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383 results about "Dichloroethane" patented technology

Dichloroethane can refer to either of two isomeric organochlorides with the molecular formula C₂H₄Cl₂: 1,1-Dichloroethane 1,2-Dichloroethane

Novel preparation method of tetra (dimethylamino) tin

The invention relates to a novel preparation method of tetra (dimethylamino) tin. The method comprises the following steps: in a nitrogen atmosphere, pumping an n-hexane solution of n-butyllithium and an n-hexane solution of dimethylamine into a pipeline through a propeller, mixing through a T-shaped joint, and reacting through a flow reactor 1 and a flow reactor 2 to obtain a lithium dimethylamide mixed solution; the method comprises the following steps: pumping a lithium dimethylamino mixed solution and a n-hexane solution of tin tetrachloride into a pipeline through a propeller, mixing through a T-shaped joint, and reacting through a flow reactor 3 and a flow reactor 4 to obtain a crude tetra (dimethylamino) tin product; and centrifuging and filtering the tetra (dimethylamino) tin crude product, adsorbing impurities by adopting a resin column, and carrying out reduced pressure distillation to remove the solvent, thereby obtaining the tetra (dimethylamino) tin. The adsorption resin column adopts modified macroporous adsorption resin, and is obtained by reacting, filtering and drying D190 macroporous styrene sulfydryl resin, dichloroethane, tetramethylguanidine, 5-allylpyrimidine-4, 6-diol and an ethylene boric anhydride pyridine complex.
Owner:ZHEJIANG BRITECH CO LTD

Catalytic combustion catalyst for treating CVOCs as well as preparation method and application of catalytic combustion catalyst

The invention discloses a catalytic combustion catalyst for treating CVOCs (Chemical Volatile Organic Compounds) as well as a preparation method and application of the catalytic combustion catalyst. The preparation method comprises the following steps: (1) impregnating and loading cerous nitrate and trimethyl phosphate on a carrier, drying, and roasting at 600-800 DEG C to form a modified carrier containing a cerous phosphate crystal phase; and (2) impregnating and loading active metal ruthenium on the modified carrier, drying and roasting to obtain the catalyst for treating catalytic combustion of the CVOCs. The catalyst provided by the invention can be used for catalytic combustion degradation of CVOCs such as dichloromethane, chlorobenzene, chloroethylene, dichloroethane, dichloroethylene, oxychloropropane and the like. For catalytic combustion degradation of CVOCs, the catalyst disclosed by the invention can show high activity, high chlorine-resistant stability, low polychlorinated by-product selectivity and thermal stability, and has certain industrial application prospects.
Owner:ENVIRONMENTAL SCI RES & DESIGN INST OF ZHEJIANG PROVINCE +1

Method for separating 1-fluoro-1, 1-dichloroethane and 1, 1, 1, 3, 3-pentafluorobutane azeotrope through extractive distillation

The invention relates to a method for separating azeotrope of 1-fluoro-1, 1-dichloroethane and 1, 1, 1, 3, 3-pentafluorobutane through extractive distillation. According to the method for separating the 1-fluoro-1, 1-dichloroethane and the 1, 1, 1, 3, 3-pentafluorobutane azeotrope through extractive distillation, an extracting agent is added into the 1-fluoro-1, 1-dichloroethane and the 1, 1, 1, 3, 3-pentafluorobutane azeotrope, and the extracting agent is one or more of n-amyl alcohol and n-heptanol. The method adopts intermittent extractive distillation or continuous extractive distillation operation, and has the advantages of simple and efficient separation process, high product purity and the like. The loss rate of the extracting agent is low, the extracting agent can be recycled, and environmental pollution can be avoided.
Owner:ZHENGZHOU UNIV

