164 results about "Fluoridation reaction" patented technology

The invention provides an ultra-pure thorium fluoride production process which comprises the following steps: preparing a nanoscale ThF4.xNH4F precursor through a gas-liquid-solid three-phase reaction, atomizing an ammonium fluoride solution into microdroplets by adopting ultrasonic atomization, and carrying out synergistic reaction with gaseous ammonium fluoride and a liquid-phase thorium nitrate solution; a microwave-plasma synergistic fluorination reaction is adopted, and the precursor is heated in a high-purity inert atmosphere to generate crude thorium fluoride; according to the ultra-pure thorium fluoride production process provided by the invention, the purity of thorium fluoride is remarkably improved through the technical means of preparation of a nanoscale precursor through a gas-liquid-solid three-phase reaction, microwave-plasma synergistic fluorination, multi-stage sublimation combined with graphene-based nano trapping membrane purification, intelligent process control, by-product closed-loop recovery and the like; the impurity content is low, and the requirements of nuclear reactor fuel substrates and high-end optical coatings on ultra-high purity are met. The method has the advantages of high yield, high process stability and small purity fluctuation among batches, and the production efficiency and the product consistency are obviously improved.

The invention discloses a synthesis method of 2, 4, 5-trifluorophenylacetic acid, which comprises the following steps: by taking cheap and easily available o-chloronitrobenzene as a raw material, reacting with sodium nitrate in a sulfuric acid and trifluoroacetic acid system, separating generated 2, 4-dinitrochlorobenzene through melt crystallization, and continuing to synthesize 2, 4-dinitrochlorobenzene in methyl chloroacetate to obtain 2, 4, 5-trifluorophenylacetic acid. The method comprises the following steps: carrying out indirect aromatic nucleophilic substitution reaction on 2, 4-dinitrophenylacetic acid under the condition of sodium hydride to generate 5-chloro-2, 4-dinitrophenylacetic acid methyl ester, separating, carrying out fluorination reaction on the 5-chloro-2, 4-dinitrophenylacetic acid methyl ester and potassium fluoride under the action of a phase transfer catalyst, carrying out rectification separation to obtain 2, 4, 5-trifluorophenylacetic acid, and carrying out hydrolytic acidification on the 2, 4, 5-trifluorophenylacetic acid in a sodium hydroxide aqueous solution to obtain 2, 4, 5-trifluorophenylacetic acid. And the process route is safer, more environment-friendly, more efficient and lower in cost.

The invention discloses a ternary positive electrode material as well as a preparation method and application thereof, and belongs to the technical field of lithium ion batteries. The method comprises the following steps: modifying a ternary matrix material in a composite doping manner of rare earth elements and transition metals, and then coating the surface of the material with a layer of amorphous ferric fluoride in a manner of combining atomic layer deposition with fluorination reaction. The ternary positive electrode material provided by the invention has higher rate capability and better cycling stability, and can maintain better chemical performance under high current density, so that the problems of capacity loss and poor electrical performance of the ternary positive electrode material of the lithium battery in a high-voltage long-cycle process are greatly relieved.

The invention provides a preparation method of an Al18F-labeled PSMA radiopharmaceutical, according to the preparation method, through adjustment of a reaction system, the labeling time efficiency, the radiochemical purity of a final product, the radiochemical conversion rate and the product yield are ensured, meanwhile, the requirement for the fluorination reaction temperature in the labeling process is effectively reduced, and the product yield is improved. The preparation method of the Al18F-labeled PSMA radiopharmaceutical provided based on the method has good applicability and thorough reaction, new impurities are not introduced into a final product due to reduction of the reaction temperature or adjustment of a reaction system, the variety and content of the impurities in the final product can be further reduced and controlled, and the preparation method is suitable for industrial production. And the medication safety of a patient is further ensured. In addition, the final product obtained by the preparation method provided by the invention has good inter-batch uniformity, and has good stability under the storage conditions of 30 DEG C + / -2 DEG C and 40 DEG C + / -2 DEG C.

