26 results about "Trichlorobenzene" patented technology

The invention relates to a flame-retardant PVC material for a drag chain cable and a preparation method of the flame-retardant PVC material, and belongs to the technical field of cable materials. According to the invention, the flame-retardant compatibilizer is prepared, a trichlorophenyl structure in the flame-retardant compatibilizer has good compatibility with a PVC phase, and a siloxane structure in the flame-retardant compatibilizer can be crosslinked with siloxane in a modified TPU master batch in a heat treatment crosslinking process, so that the compatibility with a TPU phase is improved; the flame-retardant component is creatively used as a third component compatibilizer, so that the problem of non-uniform dispersion of the flame-retardant component in the PVC / TPU composite material is solved, the interface bonding force of a PVC phase and a TPU phase is effectively improved, the modification effect of TPU on PVC is improved, and the finally obtained flame-retardant PVC material has more excellent dynamic adaptability and environmental tolerance.

The invention relates to the field of material chemistry on-line detection, in particular to a 1, 2, 4-trichlorobenzene on-line detection material and a preparation method thereof, and provides a film-forming sensitive layer material capable of being coated on the surface of a transducer, and the film-forming sensitive layer material comprises chitosan, a crosslinking component with the content of 0.1-5wt% in terms of glutaraldehyde and magnetic core-shell molecularly imprinted particles after being dried, the magnetic core-shell molecularly imprinted particle contains a ferroferric oxide magnetic inner core, a silicon dioxide middle layer and a molecularly imprinted polymer shell layer, and the shell layer is a cyclodextrin methacrylate and ethylene glycol dimethacrylate copolymer network and takes 1, 2, 4-trichlorobenzene as a template. The material keeps the membrane integrity and long-term stability under the working conditions of circulation and regeneration and also gives consideration to quick response, and the residual 1, 2, 4-trichlorobenzene is controlled to be not greater than 0.10 wt% and the residual glutaraldehyde is controlled to be not greater than 0.5 wt%. The method is used for relieving structural mass transfer contradiction and processing and coating coupling contradiction caused by high filler load, and has online detection application value.

The invention belongs to the field of medical intermediate compounds and organic synthesis, and particularly relates to a key intermediate of lotinib and a preparation method thereof, the preparation method comprises the following steps: (1) in an organic solvent, organic alkali, 2-cyanoethyl 5-acetyl-3-methylthiophene-2-carboxylic ester and 2, 2, 2-trifluoro-1-(3, 4, 5-trichlorobenzene) ethanone react to obtain an intermediate 1; (2) dehydrating the intermediate 1 into double bonds to obtain an intermediate 2; and (3) reacting the intermediate 2 with a ligand to obtain the key intermediate of lotinib. The intermediate is used for synthesizing lotinib. The preparation method provided by the invention has the advantages of extremely high chiral selectivity, mild conditions and stable yield, can be suitable for amplified production, and provides a new technology suitable for industrial production for the key intermediate of lotinia.

This invention discloses a method for preparing and applying a gold cluster scintillator protected by a stable luminescent free radical ligand. The scintillator material uses (3,5-dichloro-4-pyridine)bis(2,4,6-trichlorobenzene)methyl free radical (PyBTM) as a ligand, and a chain-like tetranuclear free radical cluster is constructed using a one-pot method. The chemical formula of the compound is [Au4(PNP)2(PyBTM)2](SbF6)4, belonging to the triclinic crystal system, space group R-3. This free radical cluster scintillator achieves 100% theoretical exciton utilization and a short radiation decay lifetime due to its unique doublet emission mechanism. These properties make it an ideal candidate material for overcoming the contradiction between high luminous yield and fast response in traditional scintillators. Due to the excellent thermal and water-oxygen stability of this system, it can be fabricated into a scintillator screen to further achieve high-quality X-ray imaging with a spatial resolution of up to 31 LP·mm. ‑1 This provides a general design strategy for high-performance radiation detection materials.

