous catalytic reduction. The method comprises the following steps: dissolving 3, 5-dichloronitrobenzene serving as a raw material in a water-alcohol mixed solvent, adding sodium taurate or sodium glycinate serving as an organic salt stabilizer, adjusting the pH value to 3.5-4.5, and feeding into a partitioned temperature tubular reactor; under the hydrogen atmosphere, under the action of a Pd / C-FeO bi-component catalyst, selective reduction is performed at the front section of 70-90 DEG C, and conversion is completed at the rear section of 100-120 DEG C; and after the outlet of the reactor is cooled to 40-60 DEG C, sequentially injecting a weakly acidic neutralizing solution and a trapping agent at an interval of 0.1-0.5 second so as to passivate and complex the intermediate and reduce the generation of byproducts. The product is subjected to flash evaporation and membrane separation to obtain 3, 5-dichloroaniline with the purity being greater than or equal to 99%, and the solvent, the stabilizer and the hydrogen can be recycled. According to the method, the polar microenvironment is constructed through the stabilizer, the selectivity and the catalyst stability are remarkably improved through the synergistic effect of zoning temperature control and outlet two-stage delayed injection, and the method is suitable for continuous production.

The invention discloses a synthesis method of 1-methoxy-1-methyl-3-(3, 4-dichlorophenyl) urea, and relates to a synthesis method of 1-methoxy-1-methyl-3-(3, 4-dichlorophenyl) urea. The preparation method comprises the following steps: S1, reacting methoxyamine hydrochloride with phosgene in an organic solvent to prepare methoxy isocyanate M1; s2, the M1 and 3, 4-dichloroaniline are subjected to a reaction, and 1-methoxy-3-(3, 4-dichlorophenyl) urea M2 is synthesized; and S3, carrying out an Eschweiler-Clarke methylation reaction on the M2, formaldehyde and formic acid, so as to obtain the 1-methoxy-1-methyl-3-(3, 4-dichlorophenyl) urea (linuron). The invention provides a new path for industrial production of the linuron. Micromolecular aliphatic amine is used for replacing macromolecular aromatic amine to carry out photochemical reaction to prepare isocyanate, so that the production capacity is improved; an anhydrous homogeneous system is adopted for preparation of M2, hydrolysis of isocyanate is effectively avoided, homogeneous reaction is more sufficient, the yield is increased, and no salt-containing wastewater is generated; in the step S3, formaldehyde and formic acid are used for methylation, by-products are pollution-free carbon dioxide and water, the method is a low-toxicity pollution-free synthetic route, and a new route is provided for industrial production of the linuron.

The invention discloses establishment and application of gobiocypris rarus eye cells, and the gobiocypris rarus eye cells Gbr-eye are constructed by utilizing the eyes of the gobiocypris rarus, and are gobiocypris rarus eye cell lines capable of realizing continuous passage. The culture method of the gobiocypris rarus eye cell line comprises the steps of primary culture, subculture, cryopreservation and recovery. A chemical and environmental water acute toxicity assessment method is established based on the gobiocypris rarus eye cell line, and the method specifically comprises the steps of inoculation of gobiocypris rarus eye cells, exposure of 3, 4-dichloroaniline and environmental water and toxic effect detection of 3, 4-dichloroaniline on the gobiocypris rarus eye cells. According to the establishment method and application of the gobiocypris rarus eye cells, the application of the gobiocypris rarus in toxicity detection of chemicals and environmental water bodies is expanded, and reference is provided for acute toxicity test based on fish cells.

