1081 results about "Side reaction" patented technology

The invention discloses an omariglitazone intermediate as well as a synthesis method and application thereof, and belongs to the technical field of pharmaceutical chemistry synthesis. The invention provides a synthesis method of an omarigliflozin intermediate and application of the intermediate in synthesis of omarigliflozin. The key of the synthesis method provided by the invention lies in the deprotection process of polycyclic indole amide, nitrile groups are not hydrolyzed, indole carboxylic acid is generated with high selectivity, molecular lactamization is avoided in the condensation process with polycyclic imine B, and expensive amidation reagents such as HATU are not needed in the process, so that the synthesis method is simple and easy to implement. And the purpose of preparing omariglitazone with low cost and high yield is achieved. The synthesis method has the advantages of easily available raw materials, mild reaction conditions, small side reaction influence, simplicity and convenience in operation and high yield, improves the yield, is easy to purify, and is suitable for industrial production of omariglitazone.

The invention provides a bio-based 1, 4-butanediol composition as well as a preparation method and application thereof, and the bio-based 1, 4-butanediol composition comprises bio-based 1, 4-butanediol, 4-hydroxybutyric acid-(4-hydroxyl) butyl ester and bis (4-hydroxyl) dibutyl ether. The total mass content of 4-hydroxybutyric acid-(4-hydroxyl) butyl ester and bis (4-hydroxyl) dibutyl ether in the bio-based 1, 4-butanediol composition is 51 to 220 ppm. The bio-based 1, 4-butanediol composition has low hygroscopicity, and can maintain low water content after long-term storage; meanwhile, when the bio-based 1, 4-butanediol composition is used for polyester synthesis, the esterification time can be shortened, the reaction efficiency can be improved, side reactions can be reduced, and a polyester product with better damp-heat resistance stability can be obtained.

The invention relates to the field of fine chemical engineering, and discloses a green process for preparing chloramine T by a continuous flow reactor. The method comprises the following steps: respectively pumping p-toluenesulfonamide, a sodium hydroxide solution and a sodium hypochlorite solution into a micro-channel mixer for instantaneous mixing, and carrying out chlorination reaction in a multi-stage temperature control tubular reaction unit; the concentration of free chlorine is detected on line at an outlet, and the flow rate of a chlorine source is dynamically adjusted through a PID algorithm, so that closed-loop control is realized; the reaction liquid is directly crystallized and separated to obtain the product without alkali wash. The system comprises a base solution and chlorine source conveying subsystem, a micro-channel mixer, a multi-stage reaction unit, an online monitoring module, a central controller and a crystallization unit. The side reaction is inhibited from the source, so that the free chlorine is less than or equal to 0.5 mg / L, the alkali washing step is omitted, the COD (Chemical Oxygen Demand) of the wastewater is reduced by more than 80%, the product purity is more than or equal to 99.5%, and the productivity is improved by 3 times.

The invention relates to the technical field of fine chemical engineering and flame retardant preparation, and discloses a preparation method of bromo-triazine capable of improving thermal stability, and the preparation method comprises the following steps: mixing phenol, water and dichloromethane, controlling the temperature, and carrying out oxidative bromination reaction to prepare an organic phase containing tribromophenol; then, under the action of an organic amine catalyst, carrying out condensation reaction on the organic phase, liquid caustic soda and cyanuric chloride; after the reaction, washing with water to remove impurities; and in the presence of process water, firstly controlling the temperature at 38-42 DEG C for azeotropic desolvation, then raising the temperature to 85-95 DEG C for high-temperature crystallization and crystal growing, and finally cooling, filtering and drying to obtain the bromo-triazine product. By utilizing the high selectivity of the organic amine catalyst and a two-stage azeotropic crystallization process, the side reaction is effectively reduced, the solvent wrapped in the crystal is eliminated, the prepared product is high in main content and extremely low in volatile component, the temperature can reach 370 DEG C or above when the thermal weight loss is 2%, and the thermal stability is remarkably improved.

