714 results about "Vacuum distillation" patented technology

The invention discloses a method for preparing 6N-grade high-purity zinc through twice vacuum distillation based on a uniform temperature field. The method comprises the following steps: pretreatment; first-stage distillation: putting the zinc ingot subjected to vacuum drying into a crucible of a vacuum distillation furnace, mounting a plurality of stages of condensation collecting trays on the top of the crucible in an overlapping manner, and then performing high-vacuum pumping, heating and heat preservation; second-stage distillation: after the heat preservation of the first-stage distillation is finished, heating and heat preservation are continued under high vacuum; a plurality of samples are respectively obtained from the multistage condensation collecting disc, and the samples with the zinc content not lower than 99.9999% are collected, namely the 6N-grade high-purity zinc product. According to the method, zinc ingots with the purity of 99.99%-99.995% are used as raw materials, a conventional vacuum distillation furnace is used as distillation equipment, multiple stages of condensation collecting plates are mounted on the top of a crucible in an up-and-down overlapping manner, a novel two-stage distillation process is developed in a matched manner, key parameters such as the vacuum degree, the heating temperature, the heating rate and the heat preservation time are accurately controlled, and the high-purity zinc ingot is obtained. And a 6N-grade high-purity zinc product is successfully prepared.

The invention discloses dibutyl adipate as well as a preparation method and application thereof, preparation raw materials comprise adipic acid, n-butyl alcohol and a catalyst, and the molar ratio of the adipic acid to the n-butyl alcohol to the catalyst is 1: (3-8): (0.001-0.005). Excessive n-butyl alcohol obtained through distillation and kettle residues obtained after vacuum rectification can be directly applied to the next batch of reaction, continuous circular reaction can be achieved by supplementing a small amount of catalyst, maximum utilization of raw materials is achieved, and the production cost is reduced. Compared with the product obtained by the prior art, the content of the product obtained by simple rectification is higher, the content of dibutyl adipate in the product is 99.8% or above, the risk of trace activated carbon residue after activated carbon adsorption treatment is avoided, and the cosmetic grade product standard is met.

The invention discloses a resource regeneration method of waste lubricating oil, relates to the technical field of petrochemical engineering, and belongs to the patent classification number C10M175 / 06. The preparation method comprises the following steps: adding a composite flocculant into the waste lubricating oil, heating and stirring, and then carrying out magnetic separation to obtain pretreated waste lubricating oil; uniformly mixing the pretreated waste lubricating oil, glycerol and a Ni / Al2O3 catalyst, then heating and reacting under pressure, and cooling to room temperature to obtain a catalytic hydrogenation product; and carrying out reduced pressure distillation on the catalytic hydrogenation product, recovering the lubricant base oil fraction, adding methanol and concentrated sulfuric acid into the distillation residual liquid, heating for esterification reaction, and separating the liquid to obtain the biodiesel. In the pretreatment process, the composite flocculant is used for removing acid and particle impurities in the lubricating oil, a traditional alkali adding neutralization precipitation process is replaced, the method is environmentally friendly, and the recovery cost of enterprises is reduced.

The invention relates to the technical field of petrochemical corrosion failure and protection, and discloses a dew point corrosion high-risk area prediction method suitable for an atmospheric and vacuum distillation unit, and the method comprises the steps: firstly obtaining the technological characteristics of a to-be-tested device and the physical property data of processing raw oil; constructing a process calculation model of the to-be-tested device according to the process characteristics and the physical property data; solving logistics parameters in the device to be tested by using the process calculation model, and analyzing logistics distribution characteristics in the device; the material flow distribution characteristics comprise phase distribution characteristics, temperature distribution characteristics, component distribution characteristics and concentration distribution characteristics; calculating the dew point temperature in the device to be measured; and finally, determining a high-risk area in which low-temperature dew point corrosion occurs in the device to be detected in combination with the material flow distribution characteristics and the dew point temperature. According to the method, quick and accurate prediction of the corrosive components in the dew point corrosion high-risk area in the atmospheric and vacuum distillation unit is realized.

The invention relates to a preparation method of soybean oil base polyhydric alcohol, in particular to a method for preparing soybean oil base polyhydric alcohol by directly using soybean oil. The soybean oil diluted by using a solvent reacts with hydrogen peroxide with the weight percentage being 30% for 2-5 hours at the temperature of 60-70 DEG C under catalysis of a catalyst with the weight percentage being 3-5%; vacuum distillation is conducted after the reaction is ended, and the solvent is evaporated; then low alcohol is added in a reactor to be subjected to a reaction for 4-6 hours under the pressure of 0.3-0.4 MPa and at the temperature of 70-80 DEG C, then the reaction is stopped, and the soybean oil base polyhydric alcohol is obtained. The method saves the using amount of hydrogen peroxide, reduces the post-treatment steps, and simplifies the production procedures, and accordingly the product cost is declined directly.