The invention discloses a method for synthesizing 2, 6-dichloroaniline through light induction, and relates to the technical field of organic synthesis.The method comprises the steps that aniline and acetic anhydride are mixed and stirred, and acetanilide is obtained; acetanilide is dropped into concentrated sulfuric acid to obtain a mixed solution, the mixed solution and concentrated sulfuric acid are subjected to a continuous flow reaction through a microchannel according to a preset molar ratio, and p-nitroacetanilide is obtained; the method comprises the following steps: mixing p-nitroacetanilide and a photocatalytic solution, placing the mixture in a photocatalytic reactor, and in an inert gas atmosphere, carrying out a catalytic chlorination reaction through irradiation of visible light with a preset wavelength to obtain 2, 6-dichloro-4-nitroacetanilide; the preparation method comprises the following steps: mixing 2, 6-dichloro-4-nitroacetanilide with a hydrochloric acid solution, and heating and refluxing to obtain 2, 6-dichloro-4-nitroaniline; the method comprises the following steps: by taking palladium on carbon as a catalyst, carrying out a denitrification reaction on 2, 6-dichloro-4-nitroaniline under the action of hydrogen to obtain 2, 6-dichloroaniline; the method can solve the technical problems of poor reaction selectivity, low yield and loss of traditional synthesis of 2, 6-dichloroaniline.

The application provides a preparation method of 3,5-dichloroaniline, and the preparation method comprises the following steps: reacting 1,3,5-trichlorobenzene with a coupling reagent ammonia source in the presence of a copper catalyst, a ligand and a base in an inert solvent to generate 3,5-dichloroaniline. The copper catalyst is adopted, and a suitable ligand and a base are selected, so that the preparation of 3,5-dichloroaniline with low cost, low reaction temperature and high yield is realized.

The application discloses a composite material for simultaneously improving soil acidification and pesticide residue, wherein nano calcium hydroxide is loaded on active carbon as a carrier, and the mass ratio of the active carbon to the nano calcium hydroxide is 1: (0.9-1.5). The composite material is prepared by adding active carbon and sodium hydroxide solution into a calcium chloride solution in sequence under a nitrogen atmosphere, washing and drying the precipitate after the reaction, and the application of the composite material in simultaneously changing the pH value of acidic soil and adsorbing diuron and 3,4-dichloroaniline in the acidic soil. The composite material of the application loads nano calcium hydroxide on active carbon, and by limiting the mass ratio of the active carbon to nano calcium carbonate, the pH value of acidic soil can be effectively improved, and diuron and 3,4-dichloroaniline in the soil can be simultaneously adsorbed, so that the application is simple, and the problems of soil acidification and pesticide residue, two soil pollution problems, are solved.

The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of N-pivaloyl 2, 4-dichloroaniline. The invention provides a preparation method of N-pivaloyl 2, 4-dichloroaniline, which comprises the following steps: mixing N-pivaloyl aniline and an organic solvent, introducing chlorine into the obtained system, and carrying out chlorination reaction to obtain the N-pivaloyl 2, 4-dichloroaniline. The N-pivaloyl aniline and the chlorine are used as raw materials, and the raw materials are low in price, so that the preparation method provided by the invention is low in cost and suitable for industrial production. In addition, the selectivity and the yield of the N-pivaloyl 2, 4-dichloroaniline in the preparation method provided by the invention are relatively high.

The invention discloses an alkali polishing additive for silicon wafers. The alkali polishing additive comprises organic amine, a complexing dispersant, inorganic salt and a surfactant. The organic amine is one or more of dichloroaniline, diethanol amine and dimethylamine, and the organic amine is 1-5 parts. The complexing dispersant is one or more of sodium benzoate, sodium alginate and sodium citrate, and the complexing dispersant is 3-8 parts. The inorganic salt is one or more of sodium sulfate, lauryl sodium sulfate, sodium pyrosulfate and sodium tartrate, and the inorganic salt is 1-5 parts. The surfactant is one or more of dodecyl dimethyl betaine, sodium alkyl naphthalene sulfonate and alkyl glycoside, and the amount of the surfactant is 5-8 parts; the additive also comprises deionized water; according to the silicon wafer alkali polishing additive, the organic amine is added, the back polishing effect of the same tower footing is obtained under the condition of low weight loss, the battery efficiency is improved, meanwhile, the additive synthesis device can stir and dissolve all the raw materials evenly, and the alkali polishing additive is obtained.

