2669 results about "Chlorobenzene" patented technology

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

The invention concretely relates to a synthetic technology for pyraclostrobin. The synthetic technology comprises: firstly performing cyclization to obtain 1-(4-chlorophenyl)-pyrazol-3-one, oxidizing the pyrazol ring under the effect of an oxidant to generate 1-(4-chlorophenyl)-3-hydroxypyrazole, then using 2-nitrobenzyl bromide to performing etherification to generate 1-(4-chlorophenyl)-3-[2-(nitrophenyl)methoxy]-1H-pyrazole, then using a reducing agent to perform nitro reducing, so as to generate N-hydroxyl-2-[N'-(4-chlorophenyl)pyrazol-3'-yloxymethyl]aniline, then using ClCO2CH3 to perform N-acylation reaction to generate methyl N-hydroxyl-N-2-{[N'-(4-chlorophenyl)pyrazol-3'-yloxymethyl]phenyl}formate, and finally performing hydroxyl methylation under an alkaline condition to generate pyraclostrobin. The technology enables all operations in the pyraclostrobin preparation process to be relatively controllable, helps to improve the stability of the preparation process and improve the product yield, successfully employs low-cost reagents and substantially reduces production cost, and also the employed reagents are relatively small in toxicity, is relatively beneficial for environment protection, and has no corrosivity on plastic pipes, so that the production safety is improved.

The invention discloses a new preparation method of 4,4-dichlorodiphenyl sulfone. The method comprises the following steps: 1) through using AlCl3 as a catalyst, and chlorobenzene and thionyl chloride as reaction raw materials, performing a Friedel-Crafts reaction at 25-35 DEG C, then hydrolyzing the mother liquor obtained through the Friedel-Crafts reaction, refluxing at 95-100 DEG C for 45-60 minutes, cooling the obtained mother liquor to less than 20 DEG C after refluxing to obtain an organic phase and an aqueous phase; 2) performing reduced pressure distillation on the organic phase, centrifuging, washing the obtained product to be neutral and be used as a product A for later use, wherein the main component of the product A is 4,4-dichlorodiphenyl sulfoxide; and 3) through using the product A and the oxidant hydrogen peroxide as raw materials and acetic acid as satalytic solvent, carrying out an oxidation reaction on the main component 4,4-dichlorodiphenyl sulfoxide of the product A to obtain crude 4,4-dichlorodiphenyl sulfone. Therefore, the existing synthesis method of 4,4-dichlorodiphenyl sulfone is changed, the production cost of 4,4-dichlorodiphenyl sulfone is low, the product quality is good and the reaction time is short.

The invention discloses a method for preparing 4.4-dichlorodiphenyl sulfone by using sulfoxide oxidation. The method comprises the following steps of: (1) performing Frieldel-Crafts reaction at the temperature of 25-35 DEG C by taking AlCl3 as a catalyst and chlorobenzene and thionyl chloride as reaction raw materials; next, hydrolyzing mother liquor after the Frieldel-Crafts reaction is finished; refluxing at the temperature of 95-100 DEG C for 45-60 minutes after hydrolysis is finished; cooling to be below 20 DEG C to divide into an organic phase and a water phase after refluxing is finished; performing reduced pressure distillation and centrifugal washing on the organic phase to be neutral to serve as a product A for later use, wherein a main component in the product A is 4.4-dichlorodiphenyl sulfone; and (2) performing oxidation reaction on the 4.4-dichlorodiphenyl sulfone by taking the product A as the raw material, hydrogen peroxide as a catalyst and dichloromethane as a reaction solvent to synthesize a 4.4-dichlorodiphenyl sulfone rough product. Thus, the method has the advantages of mild reaction conditions, high product quality and low three wastes (waste water, waste gas and industrial residues).