This invention belongs to the field of catalyst technology, specifically relating to a supported iron-ruthenium catalyst and its application in the synthesis of m-dichlorobenzene and / or para-dichlorobenzene. The iron-ruthenium catalyst comprises a support and iron and ruthenium supported on the support. The support comprises quaternary ammonium salt-modified diatomaceous earth. Based on the total weight of the catalyst, the mass percentage of iron is 5-15%, and the mass percentage of ruthenium is 3-9%. The abundant active sites on the surface of the quaternary ammonium salt-modified diatomaceous earth support can significantly improve the catalytic activity and selectivity for m-dichlorobenzene and / or para-dichlorobenzene, without the formation of trichlorobenzene. The catalyst lifetime is 5-8 times longer than that of iron catalysts. The product can be separated and purified by stripping, distillation, and crystallization. The process is simple and can obtain high-purity m-dichlorobenzene and para-dichlorobenzene products.

The application provides a kind of double ligand HOF functionalized magnetic nanomaterial and its preparation method and application, belongs to functionalized magnetic material preparation technical field.The method first synthesizes Fe3O4NPs, NH3·H2O is added to solution to be alkaline, then the temperature is heated to react, obtains Fe3O4NPs suspension liquid;Fe3O4NPs suspension liquid is added to oleic acid stirring, and the obtained Fe3O4@OA;Guanidine hydrochloride monomer is dissolved in solvent, then Fe3O4@OA is dispersed in stirring, and Fe3O4@GD is obtained;Finally, Fe3O4@GD is mixed with GD, boric acid, triethylamine and 1,2,4-trichlorobenzene containing solution stirring, and double ligand HOF functionalized magnetic nanomaterial is obtained.The functional material of the application can also effectively capture glycoprotein, and identify glycoprotein and phosphoprotein.

The invention provides a method for preparing 1, 2, 3-trifluorobenzene, which comprises the following steps: by taking 1, 2, 3-trichloro-4, 6-dinitrobenzene as a starting material, carrying out fluorination reaction, hydrogenation reduction reaction, diazotization reaction and deamination reaction to obtain the 1, 2, 3-trifluorobenzene. The initial raw material can be prepared from 1, 2, 3-trichlorobenzene through a nitration reaction, and the preparation method has the advantages of high yield, few three wastes, high safety and the like, is a green method which is high in selectivity, high in economical efficiency and environmentally friendly, and is suitable for industrial production.

The invention discloses a preparation method of deuterated dichloroacetamide, and belongs to the field of organic synthesis. The problem that dehalogenation deuterization is difficult in the prior art is solved. The method comprises the following steps: uniformly mixing 2, 2, 2-trichloro-N-phenylacetamide, TDO, heavy water, potassium carbonate and an organic solvent, then heating and stirring for reaction, after reaction, carrying out reduced pressure distillation to remove the solvent, and then carrying out silica gel column chromatography separation and purification to obtain the deuterated dichloroacetamide. The method is used for preparing the deuterated dichloroacetamide.

The invention discloses 4, 7, 2 '-trichloro-7'-phenyl-6-carboxyl fluorescein as well as a preparation method and application thereof, and relates to the technical field of fluorescein synthesis. The preparation method comprises the following steps: reacting 6-carboxyl-tetrachloro-fluorescein, phenylboronic acid, a palladium catalyst and alkali in a mixed solvent in proportion at the temperature of 50-110 DEG C for 1.5-3 hours; 6-carboxyl-tetrachloro-fluorescein is used as a raw material, and separation and purification of ketone compound isomers are avoided; the synthesis route is short, operation is simple, and reaction conditions are mild; the use of dangerous chemical reagents is avoided; the reaction selectivity is good, byproducts are few, the product purity is high, and the total yield is high; the product can be amplified to a hectogram level, and batch production is easy to realize; unreacted raw materials in the reaction can be recycled, the purification frequency is low, and the process cost is remarkably reduced. And the prepared 4, 7, 2 '-trichloro-7'-phenyl-6-carboxyl fluorescein is expected to be popularized and applied in the fields of analysis and detection and biomedicine.

