1261 results about "Fine chemical" patented technology

The invention relates to the technical field of automation, in particular to an automatic monitoring and optimizing system for a fine chemical production process, which comprises the following steps of: extracting time-frequency domain fusion characteristic quantity of stirring torque power time sequence fluctuation data in real time through an incidence matrix construction module, dynamically inverting a thixotropic index by combining a deep neural network model, and optimizing the stirring torque power time sequence fluctuation data; the problem that a traditional method is difficult to perceive material rheological characteristics in real time is solved. The dynamic coupling analysis module analyzes the material viscosity change rate based on the thixotropic index, fuzzy PID control is adopted to generate a stirring speed adjusting instruction dynamically matched with the viscosity and a jacket temperature compensation value, and the defects of uneven mixing and local overheating caused by lagging adjustment of process parameters are overcome; the multi-target collaborative optimization module locks the mass optimization weight in the viscosity sudden change stage, rapidly stabilizes the reaction condition through a feed-forward compensation algorithm, dynamically balances the stirring power consumption and the heat transfer efficiency based on Pareto frontier search in the steady state stage, and solves the conflict between the mass and the energy efficiency target.

The invention relates to the technical field of reaction kettle temperature control, and discloses a fine chemical engineering reaction kettle temperature intelligent control method based on self-adaptive search, which comprises the following steps: S1, data acquisition: acquiring operation data of a reaction kettle, including temperature in the kettle, jacket inlet and outlet temperature, fluid flow and valve opening signals; s2, heat balance calculation: establishing a heat balance equation based on the collected data, and calculating reaction heat release and an equivalent heat transfer coefficient; s3, updating the model; s4, predictive control solution is carried out; s5, performing adaptive search; s6, carrying out security constraint; s7, stage identification; and S8, performing control execution. The reaction heat release amount and the equivalent heat transfer coefficient are calculated in real time through linkage of a heat balance calculation module and a model updating module, online parameter identification is achieved through a recursive least square algorithm, a heat model can be dynamically corrected along with working condition changes, it is ensured that a prediction model is consistent with the actual reaction process, and the prediction efficiency is improved. And the temperature prediction precision and the reliability of control response are obviously improved.

The invention discloses a preparation method and application of a bio-based zinc adenine salt environment-friendly PVC heat stabilizer, and belongs to the field of fine chemical synthesis and plastic additive application. The nitrogen-containing organic metal heat stabilizer adenine zinc complex is prepared by taking adenine and zinc acetate as main raw materials through a one-step method. The method is simple and environment-friendly in preparation process, easily available in raw materials and suitable for industrial production. The prepared heat stabilizer zinc adenine is used as a heat stabilizer, can effectively absorb hydrogen chloride generated by PVC thermal decomposition, and can replace allyl chlorine atoms, so that the heat stability of a PVC product is improved, PVC has more excellent heat stability, and the heat stabilizer is expected to replace a traditional commercially available heat stabilizer.

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 discloses a method for preparing cyclohexylamine based on reductive amination of cyclohexanone, and belongs to the technical field of fine chemical engineering. The preparation method comprises the following steps: adding a reactant cyclohexanone into a reaction kettle containing a certain amount of solvent, ammonia water and hydrogen atmosphere, and carrying out reductive amination reaction in the presence of a catalyst to obtain cyclohexylamine. The catalyst is CoyAl-LDHs loaded with metal active components, the CoyAl-LDHs are layered cobalt-aluminum bimetal hydroxides, and cobalt ions and precious metal ions in laminates are subjected to spontaneous oxidation-reduction reaction, so that the precious metal ions can be efficiently reduced into active metal nanoparticles. The layered cobalt-aluminum double-metal hydroxide not only has abundant surface acid-base sites, but also has high dispersity of loaded metal nanoparticles. The catalyst preparation and reductive amination reaction conditions are mild, the yield is high, the reaction system is simple and easy to separate, and the method is suitable for industrial production of cyclohexylamine.