The invention discloses a molecular-level atmospheric and vacuum corrosion simulation method and device, and the method comprises the steps: obtaining first macroscopic property data of current crude oil according to a crude oil physical property analysis model; according to a preset corrosion molecule library and the first macroscopic property data, obtaining a first molecule concentration of corrosion molecules in the current crude oil; acquiring virtual components of corrosion molecules in the current crude oil according to a preset physical property database and the first molecular concentration; and according to preset DCS data and the virtual components of the corrosion molecules, carrying out corrosion iteration simulation on the atmospheric and vacuum distillation unit, and outputting a simulation result of the distribution of the corrosion molecules at each part in the atmospheric and vacuum distillation unit. Compared with the prior art, the accuracy and timeliness of corrosion molecule distribution prediction of each part of the atmospheric and vacuum distillation unit can be improved.

A preparation method of 5N high-purity antimony comprises the following steps: (1) hydrolysis: taking ethylene glycol antimony as a raw material, and carrying out pyrohydrolysis pretreatment to obtain antimony trioxide; (2) biological reduction: uniformly mixing antimony trioxide with an organic catalytic reduction covering agent, and carrying out reduction smelting to prepare 4N antimony; and (3) vacuum distillation: the 4N antimony is subjected to two-stage vacuum distillation, namely first-stage high-temperature vacuum distillation and second-stage low-temperature vacuum distillation, and the 5N high-purity antimony is obtained. According to the method, an ethylene glycol antimony product is adopted as a raw material and subjected to hydrolysis-biological reduction and multi-field synergistic enhanced vacuum distillation to obtain 5N high-purity antimony, the total amount of impurity elements of the product is controlled to be 10 ppm or below, the content of key impurity elements As is controlled to be 1 ppm or below, the content of Pb is controlled to be 0.2 ppm or below, the content of Bi is controlled to be 0.2 ppm or below, the content of Cu is controlled to be 0.05 ppm or below, and the content of Fe is controlled to be 0.5 ppm or below.

The invention relates to a method for preparing a rosuvastatin calcium intermediate, and belongs to the technical field of drug intermediate synthesis. The method comprises the following steps: under the protection of nitrogen, carrying out reflux reaction on raw materials including 4-fluorobenzaldehyde and ethyl 4-methyl-3-oxovalerate under the catalysis of piperidine acetate and a co-catalyst, and carrying out reduced pressure distillation recovery to obtain a compound shown as a formula V; dropwise adding 2-ethyl-2-isothiourea and a compound shown in a formula VI, carrying out cyclization reaction under a non-violent reflux condition, and then adding DDQ in batches for oxidation to obtain a compound shown in a formula IV; oxidizing the compound as shown in the formula IV, and immediately quenching by using saturated NaHCO3 after the reaction is finished to obtain a compound as shown in a formula III; the preparation method comprises the following steps: firstly, treating a compound shown as a formula III by using methylamine, and slowly dropwise adding methylsulfonyl chloride under ice bath temperature control to obtain a compound shown as a formula II; reducing the ester group of the compound shown in the formula II in anhydrous toluene by using DIBAL to obtain an alcohol intermediate; then, selective oxidation is performed to obtain a final product; the method integrally has the advantages of high product yield and purity, few byproducts and low production difficulty.

A device and method for preparing high-purity metals by vacuum distillation and bidirectional step condensation, the device comprising an atmosphere control device, a vacuum distillation device, a charging device, an intelligent control device, and an exhaust gas treatment device. The atmosphere control device comprises a nitrogen bottle and a control valve located above the bottle mouth for controlling the opening and closing of the nitrogen bottle. The vacuum distillation device comprises a vacuum distillation device and a vacuum pump connected to the vacuum distillation device via a pipeline. The charging device is located in the middle of the vacuum distillation device, and the intelligent control device is connected to the vacuum distillation device. The exhaust gas treatment device comprises an impurity removal device. The vacuum distillation device is provided with a plurality of heaters, which are arranged in parallel along the length direction of the charging device and the condensation zone on both sides of the vacuum distillation device. The present invention also includes a method for preparing high-purity metals using the device. The device of the present invention has a simple structure, is not restricted by the gravity field, is convenient for sampling, and has high impurity removal efficiency.