This invention belongs to the field of organic synthesis, specifically relating to a method for preparing 2,3,4-trifluoronitrobenzene. Specifically, it involves continuous nitration of 1,2,3-trichlorobenzene as a starting material and continuous production of 2,3,4-trifluoronitrobenzene via fluorination microchannels. This method has the advantages of simple process, low cost, high yield, high intrinsic safety, high production efficiency, and environmental friendliness. It does not require the addition of a phase transfer catalyst, does not use polar organic solvents in the reaction, and can be continuously produced, making it suitable for industrial scale-up.

The invention relates to the technical field of pesticide preparation, and particularly discloses a novel preparation method of a key intermediate 1-(2, 4, 6-trichlorophenyl)-propyl-2-ketone of a bactericide pydiflumetofen. The method comprises the following steps: by taking 3, 5-dichloro-4-fluoronitrobenzene as a starting raw material, sequentially carrying out four-step unit reactions: reacting with ethyl acetoacetate under an alkaline condition to prepare 2-(2, 6-dichloro-4-nitrophenyl)-3-oxobutyric acid ethyl ester, and reacting with ethyl acetoacetate under an alkaline condition to prepare 2-(2, 6-dichloro-4-nitrophenyl)-3-oxobutyric acid ethyl ester; carrying out degreasing under an acidic condition, so as to obtain 1-(2, 6-dichloro-4-nitrophenyl)-propyl-2-ketone; reducing the nitro group to obtain 1-(4-amino-2, 6-dichlorophenyl)-propyl-2-ketone; and performing Sandmeyer reaction to obtain a target product. The preparation method is novel in synthetic route, few in side reaction and high in total yield, the content of a target product is larger than 99%, the preparation method is suitable for industrial production, and a key support is provided for industrialization of pydiflumetofen.

The invention discloses a preparation method of 3, 4, 5-trichlorobenzonitrile, which comprises the following steps: mixing p-hydroxybenzonitrile, a Lewis acid catalyst, a phenyl phosphonic acid dialkyl ester cocatalyst and a chlorobenzene organic solvent, heating to 40-80 DEG C, introducing chlorine for chlorination reaction, heating to 120-180 DEG C, and continuing chlorination reaction to obtain the 3, 4, 5-trichlorobenzonitrile. According to the preparation method of the 3, 4, 5-trichlorobenzonitrile, the p-hydroxybenzonitrile is taken as a raw material, and the 3, 4, 5-trichlorobenzonitrile can be generated through high-selectivity and high-yield reaction by optimizing the reaction temperature under the combined action of the lewis acid catalyst and the dialkyl phenylphosphonate cocatalyst; the method has the advantages of simple process, convenience in operation, easily available raw materials, low cost, high safety, high yield, less pollution and the like, is convenient for large-scale preparation, is favorable for realizing industrial application, and can meet the requirements of different fields on 3, 4, 5-trichlorobenzonitrile.

The invention provides a method for synthesizing 2, 6-dichlorobenzoyl chloride and purifying by-products, and belongs to the technical field of synthesis of organic compounds. According to the method, 2, 6-dichlorotoluene and chlorine are subjected to a chlorination reaction, and after the reaction is finished, a chlorination reaction solution is obtained; and carrying out vacuum rectification on the chlorination reaction liquid to obtain a front fraction and a main fraction. And the front fraction is continuously subjected to reduced pressure rectification to obtain a by-product 1, 2, 3-trichlorobenzene. Carrying out hydrolysis reaction on the main fraction to obtain hydrolysis reaction liquid; and carrying out reduced pressure distillation on the hydrolysis reaction solution to obtain the 2, 6-dichlorobenzaldehyde. 2, 2, 6-dichlorobenzaldehyde and chlorine are subjected to a secondary chlorination reaction, and after the reaction is finished, a 2, 6-dichlorobenzoyl chloride crude product is obtained; and carrying out reduced pressure distillation on the crude product to obtain a 2, 6-dichlorobenzoyl chloride finished product. According to the method, the by-product 1, 2, 3-trichlorobenzene generated in the synthesis process of 2, 6-dichlorobenzoyl chloride is efficiently recycled, the resource utilization rate is increased, and the treatment burden of three wastes is relieved.

