538 results about "Dichlorobenzene" patented technology

Herein is provided a novel process for the preparation of methyl 6-(2,4-dichlorophenyl)-5-[4-[(3S)-1-(3-fluoropropyl)pyrrolidin-3-yl]oxyphenyl]-8,9-dihydro-7H-benzo[7]annulene-2-carboxylate by a Suzuki coupling of compound (3), wherein LG represents a leaving group, with an organoboron reagent:Compound (3) is obtained by activation of compound (4) with a leaving group LG, and compound (4) is obtained by alpha-arylation of methyl 5-oxo-6,7,8,9-tetrahydro-5H-benzo[7]annulene-2-carboxylate with 1-LG′-2,4-dichlorobenzene, wherein LG′ represents a leaving group:

The invention relates to a crown ether covalent organic framework material as well as a preparation method and application thereof. The preparation method comprises the following steps: dissolving a crown ether monomer and an amino monomer in an o-dichlorobenzene solvent, adding a catalyst acetic acid aqueous solution, and uniformly dispersing to form a reaction solution; the method comprises the following steps: freezing a reaction solution through a liquid nitrogen bath, vacuumizing, filling nitrogen, carrying out a heating reaction, and carrying out post-treatment operations such as washing and drying on a reaction product, so as to obtain the crown ether covalent organic framework material BADT-DB18C6-COF. The crown ether covalent organic framework material is formed by condensation of a crown ether aldehyde monomer and an amino monomer, the crown ether monomer is 4, 4 ', 4' ', 4 '''-(6, 7, 9, 10, 17, 18, 20, 21-octahydrodibenzo [B, K] [1, 4, 7, 10, 13, 16] hexaoxacyclo octadecene-2, 3, 13, 14-tetrayl) tetrabenzaldehyde, and the crown ether monomer is 4, 4 ', 4' ', 4'''-(6, 7, 9, 10, 17, 18, 20, 21-octahydrodibenzo [B, K] [1, 4, 7, 10, 13, 16] hexaoxacyclo octadecene-2, 3, 13, 14-tetrayl) tetrabenzaldehyde. The amino monomer is 4 ', 5'-bis (4-aminophenyl)-[1, 1 ': 2', 1 ''-terphenyl]-4, 4''-diamine. The crown ether covalent organic framework material BADT-DB18C6-COF prepared by the invention is mainly used as an adsorbent, is used for adsorbing and recovering uranium, thorium and americium ions from a solution, shows good adsorption capacity on radionuclides U-238, Th-232 and Am-243, and is particularly suitable for the field of spent fuel post-treatment in the nuclear industry.

The invention discloses a method for preparing a waste gas purification catalyst from red mud and electrolytic manganese residues, a product and application thereof, and belongs to the field of solid waste resource utilization. According to the method, the preparation process is simple, efficient resource utilization of the red mud and the electrolytic manganese residues can be achieved through reasonable burdening, hydrothermal reaction and pyrolysis carbonization processes, and no other waste liquid or secondary solid waste is generated in the preparation process. The prepared waste gas purification catalyst is excellent in catalytic performance and can be used for quickly converting harmful gas of 1, 2-dichlorobenzene.

The invention discloses a corrosion-resistant polypropylene edge band material and a preparation method thereof, and belongs to the technical field of preparation of edge band materials. The corrosion-resistant polypropylene edge sealing strip material is prepared from, by weight, 50-75 parts of polypropylene, 2-5 parts of an antioxidant, 3-6 parts of a corrosion-resistant agent, 2-4 parts of a composite flame retardant, 8-15 parts of calcium carbonate and 2-4 parts of dye, the corrosion-resistant agent is prepared from 2, 6-dichlorobenzonitrile, 1, 2, 4-triazole, a sulfuric acid solution, sodium nitrite and parachloroaniline, and the corrosion-resistant agent is prepared from 2, 6-dichlorobenzonitrile, 1, 2, 4-triazole, a sulfuric acid solution, sodium nitrite and parachloroaniline. The composite flame retardant is prepared from 3-glycidyl ether oxypropyl trimethoxy silane, diphenyl silanediol, barium hydroxide and boric acid. The edge band material prepared by the method has excellent corrosion resistance, flame retardance, heat resistance and mechanical properties.