The invention belongs to the technical field of octafluorocyclopentene gas preparation, and particularly relates to a catalytic synthesis method of octafluorocyclopentene. The method specifically comprises the following step: under the action of a fluorine-chlorine catalyst, carrying out gas-phase catalytic fluorination reaction on 1-chloroheptafluorocyclopentene and anhydrous hydrogen fluoride at 80-120 DEG C to obtain octafluorocyclopentene. The preparation method of the fluorine-chlorine catalyst comprises the following steps: dissolving metal chloride in water, adding a precipitant, and fully stirring for reaction to obtain slurry; filtering the slurry to remove filtrate to obtain a solid, and washing the solid with deionized water until the solid is neutral; adding aluminum nitrate into the washed solid, fully stirring and drying to obtain a precursor of the catalyst; and performing compression molding on the precursor of the catalyst, roasting, and activating to obtain the fluorine-chlorine catalyst. The method is mild in reaction condition and high in catalytic efficiency.

The invention relates to a method for high-value recovery of a positive electrode material of a waste lithium iron phosphate battery, which mainly comprises the following steps: adding a lithium iron phosphate positive electrode material, ammonium chloride and hydrogen peroxide into a ball milling tank for grinding, controlling the mass ratio of the ammonium chloride to the lithium iron phosphate positive electrode material to be 5: 2-7: 2, and controlling the volume mass ratio of the hydrogen peroxide to the lithium iron phosphate positive electrode material to be (18-22): 1mL / g; after grinding, washing out the mixture from the ball-milling tank by using deionized water, and then carrying out water leaching treatment to fully leach out metal lithium; excessive ammonium fluoride is added into the filtrate, and reaction liquid and a product lithium fluoride are obtained after reaction; and carrying out adsorption treatment on the reaction liquid by using defluorination resin, regenerating the defluorination resin through elution, combining and concentrating the collected effluent and eluent to obtain an ammonium chloride solution, and recycling the ammonium chloride solution to a chlorination reaction stage. According to the invention, through H2O2 reinforced mechanical chlorination coupling fluorination reaction, nearly total recovery of the waste lithium iron phosphate battery positive electrode material and high value of the product are realized, and the process is simpler and more environment-friendly.

The invention relates to the technical field of preparation of hydrofluoroolefin, in particular to a method for preparing 2, 3, 3, 3-tetrafluoropropene, which comprises the following steps: carrying out fluorination reaction on 3, 3, 3-trifluoro-2-chloropropene and excessive hydrogen fluoride under the action of a catalyst to generate a first mixture flow containing 1, 1, 1, 2, 2-pentafluoropropane (245cb), and separating the first mixture flow from the first mixture flow to obtain the 2, 3, 3, 3, 3-tetrafluoropropene. Then directly introducing the first mixture flow into a dehydrofluorination reactor for gas phase dehydrofluorination reaction to generate a second mixture flow containing 2, 3, 3, 3-tetrafluoropropene, hydrogen fluoride and unreacted raw materials, finally condensing the second mixture to remove hydrogen chloride, condensing and recycling hydrogen fluoride to obtain a third mixture flow, and rectifying the third mixture flow to obtain 2, 3, 3, 3-tetrafluoropropene. And 3, 3, 3, 3-tetrafluoropropene. According to the invention, unavoidable process wastes in the prior art are converted into recyclable reaction raw materials, the environmental protection and economic pressure of by-product treatment in the prior art is eliminated, meanwhile, the purpose of continuous flow reaction is effectively realized, and the process control difficulty and the process cost are reduced.

The invention relates to the technical field of batteries, in particular to a lithium carbon fluoride battery positive plate as well as a preparation method and application thereof. The method comprises the following steps: placing graphite in a fluorination reactor, filling a fluorination gas source, and carrying out fluorination reaction to obtain graphite fluoride; when the pressure in the fluorination reactor exceeds 200kPa, the pressure release valve is opened, and the fluorination gas source enters the cooler to be cooled and then enters the gas circulating pump to circulate and flow back to the fluorination reactor. According to the invention, a gas source flowing method is utilized, and the fluorination reaction is carried out safely and stably by accurately controlling the gas flow and taking away part of reaction heat, so that the potential safety hazard of chamber explosion caused by overheat reaction in the fluorination process is solved. Uniformly mixing graphite fluoride, a conductive agent, a binder and a solvent to obtain positive electrode slurry; and coating a current collector with the positive electrode slurry, drying, and rolling to obtain the positive electrode plate of the lithium carbon fluoride battery, which has excellent electrochemical performance.