Disclosed is a perovskite precursor solution for improving stability of a perovskite solar cell. Iodoformamidine and cesium iodide are added into a solvent, and bromomethylamine, lead iodide and 3,4-dichloroaniline are added after stirring to obtain the perovskite precursor solution. The perovskite precursor solution is spin-coated on a substrate, obtaining a perovskite thin film by thermal annealing as a light absorption layer of the solar cell. The perovskite precursor solution prepared by the present invention replaces an existing perovskite layer, the defects in the existing perovskite mineralization technology are solved. The perovskite stability improvement leads lower requirements for the process environment and convenient preparation method, realizes the long-time stable performance in a common environment.

The application discloses a synthesis method of a compound 1-(2,3-dichlorophenyl)piperazine hydrochloride, which takes 2,3-dichloroaniline and bis(2-chloroethyl)amine hydrochloride as raw materials, and obtains 1-(2,3-dichlorophenyl)piperazine hydrochloride through a catalyst catalyzed condensation reaction. The synthesis method is simple, the product can be obtained at a high conversion rate, and the reaction safety is high; the raw material used in the application has a low environmental protection pressure, the reaction condition is mild, the requirement on equipment is low, and the application is suitable for industrial production requirements.

The invention discloses a green preparation method of 3, 5-dichloroaniline based on a pipeline reaction. The method comprises the following steps: dissolving 3, 5-dichloronitrobenzene in a water-alcohol mixed solvent, and adding a stabilizer; feeding the obtained solution into a continuous pipeline reactor, introducing hydrogen into a first-section catalytic zone, and selectively reducing nitro groups by using a Pd / C-Fe2O3 catalyst; ammonia gas is introduced into the second-section catalytic zone, and directional ammoniation is carried out by using a Ni-B catalyst; a neutralizing solution and a sodium lactate trapping agent can be injected between the two sections to stabilize the intermediate; and carrying out flash evaporation and membrane separation treatment on the reaction product, and recycling the solvent, the stabilizer and unreacted gas to obtain the 3, 5-dichloroaniline with the purity of more than or equal to 99%. According to the method, efficient coupling of nitro reduction and ammonification reaction is realized through division and cooperation of Pd / C-Fe2O3 and Ni-B dual catalysts and combination of partitioned temperature control and intermediate stabilization measures, the proportion of by-products is remarkably reduced, the yield and the purity are improved, and the service life of the catalysts is prolonged.

The invention discloses a weather-resistant finishing paint coating and a preparation method thereof, and belongs to the technical field of building coatings. The weather-resistant finish paint is prepared from the following raw materials in parts by weight: 40 to 60 parts of pure acrylic emulsion, 0.5 to 1 part of dispersing agent, 3 to 5 parts of coalescing agent, 1 to 2 parts of light stabilizer, 0.5 to 0.8 part of thickening agent, 3 to 5 parts of zinc oxide and 0.2 to 0.4 part of defoaming agent; the preparation method comprises the following steps: firstly, reacting 4-hydroxy-2, 2, 6, 6-tetramethyl-piperidine with sodium hypochlorite to generate an intermediate 1, then reacting with 1-nonanol to generate an intermediate 2, then reacting with 2, 5-dichloroaniline to generate an intermediate 3, and finally reacting with guaiacol-based lignin to obtain the light stabilizer. The weather-resistant finish paint prepared by the preparation method disclosed by the invention has excellent weather resistance.

The technical scheme discloses a device for continuously preparing 2,5-dichloroaniline, which comprises a first mixer, a first fixed bed reactor, a first separator, a second mixer, a second fixed bed reactor and a second separator; the first mixer comprises a cover plate, a gland, a mixing head and a mixing shell; the mixing shell is fixed on the first fixed bed reactor and communicates with the inner cavity of the first fixed bed reactor; the inner cavity of the mixing shell is sequentially provided with the gland and the mixing head from top to bottom; the cover plate is fixed above the gland and seals the joint of the cover plate and the mixing shell; the mixing head is internally provided with multiple transverse and longitudinal channels; the longitudinal channels are in communication with the feed inlet of the cover plate; and the transverse channels are in communication with the channels of the mixing shell. The technical scheme can solve the technical problem of how to ensure the safe access of hydrogen and the sealing safety while reducing the cost.