The invention belongs to the field of medical intermediate compounds and organic synthesis, and particularly relates to a key intermediate of lotinib and a preparation method of the key intermediate of lotinib, the preparation method comprises the following steps: (1) in an organic solvent, organic alkali, 5-acetyl-3-methyl-2-thiophene carboxylic acid and 2, 2, 2-trifluoro-1-(3, 4, 5-trichlorobenzene) ethanone react to obtain an intermediate 1; (2) dehydrating the intermediate 1 into double bonds to obtain an intermediate 2; and (3) reacting the intermediate 2 with a ligand to obtain the key intermediate of lotinib. According to the preparation method, the steps of a synthetic route can be shortened, the period is shortened, the yield is improved, the cost is reduced, the reaction conditions are milder, and a new technology suitable for industrial production is provided for the key intermediate of lotinia.

The present invention belongs to the technical field of organic synthesis, and particularly relates to a method for preparing 1-(2,4,6-trichloro-phenyl)-propyl-2-ketone-methoxy oxime ether. The method comprises the following steps: (1) chlorination reaction: adding a chlorinating agent into aniline as a raw material in a solvent at 0-10°C, and performing a chlorination reaction to obtain 2,4,6-trichloroaniline; (2) coupling reaction: subjecting 2,4,6-trichloroaniline, isopropenyl acetate and a catalyst to a coupling reaction in a solvent under the initiation of nitroxyl ions, so as to obtain 1-(2,4,6-trichloro-phenyl)-propyl-2-ketone; (3) oximation reaction: subjecting 1-(2,4,6-trichloro-phenyl)-propyl-2-ketone and hydroxylamine hydrochloride to an oximation reaction in a solvent under the action of an alkali, so as to obtain 1-(2,4,6-trichloro-phenyl)-propyl-2-ketone-oxime; and (4) methylation reaction: subjecting 1-(2,4,6-trichloro-phenyl)-propyl-2-ketone-oxime and chloromethane to a methylation reaction in a solvent under the action of an alkali, so as to obtain 1-(2,4,6-trichloro-phenyl)-propyl-2-ketone-methoxy oxime ether.

The invention discloses a preparation method of an electrically neutral in-situ antibacterial loose nanofiltration membrane, and belongs to the technical field of nanofiltration membranes. The method comprises the following steps: S1, taking a polymeric membrane matrix material, a membrane modifier and an organic solvent as raw materials, and preparing a base membrane through a phase inversion process; s2, taking the synthesized micromolecular organic matter containing the antibacterial imidazole structure as a water-phase monomer; and S3, selection of organic phase monomers: at least one of halogenated aromatic hydrocarbons such as tribromotrimethylbenzene, sym-tribromobenzene, sym-trichlorobenzene and the like. And S4, carrying out interfacial polymerization reaction on the water-phase monomer and the organic-phase monomer on the base membrane to prepare the electrically neutral in-situ antibacterial loose nanofiltration membrane. The membrane material prepared by the invention has high flux, excellent dye / salt separation performance and efficient antibacterial performance, and remarkable application potential.