The embodiment of the invention provides a preparation method of a high-load electrode with a vertical pore channel structure and a battery, which comprises the following steps: grinding and premixing carbon fluoride and a conductive carbon material in proportion, adding a binder, carrying out high-speed ball milling to obtain fiberized powder, and rolling to prepare an electrode material, thereby obtaining the high-load electrode with the vertical pore channel structure. Compounding the carbon fluoride with a current collector through hot rolling to obtain a positive pole piece; and finally, carrying out laser pore-forming treatment on the positive pole piece to obtain the high-load carbon fluoride electrode with a vertical pore channel structure. The pore diameter of the pore channel structure is 10-100 [mu] m, the pore pitch is 1-10 times of the thickness of the electrode material, the pore depth is 50-100% of the thickness of the electrode material, the ion tortuosity of the electrode is effectively reduced and the ion transmission efficiency is improved by constructing a vertical pore channel, meanwhile, high-energy laser induces an in-situ defluorination reaction on the pore wall to generate a high-conductivity sp2 carbon phase, and the conductivity of the electrode is improved. And the limitation of sacrifice conductivity of a mechanical pore-forming technology is broken through.

The invention relates to an improved process for the manufacture of a fluorinated organic compound, wherein the process comprises a fluorination reaction of an organic precursor compound having at least one chlorine substituent and / or at least one double bond, and said organic precursor compound is reacted in liquid phase in HF (hydrogen fluoride) serving as solvent and fluorinating agent in the presence of a fluorinating catalyst, and wherein the fluorination reaction is performed in liquid phase in a SiC block chemical reactor, and wherein the reaction mixture is withdrawn from SiC block chemical reactor, and wherein the process comprises optionally isolating and / or purifying the targeted fluorinated organic compound.

The application discloses a continuous production process and equipment for a trifluoromethylbenzene tower, and belongs to the field of organic fluorine chemistry. The production process comprises the following steps: S1: continuously feeding trichloromethylbenzene and hydrogen fluoride into a tower reactor connected with a heat exchanger circulating cooling system in a reverse direction, so that a three-stage continuous fluorination reaction occurs in the tower reactor to obtain crude trifluoromethylbenzene, and unreacted hydrogen fluoride is separated into liquid at the top of the tower and then flows back into the tower reactor; S2: the crude trifluoromethylbenzene obtained in the reaction is subjected to nitrogen bubbling in a bubble tower, and then is continuously distilled in a rectifying tower to obtain finished trifluoromethylbenzene; and S3: byproduct hydrogen chloride generated in the fluorination reaction is introduced into a hydrochloric acid tank to obtain hydrochloric acid, and the content of hydrofluoric acid in the hydrochloric acid is less than 1000 ppm. The method can greatly improve the utilization rate of raw material hydrogen fluoride, improve the purity of byproduct hydrochloric acid, reduce the generation amount of waste acid, avoid the sharp change of pressure in the reaction process, and realize large-scale, continuous, stable and safe production of trifluoromethylbenzene.

The invention provides a fluorination method of a PSMA radiopharmaceutical intermediate, and further provides a preparation method of an Al18F-labeled PSMA radiopharmaceutical preparation based on the fluorination method, and the fluorination method and the preparation method have the advantages that through adjustment of a reaction system, the purity of the PSMA radiopharmaceutical intermediate is improved, and the purity of the PSMA radiopharmaceutical preparation is improved. The preparation method of the PSMA radiopharmaceutical preparation marked by the Al18F has the advantages that marking time efficiency, radiochemical purity of a final product, radiochemical conversion rate and product yield are guaranteed, requirements on fluorination reaction temperature in a marking process are effectively lowered, and the preparation method of the PSMA radiopharmaceutical preparation marked by the Al18F based on the fluorination method is good in applicability, thorough in reaction and high in yield. New impurities are not introduced into the final product due to reduction of the reaction temperature or adjustment of a reaction system, and the preparation method can further reduce and control the variety and content of the impurities in the final product, so that the medication safety of patients is further ensured. In addition, the final product preparation product obtained by the fluorination method or the preparation method provided by the invention has good inter-batch uniformity, and has good stability under the storage conditions of 30 DEG C + / -2 DEG C and 40 DEG C + / -2 DEG C.