The invention relates to the technical field of chemical automation control, and discloses an intelligent closed-loop control system for producing p-dichlorobenzene by a biomass method, which comprises a signal acquisition module, a residence time reconstruction module, a thermal coupling analysis module, a parameter self-adaptive scheduling module and an execution control module. The rheological characteristics of raw materials are monitored by collecting the current of a stirring motor, the liquid level is dynamically increased through a retention time reconstruction module to prolong the retention time of the materials, and a liquid level periodic migration strategy is introduced to prevent scaling of a gas-liquid interface; the thermal coupling analysis module and the parameter self-adaptive scheduling module are used for calculating thermal retardation post factors, temperature control parameters are corrected in real time, the upper limit of cooling output is limited, inner wall supercooling crystallization is prevented, and the problems that the conversion rate is reduced, the heat transfer efficiency is reduced and equipment is hung on the wall due to viscosity fluctuation of biomass raw materials are effectively solved. And the self-adaptive stable control of the reaction process is realized.

The invention discloses a reaction device based on dichlorobenzonitrile synthesis and a use method thereof, and relates to the field of reaction devices.According to the technical scheme, the reaction device comprises a reaction tank and a cover located at the top end of the reaction tank, a heating interlayer is arranged on the reaction tank, and a spiral conveying pipe surrounding a reaction cavity in the middle of the reaction tank is arranged in the heating interlayer; the heating medium is conveyed through the spiral conveying pipe, and the gap between the heating interlayer and the spiral conveying pipe is filled with the heat preservation material, so that the heating medium is conveyed around the reaction cavity in the heating interlayer through the spiral conveying pipe, and the spirally distributed conveying pipe can enable the heating medium to uniformly act on the outer wall of the reaction cavity; heat loss is reduced through the heat preservation material between the heating interlayer and the spiral conveying pipe, accurate control and uniform distribution of the reaction temperature are achieved, side reactions caused by local overheating are avoided, and therefore generation of polychlorinated impurities is reduced, and the purity of the dichlorobenzonitrile product is improved.

The invention discloses a cross-linking agent for rubber and a preparation method thereof. The preparation method comprises the following steps: S11, dissolving 2, 4-dichlorobenzoic acid in tert-butyl alcohol, and dropwise adding concentrated sulfuric acid to obtain a mixed solution; s12, slowly dropwise adding a hydrogen peroxide solution into the mixed solution, and oxidizing to obtain a primary oxidized solution; s13, carrying out secondary oxidation on the primary oxidation solution obtained in the step S12 to obtain a secondary oxidation solution; and S14, purifying the secondary oxidation liquid obtained in the step S13 to obtain the cross-linking agent for rubber. The application of the cross-linking agent for the rubber in the rubber comprises the following steps: S21, banburying raw materials and the cross-linking agent for the rubber to prepare a rubber material; and S22, feeding the rubber material in the step S21 into a vulcanizing machine, and vulcanizing to obtain the rubber. The prepared cross-linking agent for the rubber is good in performance, the preparation method is simple, emission of three wastes is small, the atom utilization rate is high, and after the cross-linking agent is applied to the rubber, the prepared rubber is good in tensile strength, elongation at break and wear resistance index.

The invention relates to the technical field of materials and advanced oxidation, and discloses a covalent organic framework catalyst with a benzothiadiazole structure, a preparation method of the covalent organic framework catalyst and application of the covalent organic framework catalyst in peroxymonosulfate (PMS) activation and organic pollutant degradation. The preparation method of the covalent organic framework catalyst comprises the following steps: adding precursors 1, 3, 6, 8-tetra-(p-aminophenyl)-pyrene and 2, 7-dibenzaldehyde-benzothiadiazole into a mixed solvent composed of o-dichlorobenzene and n-butyl alcohol, carrying out a reaction by using acetic acid as a catalyst through a solvothermal method, and after the reaction, carrying out multiple times of centrifugal washing and drying to obtain the covalent organic framework catalyst. The catalyst shows excellent performance in the aspect of activating PMS to degrade organic pollutants, the degradation rate constant of bisphenol A reaches 1.68 min <-1 >, and 100% removal can be achieved within 5 minutes. Meanwhile, the catalyst has the advantages of no secondary pollution, strong anti-interference performance, reusability and the like. Compared with a traditional method, the catalyst has high PMS activation efficiency, the catalysis process is energy-saving and environment-friendly, the operation is simple and convenient, the preparation process is simple and feasible, and a new solution is provided for efficient degradation of organic pollutants in water.