A dioxin closed-loop control method based on real-time detection and dynamic optimization is proposed. By deploying an online monitoring system, a tunable laser ionization time-of-flight mass spectrometer is configured at the incineration flue gas discharge port to detect the concentration of dioxin indicator trichlorobenzene in real time. Combined with sensor detection of working condition parameters, the concentration of dioxin toxicity equivalent is converted in real time using polynomial regression to form an integrated system of online monitoring and toxicity assessment. A double-layer random forest-hybrid eagle optimization model is constructed. The first layer is based on historical working condition data to train a random forest model to predict the emission trend of dioxin and the potential risk of exceeding the standard. The second layer dynamically optimizes the incineration parameter combination by improving the eagle optimization algorithm and sends it to the incineration system in real time. At the same time, a calcium-based retarder directional spraying device is deployed in the flue gas purification section to achieve uniform coverage and precise dose control of the retarder and inhibit the low-temperature recombination reaction of dioxin. Finally, the parameters of the double-layer optimization model are dynamically updated based on the error between the actual detection value and the predicted value to improve the adaptability of the model to working condition fluctuations, thereby effectively reducing dioxin emissions and improving the environmental protection and stability of the incineration process.

The present invention relates to emulsion concentrate (EC) formulations of succinate dehydrogenase inhibitor fungicides, the preparation of such formulations and their use in diluted form for the control of fungal pathogens, particularly in crops of useful plants. More specifically, the present invention relates to an emulsion concentrate of -difluoromethyl-1-methyl-1H-pyrazole-4-carboxylic acid methoxy-[1-methyl-2-(2,4,6-trichlorophenyl)-ethyl]-amide, comprising a blend of at least three surfactants and an aromatic ester solvent.

The application discloses a preparation method of 1,2,3-trichloro-4,6-dinitrobenzene, which comprises the following steps: (1) sulfuric acid and 1,2,3-trichlorobenzene are sequentially added into a batching kettle, mixed uniformly and heated to 60-75 DEG C to obtain a mixture A; (2) nitric acid and sulfuric acid are sequentially added into another batching kettle and mixed uniformly to obtain a nitrosulfur mixed acid; (3) two feed modes are adopted, the mixture A obtained in the step (1) and the nitrosulfur mixed acid obtained in the step (2) are pumped into a two-stage tubular reactor with a diameter of 10 mm respectively to carry out nitration reaction; (4) after the nitration reaction is completed, the reaction liquid obtained in the two-stage tubular reactor is transported into a receiving tank, waste acid and an organic phase are separated, the residual waste acid in the organic phase is neutralized and washed to neutral to obtain 1,2,3-trichloro-4,6-dinitrobenzene. According to the application, the conversion rate of the 1,2,3-trichlorobenzene is greater than 99%, the yield of the obtained product 1,2,3-trichloro-4,6-dinitrobenzene is greater than 98%, and the purity is greater than 99.5%.

This invention belongs to the field of organic synthesis technology, specifically relating to a method for preparing the intermediate 1-(2,4,6-trichlorophenyl)-propyl-2-one of fluopyram. The method involves reacting 1,2,3,5-tetrachlorobenzene with acetylacetone-like raw materials, followed by acidification and decarboxylation to obtain 1-(2,4,6-trichlorophenyl)-propyl-2-one. This method employs a two-step one-pot process of aryl nucleophilic substitution and decarboxylation. The synthesis route is short, with high atom utilization, mild reaction conditions, simple process, low cost, high yield, minimal waste, no scale-up effect, high intrinsic safety, high production efficiency, and is environmentally friendly, making it suitable for large-scale industrial production.

This invention belongs to the field of organic synthesis technology, specifically relating to a method for preparing 1-(2,4,6-trichlorophenyl)-propyl-2-one. Starting from 1,3,5-trichlorobenzene, 1-(2,4,6-trichlorophenyl)-propyl-2-one is prepared through chloromethylation, carbonylation, and Dakin-West reaction. This method is simple to synthesize, easy to operate, has a high safety factor, low cost, and is suitable for industrial production.