The invention belongs to the technical field of infrared focal plane sensor manufacturing, and particularly relates to a vanadium oxide etching post-processing method based on VHF wetting driving. Comprising the following steps: performing graded vacuumizing and temperature programming pretreatment on a wafer subjected to vanadium oxide etching, and continuously introducing VHF moistening mixed gas consisting of anhydrous hydrogen fluoride, ethanol steam and inert carrier gas into a treatment cavity; by accurately regulating and controlling the temperature and pressure of the cavity, anhydrous hydrogen fluoride is promoted to be subjected to a selective fluorination reaction with photoresist decomposition products and metal impurities left after etching to generate gaseous products, and ethanol steam synchronously exerts the dual effects of moistening, corrosion prevention and water molecule desorption promotion. According to the method, a gas phase processing mode is adopted in the whole process, liquid intervention is avoided, the problems of vanadium oxide pixel adhesion and film corrosion can be effectively solved, meanwhile, residual impurities are thoroughly removed, the electrical property stability of the vanadium oxide film is guaranteed, the yield and detection precision of the infrared focal plane sensor are remarkably improved, and the method has good industrial application prospects.

The present invention relates to the technical field of chemical synthesis, and provides a method for synthesizing 2,4-difluoronitrobenzene, which includes the following steps: under the action of a catalyst, 2,4-dichloronitrobenzene and a fluorinating agent are subjected to a fluorination reaction to obtain 2,4-difluoronitrobenzene; the catalyst includes tetrabutylammonium bromide and tetrabutylammonium chloride, and the mass ratio of tetrabutylammonium bromide to tetrabutylammonium chloride is 1:5 to 5:1. Through the above technical solution, the problems of low yield and low purity in the synthesis of 2,4-difluoronitrobenzene in the related art are solved.

The invention discloses a ruthenium complex with fluorine ions as counter anions and a synthesis method and application thereof, and belongs to the technical field of organic synthesis.The ruthenium complex is selected from a compound with the structural formula such as Ru-A or Ru-B or a hydrate of the compound with the structural formula such as Ru-A or Ru-B. The synthesis method is simple, operation is easy, and the ruthenium complex is suitable for industrial production. The ruthenium complex can be used as a catalyst for catalyzing a fluorination reaction of a trifluoromethoxy aromatic compound, has the advantages of high catalytic activity, good substrate compatibility, high product yield and no need of an activating reagent, can be used for later-stage functional modification of complex molecules, and has a good application prospect in the field of organic synthesis; .

The utility model discloses a fluorination reactor's gas leakage monitoring alarm equipment, including blower, high-efficiency collection structure and monitoring alarm structure, the high-efficiency collection structure is provided on the blower, the monitoring alarm structure is provided on the blower, the high-efficiency collection structure includes suction pipe, base, annular pipe and air inlet, the suction pipe is connected to an air inlet of the air blower, the base is fixedly arranged below the suction pipe, and the lower portion of the annular pipe is arranged on the base and communicated with the suction pipe. The utility model belongs to the technical field of fluorination reaction equipment, particularly relates to gas leakage monitoring and alarming equipment of a fluorination reactor, and effectively solves the problems that most of the gas leakage monitoring and alarming equipment of the fluorination reactor is provided with a monitoring device at the outer side of the fluorination reactor, and because the density of hydrogen fluoride is greater than that of control air, the leakage is influenced. And the hydrogen fluoride flows downwards and gathers on the ground, so that the leakage monitoring alarm is delayed, and the environmental safety is influenced.