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 a mechanical force-induced fluorescence discoloration sensor material as well as a preparation method and application thereof, and relates to the technical field of organic synthesis and fine chemical engineering. The preparation method comprises the following steps: step 1, carrying out heating reaction on 4-(1, 2, 2-triphenyl vinyl) benzaldehyde, 3-(2, 2-dicyano-1-(3, 4-diaminophenyl) vinyl) benzene-1-yl and a catalyst to prepare a compound 1-1; and 2, carrying out heating reaction on the obtained compound 1-1 and methyl iodide under the action of alkali and a solvent, and analyzing and purifying to obtain a compound 1-2. The compound disclosed by the invention is low in preparation cost, simple and convenient to operate and simple in method, the compound shows the material characteristic of mechanical force-induced fluorescence discoloration and can be applied to the fields of sensors, dyes, anti-counterfeiting and the like, and meanwhile, the synthesis method can be used for synthesis in the fields of fine organic chemical engineering such as luminescent materials, printing and dyeing technologies and the like.

The invention discloses a fine chemical engineering adaptive control optimization system based on digital twinning, and belongs to the field of chemical engineering control. Comprising an acquisition processing module, a process twinning module, a fusion calibration module, a sensing prediction module, a decision optimization module, an execution optimization module, a simulation verification module, a causal diagnosis module, a self-healing control module and a tracking monitoring module. According to the method, adaptive updating and high-fidelity prediction of the model are realized, the deviation of the traditional mechanism model is effectively reduced, the system has the capability of identifying abnormity and risk in advance, the intelligent level of control decision is improved, process disturbance can be responded in real time, operation parameters can be rapidly adjusted, and the stability and robustness of the production process are improved.

The invention discloses a microfluidic nitration reaction platform based on in-situ Raman and a reaction optimization method. The platform integrates a microreactor, an in-situ Raman detection module, a spectrogram processing and quantifying module, an experimental optimization module and a central control module, and is suitable for monitoring and optimizing complex reactions under a non-mutual solution phase plunger flow system. According to the method, an indirect hard modeling (IHM) method is used for processing an overlapped Raman spectrogram, a standard curve is combined for establishing a multi-component concentration prediction model, and high-precision quantification of reactants and products is realized. According to the platform, a Gaussian process model is combined with dynamics prior, a multi-target Bayesian optimization process based on expected hypervolume improvement (EHVI) is driven, and Pareto optimal conditions in a temperature and residence time space are effectively explored. The system has the functions of automatic focusing sampling, spectrogram real-time decoupling, concentration inversion and experimental condition decision making, and is suitable for intelligent reaction development and optimization in the fields of fine chemical engineering, high-throughput reaction screening and the like.

The invention discloses a boron-containing copper-based three-dimensional metal organic framework material as well as a preparation method and application thereof, and belongs to the technical field of fine chemical engineering. The preparation method comprises the following steps: preparing Zn-based MBON from zinc salt, boric acid and imidazole through a hydrothermal method, and then completely replacing the zinc component with copper to obtain Cu-based MBON, namely the boron-containing copper-based three-dimensional metal organic framework material. The specific surface area of the material is large, and a three-dimensional nano flower-shaped unique structure is formed. The prepared material is used as a catalyst for furfural electro-hydrogenation and carbon dioxide reduction reaction, the diffusion efficiency of reactants (such as furfural and CO2) can be enhanced, rapid desorption of products (such as furfuryl alcohol and ethylene) can be promoted through the surface capillary action, meanwhile, generation of by-products caused by excessive reaction is inhibited, and the selectivity of target products is improved.

The invention relates to the technical field of purification of fine chemical intermediates, in particular to a purification method of a mannitol carbonate sulfate preparation process intermediate, which comprises the following steps: S1, synthesizing diacetone-D-mannitol; s2, preparing an organic solution containing solids; s3, performing deprotection reaction to prepare a solid crude product; s4, removing unreacted solids; s5, extracting and separating by-product solids; and S6, purifying the target product solid and recovering mannitol. Through system separation and multi-component recovery, preparation of a high-purity product and cyclic utilization of unreacted substances, byproducts and raw materials are realized, the yield is remarkably improved, the cost is reduced, and the quality of a final product is guaranteed.