The invention belongs to the field of separation and purification of bio-based chemicals, and particularly relates to a method for separating and purifying levoglucosenone from bio-oil. According to the method, the bio-oil obtained in the process of preparing levoglucosenone (LGO) through selective pyrolysis of biomass is used as a raw material, organic acid in the bio-oil is removed through a supersaturated carbonate solution, and then an oil phase is obtained through step-by-step extraction. And then adjusting working conditions, carrying out echelon reduced pressure distillation on the oil phase, and sequentially removing the extracting agent, low-boiling-point impurities and high-boiling-point oligomers, so as to obtain high-purity LGO. The pyrolysis bio-oil is subjected to coupling treatment of deacidification, step-by-step extraction and echelon reduced pressure distillation, so that the aim of separating and purifying high-added-value chemicals from low-value and complex-component bio-oil is fulfilled. The raw materials are cheap and easy to obtain, the process is simple, and the method is a biomass resource utilization method with great prospects.

The invention discloses lithium sulfide and a preparation method thereof. The preparation method comprises the following steps: (1) carrying out ball-milling mixing on iron powder, sodium sulfide and lithium sulfate in a first inert atmosphere to obtain a mixture; (2) calcining the mixture in a second inert atmosphere for the first time to obtain a reaction material; (3) stirring and washing the reaction material with an alcohol solvent in a third inert atmosphere, filtering to obtain filtrate and a filter cake, performing reduced pressure distillation on the filtrate to obtain a lithium sulfide crude product, washing the filter cake with deionized water, and filtering to obtain a solid by-product; and (4) carrying out secondary calcination on the lithium sulfide crude product in a fourth inert atmosphere to obtain lithium sulfide. The preparation method provided by the invention has the advantages of few synthesis steps, simple product purification and environmental protection.

The invention discloses a photoresist stripping waste liquid recovery method, which belongs to the technical field of waste liquid treatment, and comprises the following steps: carrying out centrifugal separation treatment on photoresist stripping waste liquid to remove polymer solid impurities in the photoresist stripping waste liquid to obtain pretreated stripping waste liquid; adding a bentonite-based adsorption material into the pretreated stripping waste liquid, stirring, and performing magnetic separation through a magnet to obtain purified stripping waste liquid; carrying out reduced pressure rectification treatment on the purified stripping waste liquid to obtain a recovered stripping liquid and a high-boiling-point substance; according to the recycling method, the high-concentration stripping liquid can be recycled, meanwhile, metal ions, moisture and high-molecular solid impurities influencing the product quality are removed, a dehydrating tower is not needed for dehydration treatment, and the recycling method has the advantages of being simple in process, small in occupied area of equipment and the like; and meanwhile, the pollution of the stripping waste liquid to the environment is also reduced.

The utility model relates to low-temperature vacuum distillation equipment convenient for material separation, and aims to solve the technical problems that the stirring range is still limited because stirring blades of the low-temperature vacuum distillation equipment can only stir in a horizontal fixed direction, the stirring is insufficient, the temperature rise of materials is non-uniform, and the material separation efficiency is reduced, and the low-temperature vacuum distillation equipment comprises a low-temperature distillation tank, according to the device disclosed by the utility model, the rotating shaft is effectively driven to rotate through the motor, so that the spiral blade and the stirring rod are driven to rotate, materials can be stirred in the vertical direction through the rotation of the spiral blade, and the materials can be stirred in the horizontal direction through the rotation of the stirring rod; the stirring effect is improved, uniform temperature rise of materials is facilitated, accordingly, the material separation efficiency is improved, the stirring rod can effectively drive the scraping plate to move when rotating, the scraping plate effectively scrapes and cleans the inner wall of the tank body, and adhesion of the materials to the inner wall of the tank body is reduced.

The invention belongs to the field of high-purity indium preparation, and provides a method for preparing high-purity indium based on ultrasonic vacuum distillation-electromagnetic pulse zone melting purification, the method combines vacuum distillation and zone melting purification technologies, ultrasonic waves are applied in the vacuum distillation process to assist in removing low-boiling-point impurities such as Cd, Zn and the like, and the purity of the high-purity indium is improved. In the zone melting process, pulse current is applied through an induction coil to assist in removing impurities mainly including Sn, Pb and Fe, and stable preparation of a high-purity indium product with the purity larger than or equal to 99.9995% and the oxygen content smaller than or equal to 2 ppm is achieved by screening and controlling technological conditions. According to the method, the requirement for the purity of the raw material indium is low, and the preparation cost of a high-purity indium product can be reduced.