Antistatic agent for fuel oil and preparation method thereof

The invention provides an antistatic agent for fuel oil and a preparation method thereof, and belongs to the technical field of petrochemical engineering, and the preparation method comprises the following steps: S1, adding soybean lecithin and chlorosulfonic acid into dichloroethane, uniformly mixing, under the protection of nitrogen, heating and stirring for reaction, neutralizing reaction liquid, and performing rotary evaporation to obtain sulfonated soybean lecithin; the preparation method comprises the following steps: adding sulfonated soybean lecithin and ethidene diamine into absolute ethyl alcohol, then adding p-toluenesulfonic acid, heating and stirring for reaction, and carrying out reduced pressure distillation to obtain modified soybean lecithin; s2, dispersing the SiO2 particles in absolute ethyl alcohol, adding KH-550, and performing ultrasonic treatment, centrifugation and drying to obtain pretreated SiO2 particles; and uniformly mixing the modified soybean lecithin and the pretreated SiO2 particles, adding the mixture into a supercritical fluid reactor, heating and pressurizing, ultrasonically dispersing, and drying to obtain the antistatic agent. The antistatic agent has the advantages of good dispersibility, strong stability and strong antistatic capability.
Owner:ZIBO KAIMEIKE IND & TRADE CO LTD

Purity analysis method for crude vinyl chloride in conversion process

The invention discloses a purity analysis method for crude vinyl chloride in a conversion process, which comprises the following steps: after sampling, carrying out qualitative and quantitative analysis on small molecule components in the crude vinyl chloride, then analyzing acetylene and high-boiling residues in the crude vinyl chloride, and calculating the purity of the crude vinyl chloride according to a deduction method. Compared with the prior art, the aluminum foil sampling bag is adopted for sampling, so that the problem of poor sample representativeness is solved; the content of the high-boiling residues in the crude vinyl chloride can be accurately analyzed by adopting gas chromatography, so that the accuracy and precision of analysis data are improved; according to the method, gas chromatography is adopted to completely replace a dichloroethane absorption method, so that the working intensity of workers is reduced, and the method has the effects of safety, environmental protection and low energy consumption.
Owner:TANGSHAN SANYOU CHLOR ALKALI

Hypercrosslinked polyionic liquid modified MXene nanocomposite as well as preparation method and application thereof

The invention relates to a hyper-crosslinked polyionic liquid modified MXene nano composite material as well as a preparation method and application thereof, and belongs to the field of nano functional materials. The invention relates to a preparation method of a hyper-crosslinked polyion liquid modified MXene nanocomposite, which comprises the following steps: dissolving vinylated MXene nanosheets and 1-vinyl-3-butylimidazolium bromide in toluene, adding styrene into the obtained solution, adding azodiisobutyronitrile, and reacting to obtain the polyion liquid modified MXene nanocomposite. Adding the obtained polyion liquid modified MXene composite material and dimethoxymethane into dichloroethane to uniformly disperse the polyion liquid modified MXene composite material, then adding anhydrous ferric trichloride into the solution, and reacting to obtain the hypercrosslinked polyion liquid modified MXene nano composite material. When the composite adsorbent provided by the invention is used for adsorbing the IBP, the highest removal rate can reach 93.2%, and the composite adsorbent is simple to operate, high in stability and environment-friendly.
Owner:DONGGUAN UNIV OF TECH

Preparation method of lithium difluorobisoxalato phosphate concentrated solution

The invention relates to a preparation method of a lithium difluoro bis (oxalate) phosphate concentrated solution, and belongs to the technical field of lithium battery electrolyte additives. Adding lithium oxalate into a solvent, stirring and dissolving to obtain a lithium oxalate solution; the method comprises the following steps: adding a modified fluorine ion chelating agent into a lithium oxalate solution, stirring, filtering, putting into a reactor, and slowly introducing phosphorus pentafluoride gas; after the introduction is finished, heating and stirring for reaction; after the reaction is finished, filtering reaction liquid to remove unreacted solid impurities, so as to obtain a lithium difluoro bis (oxalate) phosphate concentrated solution; the modified fluorine ion chelating agent is prepared from D301 ion exchange resin, dichloroethane, propylene-1-base boronic acid pinacol ester, mercaptoethyl guanidine dihydro bromide and sodium tert-butoxide. The lithium difluoro bis (oxalate) phosphate prepared by the method is high in purity and high in yield, and meets the use requirements of lithium ion battery electrolyte on lithium salt.
Owner:HANGZHOU WANLIDA NEW ENERGY TECH CO LTD