The invention belongs to the technical field of fine chemical engineering, and particularly discloses a method for preparing a broad-spectrum bactericide 2-n-butylbenzo [d] isothiazole-3 (2H)-ketone by a molecular editing method. The preparation method comprises the following specific steps: taking 3H-1, 2-benzodisulfophenol-3-ketone and n-butylamine as raw materials, taking Selectfluor as an additive, adding the raw materials and the additive into a mixed solvent, and carrying out heating and stirring reaction, so as to obtain the target product 2-n-butylbenzo [d] isothiazole-3 (2H)-ketone (BBIT). The method is simple and convenient to operate, the raw materials are easy to obtain, the yield is high, thiophenol raw materials or excessive alkali are prevented from being used, and potential application value is achieved.

The utility model discloses an automatic pressure relief device of a reaction kettle, and belongs to the field of fine chemical engineering. The automatic pressure relief device of the reaction kettle comprises a connecting nozzle arranged on a reaction kettle body, and further comprises a pressure relief pipe fixedly arranged on the connecting nozzle, the top cover is arranged at the top of the pressure relief pipe; the multiple groups of exhaust holes are circumferentially formed in the pressure relief pipe at equal intervals; the top plate is arranged in the pressure relief pipe; the sliding rod is arranged on the top plate in a sliding manner; the pressure relief groove is formed in the connecting nozzle; the sealing head is fixedly arranged on the sliding rod, and the sealing head corresponds to the pressure relief groove; the spring is fixedly arranged between the sealing head and the top plate; the reaction kettle disclosed by the utility model can be used for effectively preventing a worker from being influenced by over-high speed of gas leaked from the reaction kettle body, and can be used for adjusting a pressure balance value in the reaction kettle body.

The present application relates to the field of fine chemical industry, and particularly to a preparation method of sodium tetrafluoroborate; the present application uses hydrofluoric acid, boric acid and soda to prepare sodium tetrafluoroborate; the present application uses evaporation, polar organic solvent dissolution, separation, modified polytetrafluoroethylene membrane fine filter filtration, cooling crystallization and the like to purify sodium tetrafluoroborate; the present application uses a polytetrafluoroethylene membrane filter core, vinyl guanidine, sodium acrylate, 1-allyl-3-ethyl imidazole tetrafluoroborate, an initiator and deionized water to prepare a modified polytetrafluoroethylene membrane filter core; the modified polytetrafluoroethylene membrane filter core prepared by the present application can effectively improve the purity of sodium tetrafluoroborate; the present application has the characteristics of low cost, simple process, low toxicity and environmental friendliness; the present application has mild reaction conditions in the preparation process, is easy to operate, has low energy consumption and high product purity.

The invention discloses a double-morphology boron-containing Zn / Cu metal organic framework composite material as well as preparation and application thereof, and belongs to the technical field of fine chemical engineering. The double-morphology boron-containing Zn / Cu metal organic framework composite material is prepared through a one-pot hydrothermal reaction, and the double morphology comprises a three-dimensional nanoflower structure and a three-dimensional rod / columnar structure. Specifically, by adjusting the molar ratio of Zn to Cu in the coordination process with corresponding ligands, when the molar ratio of Zn to Cu reaches 1: 1, the original single nanoflower structure can generate a new three-dimensional rod / columnar structure, so that two composite forms are formed. The double-morphology boron-containing Zn / Cu metal organic framework composite material shows high activity and high selectivity when being used for two key reactions of electrochemical hydrogenation reduction and electrochemical oxidation of furfural.

The invention discloses a difunctional electrocatalyst for carbon dioxide reduction and PET plastic oxidation and a preparation method and application of the difunctional electrocatalyst, and belongs to the field of application of electrocatalytic materials. The preparation method comprises the following steps: precipitating copper chloride and sodium hydroxide to obtain a precursor of copper hydroxide, and freeze-drying, washing and drying the precursor. The problem that the voltage required by the anode reaction is large when carbon dioxide is electrolyzed is solved. And meanwhile, the material has the advantages of excellent negative and positive electrode bifunctional activity and simultaneous generation of chemicals with high added value at the two electrodes, and has certain commercial application value. Meanwhile, the preparation method is simple, and technical feasibility is provided for large-scale preparation of fine chemicals through carbon dioxide reduction.