The utility model discloses a device for preventing trichlorobenzene from being solidified in a benzoyl chloride device, which comprises a rectifying tower, the tower top of the rectifying tower is fixedly connected with a tower top condenser, the tower top condenser is fixedly connected with a hot water heat exchanger through a third connecting pipeline, and the hot water heat exchanger is fixedly connected with a circulating water return pipeline. A circulating water feeding pipeline is fixedly connected to the hot water heat exchanger, a second valve is arranged on the circulating water feeding pipeline, the hot water heat exchanger is fixedly connected with a hot water expansion tank through a fourth connecting pipeline, a thermometer is fixedly connected to the fourth connecting pipeline, a liquid level meter is fixedly connected into the hot water expansion tank, and an air pipeline is fixedly connected to the hot water expansion tank. A water supplementing pipeline is fixedly connected to the hot water expansion tank, a first valve is arranged on the water supplementing pipeline, the hot water expansion tank is fixedly connected with a hot water circulating pump through a first connecting pipeline, and the hot water circulating pump is fixedly connected with the tower top condenser through a second connecting pipeline. And the problem of production interruption caused by solidification of trichlorobenzene in the tower top condenser can be avoided.

The present invention relates to the fields of pharmaceutical intermediate compounds and organic synthesis, and specifically relates to a key intermediate of lotilaner and a preparation method therefor. The preparation method comprises: (1) reacting an organic base, 2-cyanoethyl 5-acetyl-3-methylthiophene-2-carboxylate, and 2,2,2-trifluoro-1-(3,4,5-trichlorophenyl)ethanone in an organic solvent to obtain an intermediate 1; (2) dehydrating the intermediate 1 to form a double bond to obtain an intermediate 2; and (3) reacting the intermediate 2 with a ligand to obtain a key intermediate of lotilaner. The intermediate is used for synthesizing lotilaner. The preparation method of the present invention has extremely high chiral selectivity, mild conditions, and stable yield, can be suitable for scale-up production, and provides a new technique suitable for industrial production for the key intermediate of lotilaner.

This invention relates to the field of online detection in materials chemistry, specifically an online detection material for 1,2,4-trichlorobenzene and its preparation method. It provides a film-forming sensitive layer material that can be coated onto the surface of a transducer. After drying, it comprises chitosan, a crosslinking component (calculated as 0.1–5 wt% of glutaraldehyde), and magnetic core-shell molecularly imprinted particles. The magnetic core-shell molecularly imprinted particles contain a magnetite magnetic core, a silica intermediate layer, and a molecularly imprinted polymer shell. The shell is a copolymer network of cyclodextrin methacrylate and ethylene glycol dimethacrylate, using 1,2,4-trichlorobenzene as a template. The material maintains membrane integrity and long-term stability while ensuring rapid response under circulation and regeneration conditions, and controls residual 1,2,4-trichlorobenzene to no more than 0.10 wt% and residual glutaraldehyde to no more than 0.5 wt%. This material alleviates structural mass transfer contradictions and the coupling contradiction between processing and coating caused by high filler loading, and has value for online detection applications.

This invention relates to the field of cable technology and proposes a heat-resistant overhead insulated cable and its manufacturing process. The heat-resistant overhead insulated cable includes a conductor, a shielding layer, and an insulation layer arranged sequentially from the inside out. The insulation layer comprises the following components by weight: 100 parts polyvinyl chloride, 5-8 parts chlorinated polyethylene, 30-40 parts plasticizer, 4-5 parts stabilizer, 10-15 parts filler, 1-3 parts antioxidant, 2-4 parts lubricant, and 8-10 parts phenylmaleimide compound. The phenylmaleimide compound is composed of 2,4,6-trichlorophenylmaleimide and N-phenylmaleimide in a mass ratio of 1:1.5-2. The heat-resistant overhead insulated cable provided by this invention solves the technical problems of insufficient heat resistance, easy softening and deformation at high temperatures, low mechanical property retention after long-term thermal aging, and easy brittle fracture in existing overhead insulated cables.