The invention discloses an internal-acid and external-alkali type organic-inorganic hybrid molecular sieve catalyst as well as a preparation method and application thereof, and belongs to the technical field of heterogeneous catalytic materials and chemical processes. According to the catalyst, a hydrogen type Beta molecular sieve is used as an acidic inner core, polyvinylpyrrolidone (PVP) is used as an organic shell, and a unique inner-acid outer-alkali structure is formed. The preparation method comprises the following steps: hydrothermally synthesizing a hydrogen type Beta molecular sieve with a specific silica-alumina ratio, and then coating PVP through surface adsorption. The catalyst is used for catalyzing the condensation of methylal and trioxymethylene under mild conditions (40-70 DEG C and normal pressure) to prepare polyoxymethylene dimethyl ethers (DMMn). The PVP shell covers acidic sites on the outer surface of the molecular sieve to form an external neutral / weak base and internal strong acid microenvironment, so that the secondary side reaction of the product is effectively inhibited, the trioxymethylene conversion rate of more than 98% and the DMMn selectivity of more than 96% can be obtained in the reaction at 50 DEG C and normal pressure, the product distribution can be regulated and controlled, and the traditional Anderson-Schulz-Flory distribution limitation is broken through. The catalyst disclosed by the invention has the advantages of high activity, high selectivity, mild conditions and easiness in separation, and has a good industrial application prospect.

The synthesis process comprises the following steps: (1) introducing inert gas into a reactor, adding a solvent, a Lewis acid catalyst and diphenyl ether, then dropwise adding an acyl chloride monomer solution, and synthesizing an intermediate M with a short-chain small molecular structure; (2) continuously dropwise adding an acyl chloride monomer solution into the reactor for reaction, and then adding an end-capping reagent for reaction; and (3) quenching, washing and drying the reaction product in the step (2) to obtain the product. Under the condition that only the Lewis acid is used as the catalyst, the one-pot method is adopted for synthesizing PEKK in two steps, side reactions can be reduced, meanwhile, the dosage of the catalyst is reduced, the production cost is reduced, the post-treatment process is simplified, and the obtained polyether ketone ketone is high in molecular weight and good in heat resistance and mechanical performance.

The invention discloses lithium sulfide, a two-step double decomposition preparation method and application of the lithium sulfide in an all-solid-state battery, and belongs to the technical field of solid-state batteries. According to the preparation method, a two-step decomposition synthesis technology is adopted, lithium carbonate and ammonium thiocyanate are used as raw materials, the raw materials are uniformly mixed and then placed in a high-temperature reactor, a step heating sintering procedure is completed in an inert gas atmosphere, and the purpose of fully decomposing and converting the raw materials is achieved by accurately controlling the temperature and the time; after a product is obtained through reaction, the high-purity lithium sulfide material is obtained after the product is cooled to the room temperature. The method for preparing the lithium sulfide is low in raw material cost, simple in reactant formula and free of side reaction in the reaction process, and the finally generated product is few in impurity, high in purity and good in crystallinity.

The invention discloses a copper-based catalyst for preparing acetaldehyde through ethanol dehydrogenation as well as a preparation method and application of the copper-based catalyst. The preparation method comprises the following steps: S1, carrying out alkalization treatment on protic mordenite in a strong alkali solution to increase the number of surface hydroxyl groups of the protic mordenite; and S2, adding the mordenite obtained in the step S1 into a copper salt solution to load copper ions, and then sequentially carrying out low-temperature drying shaping and medium-temperature activation stages to obtain the copper-based catalyst with networked Cu-OH-Si-O bonds on the surface. Through the synergistic effect of alkali liquor regulation and control and staged oxygen roasting, the dispersity and stability of a Cu active center in the catalyst are improved, the acetaldehyde selectivity of the reaction of preparing acetaldehyde through ethanol dehydrogenation is also improved, and side reactions are inhibited. Carrying out heat treatment regeneration on the inactivated copper-based catalyst in an oxygen-containing atmosphere; and after regeneration, the networked Cu-OH-Si-O bond on the surface of the copper-based catalyst is reconstructed.