The invention discloses a preparation method of high-purity 2-fluoroethanol, and particularly relates to the technical field of preparation of 2-fluoroethanol, which comprises the following steps: S1, in a dual-catalyst system consisting of a phase transfer catalyst and a Lewis acid catalyst and an organic solvent, carrying out fluoridation reaction on 2-chloroethanol and anhydrous potassium fluoride at 60-120 DEG C for 2-10 hours to obtain 2-chloroethanol; and S2, sequentially carrying out integrated purification of filtration, reduced pressure distillation, adsorption treatment and rectification on the reaction mixture. According to the invention, through synergistic activation and mass transfer of double catalysts, the reaction rate and selectivity are significantly improved, the water segregator is utilized to remove reaction water to push equilibrium movement, the conversion rate is improved, and water and impurities are systematically removed by virtue of composite adsorption and precise rectification of molecular sieves and activated carbon, so that high-quality 2-fluoroethanol with high purity and low moisture is finally obtained. The whole preparation process is mild in condition, high in yield, good in safety and suitable for industrial production.

The present application discloses a full-process continuous process for synthesizing 1,1,1,3,3-pentafluoropropane, including a telomerization reaction: vinyl chloride, carbon tetrachloride, catalyst 1 and a cocatalyst are added to a pre-reactor mixer for premixing to obtain mixture 1, mixture 1 is pumped into a reactor system for telomerization reaction to obtain the material of the telomerization reaction, the material of the telomerization reaction is continuously pumped out and separated to obtain R240fa, and the separated vinyl chloride, carbon tetrachloride, catalyst 1, cocatalyst and unseparated R240fa are returned to the pre-reactor mixer for continuous reaction; a fluorination reaction: the R240fa, chlorine gas and anhydrous hydrogen fluoride obtained from the telomerization reaction are continuously introduced into a fluorination reaction kettle containing activated catalyst 2 for fluorination reaction to obtain a fluorination reaction product, the fluorination reaction product is separated to obtain 1,1,1,3,3-pentafluoropropane, and the remaining product after separating 1,1,1,3,3-pentafluoropropane is returned to the fluorination reaction kettle for continuous reaction.

The application provides a purification method of lithium fluoride, high-purity lithium fluoride, lithium hexafluorophosphate, an electrolyte and a device, and the purification method of the lithium fluoride comprises the following steps: performing water washing treatment on the lithium fluoride to be purified at 0-50 DEG C to obtain a mixture containing a first solid-phase product; performing ultrasonic treatment on the mixture at 20-25 kHz to obtain a second solid-phase product through filtration; performing fluorination reaction on the second solid-phase product with electronic-grade anhydrous hydrofluoric acid to obtain a third liquid-phase product; performing ion exchange on the third liquid-phase product by using a chelating resin at 0-80 DEG C, and then performing cooling evaporation crystallization, and obtaining a fourth solid-phase product through filtration; and performing cleaning treatment on the fourth solid-phase product by using inert gas at 150-250 DEG C to obtain high-purity lithium fluoride. The high-purity lithium fluoride obtained by the purification method has low content of lithium carbonate and other impurities, and is beneficial to improving the performance and stability of subsequent products.

The invention relates to the technical field of energetic materials, in particular to nickel fluoride catalyzed ammonium perchlorate / aluminum composite fuel and a preparation method and application thereof. The ammonium perchlorate / aluminum composite fuel consists of the following components in percentage by mass: 50-70% of ammonium perchlorate, 0-10% of nickel fluoride and the balance of aluminum powder. Due to the addition of NiF2, high and low decomposition peaks of AP are combined into a violent exothermic peak, and the temperature of the high-temperature decomposition peak is reduced by about 30 DEG C, which means that the burning rate of the propellant can be greatly improved; the heat effect of the fluorination reaction (55.98 kJ. G <-1 >) of aluminum is far higher than the heat effect of the oxidation reaction (31.05 kJ. G <-1 >) of aluminum, so that the explosion heat is improved by about 10% while the reaction path is optimized. Besides, the anhydrous NiF2 used in the formula is stable in physical and chemical properties and does not absorb moisture and deliquesce, the problem of long-term storage of common fluorides such as CuF2 and FeF3 is solved, and the product reliability is extremely high.