System for producing vinyl chloride through oxychlorination

The utility model provides a system for producing vinyl chloride through oxychlorination, and belongs to the field of vinyl chloride synthesis. According to the system for producing vinyl chloride through oxychlorination, dichloroethane is prepared through the oxychlorination reaction unit, then the dichloroethane is refined through the refining unit, then the refined dichloroethane is cracked in the cracking unit to prepare vinyl chloride, and finally the vinyl chloride is obtained through purification in the vinyl chloride refining unit. Dichloroethane is prepared through a direct chlorination reaction unit, so that the yield of dichloroethane is increased, and a raw material is provided for cracking of dichloroethane; according to the system for producing vinyl chloride through oxychlorination, dichloroethane is prepared through the oxychlorination reaction unit and the direct chlorination unit, so that the working efficiency of the system is improved.
Owner:INNER MONGOLIA RUIDAXIN TECH CO LTD

Preparation method of deuterated methylamine hydrochloride and solid-phase continuous flow synthesis system

The invention discloses a preparation method of deuterated methylamine hydrochloride and a solid-phase continuous flow synthesis system, and relates to the technical field of deuterated synthesis. The preparation method comprises the following steps: adding out-of-phase polykadexide into methyl trifluoromethanesulfonate and 1, 2-dichloroethane for heating reaction, then adding methanol for quenching reaction, washing and drying to obtain an out-of-phase polykadexide type methyl reagent; the method comprises the following steps: adding a heterophase polysulfide-type methyl reagent into a mixed solvent of a polar solvent and heavy water, and carrying out alkali treatment to complete deuteration conversion, so as to obtain a heterophase polysulfide-type deuterated methyl reagent; the preparation method comprises the following steps: dissolving o-phenylsuccinimide in acetonitrile, and adding a heterophase polysulfide deuterium methyl reagent and inorganic alkali to react, so as to obtain N-(1, 1, 1-trideuterium methyl) benzo-succinimide; the preparation method comprises the following steps: hydrolyzing N-(1, 1, 1-trideuterium methyl) benzo-succinimide and hydrochloric acid in an aqueous solvent to obtain deuterated methylamine hydrochloride. The preparation method is simple, the deuterium source is cheap, the atom utilization rate is high, the deuteration rate is high, and the production cost is low.
Owner:SHENZHEN UNIV

Refining method of carbon dioxide-based polycarbonate diol

PendingCN120137156AChlorobenzeneEthyl phenylacetate
The present invention relates to the technical field of polymer synthesis, and provides a carbon dioxide-based polycarbonate diol refining method, which comprises: S1, mixing carbon dioxide-based polycarbonate diol, an extraction agent and water, and washing to obtain a glue liquid; s2, the glue liquid is subjected to flash evaporation and devolatilization, and a carbon dioxide-based polycarbonate diol refined product is obtained; the extracting agent comprises methylbenzene or a mixture of one of methylbenzene, chlorobenzene and ethyl acetate and dichloroethane. According to the technical scheme, the problem of low yield of polycarbonate diol prepared in related technologies is solved.
Owner:HUANGHUA XINNUOLIXING FINE CHEM +1

Oxychlorination Process

In a process for producing 1,2-dichloroethane, the process includes the steps of: (i) providing a fluidizable catalyst; (ii) charging a fluidizable catalyst into a fluidized bed reactor; (iii) fluidizing the catalyst in the reactor; (iv) heating the catalyst in the fluidized bed reactor to a temperature greater than 150° C. for more than 6 hours while fluidizing the catalyst in the reactor, wherein the fluidizing and heating steps are performed in the absence of ethylene conversion; and (v) converting ethylene to 1,2-dichloroethane in the presence of the catalyst after the heating step.
Owner:OXY VINYLS LP

Monofluorodichloroethane waste liquid recycling device

The utility model belongs to the technical field of waste liquid recycling equipment, and particularly relates to a dichlorofluoroethane waste liquid recycling device which comprises a waste liquid cylinder, the interior of the waste liquid cylinder is of a cavity structure, waste liquid is layered after being poured into the waste liquid cylinder for standing, and the waste liquid in the cylinder is divided into three layers, namely an upper floating oil layer, a middle standing layer and a lower particle layer; an observation window and an air filter are respectively arranged at the top of the waste liquid cylinder; a waste liquid outlet communicated with the waste liquid cylinder is formed in one side of the bottom of the waste liquid cylinder; a collector communicated with the waste liquid cylinder is arranged outside the waste liquid cylinder; and a recycling part is also arranged in the cylinder body of the waste liquid cylinder. According to the recycling device, the recycling component is arranged in the waste liquid cylinder, the purposes of recycling and reusing the dichlorofluoroethane waste liquid and reusing the dichlorofluoroethane waste liquid by using a middle standing layer are achieved by adopting a physical method and through natural standing, layering, semi-automatic liquid taking and filtering of the waste liquid, the purposes of no power consumption, safety and environment-friendly recycling are achieved, the using cost is low, and the recycling device is suitable for industrial production. And benefits are brought to enterprises.
Owner:STATE-OWNED LUOYANG DANCHENG RADIO FACTORY