The invention belongs to the field of chemical production, and particularly relates to a method for catalytically synthesizing propiconazole by using ionic liquid. And carrying out condensation reaction on the brominated substance 2-bromomethyl-2-(2, 4-dichlorophenyl)-4-propyl-1, 3-dioxopentane and triazole under the catalysis of the ionic liquid to generate propiconazole. The ionic liquid is one of [Emim] BF4, [Emim] PF6, [BMIM] PF6 and [BMIM] OH. According to the invention, the imidazole cation ionic liquid is used as a catalyst and a solvent to catalyze the N-alkylation reaction of 2-bromomethyl-2-(2, 4-dichlorophenyl)-4-propyl-1, 3-dioxopentane and triazole, and the research finds that the alkaline imidazole cation liquid has good catalytic performance, high yield and good selectivity, and can be used as a catalyst for catalyzing the N-alkylation reaction of 2-bromomethyl-2-(2, 4-dichlorophenyl)-4-propyl-1, 3-dioxopentane and triazole. And the reaction conditions are mild, the operation is simple, the ionic liquid is easy to recover, and the catalytic activity is not obviously reduced after being applied for five times.

According to the method, a polysaccharide derivative bonding type chiral chromatographic column with silica gel surface bonded amylose-tri (3, 5-dichlorophenyl carbamate) as a filler is adopted, a mixed solution of n-hexane and isopropanol is used as a mobile phase, the column temperature is 28-32 DEG C, the flow velocity is 1.1-1.3 ml / min, the column temperature is 20-30 DEG C, the column temperature is 20-30 DEG C, the column temperature is 20-30 DEG C, the column temperature is 20-30 DEG C, the column temperature is 20-30 DEG C, and the column temperature is 20-30 DEG C; an ultraviolet detector is adopted, the wavelength is 205-220 nm, and effective separation of the etomidate intermediate and the enantiomer thereof is achieved. The method is good in detection result accuracy and high in sensitivity, and compared with an existing analysis method, the method is better in separation effect, simpler in mobile phase composition, more durable in chromatographic column and lower in cost, so that a good guarantee is provided for quality control of the etomidate intermediate and etomidate.

The invention relates to the field of cosmetics, in particular to a nicotiana benthamiana callus extract, a preparation method thereof and cosmetics. The method comprises the following steps: inoculating an induction medium with young leaves of nicotiana benthamiana as explants, and inducing the explants to form calluses; the induction culture medium is prepared from 1.0 to 3.0 mg / L of 6-benayl aminopurine; 0.2 to 1.0 mg / L of naphthylacetic acid; inoculating the callus on a subculture medium for multiplication culture; the subculture medium is prepared from the following components: 0.5 to 2.0 mg / L of 6-benayl aminopurine, 0.0 to 1.0 mg / L of naphthylacetic acid and 0.0 to 2.0 mg / L of 2, 4-dichlorphenoxyacetic acid; and extracting the calluses of the nicotiana benthamiana after multiplication culture by using water as a solvent according to a material-liquid ratio of 1: (5-20). According to the method, the Bensi tobacco callus with high dedifferentiation degree, good loosening degree and high growth speed is obtained, and the callus extract with the DPPH removal rate reaching 85% or above is obtained through extraction.

The invention discloses a phenolphthalein-based polyaryletherketone polymer and a preparation method thereof, and the phenolphthalein-based polyaryletherketone polymer is prepared from the following raw materials: 240 to 370 parts of phenolphthalein monomer, 45 to 150 parts of modified phenolphthalein, 140 to 220 parts of 2, 6-dichlorobenzonitrile and 3 to 12 parts of alkyl halide. The modified phenolphthalein is prepared from phenolphthalein and a modifier; the modifying agent is selected from at least one of 3-amino propyl trimethoxy silane, 3-amino propyl triethoxy silane, bis (aminopropyl) polydimethylsiloxane, and aminopropyl terminated polydimethylsiloxane. By introducing a siloxane side chain and a cyano side bond and using long-chain aliphatic hydrocarbon for end capping, the bonding capacity of the polymer and other materials is improved, and meanwhile, the high temperature resistance and toughness of the polymer are kept.