The invention relates to neutral mononuclear copper (I) complexes for emitting light and with a structure according to formula (A) in which: M represents: Cu(I); L∩L represents: a single, negatively charged, bidentate ligand; N∩N represents: a diimine ligand (substituted with R and FG), in particular a substituted 2,2′-bipyridine derivative (bpy) or a substituted 1,10-phenanthroline derivative (phen); R represents: at least one sterically demanding substituent for preventing the planarisation of the complex in the excited state; FG=functional group, and represents: at least one second substituent for increasing solubility in organic solvents. The substituent can also be used for electron transport or alternatively for hole transport, said functional group being bound to the diimine ligands either directly or by means of suitable bridges; and the copper (I) complex: having a ΔE(S₁−T₁) value of less than 2500 cm⁻¹ between the lowest excited singlet state (S₁) and the triplet state (T₁) which lies below; having an emission lifespan of at most 20 μs; having an emission quantum yield of greater than 40%, and a solubility of at least 1 g/L in organic solvents, in particular polar organic hydrocarbons such as acetone, methyl ethyl ketone, benzene, toluene, chlorobenzene, dichlorobenzene, dichloromethane, chloroform, dichloroethane, tetrachloroethylene, alcohols, acetonitrile or water.

The invention discloses a synthetic process for efficiently and continuously producing 4,4-dichlorodiphenyl sulfone, which comprises the following steps: carrying out Friedel-Crafts acylation on thionyl chloride and excessive chlorobenzene under the action of a lewis acid catalyst, carrying out pyrohydrolysis and adding chlorobenzene to carry out layering after the reaction is finished, adding anoxidizing agent into a sulfoxide organic layer to carry out oxidization, adding activated carbon to carry out decoloration and filtering; cooling filtrate and carrying out rejection filtration to obtain 4,4-dichlorodiphenyl sulfone. The synthetic process has the advantage that chlorobenzene not only is a raw material, but also is a reaction solvent, so that cross use of various solvents is avoided. Particularly, use of a great amount of acetic acid used as an oxidation reaction solvent is avoided, and corrosion to equipment and environmental pollution are avoided. In the integral process flow,separation and extraction of an intermediate 4,4-dichlorodiphenyl sulfoxide are avoided, so that production time of the product is greatly shortened, and production cost is saved. By using hydrogen peroxide, acetic acid and concentrated sulfuric acid as mixed oxidizing agents, oxidization capacity of hydrogen peroxide is greatly improved, yield and purity of the product are greatly improved, yield of the product reaches 90% or more, and purity of the product is greater than 99.8%.

The invention relates to a high oil absorption polyurethane foam which comprises the following components in parts by weight: 20 to 40 parts of isocyanate, 35 to 60 parts of polyol, 0.5 to 3 parts of catalyst, 0.5 to 3 parts of foam stabilizer, 5 to 10 parts of foaming agent, 2 to 10 parts of opening agent,5 to 20 parts of flame retardant, 5 to 15 parts of silicon rubber spherical micro powder and 0.5 to 2 parts of coupling agent. The preparation method comprises the following technology steps of weighing, prepolymerization, dispersing, polymerization foaming reaction, curing and peeling at room temperature and cutting. The high oil absorption polyurethane foam can be used for the absorption and recycle of various oil products (crude oil, engine oil, diesel fuel, gasoline, kerosene and the like) on water surfaces, ground or surfaces of other objects, and various oil soluble organic compounds (benzene, methylbenzene, dimethylbenzene, chloroform, nitrobenzene, chlorobenzene and the like). The invention has the advantages of simple technology and low cost, obviously improves the dispersing effect of the silicon rubber spherical micro powder in a polymerization system by using ultrasonic technique, and greatly increase the oil absorption quantity and oil absorption rate of the polyurethane foam by adding the silicon rubber spherical micro powder.