The invention discloses a pyridine quaternized cellulose derivative and a preparation method thereof, and belongs to the field of modified cellulose derivatives. According to the method, sodium carboxymethyl cellulose is taken as a raw material, and a target product is prepared through a three-step method of epoxy group grafting, sulfydryl-epoxy click chemical reaction and pyridine quaternization reaction in sequence. According to the method, the high efficiency of click chemistry and the modular design concept are innovatively introduced into the field of cellulose derivative modification, the problems that a traditional quaternization method is uncontrollable in substitution degree, many in side reaction and poor in molecular design flexibility are solved, and the method has the advantages of being mild in reaction condition, high in efficiency and clear in product structure.

The invention discloses a preparation method of a sulfonic acid type covalent organic framework material and a preparation method of 5-hydroxymethylfurfural. The material is prepared by carrying out covalent condensation reaction on a monomer containing a sulfonic acid group precursor and a connecting ligand of a skeleton through a hot solvent method, and the catalyst has the characteristics of high crystallinity, large specific surface area, ordered pore structure, high sulfonic acid group density and uniform distribution. The preparation method is simple, convenient, efficient, mild in condition and high in yield. Compared with a traditional lewis acid catalyst for preparing 5-hydroxymethylfurfural through fructose dehydration, the material has the advantages of being uniform and adjustable in porosity, higher in active site, capable of promoting fructose hydrolysis and the like, efficient conversion can be achieved, side reactions and product transition polymerization are inhibited, and better industrialization prospects are shown.

A non-aqueous electrolyte comprises a lithium salt, an organic solvent, and an additive, wherein the additive includes a compounds represented by Formula 1, and such non-aqueous electrolyte may be capable of suppressing the degradation of the positive electrode, reducing side reactions between the positive electrode and the electrolyte, and forming a stable SEI film on the negative electrode, thereby improving high-temperature cycle properties and high-temperature storage properties:wherein all the variables are described herein.

The application provides a synthesis method of p-benzoquinone dioxime. The synthesis method comprises the following steps: (1) adding solid acid into an ethanol solution of phenol to obtain a mixed solution A, then vacuumizing and filling with inert gas; dissolving nitrite into ethanol, uniformly mixing to obtain an ethanol solution of nitrite, then vacuumizing and filling with inert gas; in an inert gas atmosphere, adding the ethanol solution of nitrite into the mixed solution A dropwise to perform nitrosation reaction, to obtain a reaction liquid B; in the inert gas atmosphere, adding an ethanol solution of hydroxylamine into the obtained reaction liquid B to perform oximation reaction; after the reaction is completed, filtering the obtained reaction liquid C, performing reduced pressure distillation on the obtained filtrate, and performing washing, filtering and drying on the obtained residual liquid of the reduced pressure distillation, to obtain p-benzoquinone dioxime. The method provided by the application reduces the occurrence of side reactions, improves the conversion rate of the reaction, and improves the yield and purity of p-benzoquinone dioxime.

The invention discloses a preparation method and application of a betaine-induced branch structure CoFe-based catalyst, and relates to a preparation method and application of a CoFe-based catalyst. The technical problem that an existing CoFe-based catalyst is poor in activity and stability is solved. The preparation method of the betaine-induced branched structure CoFe-based catalyst comprises the following steps: immersing clean foamed nickel into an isopropanol-water heterogeneous solution containing Co < 2 + > and Fe < 2 + > for in-situ growth, then introducing betaine to induce to form a branched structure, and anchoring an acidic group on the surface of a CoFe matrix to enhance the structural stability; the alkaline group faces an electrolyte interface under the action of an electric field, regulates interface charge distribution, selectively adsorbs part of Cl <-> and repels the other part of Cl <-> at the interface, so that chlorine evolution side reaction is inhibited. When the industrial-grade current density is 500 mA cm <-2 > during seawater hydrogen production, only 280 mV overpotential is needed, and stable operation can be carried out for more than 1000 h. The method can be used in the seawater hydrogen production field.