The invention relates to the technical field of yellow pigment processing, in particular to a sun-proof yellow pigment preparation process and a product thereof, and the process comprises the following steps: under the protection of nitrogen, preparing a diazonium solution from polyvinylpyrrolidone, hydrochloric acid, dichloroaniline and sodium nitrite; preparing a coupling solution from sodium hydroxide, phenyl methyl pyrazolone and hexadecyl trimethyl ammonium bromide; mixing the modified titanium dioxide with sodium dodecyl benzene sulfonate, rosin soap and ethylene diamine tetraacetic acid, carrying out four-stage pH regulation and gradient heating, finally adding the modified titanium dioxide, and carrying out heat preservation, filter pressing and drying. On the premise of not changing the traditional azo core reaction, the sun-proof grade of the pigment is improved to 7-8 grade from 4-5 grade through assistant synergy and crystal form regulation and control, and the pigment has high tinting strength, excellent dispersity and batch stability, is suitable for building exterior wall coatings, automobile plastic ornaments and high-end light-color ink, and thoroughly solves the problem of outdoor yellow color fading.

The invention relates to the technical field of catalysts, and discloses a catalyst and an application thereof in preparation of 3, 4-dichloroaniline. Platinum (Pt) and zinc (Zn) nano layers are deposited on the surface of a carrier, a bimetallic structure in which Pt and Zn are in contact is achieved through respective deposition of a Pt precursor and a Zn precursor, an amine ligand auxiliary is added into a reduced raw material solution, and the 3, 4-dichloroaniline is prepared through a hydrothermal method. The preparation method has the advantages that the probability that halogen is in contact with acid sites is reduced, the activity and selectivity of the catalyst are improved, the stability of the catalyst is improved by fixing the active sites through a CVD (chemical vapor deposition) technology and using a proper amount of carbon, and the problem that active metal particles are expanded in the secondary activated sintering process of the catalyst can be obviously resisted without reducing the activity of the catalyst; the metal nanoparticles are effectively prevented from being gathered or sintered at a high temperature, and the wrapping layer can provide a physical barrier, reduce migration of the metal nanoparticles and maintain small particle size of the metal nanoparticles, so that high catalytic activity is maintained, the service life of the catalyst is prolonged, and poison of halogen elements to the catalyst is reduced.

The invention discloses a preparation method of pigment red 2, and belongs to the technical field of pigments. The method comprises the following steps: adding 2, 5-dichloroaniline into hydrochloric acid, and dropwise adding a sodium nitrite solution into a 2, 5-dichloroaniline hydrochloride suspension to obtain a solution A; adding water into a grinding machine, then adding 3-hydroxy-N-phenyl-2-naphthylamide and a surfactant, and grinding to obtain a solution B; adding water and a phase transfer catalyst into a grinding machine, dropwise adding the solution A and the solution B at the same time, and reacting while grinding; after the reaction is finished, heating and preserving heat for a certain time, and finally filtering, washing and drying a product to obtain a pigment red 2 finished product. The method is simple and mild in preparation process, low in wastewater discharge amount, environment-friendly and suitable for large-scale production.

The present invention relates to the technical field of preparation of organic compounds, and in particular to 2-chlorophenylhydrazine hydrochloride and a preparation process thereof: 500-600 parts of ethanol, 500-600 parts of stannous chloride solution, 300-350 parts of hydrochloric acid solution, 100-120 parts of 2,4-dichloronitrobenzene, and 10-12 parts of reduced iron powder. In the present invention, 2,4-dichloronitrobenzene is used as an initial raw material to first prepare 2,4-dichloroaniline hydrochloride. Due to its relatively more stable structure, the intermediate product can better maintain its chemical properties unchanged during storage, transportation, and subsequent reaction waiting steps throughout the entire preparation process. This stability can effectively prevent the intermediate product from undergoing unnecessary chemical reactions or degradation due to external environmental factors, thereby ensuring that the subsequent step of extracting 2-chloroaniline hydrochloride can be performed based on the stable starting material, thereby improving the stability basis for extraction of the final product.