The invention discloses a low-melting-point metal vacuum distillation-zone melting impurity removal device, the interior of the device is divided into a vacuum distillation zone and a zone melting zone which are communicated, the vacuum distillation zone comprises a graphite crucible and a special-shaped condensation cover, the inner side wall of the special-shaped condensation cover is provided with a triangular airflow separator, and the inner bottom wall of the special-shaped condensation cover is provided with a plane airflow splitter plate; a bottom outlet is communicated with a flow guide pipe and is connected with a zone melting pipe of the zone melting zone through a flow guide branch pipe; the method comprises the steps that firstly, low-melting-point metal is added, and all parts are installed; 2, carrying out vacuum distillation on the low-melting-point metal; and 3, carrying out regional purification on the vacuum distillation material in the regional melting pipe. According to the device, the vacuum distillation zone and the zone melting zone which are communicated are arranged, so that zone melting impurity removal is directly carried out after low-melting-point metal is subjected to vacuum distillation impurity removal, and the defects of air oxidation, pollution introduction, long charging time and the like caused by segmented charging are overcome; the method enhances the impurity removal effect and is suitable for the field of metal purification.

The invention discloses a lining high-vacuum regulating valve, which comprises a valve body and a valve rod arranged in the valve body, and further comprises a valve core connected with the valve rod and a valve cover provided with a stuffing box, and is characterized in that the inner surface of the valve body is coated with a first lining layer, and the first lining layer and the valve body form a conformal coating structure through a thermal forming process; the outer surface of the valve element is coated with a second lining layer, and the second lining layer and the valve element form a common coating structure through the thermal forming technology. Through the means of combining a high-temperature mold pressing injection molding process and a dovetail groove rivet composite structure, the industrial problems of stripping deformation of a lining material and a metal valve body and medium leakage under the high-vacuum working condition are solved, and the structural stability of the lining layer under the extreme negative pressure and the zero leakage effect of gas-liquid media are obtained; and the equipment reliability and environmental safety of vacuum distillation, negative pressure reaction and other processes in the fields of chemical industry, pharmacy and the like are remarkably improved.

The invention discloses a preparation method of bis (trifluoromethylsulfonyl) imide salt, and belongs to the technical field of metal ion battery electrolyte materials, and the preparation method comprises the following steps: mixing trifluoromethylsulfonyl fluoride and organic amine alkali to obtain a mixed solution A; dropwise adding the mixed solution A into a reaction kettle filled with ammonia gas, and completely reacting to generate bis (trifluoromethanesulfonyl) imide quaternary ammonium salt; carrying out reduced pressure distillation on the reaction product to obtain pure bis (trifluoromethanesulfonyl) imide quaternary ammonium salt; the preparation method comprises the following steps: mixing bis (trifluoromethylsulfonyl) imide triethylamine salt and metal salt according to a molar ratio of 1: (1-3), and completely reacting in an organic solvent to generate bis (trifluoromethylsulfonyl) imide salt; and filtering the reaction liquid, and carrying out reduced pressure distillation to obtain the final product bis (trifluoromethylsulfonyl) imide salt. The preparation method provided by the invention has the characteristics of simple process, high yield and high product purity, and solves the problems of complex process, low yield, low product purity and the like in the existing preparation method.

The invention discloses a preparation method of a polyoxyethylene ether surfactant with a piperazine group, and belongs to the technical field of surfactant preparation. The preparation method of the polyoxyethylene ether surfactant with the piperazine group comprises the following steps: 1, adding piperazine into a container filled with deionized water, stirring and dissolving, adding ethylene oxide, heating and stirring to react, adding sodium hydroxide, continuing to react, and carrying out reduced pressure distillation to obtain an intermediate; 2, adding a compound stabilizer into deionized water, performing ultrasonic treatment to obtain a compound stabilizer solution, adding the compound stabilizer solution into the intermediate, and performing stirring and mixing to obtain a mixed solution; and 3, adding the modified ionic liquid into the mixed solution, heating and stirring for reaction, cooling, filtering, extracting, and freeze-drying to obtain the polyoxyethylene ether surfactant with the piperazine group. The surfactant prepared by the method has excellent stability, emulsibility, dispersity and interfacial activity.