Synthesis method and application of catalyst for preparing vinyl chloride through catalytic cracking of 1, 2-dichloroethane

The invention discloses a synthesis method of a catalyst for preparing vinyl chloride through catalytic cracking of high-activity 1, 2-dichloroethane, and active components in the catalyst are uniformly dispersed on nitrogen-doped carbon dots loaded on activated carbon. The method comprises the following steps: firstly preparing nitrogen-doped carbon dots containing active components, and then loading the nitrogen-doped carbon dots on activated carbon to prepare the composite catalyst. The catalyst can efficiently catalyze the reaction of cracking 1, 2-dichloroethane to prepare vinyl chloride. Compared with the existing catalyst for preparing vinyl chloride by cracking 1, 2-dichloroethane, the active component has better dispersity, the energy consumption can be greatly reduced, the production cost is reduced, and the catalyst has a very good industrial prospect.
Owner:WANHUA CHEM GRP CO LTD

Synthetic method of isoxazole compound under visible light catalysis condition

PendingCN121974865AOrganic chemistryOrganic synthesisN-butyl nitrite
The invention belongs to the technical field of organic synthesis, and particularly relates to a synthesis method of an isoxazole compound under a visible light catalysis condition. The method comprises the following steps: dissolving a compound 1 in 1, 2-dichloroethane, then adding tert-butyl nitrite, tribromomethane, alkali and a photocatalyst, in an inert gas environment, irradiating with visible light and stirring at room temperature to react, after the reaction is completed, reducing pressure to remove a solvent, and then performing silica gel column purification on a crude product to obtain a product, namely the isoxazole compound. The brand-new method for preparing the isoxazole compound through visible light catalysis is developed, the conditions of high temperature and high pressure in a traditional synthesis method are avoided, energy consumption and environmental pollution are remarkably reduced, and the yield of the isoxazole compound is effectively increased by regulating and controlling reaction conditions and optimizing raw material selection and proportion.
Owner:GUANGDONG UNIV OF PETROCHEMICAL TECH

A bio-based anionic superdispersant and preparation method thereof

The present invention discloses a bio-based anionic super dispersant having a structure shown in formula I or formula II. The super dispersant shown in formula I is formed by rigid terephthalate and flexible vinyl linked by ether bonds; the super dispersant shown in formula II is formed by rigid terephthalate and flexible glycerol linked by ether bonds. The preparation method of the super dispersant in the present invention is: succinylsuccinic acid dimethyl ester is oxidized to obtain 2,5-hydroxy terephthalic acid dimethyl ester, and then condensed with 1,2-dichloroethane (or epichlorohydrin) and the like to form an ether, and then the ester bond is saponified under an alkali agent to obtain. The preparation method of the super dispersant provided by the present invention is simple, has a high biochar content, a high yield, good pigment dispersion performance, and good stability of the obtained pigment paste.
Owner:JIANGSU LYNWON TECH CO LTD

Preparation method of cefotaxime

ActiveCN119285653Ahigh purityUniform and stable dispersionOrganic chemistryCefotaximeOrganic solvent
The invention relates to the technical field of pharmaceutical compounds, and particularly discloses a preparation method of cefotaxime. The preparation method comprises the following steps: dissolving 7-ACA in an organic solvent A, then adding porous silica gel spheres, mixing for 90-120 minutes, washing and drying to obtain the porous silica gel sphere loaded 7-ACA; and uniformly dispersing the porous silica gel ball-loaded 7-ACA, AE-active ester, an antioxidant and triethylamine in an organic solvent B, reacting at 10-25 DEG C for 60-90 minutes, and carrying out solid-liquid separation, extraction, acidification, crystallization, washing and drying to obtain the cefotaxime. The organic solvent B comprises dichloroethane and isopropanol. The cefotaxime prepared by the preparation method disclosed by the invention has relatively good yield and purity.
Owner:SHANDONG ANHONG PHARM CO LTD