The invention provides phenyl-containing polysiloxane silicone oil for personal care and a preparation method of the phenyl-containing polysiloxane silicone oil. The mass of dichlorobenzene in the phenyl-containing polysiloxane silicone oil is 1-20 ppm, the dichlorobenzene has two structures, and the proportion of p-dichlorobenzene in the total content of dichlorobenzene is less than 75 wt%. The phenyl-containing polysiloxane silicone oil has the advantages of being colorless, odorless and low in residue, can be used as an additive of personal care products such as skin care products and hair conditioners, is extremely low in color number, completely odorless and good in compatibility with most personal care product raw materials, and solves the use problem of low-odor and low-color-number additives in the daily chemical industry.

The invention relates to a synthesis process of p-chlorophenylboronic acid, which comprises the following steps: by taking tetrahydrofuran as a solvent and p-dichlorobenzene as an initial raw material, firstly preparing p-chlorophenylmagnesium chloride through Grignard reaction, then reacting the p-chlorophenylmagnesium chloride with boric acid ester in a microchannel reactor to obtain a p-chlorophenylboronic acid ester crude product, and then hydrolyzing, layering and carrying out oil-phase azeotropic distillation to obtain the p-chlorophenylboronic acid ester. And finally, recrystallizing by adopting a mixed system of an alcohol solvent and a benzene solvent to obtain p-chlorophenylboronic acid with the content of 98% or above. The synthetic process of the p-chlorophenylboronic acid is mild in reaction condition, simple and convenient to operate, low in cost, high in safety, high in product content and very suitable for being applied to industrial large-scale production.

The invention discloses colloid, porous carbon and a preparation method and application thereof. The preparation method of the colloid comprises the following steps: S1, extracting aromatic hydrocarbon-rich oil by adopting a first solvent to obtain a soluble component which is a component A; wherein the first solvent is selected from one or more of o-dichlorobenzene, dipropyl ether and 3-pentanone; s2, the component A is adsorbed to an aluminum oxide chromatographic column, petroleum ether or n-heptane, methylbenzene and a second solvent are sequentially adopted to wash the chromatographic column, then desorbed matter is obtained, and the second solvent is a mixture of methylbenzene and ethyl alcohol. The colloidal pyrrole is high in nitrogen content, and the porous carbon prepared from the colloidal pyrrole is excellent in conductivity.

The invention relates to the technical field of high polymer materials, and discloses a synthesis method of low-chlorine polyphenylene sulfide nitrile, which comprises the following steps: carrying out pressurized prepolymerization reaction on a sodium sulfide solution and p-dichlorobenzene to obtain a first prepolymerization reaction product; carrying out copolymerization prepolymerization reaction on the first prepolymerization reaction product and 2, 6-dichlorobenzonitrile to obtain a second prepolymerization reaction product; carrying out heating polymerization reaction on the second prepolymerization reaction product and benzyl chloride to obtain a heating polymerization reaction product; and raising the temperature of the polymerization reaction product, and carrying out phase separation to obtain the low-chlorine polyphenylene sulfide nitrile. Under the condition of no auxiliary agent, the polymerization process of inert gas pressurization and phase separation is adopted, benzyl chloride is applied to adjust the end group, low-chlorine high-molecular-weight polyphenylene sulfide nitrile can be obtained in a short time, the production efficiency of synthesizing polyphenylene sulfide nitrile can be improved, the purification process of byproduct sodium chloride is shortened, auxiliary agent recovery is omitted, and the production cost is reduced. The engineering construction investment is reduced, and the production cost for manufacturing the polyphenylene sulfide nitrile is greatly reduced.

The invention discloses an imidazole derivative molecule modified solar cell and a preparation method thereof, and belongs to the technical field of solar cells. The cell sequentially comprises an ITO (Indium Tin Oxide) conductive glass layer, a nickel oxide passivation layer, a [4-(3, 6-dimethoxy-9H-carbazole-9-yl) butyl] phosphonic acid hole transport layer, an ITO (Indium Tin Oxide) conductive glass layer and a nickel oxide passivation layer from bottom to top, the thin film solar cell is characterized in that the thin film solar cell comprises a substrate, a metal Ag electrode layer, a Cs0.05 (FA0. 95MA0. 05) 0. 95Pb (I0. 95Br0. 05) 3 narrow-band gap perovskite thin film PVSK modified by 2-(2 ', 6'-dichloroanilino)-2-imidazoline, a (6, 6)-phenyl-C61-butyric acid methyl ester electron transport layer, a 2, 9-dimethyl-4, 7-biphenyl-1, 10-phenanthroline hole blocking layer and a metal Ag electrode layer; according to the scheme, perovskite defects are passivated through imidazole derivative molecules, double-interface passivation and crystallization regulation are achieved, the film quality is improved, and the crystal quality of the perovskite film is remarkably improved; due to effective passivation of the double interfaces, ion migration is obviously inhibited, the carrier transmission efficiency is effectively improved, and the moisture resistance of the perovskite thin film and the device stability are improved.