The present invention belongs to the technical field of phosphorus pentafluoride preparation, and in particular to a method for efficiently synthesizing phosphorus pentafluoride using phosphoric acid and hydrogen fluoride. The synthesis method comprises the following steps: adding phosphoric acid and anhydrous hydrogen fluoride into a reactor at a temperature of 20°C to 10°C and mixing them uniformly, then passing SF4 into a mixed reaction, introducing the reaction mixture into a thermal decomposition kettle for thermal decomposition, and performing rectification and separation on the gas phase product obtained by decomposition to obtain high-purity phosphorus pentafluoride; wherein the molar ratio of the phosphoric acid and anhydrous hydrogen fluoride added is 1:1~2; the molar ratio of the SF4 to phosphoric acid is 2~2.5:1. The present invention uses phosphoric acid and anhydrous hydrogen fluoride as raw materials, and by adding SF4 as a dehydrating agent and an auxiliary fluorinating agent, the efficiency of the fluorination reaction can be significantly improved, and the product quality and yield can be improved. The synthesis method of the present invention has the advantages of mild conditions, simple process, low equipment requirements, and environmental protection and high efficiency.

The application provides a preparation method of fluoroethylene carbonate. The method comprises the following steps: uniformly mixing potassium fluoride, a novel solid base catalyst and an organic solvent, then adding chloroethylene carbonate to perform fluorination reaction; after the reaction is completed, the obtained reaction liquid is filtered and distilled to obtain a crude product, and the obtained crude product is subjected to rectification and crystallization to obtain fluoroethylene carbonate; the novel solid base catalyst is composed of a magnesium-aluminum composite oxide coated magnetic nano Fe3O4 carrier and a double-metal fluoride, and the double metal in the double-metal fluoride is a combination of Rb and Co. Compared with the prior art, the application has the following prominent points: (1) less solvent can be used for reaction, and the reaction condition is mild; (2) high selectivity, high activity, less side reaction and high product yield; (3) simple post-treatment, the solvent can be recycled after being evaporated, the generation of three wastes is less, and the industrial production is green and environmentally friendly.

The invention belongs to the field of metal fuels, and discloses an in-situ fluorination activity protection process and application of an aluminum-lithium alloy fuel, a fluorination method comprises the following steps: putting aluminum-lithium alloy fuel particles to be fluorinated into a fluidized bed filled with a protective gas, and forming a fluidized state; and then mixed gas of protective gas and fluorine gas is introduced into the fluidized bed, fluoridation reaction is carried out on the aluminum-lithium alloy fuel particles based on a fluidized bed-chemical vapor deposition process, and the aluminum-lithium fluoride alloy fuel particles with fluoride protective layers on the surfaces can be obtained. A fluidized bed-chemical vapor deposition process is used for carrying out fluorination reaction on aluminum-lithium alloy fuel particles, so that the metal fuel with a fluorinated protective layer, good compatibility and good oxidation resistance is obtained; the problems that aluminum-lithium alloy powder in existing alloy fuel is difficult to be compatible with other components in a solid propellant, easy to oxidize and difficult to store for a long time are solved.

The application designs a method for preparing optically active methyl fluoropropionate by using diethylamine sulfur trifluoride, comprising the following steps: fluorination reaction: under the protection of nitrogen, methyl S-lactate is added to a dry reaction kettle as raw material, the kettle temperature is cooled to a first reaction temperature, diethylamine sulfur trifluoride is added dropwise into the reaction kettle, after dropping, the reaction kettle is heated to a second reaction temperature, after the reaction is completed, the reaction mixture is added dropwise into saturated sodium / potassium bicarbonate aqueous solution to obtain R-2-fluoropropionic acid methyl ester; the molar ratio of diethylamine sulfur trifluoride to methyl S-lactate is 1-1.5:1, the method is high in efficiency, low in three-waste amount, short in reaction path, suitable for industrial production, and has economic value.

The invention relates to a preparation method of liquid lithium hexafluorophosphate, which comprises the following steps: in a reactor, taking a non-aqueous organic solvent as a dispersing agent, taking simple substance phosphorus, phosphorus oxide (not containing hydrogen) or phosphorus halide as a phosphorus source, taking lithium halide as a lithium source, carrying out one-pot fluorination reaction on excessive F2-containing gas at 5-20 DEG C for 50-350 minutes, and carrying out flash evaporation to remove the solvent after the reaction is finished, so as to obtain a lithium hexafluorophosphate solid; and dissolving the solid product in an ester organic solvent, filtering, and removing impurities from resin to obtain the liquid lithium hexafluorophosphate. The method has the advantages of simple process flow, low cost, high fluorination efficiency, high product yield, high purity and the like.