Pd-Ba / C catalyst and preparation method and application thereof

The invention discloses a Pd-Ba / C catalyst as well as a preparation method and application thereof. The preparation method comprises the following steps: step 1, pretreating a carbon carrier; step 2, preparing a complexing solution containing a barium complex; step 3, carrying out wet impregnation to obtain a carbon carrier adsorbed with a barium complex; 4, performing low-temperature pyrolysis to obtain a barium pre-modified carrier; 5, a complexing solution containing palladium and barium complexes is prepared; step 6, co-adsorption of bimetals is realized through wet impregnation, and a bimetal adsorption carrier is obtained; step 7, freeze drying; 8, the precursor obtained after freeze drying is subjected to hydrogen reduction, and the Pd-Ba / C catalyst is obtained. The invention provides application of the Pd-Ba / C catalyst in preparation of ethylene by hydrodechlorination of 1, 2-dichloroethane. According to the invention, pre-loaded barium occupies a strong adsorption site on the surface of the activated carbon, so that the stability and dispersity of a palladium active center can be enhanced, and synergistic improvement of chlorine poisoning resistance and catalytic performance of the catalyst is realized.
Owner:ZHEJIANG UNIV OF TECH

A preparation method and application of an oxygen cephalosporin intermediate OZ

ActiveCN118440097Bshort process routeEasy to separate and recycleOrganic chemistryOrganic solventFluid phase
The present invention provides a method for preparing an oxygen cephalosporin intermediate OZ, the preparation method comprising using a compound shown in formula I as a raw material, triphenylphosphine as a desulfurizing agent, toluene and dichloroethane as solvents for reflux reaction, and preparing an oxygen cephalosporin intermediate OZ shown in formula II. The present invention tests the effects of different organic phosphines on the reaction. According to liquid phase reaction monitoring data, triphenylphosphine is the best. By using a specific precipitation solvent, the crystallization effect is good, and the purity of the product is improved. At the same time, the present invention tests the effects of different organic solvents on the reaction. Among them, a mixed solvent of toluene and dichloroethane is the best for the reaction, and the reaction conversion rate can reach more than 80%. The present invention has a short process route, mild reaction control conditions, simple operation, high yield, low cost, and is suitable for industrial production.
Owner:GUANGDONG LIGUO PHARMACY

A method for preparing brominated polystyrene

ActiveCN119529143BImidePtru catalyst
The invention discloses a method for preparing brominated polystyrene, and belongs to the technical field of brominated polystyrene preparation. The method comprises: preparing a main chain bromination inhibitor, preparing a catalyst, and reacting; in the reaction, polystyrene and ethylene dichloride are mixed, stirred at 35-40°C for 30-40min under the protection of nitrogen, then cooled to 0-2°C, the main chain bromination inhibitor and the catalyst are added, stirred for 20-30min, and a dichloroethane solution of N-bromosuccinimide is added dropwise, and after the addition is completed, the mixture is stirred at room temperature for 1.5h, the reaction is terminated, and the mixture is washed with a sodium hydroxide aqueous solution, washed with water, and then filtered, and the filtrate is evaporated and crystallized, filtered, and vacuum dried to obtain brominated polystyrene; the brominated polystyrene prepared by the invention has good color performance and thermal stability, high bromine content, narrow molecular weight distribution, good reaction controllability, and short reaction time.
Owner:SHANDONG DONGXIN NEW MATERIALS TECH CO LTD

Preparation and application of hydroxyl-functionalized quaternary phosphonium salt polyion liquid super-crosslinking heterogeneous catalyst