The invention relates to a method for preparing (S)-(4-chlorphenyl)-(pyridine-2-yl)-methanol by utilizing microbial catalysis, and belongs to the technical field of biological catalysis. According to the method, 4-chlorphenyl-(pyridine-2-yl)-ketone is subjected to asymmetrical reduction by utilizing kluyveromycessp (CCTCCM 2011385) whole cells to synthesize the (S)-(4-chlorphenyl)-(pyridine-2-yl)-methanol. The method comprises the following steps of: sieving a microbe which has high-stereoselectivity carbonyl reductase activity on a prochiral ketone substrate, determining a series of conditions of asymmetrical reduction reaction, such as reaction temperature, pH, the concentration of cells, the concentration of the substrate and reaction time and additives (including various secondary solvents, polyethyleneglycol (PEG), phosphates and the like), wherein the enantiomer excess value and yield of the (S)-(4-chlorphenyl)-(pyridine-2-yl)-methanol serving as a product can reach 86.7 percent e.e and 92.1. The product is separated and extracted initially by silicagel column chromatography, so that the purity of the separated product is 99.2 percent, and the extraction yield is 56.7 percent.

The invention relates to a method for recovery of contaminated groundwater through in situ enhanced aeration, which comprises the following steps: digging more than one surfactant injection well, an aeration well and an extraction well in an area with the groundwater contaminated, injecting surfactant into the area with the groundwater contaminated through the surfactant injection well to dissolve the surfactant into the groundwater so as to form surface tension in the area with the groundwater contaminated, starting the extraction pump to pump an aeration zone into negative pressure, and starting the aeration pump for continuous aeration. The invention effectively solves the problem that the majority of pollutants can be removed only after flowing into the porous channel through diffusion due to the narrow porous channel near the aeration well, and improves the saturation degree of the air in the groundwater, thereby increasing opportunities of exposure the pollutants to the air. Tests show that, when the aeration rate is 100ml/min, the surface tension is reduced to 50.4dyn/cm from 70.5dyn/cm, the half-life for removal of the pollutant chlorobenzene is reduced to 16min from 31min, and simultaneously the trailing concentration is reduce to 5.1mg/L from 22.08mg/L. The removal rate can be increased to 98.5 percent from 89.2 percent after 420 minutes. The invention has the advantages of simple process, low cost, low surfactant injection and less impact on the environment.

The invention relates to Rhodococcus ruber and application of Rhodococcus ruber in degradation of phenol pollutants. The Rhodococcus ruber is designated as Rhodococcus ruber SD3, which is preserved in a preservation unit appointed by SIPO (State Intellectual Property Office), wherein the preservation unit is a China Center for Type Culture Collection, the preservation date is February 26, 2012, the accession number is CCTCC NO: M 2012035, and the Latin name is Rhodococcus ruber SD3. The Rhodococcus ruber has the following technical effect: after Rhodococcus ruber SD3 in an inorganic salt medium of phenol (phenol concentration is 1.0g/L) is subjected to shaking table vibration culture at 35 DEG C and 200r/min for 72h, the phenol degradation rate is 99.73%. The Rhodococcus ruber SD3 can also degrade substances such as isooctane, cyclohexane, benzene, n-heptane, methylbenzene, acetonitrile, chlorobenzene, naphthalene, n-hexane, and 1-naphthol.

The invention belongs to the technical filed of medicines, and concretely relates to optically pure benzyl-4-chlorophenyl C-glucoside derivatives represented by formula (II) and formula (III), a method for preparing the above compounds and intermediates thereof, a medicinal preparation and a medicinal composition containing the compounds, and an application of the optically pure benzyl-4-chlorophenyl C-glucoside derivatives in the preparation of medicines for treating and/or preventing insulin-dependent diabetes, non-insulin dependent diabetes, insulin resistance diseases or obesity, various diabetes and relevant diseases as a sodium-glucose cotransporter (SGLT) inhibitor.