The invention discloses a COF aerogel composite material for PFAS treatment and a preparation method and application thereof, and relates to the field of pollutant adsorption, the COF aerogel composite material comprises the following components: 68.18%-70% of a COF material, 22.73%-90.91% of a CS solution, and 9.09% of a TP solution; the COF material is prepared from 0.0764 mmol of ETTA (Ethylene Terephthalic Acid), 30 mg of ETTA, 0.1528 mmol of a side functional monomer and 3 mL of an o-dichlorobenzene / n-butyl alcohol solvent. The volume ratio of orthodichlorobenzene to n-butanol in the orthodichlorobenzene / n-butanol solvent is 1: 1; and the side functional monomer comprises 0.025 mmol of TFTDA (Trifluorotoluene Diisocynate) / 0.127 mmol of BFB1M, and is named as COF-F1N5. A series of COF / aerogel synthesized by the method provided by the invention has the characteristics of ultralight weight, compression resistance, good stability and small specific surface area loss, overcomes the application limitation of COF powder, is easy to recover, and has better adsorption performance on PFAS.

The invention discloses a high-temperature durable epoxy resin coating and a preparation method thereof, and relates to the technical field of epoxy resin coatings. The novel epoxy resin is prepared from 1, 3, 5-tris (2-propynyloxy) benzene, 3-azido butanol and glycidyl methacrylate as raw materials, the novel epoxy resin has multiple functional groups, the crosslinking degree of the coating can be improved, the epoxy resin coating can have high thermal stability due to introduction of a benzene ring and a triazole structure, and the epoxy resin coating can be applied to the field of coating materials. The heat resistance of the coating is improved; secondly, grafting 2-benzoyl-4, 5-dichlorobenzoic acid onto calcium silicate, and then hydrolyzing to prepare a novel hindered phenol antioxidant; calcium silicate is used for loading the antioxidant, a stable loading platform can be provided for the antioxidant, and active groups on the surface and the antioxidant generate a synergistic effect, so that the oxidation resistance is further improved, the anti-aging performance of the coating is improved, and the service life of the coating is prolonged. The high-temperature durable epoxy resin coating prepared by the invention has the effects of high temperature resistance and durability.

The invention belongs to the technical field of pesticides, and discloses a heterocarboxylic acid dimer as well as a preparation method and application thereof. Herbicides such as 2, 4-dichlorphenoxyacetic acid, 2-methyl-4-chlorophenoxyacetic acid and fluroxypyr acting on a TIR1 target point and herbicides such as dicamba and halauralid acting on an AFB5 target point are connected through a connecting arm containing groups such as O, S and N, so that the heterologous carboxylic acid dimer is constructed. The herbicidal activity and crop safety determination results show that compared with the single use or mixed use of the parent compound, the synthesized heterocarboxylic acid dimer has higher herbicidal activity and better crop safety. In addition, the preparation method of the heterologous carboxylic acid dimer is safe, simple and feasible.

The invention discloses a tail gas treatment device for chemical dichlorobenzonitrile production, which relates to the technical field of chemical dichlorobenzonitrile production and comprises a spray tower, a spray mechanism and an airflow retarding mechanism. Acidic tail gas enters the spray tower from the gas inlet, and is sprayed by an alkaline solution of the spray mechanism to remove pollutants; the airflow retarding mechanism intermittently controls the tail gas flowing speed through the staggered design of air holes of a fixed plate disc and a rotating plate disc, and the contact time of tail gas and spraying liquid is prolonged; the rotational flow plate further enhances the rotational flow effect of the tail gas and improves the spraying treatment efficiency; the intermittent transmission assembly and the angle adjusting assembly can adjust the flow of the tail gas and the inclination angle of the rotational flow plate according to the communication state of the air holes, and it is ensured that harmful substances in the tail gas are fully absorbed. The device has the characteristics of efficient purification, energy conservation, automatic adjustment and the like, and is suitable for tail gas treatment in chemical production.