The invention discloses a preparation method of a hydroxyl-functionalized quaternary phosphonium salt polyion liquid super-crosslinked heterogeneous catalyst and an application of the catalyst in catalysis of a cycloaddition reaction of CO2 and epoxide. Trimethoxytriphenylphosphine and dibromo-p-xylene are firstly subjected to quaternary phosphating to form triphenylphosphine-based ionic liquid, and then the triphenylphosphine-based ionic liquid and biphenyl benzyl dichloride can be subjected to aromatic electrophilic substitution reaction in the presence of 1, 2-dichloroethane serving as a solvent and anhydrous aluminum chloride serving as a Lewis acid catalyst to realize cross-linking, so that the triphenylphosphine-based ionic liquid can be prepared. And methoxy can be removed to form hydroxyl, so that the hydroxyl-functionalized quaternary phosphonium salt polyion liquid super-crosslinked polymer is prepared in one step. The resulting heterogeneous catalyst effectively converts CO2 to cyclic carbonates under milder conditions (80 DEG C, 1 atm) in the absence of a soluble co-catalyst.
Owner:ZHEJIANG SCI-TECH UNIV

Process for preparing fipronil and intermediate thereof

The invention belongs to the technical field of synthesis of organic compounds, and particularly relates to a process for preparing fipronil and an intermediate thereof. Toxic 1, 2-dichloroethane is comprehensively replaced by bio-based gamma-valerolactone, low-toxicity cyclopentyl methyl ether is matched, and N, N-dimethylformamide necessary for the process is recycled, so that consumption is greatly reduced; the continuous processes of amination, diazotization and the like are realized through a tubular reactor, a micro-reactor and a static mixer, and separation technologies such as pervaporation membrane and vacuum distillation are combined, so that the reaction time is shortened, the solvent recovery rate is increased, and the production is promoted to be continuously transformed to green. The supported FeCl3 / SiO2-NH2 catalyst disclosed by the invention can be repeatedly used, and byproducts and tail gas can be recycled and reused. In addition, diazonium salt residues are controlled to be smaller than or equal to 0.5% through near infrared spectroscopy, citric acid is subjected to stable oxidation reaction, a purification process is combined, it is ensured that the finished product is high in purity, excellent in yield and small in batch fluctuation, and efficiency and safety are both considered.
Owner:长青(湖北)生物科技有限公司

1-nitroanthraquinone continuous production process based on dynamic liquid membrane continuous flow reactor

The invention relates to the field of chemical equipment, in particular to a 1-nitroanthraquinone continuous production process based on a dynamic liquid membrane continuous flow reactor, which comprises a solid feeding device, a homogeneous emulsifier, a quenching kettle, a solid-liquid separator, a centrifugal separator and a dynamic liquid membrane reactor, a sulfuric acid storage tank is divided into two branches through a sulfuric acid feeding pump, one branch is connected to the dynamic liquid membrane reactor, the other branch is connected to the dynamic liquid membrane reactor through a flow self-control valve, the quenching kettle is connected to a solid-liquid separator, the solid-liquid separator is divided into two branches, one branch is connected to an anthraquinone crude product storage tank, the other branch is connected to a centrifugal separator, and the other branch is connected to a gas-liquid separator. The centrifugal separator is divided into two branches, one branch is connected to the acid water storage tank, and the other branch is connected to the dichloroethane storage tank, so that the reaction selectivity of the anthraquinone nitration reaction can be effectively improved, high-viscosity solids are prevented from being blocked, and the conversion rate of raw materials in the continuous reaction of the anthraquinone nitration reaction is improved.
Owner:QINGDAO TIANHUICHEN TECH CO LTD +1

A method for continuously preparing flake diquat dichloride by a microfluidic reactor

The invention discloses a method for continuously preparing flake diquat dichloride by a microfluidic reactor, which includes: using a feeding pump to input liquid 2,2'-bipyridine or a 2,2'-bipyridine solution dissolved in a solvent, dichloroethane or a dichloroethane solution into the microfluidic reactor, quickly mixing and precipitating, separating solid from liquid, washing with toluene, and drying to obtain flake diquat dichloride; a dispersant is added to the liquid 2,2'-bipyridine or the 2,2'-bipyridine solution dissolved in a solvent, dichloroethane or the dichloroethane solution, either both or one of them. The method of the invention has the advantages of simple operation, stable process, strong safety, and continuous and stable production. The synthesized diquat dichloride is in a flake structure, which can effectively avoid dust and is helpful for the production and packaging of various pesticide formulations. The method of the invention uses a surfactant, which effectively avoids the agglomeration phenomenon of diquat dichloride.
Owner:MAANSHAN RED SUN BIOCHEMICAL CO LTD