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

The invention discloses a treatment technique of tetrabromobisphenol A production wastewater, belonging to organic chemical industry wastewater recycling and harmless environmental-protection treatment technologies. The treatment technique of tetrabromobisphenol A production wastewater is an acidification precipitation-resin adsorption-advanced oxidation combined technique, and mainly comprises the following steps: 1. regulating the pH value of the wastewater to recycle the tribromophenol in the wastewater by acidification precipitation; 2. filling the wastewater, in which abundant tribromophenol is removed, into an adsorption column by using a macroporous adsorbent resin subjected to conventional pretreatment, and passing the wastewater through a bed bottom at a certain flow rate so that chlorobenzene is adsorbed by the resin, wherein the resin adsorption is utilized to remove most chlorobenzene, bisphenol A and other nondegradable organic substances in the recycled wastewater, thereby effectively reducing COD (chemical oxygen demand) of the wastewater and relieving the treatment load of the wastewater; and 3. carrying out electrocatalytic oxidation on the wastewater subjected to acidification precipitation-resin adsorption to finally remove harmful and nondegradable substances in the wastewater, thereby achieving the goal of harmless discharge after reaching the standard.

The invention provides an industrialization production process of entecavir-monohydrate. The special features of the process different from the other process are that: methyldiphenylchlorosilane is used as the silanization protector and special catalyst, thus the reaction temperature is -40 DEG C and the object product is smoothly produced (the reaction temperature is -78 DEG C in the prior process). Thus the production process is more suitable for industry production and because the silanization protector is cheaper and easily obtained, the production cost is greatly reduced. The invention comprises the preparation of methyldiphenylchlorosilane as the silanization protector which is obtained by directly synthesizing the methylphenyldichlorosilane and Grignard reagent of chlorobenzene under the action of special catalyst.

The invention relates to a detection method for plant growth regulator residues in fruits. The detection method comprises the following steps: the QuEChERS method is adopted to extract and purify the plant growth regulator residues in fruits, so as to enable the adding standard recovery rate of the target compound to reach 71%-98%; the RSD ( relative standard deviation) is not higher than 6%; the sensitivity and selectivity are favorable and the recovery rate is stable; the liquid chromatograph tandem mass spectrogram detection method is adopted to simultaneously detect forchlorfenuron, ethephon, 4-sodium chlophenoxycetate and 2,4- sodium acetate-dichlorobenzene oxygen; the detection limits range from 0.5 microgram/kg to 100 microgram/kg respectively; the sensitivity requirement of national limited standard is met. The detection method has favorable sensitivity and selectivity and can serve as a method for detecting the plant growth regulator residues in fruits.

The invention provides a chloration method for phenoxyacetic acid and derivatives thereof, which comprises the following steps that: raw materials of the phenoxyacetic acid or the derivatives of the phenoxyacetic acid and chlorinating agents take reaction at a certain temperature in organic solvents under the effect of catalysts, wherein the chlorinating agents can be chlorine gas, sodium hypochlorite, calcium hypochlorite and sulfuryl chloride, the catalysts can be lewis acid and sulfurated substances, and solvents can be dichloromethane, dichloroethane, trichloromethane, carbon tetrachloride, formic acid, ethyl acetate, benzene, toluene, dimethylbenzene, chlorobenzene and o-dichlorobenzene. The method has the advantages that the operation can be carried out under the waterless condition, the generation of a large amount of industrial waste water is avoided, the used catalysts are safe and are easy to obtain, the solvents can be cyclically used, and the industrialization is easy.

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

The invention discloses a preparation method of Boscalid, which comprises the following steps that Suzuki coupling reaction occurs between o-iodoaniline and 4-chlorobenzene boronic acid to produce an intermediate product 4'-chlorinated biphenyl-2-amine under the catalytic effect of Pd/C by using methylbenzene and alkaline water as mixed solvent; and condensation reaction occurs between the 4'-chlorinated biphenyl-2-amine and 2-chloronicotinyl chloride to produce the Boscalid. The preparation method of the Boscalid has the advantages that the production cost is reduced, the yield of the intermediate product 4'-chlorinated biphenyl-2-amine is improved, the total yield of the two steps exceeds 84 percent and the industrial production is expected to be realized.