The invention belongs to the technical field of fine chemical organic synthesis, and discloses a synthesis method of 1, 3-propane sultone without generation of three wastes. The synthesis method comprises the following steps: by taking allyl alcohol, sulfite and hydrosulfite as raw materials, generating 3-hydroxy propanesulfonate; then removing part of water, adding a solvent A to separate out sulfite, filtering, and adding sulfuric acid into filtrate for acidification; and adding a solvent B to separate out sulfate, filtering and separating out the sulfate, and adding a dehydrating agent to carry out dehydration cyclization reaction to prepare the 1, 3-propane sultone. According to the synthesis method provided by the invention, a 1, 3-propane sultone product with the yield not lower than 95% and the purity reaching 99.9% or above and a sulfate byproduct with the purity reaching 99.6% or above can be obtained; no waste gas, waste solid or waste water is generated in the reaction process, the catalyst sulfite can be repeatedly used, and the used solvent is easy to recover and can be repeatedly used.

The invention provides a catalytic material, a preparation method thereof and application of the catalytic material in high-purity ethyl aliphatic amine, and belongs to the technical field of fine chemical engineering. The catalytic material provided by the invention has a porous structure, so that the specific surface area of the catalytic material can be remarkably increased, more active sites can be used for contact between reaction raw materials and a catalyst, the reaction process is accelerated, meanwhile, the retention time of the reaction raw materials on the surface of the catalyst is prolonged by the porous structure, and the conversion rate of the reaction raw materials (liquid ammonia) is further improved; active components are loaded on the surface of the AB2O4 type porous composite transition metal oxide, so that the number of active sites can be further increased, and the conversion rate of liquid ammonia is further improved. Results of the embodiment show that when the catalytic material provided by the invention is used for preparing ethyl aliphatic amine by an ethanol catalytic amination method, the conversion rate of liquid ammonia is 95% or above.

The invention belongs to the technical field of fine chemical engineering, and discloses hydroxypropyl crosslinked starch as well as a preparation method and application thereof. The preparation method of the hydroxypropyl crosslinked starch comprises the following steps: mixing starch and water to prepare starch milk; adding sodium phytate and urea; adding sodium sulfate and sodium hydroxide after cooling; adding epoxypropane for reaction; and adding sodium trimetaphosphate to react to prepare the hydroxypropyl crosslinked starch. The hydroxypropyl crosslinked starch prepared by the preparation method disclosed by the invention has excellent shear resistance, acid resistance and oxidation resistance.

The invention provides a chemical industry-oriented multi-scale multi-dimensional intelligent production scheduling method and system, and the method comprises the steps: obtaining various production scheduling related data based on a factory model, a production management system, an inventory management system, a sales management system and an equipment management system which are established in advance; performing production scheduling according to the various production scheduling related data, a predetermined production quantity standard and gross profit data of different products, and determining a production plan of a target time granularity; and carrying out production according to the production plan, obtaining order insertion data and / or production abnormal information in real time, and updating the production plan. At least efficient, collaborative and benefit-maximized production scheduling can be realized, multi-objective optimization, dynamic order insertion, multi-system data integration and real-time collaboration are supported, and the actual demand of the fine chemical industry field for efficient production scheduling is met.

The present invention discloses a pyridone azo dye and a preparation method thereof, belonging to the field of fine chemical technology. The general structural formula of the pyridone azo dye is as follows: wherein X1, X2, X3, X4, and X5 are each independently selected from one of nitro, hydrogen, fluorine, chlorine, bromine, cyano, and substituted or unsubstituted phenyl; the R substituent is selected from one of the following structures: By introducing an R substituent at the N position of pyridone, the problem of low solubility of pyridone azo dye in organic solvents can be effectively solved. The solubility of the pyridone azo dye disclosed in the present invention in organic solvents is between 5-9 g / 100 mL, and the molar absorption coefficient of this type of dye is between 20,000-120,000 L·mol ‑1 cm ‑1 It has excellent light and heat stability within the range and is feasible for preparing optical devices and full-color high-stable display materials.