This invention belongs to the field of lithium-ion battery technology, specifically relating to a method for constructing Si@COF-Co materials using porphyrin COF as a conductive nano-protective layer for nano-silicon and its application. The invention first adds a methanol solution of PEI to a methanol solution of nano-silicon, then dries it at high temperature to obtain PEI-modified nano-silicon Si-PEI. Next, Si-PEI and PVP are dispersed in o-dichlorobenzene / n-butanol, and then COF monomer and glacial acetic acid are added. After maintaining the mixture at 110-130℃ for 70-80 hours, it is washed, dried, and ground to obtain Si@COF. Finally, Si@COF and cobalt acetate tetrahydrate are dispersed in methanol, reacted at room temperature, and then washed, dried, and ground to obtain Si@COF-Co. This invention offers a simple, high-yield, and effective method. The synthesized material effectively alleviates the volume expansion of nano-silicon, improves the stability and reversibility of the electrode material, and can be used as a negative electrode material for lithium-ion batteries.

The invention relates to the technical field of organic synthesis, in particular to a preparation method of N, N '-dichloro-1, 4-benzenedicarboxamide, which comprises the following steps: taking terephthalamide as an initial raw material and tert-butyl hypochlorite as a chlorination reagent; the method comprises the following steps: carrying out a chlorination reaction on terephthalamide and tert-butyl hypochlorite in a solvent under the protection of inert gas by controlling the reaction temperature, and after the reaction is finished, carrying out post-treatment to obtain N, N-dichloro-1, 4-phthalimide. The preparation method of the N, N '-dichloro-1, 4-benzenedicarboxamide comprises the following steps: taking terephthalamide and tert-butyl hypochlorite as raw materials, and carrying out one-step reaction to generate a dichloro product. Compared with a traditional N, N '-dichloro-1, 4-benzenedicarboxamide production method, the preparation method has the advantages that the amount of three wastes generated is small, the product yield is high, the product purity is high, the operation is safe and convenient, and the preparation method is more suitable for industrial application.

The invention provides a culture medium composition for saussurea involucrate tissue culture and application thereof, and belongs to the field of plant tissue culture. On the basis of the MS culture medium, the culture medium composition also comprises the following components: 9 to 11 g / L of fructose, 9 to 11 g / L of glucose, 9 to 11 g / L of sucrose, 5 to 7 g / L of agar, 0.5 to 1.5 mg / L of 2, 4-dichlorphenoxyacetic acid, 0.05 to 0.1 mg / L of naphthylacetic acid, 0.05 to 0.2 mg / L of N-phenyl-N '-1, 2, 3-thiadiazole-5-urea, 400 to 600 mg / L of lactoalbumin hydrolysate, 0.2 to 0.4 g / L of activated carbon and 10 to 25 mg / L of methyl jasmonate. By integrating hormone, functional additives (lactoalbumin hydrolysate and activated carbon) and a nano material (silver / copper doped nano zinc oxide), a multi-level synergistic effect is formed, so that the yield of flavonoid compounds is improved on the basis of improving the callus induction rate of saussurea involucrata.

The invention discloses a fullerene C60 tetra-addition derivative as well as a preparation method and application thereof. The structure of the fullerene C60 tetra-addition derivative is shown as a formula I. The specific preparation method comprises the following steps: under the protection of inert gas, taking fullerene C60, tetrabutyl ammonium hydroxide hydrate, benzyl bromide and a TBAOH methanol solution as raw materials, taking o-dichlorobenzene or methylbenzene as a solvent, and reacting at 60-80 DEG C to obtain the target fullerene C60 tetra-addition derivative. The preparation method of the fullerene C60 tetra-addition derivative has the advantages of simple operation steps, safety, easiness in control, high selectivity and the like. A photovoltaic device prepared by using the fullerene derivative as an acceptor material has high open-circuit voltage, and is a very potential photovoltaic material. # imgabs0 #