The invention discloses a method and system for continuously synthesizing 2, 4-dichloroacetophenone, and the method for continuously synthesizing 2, 4-dichloroacetophenone comprises the following steps: S1, mixing m-dichlorobenzene and a catalyst to form a turbid liquid, and continuously inputting the turbid liquid into a tubular reactor; s2, enabling gas-phase acetyl chloride to pass through a micro-interface generator to form micron-sized microbubbles, continuously inputting the micron-sized microbubbles into a tubular reactor, and carrying out mixed reaction on the micron-sized microbubbles and the turbid liquid to obtain a mixed reaction liquid; and S3, continuously inputting the mixed reaction liquid and water into a hydrolysis reactor, and carrying out hydrolysis and separation to obtain 2, 4-dichloroacetophenone. According to the invention, the traditional kettle type stirring reaction is changed into micro-interface reaction, and the mass transfer area and the total mass transfer rate among multiple phases can be multiplied, so that the reaction rate is greatly improved, the side reaction is effectively controlled, and meanwhile, the product yield, the reaction safety and the like are improved.

This invention provides a method for preparing dibenzoyl-p-benzoquinone dioxime using a microchannel reactor. The method includes the following steps: 1,3-dicyclohexylcarbodiimide and a catalyst are mixed uniformly and preheated to obtain a premix; a chloroform solution of p-benzoquinone dioxime, a chloroform solution of benzoic acid, and the premix are simultaneously introduced into the microchannel reactor for reaction; the resulting reaction solution is subjected to vacuum distillation, washing, filtration, and drying to obtain dibenzoyl-p-benzoquinone dioxime. The synthesis method of this invention features high reaction conversion rate, high production efficiency, few side reactions, and high safety. The obtained dibenzoyl-p-benzoquinone dioxime product has stable quality. Furthermore, the organic solvent used can be recovered and reused after vacuum distillation, overcoming the problems of inaccurate temperature control, poor safety, numerous side reactions, and difficult waste treatment in traditional processes. This provides a new approach for the synthesis of dibenzoyl-p-benzoquinone dioxime.

A method for preparing ethylbenzene by using nanosheet molecular sieve as catalyst, the hydrogen type nanosheet molecular sieve is broken and loaded into a fixed bed reactor, benzene and ethanol are used as raw materials, nitrogen is used as carrier gas, the reaction is carried out at 280-350 DEG C and 0.1-1.0 MPa; the hydrogen type nanosheet molecular sieve is ZSM-5 molecular sieve, the length of b axis direction is 70-100 nm, the length ratio L b / L a is less than 0.40. The method for preparing ethylbenzene provided by the application can be directly used for catalyzing ethanol and benzene to prepare ethylbenzene without secondary treatment such as modification of acid, alkali and alkali metal and rare earth metal elements based on the special structure of the nanosheet molecular sieve with ultra-short b axis, can ensure that the product is desorbed and diffused from the surface of the catalyst in time, reduces the probability of deep reaction of the product molecules, realizes high selectivity of the product ethylbenzene, and reduces the cracking and other side reactions.

The application discloses a catalyst for preparing methylaniline and a preparation method and application thereof, and belongs to the technical field of catalysts. The catalyst is prepared by modifying an activated carbon carrier with zirconium, cerium or nickel, treating the carrier with high-temperature nitrogen, loading active components Pd and pH-responsive polymers, solving the problems of low dispersion of the active components, easy poisoning and activity attenuation, and having good pH responsiveness and environmental adaptability. The preparation method optimizes a carrier modification process, adopts an impregnation method combined with timed stirring, controls reaction parameters, improves catalyst performance, realizes high selectivity and high yield of methylaniline, and has the advantages of high selectivity of the catalyst for methylaniline, inhibition of side reactions, adoption of a fixed bed reactor, simplification of operation, reduction of safety hazards, efficient reaction at a lower reaction temperature and pressure, and reduction of energy consumption and production cost.