The invention belongs to the field of fine chemical engineering, and discloses a method for synthesizing 2, 3-dimethyl-2-isopropyl butyronitrile, which comprises the following steps of: adding an organic amine solvent into a high-pressure reaction kettle, adding sodium amide, sodium iodide and a phase transfer catalyst into the reaction kettle under the protection of nitrogen and in a stirring state, stirring for a certain period of time, and reacting for 2-3 hours to obtain 2, 3-dimethyl-2-isopropyl butyronitrile. Dropwise adding a mixed solution of propionitrile and 2-bromopropane into the reactor, controlling the dropwise adding speed and the reaction temperature, continuously reacting for a period of time after the dropwise adding is finished to obtain a reactant solution, cooling the reactant solution, adding water, standing for layering, collecting an organic phase, distilling the organic phase at normal pressure to recover a solvent, and rectifying at reduced pressure to obtain 2, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3, 5-trimethyl-1, 3-pentanediol. According to the method, the sodium iodide, the phase transfer catalyst and the organic amine have a synergistic effect, so that the reaction time is shortened, and the yield of the product is improved.

The invention belongs to the technical field of fine chemical engineering, and discloses a synthesis method of a malonate compound, which comprises the following steps: under the action of a heterogeneous catalyst, carrying out hydrolysis-esterification reaction on cyanoacetic acid and alcohol, and after the reaction is finished, carrying out post-treatment to obtain the malonate compound, the heterogeneous catalyst comprises a carrier and an active component; the active component comprises ionic liquid and active metal; the carrier is an ordered mesoporous material; the active metal is alkaline earth metal. According to the method, malonate products can be obtained, the problems of low yield, serious equipment corrosion and large amount of three wastes are solved, efficient synthesis of malonate compounds is realized, meanwhile, the production efficiency is improved, and the environmental pollution is greatly reduced.

The invention relates to the technical field of fine chemical engineering, and discloses a fuel cell cooling liquid and a preparation method thereof, and the preparation method comprises the following steps: preparation of a basic liquid, construction of a corrosion inhibition system, ion inhibition treatment, addition of a functional auxiliary agent and post-treatment. According to the composite corrosion inhibitor, zinc ions are anchored to gap sites of a silicate framework through the surface loading effect of sodium silicate and nano-zinc oxide under the shear dispersion condition, a compact composite passivation film is formed on the surface of a metal pipeline, and an electrode potential active area is covered; meanwhile, molybdate ions are subjected to a self-repairing reaction at the defect position of a passivation film preferentially by virtue of the oxidation-reduction characteristic of the molybdate ions, and formation of a galvanic corrosion microbattery is blocked by dynamically filling microcracks, so that the integrity of a corrosion inhibition system is improved; all the components of the composite corrosion inhibitor generate a synergistic effect in a specific proportion, so that the cooling liquid can maintain stable corrosion resistance for a long time.

The invention discloses a multi-dimensional data fusion analysis method and system for fine chemical production, and belongs to the technical field of industrial process control, and the method comprises the steps: obtaining multi-source production data, and generating a unified time sequence data set through timestamp alignment and redundant data filtering; extracting multi-scale features and fusing the multi-scale features and the process knowledge parameters into a joint feature vector; calculating a production state score and grade through weighted fuzzy reasoning; predicting a deviation trend of the key parameters based on the score and historical optimal production data; actual sampling data are obtained, deviation comparison is carried out on the actual sampling data and the deviation trend data, and optimization calculation is triggered to generate optimization control parameters; the reaction condition is adjusted through the distributed actuator, and the new data is used for updating the unified time sequence data set. According to the method, state evaluation is carried out by fusing process knowledge and multi-scale features, and deviation trend prediction and closed-loop optimization control are carried out in combination with the state transition probability, so that predictability, stability and adaptive optimization capability of the production process can be improved.