N-substituted derivatives of l-(l-phenyl-3-aryl)-lff-pyrazol-4-yl)methanainine, method for their production and their applications

The subject of the invention is N-substituted derivatives of l-(l-phenyl-3-aryl)-lH-pyrazol-4-yl)methanamine with the general formula 1, where ¥ represents CH or N, R1 represents hydrogen, R2 represents no substituent, R3 represents hydrogen, while R4 represents N-propylbenzamide, benzo[b]furan, dihydrobenzo [b] furan, methylenedioxybenzene, ethyl benzoate, or propyl benzoate, substituted accordingly, their method of production and application, and the method of obtaining and application of N-substituted derivatives of l-(l-phenyl-3-aryl)-IH-pyrazol-4-yl)methanamine with the general formula 1, where Y represents C, CH, or N, R1 represents hydrogen or a methyl group, R2 represents a methyl group or no substituent, R3 represents hydrogen or a methyl group, while R4 represents dimethylpyrazole, methylpyrazole, dimethylimidazo[l,2-a]pyrimidine, or isopropoxybenzene, substituted accordingly. The compounds that are the subject of the invention are obtained through reductive amination using borohydride derivatives as the reducing agent, advantageously sodium triacetoxyborohydride, in the amount of 1.4-2.0 eq, amine in the amount of 1.0-1.1 eq, advantageously in slight excess, base, advantageously triethylamine in the amount of 1.0-1.1 eq (in the case of using amine in the form of hydrochloride), and the starting aldehyde. The reaction is conducted in a nonpolar solvent environment, advantageously dichloroethane at a concentration of about 0.1 M. The crude product is purified by column chromatography on silica gel using a methanol in dichloromethane mixture as the eluent, in concentration ranges from 2% to 5%. In order to obtain a solid form and improve the physicochemical parameters, the free bases are converted into hydrochloride form, and then crystallized from a polar solvent, advantageously ethanol or propanol.
Owner:UNIWERSYTET MEDYCZNY W LUBLINIE

Macroporous cation exchange resin and method of making and using same

A macroporous cation exchange resin and its preparation and application method are disclosed. The method involves dispersing polystyrene-divinylbenzene microspheres in dichloroethane to obtain a microsphere suspension. A sulfonating agent, a mixture of fuming sulfuric acid and chlorosulfonic acid, is then slowly added dropwise under cooling and stirring conditions. After the addition is complete, heating is initiated to trigger a polysulfonation reaction. Once the reaction is complete, the reaction mixture is slowly poured into ice water and continuously stirred and diluted until the solution pH reaches 2.5. The solution is then filtered, washed, and dried to obtain a solid resin. This invention simultaneously introduces a matched number of sulfonic acid groups and sulfone groups onto the polystyrene-divinylbenzene backbone. Utilizing the electron-withdrawing effect of the sulfone groups and the rigid framework they form, the stability of the C-H and C-S bonds in the resin is enhanced. This solves the problems of resin structure damage, rapid decline in separation performance, and significantly shortened service life associated with existing cation exchange resins used in treating chromium plating aging solutions.
Owner:SHANGHAI JIAOTONG UNIV

Distillation and purification device for pesticide precursor production

The utility model discloses a distillation and purification device for pesticide precursor production, which relates to the technical field of distillation and purification and comprises a distillation kettle, a circular cover body is arranged at the top end of the distillation kettle, a heating component sleeved on the outer side of the distillation kettle is fixedly connected to the bottom end of the circular cover body, and a mixing component is arranged in the middle of the top end of the circular cover body in a penetrating manner. A vacuum pump penetrates through one side of the top end of the circular cover body, a condensation assembly penetrates through the other side of the top end of the circular cover body, a mother liquor recovery tank is arranged at the bottom end of the condensation assembly, a water injection port penetrates through one side of the mother liquor recovery tank, a backflow assembly penetrates through the bottom end of the mother liquor recovery tank, and a material transferring pipe is arranged at one end of the backflow assembly. One end of the material transfer pipe penetrates through the heating assembly and is connected with the distillation kettle. The dichloroethane distillation kettle is reasonable and reliable in structure, the heat exchange area is greatly increased through the double-layer jacket design, the uniform distribution of the temperature in the distillation kettle is ensured, and the distillation effect of dichloroethane and low-boiling-point organic matters is improved.
Owner:XINJI ALPHA BIOTECHNOLOGY CO LTD