This invention provides a composite catalyst, its preparation method, and its application, as well as a method for the catalytic oxidation of alcohols to aldehydes, belonging to the field of organic synthesis technology. In the composite catalyst provided by this invention, elemental chromium improves the dispersibility of elemental silver on modified γ-Al₂O₃, thereby enhancing the oxidation activity of the composite catalyst for ethanol, reducing side reactions (further oxidation of aldehydes to acids or decomposition) during the catalytic oxidation of alcohols to aldehydes, and improving the selectivity, yield, and purity of aldehydes. The modified γ-Al₂O₃ has a more developed pore structure than uncalcined γ-Al₂O₃, and when used as a support, it improves the mechanical strength of the composite catalyst. Moreover, the composite catalyst provided by this invention reduces the reaction temperature and energy consumption for the catalytic oxidation of alcohols to aldehydes without affecting the alcohol conversion rate and aldehyde selectivity, thus reducing the cost of aldehyde preparation and making it more suitable for industrial use in the catalytic oxidation of alcohols to aldehydes.

The invention belongs to the technical field of preparation of tetraisopropyl alcohol-based ethylenediamine, and particularly relates to a catalyst for preparing tetraisopropyl alcohol-based ethylenediamine as well as a preparation method and application of the catalyst. The catalyst is formed by chelating two amine nitrogen atoms with aluminum ions by taking an Al < 3 + > center as tetra-coordination and 1, 1-dimethoxytrimethylamine as a ligand, and has a structure as shown in a formula I in the specification. The two-component composite catalyst is formed on the basis of coordination and chelation of the organic metal compound and the organic amine, the organic metal compound can promote the antistatic performance of the tetraisopropyl alcohol ethylenediamine, and the organic amine can promote the compatibility of the tetraisopropyl alcohol ethylenediamine and a high polymer material, so that the antistatic property of the tetraisopropyl alcohol ethylenediamine is improved. Compared with a pure organic amine catalyst, the composite catalyst has the advantages of high reaction activity, side reaction inhibition, improvement of the conversion rate and selectivity of tetraisopropanolethylenediamine, no need of separation from the product, promotion of the product, reduction of the impurity separation problem in the subsequent process, reduction of the reaction pressure, low equipment requirement and reduction of the equipment investment.

This invention discloses a supported zirconium-based catalyst, its preparation method, and its application. It includes a zirconium-based support and a noble metal supported on the zirconium-based support. The zirconium-based support includes one or more of a zirconium-based composite oxide support and a zirconium-based metal-organic framework material. The zirconium-based composite oxide support includes a composite of zirconium oxide and other oxides, and the other oxides include oxides of one or more elements selected from Si, P, Ce, and Mg. The above-mentioned supported zirconium-based catalyst increases the interaction between the supported noble metal and the support by introducing Si, P, Ce, or Mg into the zirconium-based support to adjust the electron cloud density or oxygen vacancy concentration of the zirconium-based support. By using a zirconium-based metal-organic framework material with regular channels to support the noble metal, reactants and products can diffuse relatively quickly and smoothly, thereby avoiding excessive side reactions and carbon deposition caused by excessive retention of reaction intermediates or products.

This application relates to a UV-3 ultraviolet absorber and its preparation method, belonging to the field of chemical synthesis technology. The preparation method employs a one-pot process, in which benzocaine reacts with triethyl orthoformate in xylene solvent. This step utilizes reactive distillation coupling control, continuously removing the generated alcohol distillate through a distillation separation device to promote reaction equilibrium shift, obtaining a xylene solution of the intermediate NET. Subsequently, the solution is heated to a reaction temperature of 135–145°C, and benzyl chloride is added dropwise for N-alkylation, while a tail gas absorption device absorbs byproduct gases. The reaction slurry is then cooled for crystallization, solid-liquid separation, and drying to obtain the UV-3 product. This invention simplifies the production process through a one-pot process, avoids the use of toxic DMF solvent, and solves the technical problem of raw material residues leading to subsequent side reactions in the one-pot process through reactive distillation coupling control, resulting in a final product with high purity and high yield.