The invention belongs to the field of fine chemical engineering, and discloses a preparation method of halauxifen-methyl, which comprises the following steps: by taking a compound I and a compound II as raw materials and acetonitrile or an acetonitrile-water mixed solution as a reaction solvent, under the protection of nitrogen, taking a palladium catalyst as a catalyst and under the condition that a cocatalyst exists or does not exist, carrying out a reaction on the compound I and the compound II to obtain the halauxifen-methyl. And carrying out Suzuki coupling reaction on the compound I and the compound II to obtain the halauxifen-methyl. The method for preparing the halauxifen-methyl is high in novelty, the product selectivity can be improved by adding the cocatalyst, the product yield is high and at least reaches 80%, and the product purity is high. # imgabs0 #

The invention discloses a fine chemical production gas treatment device, belongs to the technical field of gas treatment devices, and aims to solve the problems that pollutants in waste gas cannot be fully degraded by microorganisms, local areas are unsmooth in ventilation and the waste gas is polluted due to the fact that pores of a biological membrane are easy to drop when the waste gas is treated by a biological agent for a long time. The device comprises a treatment tank and a gas inlet communicated with one side of the lower part of the treatment tank, and when the porosity of gas inlet hole gaps in the lower surface of a first treatment mechanism is reduced due to overgrowth of a biological membrane and deposition of particulate matters, or the flow and pressure of introduced waste gas are suddenly increased, the gas inlet hole gaps in the lower surface of the first treatment mechanism can be subjected to secondary treatment, so that the effective reaction space is reduced, and the ventilation treatment efficiency is improved. The pressure of the first treatment mechanism is shared by the second treatment mechanism, so that the device can automatically adjust ventilation along with the change of air pressure, the degradation capacity is instantly supplemented, and the problems that the stability of the device is damaged, the waste gas treatment effect becomes poor, or the waste gas cannot be treated and is directly discharged to cause pollution are solved.

The present application relates to fine chemicals, and in particular to a method for preparing 2-imidazolidinone by using carbon dioxide. The method comprises reacting CO2 and ethylenediamine in the presence of inorganic sulfide to obtain 2-imidazolidinone. The method uses cheap and readily available sulfur-containing compounds as catalysts for activating CO2 for the first time, and converts ethylenediamine and CO2 into 2-imidazolidinone under relatively low temperature and supercritical conditions. Compared with the prior art, the reaction conditions of the present application are more simple and controllable, and do not require expensive and complex catalysts for post-processing, have the advantages of low energy consumption and low cost, and have extremely high popularization and application value.

The invention relates to the fields of medicine, organic chemical industry and fine chemical industry, in particular to a method for synthesizing 1, 4-diketone by catalyzing alkenyl amide and alpha-carbonyl oxidized sulfonium ylide through photooxidation reduction. The preparation method comprises the following steps: under the protection of inert gas, reacting alkenyl amide and alpha-carbonyl oxidized sulfonium ylide serving as substrates in an organic solvent by taking a photosensitizer as a catalyst under the action of blue light irradiation and alkali at 30 DEG C for 18 hours to obtain an alkenyl amide alpha-carbonyl alkylate, and then hydrolyzing under an acidic condition to synthesize various asymmetric 1, 4-diketone compounds. The 1, 4-diketone compound is synthesized by a two-step method by taking alkenyl amide and alpha-carbonyl oxidized sulfonium ylide as initial raw materials, and the method has the remarkable advantages of wide substrate raw material sources, simplicity and convenience in operation, mild reaction conditions, high reaction efficiency, good universality, excellent functional group compatibility and the like.

Belonging to the technical field of fine chemical product separation and purification, the invention discloses a beta-bromophenylethane rectification purification process, which comprises the steps of system negative pressure pretreatment, falling film evaporation directional separation, structured packing layer gas-liquid mass transfer, precise reflux ratio regulation and control, segmented collection (front fraction-qualified product), and residual liquid treatment and system circulation. According to the process, the negative pressure of a system is stabilized at 800-1200 Pa, the material temperature of a falling film evaporation discharging end is controlled at 125-135 DEG C, the feeding flow is stabilized at 1.8-2.2 m / h, the reflux ratio is regulated and controlled at 0.8: 1-1.2: 1, and the process realizes efficient purification of beta-bromopheny ethane through precise negative pressure control, synergistic linkage of falling film evaporation and a rectifying tower, segmented material collection and a circular treatment mechanism, so that the process is suitable for industrial production of beta-bromopheny ethane. According to the method, the purity of beta-bromopheny ethane can stably reach 99.5% or above, the material recovery rate is increased to 92% or above, energy consumption is reduced by 15-20% compared with that of a traditional process, material thermal decomposition loss is avoided, and the method is suitable for industrial large-scale production.