Treatment compositions and methods for treating and / or preventing human hair thinning or hair loss comprising applying a chlorin treatment composition to an area of skin / scalp in need of treatment. A treatment composition preferably comprises a copper chlorin, such as a sodium copper chlorophyllin complex, trisodium copper chlorin p6, disodium copper isochlorin e4, or trisodium copper chlorin e6. A treatment composition comprises around 0.02 to 0.1% by weight of a chlorin, preferably a copper chlorin. A density and / or diameter of hair in an area being treated may be increased by at least 5%, more preferably at least 15%. Immune privilege in an area being treated may also be restored as measured by change in certain immunoglobulin antibodies.

This invention discloses a self-adhesive coating for amorphous silicon steel sheets and its preparation method, belonging to the field of coating preparation technology. First, an epoxy resin is generated by polymerizing epichlorohydrin with 4-aminoquinoline, improving thermal stability and effectively reducing mechanical losses after coating. Then, it is reacted with phloroglucinol to obtain a modified epoxy resin, which exhibits tight inward molecular aggregation, increasing crosslinking density. Next, the ring-opening reaction of ethylene glycol diglycidyl ether with 3,5-dichloroaniline enhances crosslinking properties, followed by a reaction with lacquer resin to improve coating stability. The resulting self-adhesive coating can bond tightly to the iron core, reducing NVH levels, decreasing eddy current losses and iron losses, improving the energy conversion efficiency of the motor, and enhancing hydrophobicity.

The invention belongs to the technical field of chemical synthesis, and particularly relates to a method for safely producing 3, 5-dichloro-1-bromobenzene. The method comprises the following steps: by taking 3, 5-dichloroaniline as an initial raw material, firstly adding an organic solvent and 48% hydrobromic acid for salifying, after salifying is completed, carrying out reflux water separation, after moisture is detected to be qualified, dropwise adding nitrite at a controlled temperature, after dropwise adding is completed, carrying out heat preservation reaction, after the reaction is completed, carrying out acid pickling, alkali washing, water washing and concentration drying on an organic phase, adding ethanol, and recrystallizing to obtain the 3, 5-dichloro-1-bromobenzene. According to the method for safely producing the 3, 5-dichloro-1-bromobenzene, the problems that reaction heat release is violent and difficult to control, reaction selectivity is poor, impurities are large, treatment and purification after reaction are complex, the yield is low, the cost is high, the amount of waste liquid is large and difficult to treat and the like are solved at the same time, and in industrial large-scale production, the method is more obvious in safety, economical efficiency, greenness and environment friendliness.

The invention discloses a synthesis method of 2, 2, 2-trifluoro-1-(3, 4, 5-trichlorobenzene) ethanone, and belongs to the field of medical intermediates. The method comprises the following steps that 2, 6-dichloroaniline serves as a raw material, 3, 4, 5-trichlorobromobenzene is obtained through continuous bromination / oxidation and diazotization / chlorination, 2, 2, 2-trifluoro-1-(3, 4, 5-trichlorobenzene) ethanone is obtained through Grignard / acylation reaction, and the total yield is 65% or above. The process has the advantages of easily available raw materials, short period, mild conditions, high yield, less three wastes and low requirements on equipment, and is suitable for industrial production.

The invention relates to an oil exploitation auxiliary agent, in particular to a novel Gemini anionic surfactant as well as a preparation method and application thereof, fatty alcohol-polyoxyethylene ether, 3, 5-dichloroaniline, 1, 3-propane diamine and sodium 2-chloroethane-1-sulfonate are used as raw materials, and the Gemini anionic surfactant containing multiple hydrophilic chain segments and hydrophobic chain segments is synthesized by rigid benzene rings. The anionic surfactant is easy to dissolve in water, has higher surface activity, is small in dosage, and saves the cost in actual use. The oil-based mud flushing agent is formed by the oil-based mud flushing agent, the nonionic surfactant, the cosolvent, the chelating agent and the penetrating agent, all the components cooperate with one another to form the flushing agent with excellent flushing efficiency at high temperature and high salt, and the oil-based mud flushing agent is good in compatibility with cement paste and oil-based mud.