The utility model discloses a continuous fluorination reaction system which comprises a feeding assembly and a reaction assembly, the feeding assembly is connected with the reaction assembly through a pipeline, the feeding assembly is formed by connecting a plurality of mixing kettles in parallel, and the reaction assembly is formed by connecting a plurality of reaction kettles in series. According to the continuous fluorination reaction system provided by the utility model, a plurality of mixing kettles are used for mixing and feeding materials into the reaction kettles in turn, so that continuous reaction and no interruption in the reaction kettles are ensured, meanwhile, the whole system works in a totally closed manner, workers cannot be in contact with toxic raw materials during production, the production efficiency is high, the labor intensity is low, and the product quality is stable.

This invention discloses a process and apparatus for the continuous fluorination preparation of 2,6-dichlorobenzonitrile under mild conditions. The apparatus includes sequentially connected units for 2,6-dichlorobenzonitrile preparation, raw material preparation, online dehydration, continuous metering feeding, continuous reaction, and post-treatment, with a supporting control system for precise parameter control. The process first involves the continuous preparation and purification of 2,6-dichlorobenzonitrile at 70–90℃ and 0.1–0.3 MPa. Then, a raw material solution and a fluorination suspension are prepared and deeply dehydrated. Subsequently, a continuous fluorination reaction is carried out at 80–150℃ and 0.1–1.0 MPa. Finally, the finished product is obtained through post-treatment. This invention achieves continuous production throughout the entire process, with mild reaction conditions, a solvent recovery rate ≥95%, a finished product purity ≥99.8%, high production efficiency, low cost, wide equipment adaptability, and easy industrialization.

The utility model discloses a monochlorodifluoromethane production and separation device, which comprises a fluorination reaction kettle (1) and a fluorinated product concentration tower (2) connected with the fluorination reaction kettle (1), the fluorinated product concentration tower (2) is connected to a monochlorodifluoromethane product tank, the fluorinated product concentration tower (2) is also connected to a disproportionation reactor (3), and the disproportionation reactor (3) is connected with the fluorination reaction kettle (1). The disproportionation reactor (3) is connected to a disproportionation product concentration tower (4) through a pre-concentration tower (5), a pre-cooler (7) is arranged on the periphery of the pre-concentration tower (5), a tower top condenser (6) is arranged on the periphery of the top of the disproportionation product concentration tower (4), and the bottom of the pre-concentration tower (5) is connected to the fluorination reaction kettle (1) through a second return pipe (9). Reaction products are effectively separated, the utilization rate of all materials is high, continuous production and operation can be achieved, energy consumption is reduced, and operation is convenient.

The invention discloses a preparation method of a low-oxygen magnesium fluoride crystal, and belongs to the technical field of crystal preparation. After the raw materials are molten, the mixed gas activated by the catalytic net is introduced into the crystal furnace in an intermittent pulse mode, active fluorine species in the mixed gas and oxygen impurities on the surface of the melt can be subjected to fluorination reaction so as to reduce the content of the oxygen impurities, airflow in the intermittent pulse ventilation mode is matched with rotation of the crucible to disturb the melt, a reaction interface is updated, and the reaction efficiency is improved. And finally, the low-oxygen magnesium fluoride crystal is obtained through a pulling method.

This invention relates to an alkyl sulfonyl fluoride resin, its preparation method, and its applications. The structural formula of the alkyl sulfonyl fluoride resin is shown below: where n1 is 1~10000; n2 = 0~2. The preparation method includes: mixing compound 1 as shown in Formula I with a nitrite reagent and boron trifluoride diethyl ether and performing a diazotization reaction to obtain compound 2 as shown in Formula II; and then performing a fluorination reaction of compound 2 with a sulfur source, a fluorine source or a fluorosulfonylating reagent and an acid under the action of a catalyst to obtain the resin. Compared with the prior art, the preparation method of this invention is simple, the raw materials are readily available, and the prepared sulfonyl fluoride resin has high reactivity and good stability, and can be used as a high-efficiency matrix resin for the preparation of novel functional resins.