The invention relates to a method for continuously producing poly (p-dioxanone), which comprises the following steps: premixing glycollic acid or a glycollic acid derivative with a ring formation catalyst, and introducing the obtained mixed material and ethylene oxide into a synthesis reaction kettle for reaction; separating and purifying the obtained reaction product, introducing the obtained purified monomer into a polymerization reaction kettle, and adding a polymerization catalyst for polymerization; after polymerization is finished, discharging is conducted, residual materials in the polymerization reaction kettle are subjected to depolymerization treatment to clean the kettle body, after depolymerization is finished, depolymerization products generated in the depolymerization treatment process are discharged, the kettle does not need to be opened for cleaning, and the next round of polymerization production is directly conducted. According to the method disclosed by the invention, the steps of synthesizing the p-dioxanone monomer, separating and purifying the monomer, catalyzing and polymerizing, depolymerizing and cleaning the kettle body and the like are continuously carried out, so that the continuous production of the poly (p-dioxanone) is realized, the side reaction of oligomerization and degradation of the p-dioxanone in storage and transportation can be avoided, and the production cost of the poly (p-dioxanone) is obviously reduced.

The application relates to the technical field of organic synthesis, and discloses a synthesis method of benzthiazuron, which comprises the following steps: step 1, addition reaction of alpha-methyl styrene and hydrogen chloride gas, and degassing to obtain a first reaction liquid; step 2, substitution reaction of the first reaction liquid and cyanate in the presence of a zinc chloride catalyst, and filtration to obtain a second reaction liquid containing isocyanate; and step 3, construction of an inorganic salt aqueous solution system with a density of 1.05-1.10 g / ml and a pH of 9-10, dropwise addition of the second reaction liquid into the system for condensation reaction with o-chlorobenzylamine, and post-treatment and refinement to obtain a target product. The non-phosgene route of chloro-isocyanate substitution is adopted, and the use of the toxic phosgene is completely avoided; the salting-out effect and interface control generated by the specific high-density salt solution effectively inhibit the isocyanate hydrolysis side reaction, and the reaction yield and product purity are obviously improved.

The invention relates to the technical field of sugar alcohol preparation, and discloses a preparation method of high-purity crystalline maltitol, which comprises the following steps: firstly, by taking corn starch milk as a raw material, preparing ultrahigh-content maltose syrup with the maltose content of more than or equal to 91%, the wheat triose content of less than or equal to 0.4% and the glucose content of less than or equal to 4% through an enzyme conversion method; carrying out hydrogenation reaction on the syrup by adopting a Raney nickel catalyst, and controlling the hydrogenation side reaction to be 2% or below, so as to obtain hydrogenated liquid with maltitol content of more than or equal to 88%; and then, a pigment separation procedure in a traditional process is omitted, and the hydrogenated liquid is directly subjected to decoloration, ion exchange, evaporation concentration, crystallization, centrifugation and drying treatment to finally prepare crystalline maltitol. According to the method, by screening a specific compound enzyme system and finely regulating the pH value and temperature control environment of a saccharification reaction system, the generation of maltose is effectively promoted, and side reactions such as excessive hydrolysis of glucose and reverse synthesis of trisaccharide are inhibited at the same time, so that the high-purity maltose syrup precursor is obtained.

This invention belongs to the field of mineral flotation technology, and discloses a flotation collector for non-ferrous metal sulfide ores, its preparation method, and its application. The collector uses O,O-dialkyldithiophosphate as a starting material, and reacts sequentially with a halocarboxylic acid ester, hydrazine hydrate, potassium hydroxide, and carbon disulfide in anhydrous ethanol in a three-step reaction to obtain the target product, O,O-dialkyldithiophosphate hydrazide-N′-dithiocarbamate potassium. Its molecular structure simultaneously contains three active groups: a dithiophosphate group, an hydrazide group, and a dithiocarbamate group. This invention achieves efficient process connection and smooth transition by optimizing the material ratio, temperature, and time of each reaction step, and has advantages such as mild reaction conditions, simple operation, few side reactions, high yield, and stable product. The prepared collector exhibits excellent collecting performance and good selectivity for non-ferrous metal sulfide ores such as chalcopyrite, and is suitable for widespread application in sulfide ore flotation processes.

The application provides a preparation method of citral. By controlling the content of isopentenoic acid in a citral intermediate composition in the range of 10-2000 ppm, and then performing a thermal rearrangement reaction, citral product is prepared. The method can effectively reduce the selectivity of isomerization side reactions, and the yield of the final product citral is increased to more than 95%.