The invention discloses a preparation method of a BPPO (Brominated Polystyrene) and PVA (Polyvinyl Alcohol)-based organic-inorganic hybrid anion exchange membrane. The preparation method comprises the following steps: (1), dissolving the BPPO in chlorobenzene, and adding DMF (Dimethyl Formamide), tertiary amine solution, two micromolecule alkoxy silanes and water so as to obtain BPPO (+)/SiO2 materials; (2) dissolving the obtained BPPO (+)/SiO2 materials into DMF mixed solution so as to BPPO (+)/SiO2 solution; (3) dropping the BPPO (+)/SiO2 solution into PVA solution so as to prepare coating liquid; and (4) coating the coating liquid on a basal body so as to form a diaphragm, and drying the diaphragm to obtain the organic-inorganic hybrid anion exchange membrane. According to the invention, quaternary ammonium BPPO, PVA and micromolecule alkoxy silanes are utilized to prepare the hybrid anion exchange membrane containing the quaternary ammonium group and-OH base, the content of the PVA in the membrane can be controlled, and a cross-linked structure can be formed, so that the stability and mechanical performance of the membrane can be reinforced; and moreover, the -OH base in the PVA can promote the H+ ion to transfer, so that the prepared hybrid anion exchange membrane is particularly suitable for diffusion dialysis process, and can separate and recycle acid waste liquid.

The invention discloses rhodococcus ruber FQ-2 and an application thereof in degradation of acetone and other common industrial organic pollutants. The application method comprises the steps: an inorganic salt culture medium containing acetone and other common industrial pollutants is inoculated with the rhodococcus ruber FQ-2, a degradation reaction is carried out under the conditions of the temperature of 30 DEG C and the rotating speed of 160 r/min, and thus the organic pollutants are degraded; the common organic pollutants comprise acetone, n-hexane, carbon disulfide, chlorobenzene, butylacetate, ethyl acetate or alpha-pinene. The rhodococcus ruber FQ-2 is taken from activated sludge of an aeration tank of a pharmaceutical factory in Zhejiang province, has good degradation effect on VOCs organic pollutants, especially acetone, and can completely convert acetone into harmless substances such as CO2, H2O, cell biomass and the like; at the same time, the bacterial strain also can degrade common industrial pollutants such as carbon disulfide and chlorobenzene in different extent, so the bacterial strain has broad application prospects in biological purification of industrial wastegas and wastewater.

The invention relates a three-system organic photovoltaic device based on graphene quantum dots and a preparation method of the three-system organic photovoltaic device. According to the preparation method, the design limitation of an original binary organic photovoltaic device is broken through, and a spin coating technique and a thermal evaporation film plating technique are adopted on transparent conductive glass to reach the purpose of enhancing the device energy conversion efficiency. The three-system organic photovoltaic device uses a three-system coexistence system including an organic donor and an organic acceptor as well as the graphene quantum dots as an organic active layer, the donor and the acceptor are dissolved in chlorobenzene containing the graphene quantum dots in a certain proportion, and a three-system coexistence structure active layer is prepared only by only requiring the spin coating, so that the cost is low, the operation is simple and the conversion efficiency of the organic photovoltaic device is effectively improved.

The invention discloses a method for preparing a graphene organic dispersion solution from hyperbranched polyethylene, which comprises the following steps: (1) proportionally mixing graphite powder, organic solvent B and hyperbranched polyethylene, and then performing ultrasonic dispersion on the obtained mixture to obtain a graphene initial dispersion solution C; and further performing low-speed centrifugation and standing treatment to obtain a graphene dispersion solution D containing excessive hyperbranched polyethylene, wherein the organic solvent B is selected from one of the following chemically pure or analytically pure agents: tetrahydrofuran, trichloromethane, n-heptane, chlorobenzene and dichloromethane; and (2) performing ultra-high-speed centrifugation or vacuum filtration on the graphene dispersion solution D obtained in the steps (1) to remove the contained excessive hyperbranched polyethylene, and further performing ultrasonic dispersion in the organic solvent B to obtain the graphene organic dispersion solution. The preparation process causes less damage to the surface structure of graphene; and the obtained graphene is low in surface defect concentration and can better take the performance advantages.