The invention is suitable for the technical field of chemical purification, and provides a high-purity 2, 4-dichlorobenzonitrile preparation method, which comprises: carrying out cooling crystallization treatment on a 2, 4-dichlorobenzonitrile liquid crude product at a cooling rate of 0.5-5 DEG C / h and a cooling end point of 50-53 DEG C, and carrying out heat preservation for 1-1.5 h; and performing heating sweating treatment on the crystal obtained by the cooling crystallization treatment at a heating rate of 0.5-3 DEG C / h, heating to 57-61 DEG C, and keeping the temperature for 0.5-1 h. According to the method, the high-purity 2, 4-dichlorobenzonitrile product with the purity being greater than or equal to 99.5% can be obtained, no additional solvent is needed, no other three-waste treatment is needed, the product purity is high, and the method is a green separation and purification process; in addition, the preparation process is simple and efficient, the investment of melt crystallization equipment is low, the operation condition is mild, the risk is low, the production safety coefficient is high, the total yield of purification is high after coupling with an upstream rectification process, and the method is suitable for industrial production.

The present invention belongs to the technical field of organic synthesis, and specifically relates to a synthesis process of high-yield 1,4-bis(4-phenoxybenzoyl)benzene. The process is mainly prepared by using excess diphenyl ether and terephthaloyl chloride as reaction raw materials, using o-dichlorobenzene as reaction solvent, and under the catalytic action of aluminum chloride. The synthesis process of 1,4-bis(4-phenoxybenzoyl)benzene provided by the present invention successfully overcomes many challenges existing in traditional synthesis methods, such as many side reactions, low yield, and purification difficulties, by optimizing key parameters such as reaction conditions, solvent selection, catalyst dosage, and sample addition order. It is not only easy to operate, but also significantly improves the yield of the target compound, and also ensures the high purity and low impurity content of the product.

The invention belongs to the field of high polymer material synthesis, and provides a method for preparing polyphenylene sulfide from high-purity p-dichlorobenzene, which adopts the whole process design of pre-construction of a composite sulfur source intermediate, regulation and control of an end group controllable oligomerization polyphenylene sulfide intermediate, segmented polymerization of the high-purity p-dichlorobenzene and precise dehydration-washing-drying. The ultra-low impurity level of 0.05-0.25 wt% of burning residues of the polyphenylene sulfide product, the sodium ion content of 10-200 mg / kg and the chloride ion content of 10-500 mg / kg is achieved, and meanwhile the high-performance stability of the melting point of 270-300 DEG C, the gel fraction of 92-99 wt% and the water content of 0.01-0.20 wt% is kept. The problems of deep removal of inorganic ions and ash content, balance of gel fraction and processability and control of residual solvents in the traditional polyphenylene sulfide preparation process are solved, and the method has wide application value in the fields of high-performance engineering plastics, special fibers, electronic packaging materials and the like.

The invention discloses a paradichlorobenzene refining and separating tower and a using method thereof, and relates to the technical field of dichlorobenzene separation.The paradichlorobenzene refining and separating tower comprises a dichlorobenzene refining and separating tower body, a discharging pipe, a feeding pipe, a detecting mechanism, a stirring mechanism and a control mechanism, and the right end of the top of the dichlorobenzene refining and separating tower body is fixedly connected with the discharging pipe; a feeding pipe is fixedly connected to the center of the bottom of the dichlorobenzene refining and separating tower, a detection mechanism is fixedly connected to the center of the left end of the dichlorobenzene refining and separating tower, the detection mechanism is arranged, and through cooperation of a spectrum detector and a photoelectric detector, detection of the boiling point of dichlorobenzene mixed liquid is achieved; therefore, the working conditions of the dichlorobenzene refining and separating tower can be accurately controlled in the later period, and separation is prevented from being affected by too high or too low temperature.

The invention relates to the technical field of electrocatalytic oxygen reduction, in particular to a three-dimensional covalent organic framework material and a preparation method and application thereof. The preparation method of the novel material comprises the step of enabling a monomer 4, 4 ', 4', 4 '''-(1, 4 (1, 4)-dibenzocyclohexanoic acid-12, 13, 42, 43-tetrayl) tetrabenzaldehyde with a three-dimensional structure to react with 5, 10, 15, 20-tetraaminophenyl cobalt porphyrin, 1, 2-dichlorobenzene, 1-butanol and acetic acid according to a certain proportion to obtain the novel material. The novel material provided by the invention is simple in preparation process and good in stability, has very excellent catalytic capability on the oxygen reduction reaction of the cathode of the fuel cell, is stable in performance, and is a new energy material with great development potential and wide market prospect.