Synthetic method of isoxazoline compound

The invention belongs to the technical field of organic synthesis, and particularly relates to a synthesis method of an isoxazoline compound. The preparation method comprises the following steps: dissolving a compound 1 and ethyl acrylate in dichloroethane, then adding tert-butyl nitrite, alkali and K2S2O8, in an air environment, irradiating with a 35 W blue LED light source and stirring at room temperature for 12 hours, after the reaction is completed, reducing pressure to remove a solvent, and then performing silica gel column chromatography on a crude product to obtain a product, namely the isoxazoline compound. The synthesis method provided by the invention avoids the problem of residue of a traditional metal catalyst, and provides a new normal form for green synthesis of the isoxazoline compound. As a key intermediate, isoxazoline can derive beta-lactam, beta-amino alcohol and other structures, and a new path is provided for complex molecule synthesis.
Owner:GUANGDONG UNIV OF PETROCHEMICAL TECH +1

A process for the preparation of 1-(2-aminoethyl)pyrrolidine

The application discloses a preparation method of 1-(2-aminoethyl) pyrrolidine and belongs to the field of chemical synthesis. The application provides a novel synthesis method of 1-(2-aminoethyl) pyrrolidine, which is prepared from 1,2-dichloroethane and pyrrolidine as raw materials, addition of a solvent and alkali, heating reaction, extraction, acidification and reduced-pressure distillation after the reaction is finished to obtain N-(2-chloroethyl) pyrrolidine solution; N-(2-chloroethyl) pyrrolidine and ammonia water are used as raw materials, high-pressure heating reaction is carried out, extraction and reduced-pressure distillation are carried out after the reaction is finished to generate 1-(2-aminoethyl) pyrrolidine. The application has the advantages of simple operation process, green process synthesis, convenient product purification and high product purity.
Owner:UNIV OF JINAN

Method for preparing vinyl chloride through electro-catalysis of 1, 2-dichloroethane

The invention discloses a method for preparing vinyl chloride by electrocatalytic dechlorination of 1, 2-dichloroethane, a working electrode of the method takes a metal oxide as a catalyst, and the metal oxide is selected from at least one of the following metal oxides: Pd, Mn, Fe, Co, Ni, Cu, Ru and Mo. According to the invention, the metal oxide powder is used as the electrocatalyst, the catalyst is coated on the electrode material to prepare the working electrode, the working electrode is applied to electrocatalytic dechlorination reaction of 1, 2-dichloroethane, vinyl chloride can be generated at high selectivity at room temperature, a new way is opened up for production of vinyl chloride by electrocatalytic dechlorination, and the method has wide application prospect. And a green and low-cost solution is provided for efficient synthesis of vinyl chloride.
Owner:ZHEJIANG UNIV OF TECH

Amino-modified hypercrosslinked resin as well as preparation method and application thereof

The invention discloses amido-modified hypercrosslinked resin, a preparation method thereof and application of the amido-modified hypercrosslinked resin to adsorption of chlorine-containing VOCs (Volatile Organic Compounds). The preparation method comprises the following steps: chloromethylation: swelling hypercrosslinked NDA-88 resin in 1, 2-dichloroethane, adding anhydrous FeCl3 as a catalyst, and carrying out chloromethylation reaction at 35-40 DEG C to obtain chloromethylated resin; and amination: mixing the chloromethylated resin with an amination reagent diethylenetriamine, carrying out amination reaction at 140-150 DEG C, and carrying out post-treatment to obtain the amino modified hypercrosslinked resin. The amino-modified hypercrosslinked resin has high adsorption capacity and long penetration time for chlorine-containing VOCs (Volatile Organic Compounds) such as dichloromethane, chlorobenzene and the like, is stable in performance under the relative humidity of 50%, and is small in adsorption performance attenuation after multiple times of thermal regeneration. The resin is simple in preparation method, excellent in performance and suitable for efficient purification treatment of industrial chlorine-containing VOCs waste gas.
Owner:ENVIRONMENTAL SCI RES & DESIGN INST OF ZHEJIANG PROVINCE