The present application relates to a kind of preparation methods of 2-methylamino-3-formylpyridine, comprising the following steps: 3-cyanopyridine and dimethyl sulfate are heated to reflux reaction in organic solvent I, then base is added, continue to react under heating reflux condition, and obtain intermediate product 2-methylamino-3-formylpyridine.The raw material used in the preparation method of the present application is cheap and easy to obtain, the preparation process has few side reactions, and is easy to purify.Only the steps of extraction and heavy crystallization are needed to achieve high purity, and strict control of anhydrous reaction conditions is not required.The yield and purity are high, and the prepared 2-methylamino-3-formylpyridine is suitable for industrial large-scale production of 2-methylamino-3-hydroxymethylpyridine, and further preparation of eslicarbazepine acetate and / or eslicarbazepine acetate sulfate.

The invention belongs to the technical field of drug synthesis, and particularly relates to an improved preparation method of a fenerenone intermediate 2-cyanoethyl 4-(4-cyano-2-methoxybenzyl)-2, 8-dimethyl-5-oxo-1, 4, 5, 6-tetrahydro-1, 6-naphthyridine-3-carboxylate, which comprises the following three steps: S1, preparing an intermediate I; s2, preparing an intermediate II; and S3, preparing an intermediate V, namely, the fenerenone intermediate, namely, 2-cyanoethyl 4-(4-cyano-2-methoxybenzyl)-2, 8-dimethyl-5-oxo-1, 4, 5, 6-tetrahydro-1, 6-naphthyridine-3-carboxylate. The preparation method of the fenerenone intermediate comprises the following steps of: 1, preparing an intermediate A, and 2, 4-dimethyl-5-oxo-1, 4, 5, 6-tetrahydro-1, 6-naphthyridine-3-carboxylate. The method has the advantages of short reaction flow and few operation steps, is favorable for improving the production efficiency, effectively reduces the possibility of material loss and side reaction increase caused by tedious steps, reduces the safety risk in the production process, reduces the potential pollution to the environment, also improves the continuity and stability of the production process, and reduces the production cost. The industrial large-scale production is convenient to realize, the large demand of the market on the fenerenone intermediate is met, and the method has a good industrial application prospect.

This invention relates to the field of organic synthesis technology and discloses a method and system for preparing adiponitrile. The method includes: S1: atomizing molten adipic acid and mixing it with ammonia gas, followed by an ammoniation reaction to generate an ammoniation product; S2: dividing the ammoniation product into two parts, a and b. Part a undergoes a countercurrent, non-contact heat exchange with hot material to generate crude adiponitrile through heating and dehydration, while part b is recycled back to step S1 to participate in the reaction. The ratio of the ammoniation product in part a to that in part b is (1~5):1. The temperature of the hot material is higher than the temperature of the ammoniation product in part a. This invention improves the efficiency of the ammoniation reaction, reduces the decomposition side reactions of adipic acid and the residue of adipic acid, and significantly improves the conversion rate of the dehydration reaction and the selectivity of adiponitrile.

The invention relates to a catalytic quasi-solid ionic conductor, a preparation method and application thereof, and an aqueous zinc ion battery, and belongs to the field of aqueous zinc ion battery electrolyte preparation. The preparation method of the catalytic quasi-solid ionic conductor comprises the following steps: mixing ZSM-5 molecular sieve powder with a metal nitrate solution, carrying out a hydrothermal reaction, centrifuging, washing and drying after the reaction is completed to obtain a monatomic-loaded molecular sieve, then preparing the monatomic-loaded molecular sieve into a sheet, dropwise adding a trace amount of electrolyte for infiltration, and drying to obtain the catalytic quasi-solid ionic conductor. The catalytic quasi-solid ionic conductor is obtained. The catalytic quasi-solid ionic conductor has the following advantages: (1) rich monatomic catalytic sites can accelerate iodine conversion, reduce accumulation of polyiodide, and inhibit the shuttle effect through strong adsorption, thereby avoiding capacity fading and cathode corrosion; (2) molecular sieve pore channels can limit the activity of water molecules and inhibit side reactions; (3) zinc ions can be guided to be uniformly deposited, and dendritic crystal growth is inhibited; and (4) the cathode material has good adaptability.