The invention relates to the technical field of organic chemical synthesis, and discloses a continuous production process of a cationic etherifying agent, which comprises the following steps: taking trimethylamine hydrochloride and epoxy chloropropane as raw materials; the method comprises the following six steps: raw material pretreatment, premixing, continuous reaction, continuous separation, refining and product storage: mixing and dissolving trimethylamine hydrochloride and a solvent, preparing a catalyst solution, uniformly mixing the three materials through a static mixer, feeding into a multi-stage tubular reactor, and carrying out segmented temperature control continuous reaction, and performing flash evaporation solvent removal and rectification on the reaction product to obtain a crude product, and performing ion exchange impurity removal and reduced pressure distillation refining to finally obtain a high-purity product. The method solves the problems of low yield and more byproducts in the traditional process, and is suitable for industrial large-scale production.

The invention discloses a method for separating and refining fusel oil in Fischer-Tropsch synthesis, which comprises the following steps: carrying out pressurized rectification treatment on fusel oil to remove acids, C4 + alcohol and part of n-butyl alcohol, carrying out dehydration treatment on tower top steam after removal through membrane separation, carrying out normal-pressure rectification treatment on a dehydrated intermediate product to remove light components, and carrying out vacuum distillation treatment on the dehydrated intermediate product to obtain the fusel oil. Carrying out reduced pressure rectification treatment on the tower bottoms after the light components are removed to remove propyl alcohol and butanol, carrying out tower top steam condensation on one part of the tower bottoms, returning the other part of the tower bottoms to the tower, extracting an ethanol finished product, carrying out normal pressure rectification treatment on the tower bottoms to remove isopropyl alcohol, carrying out normal pressure rectification treatment on the tower bottoms after removal for separation, and obtaining an n-propyl alcohol finished product at the tower top; and obtaining an n-butyl alcohol finished product from the tower kettle. Through cooperative coupling of multistage rectification and membrane separation, stage-by-stage efficient separation and resource utilization of components with different polarities and boiling points in fusel oil are realized, and three types of products of ethanol, normal propyl alcohol and normal butanol are synchronously produced.

The invention provides sulfonated ionic liquid as well as a preparation method and application thereof, the preparation method of the sulfonated ionic liquid comprises the following steps: dropwise adding sultone into an organic solution of 2-amino-5-sulfydryl-1, 3, 4-thiadiazole, and carrying out condensation reflux reaction at 90 DEG C for 24 hours; carrying out reduced pressure suction filtration to remove the solvent, washing the solid, and drying to obtain an ionic liquid onium salt precursor; dissolving the ionic liquid onium salt precursor in water, slowly dropwise adding inorganic acid, and reacting at 90 DEG C for 10 hours; and after the reaction is finished, performing reduced pressure distillation to remove water, washing the solid to remove the inorganic acid, the residual raw materials and byproducts, performing reduced pressure distillation to obtain a solid, and drying to obtain the sulfonated ionic liquid. The sulfonated ionic liquid does not corrode equipment, can efficiently catalyze oleic acid esterification reaction to prepare biodiesel, and can be recycled. The sulfonated ionic liquid disclosed by the invention has good application prospects and large-scale popularization potential in the field of catalyzing oleic acid to prepare biodiesel.

The invention provides a process for preparing high-purity lithium sulfide through layer interface induction strengthening, which comprises the following steps: dissolving lithium chloride and sodium sulfide in N-methyl pyrrolidone, and stirring to form uniform slurry; pumping the obtained slurry into a fixed bed reactor filled with a molybdenum disulfide catalyst layered module, and reacting to obtain turbid liquid; performing temperature-controlled crystallization on the turbid liquid, filtering and separating to obtain sodium chloride crystals; performing reduced pressure distillation on the filtrate to obtain a lithium sulfide crude product; and dissolving the lithium sulfide crude product in absolute ethyl alcohol for washing, and carrying out suction filtration and drying to obtain lithium sulfide. According to the method disclosed by the invention, fixed bed catalytic reaction and programmed cooling crystallization separation are integrated, and process parameters are optimized, so that the core pain points of high energy consumption, poor safety, difficulty in separation, easiness in catalyst deactivation and the like in a traditional method are successfully solved; a green closed loop of the whole process flow is realized, and a reliable technical path is provided for industrial production of the high-performance lithium sulfide material.

The present application relates to a kind of dimethylamine piperidine continuous synthesis dimethylamine piperidine method of oxy group, by using reaction raw material mixed solution into continuous flow packed bed reaction zone, i.e.catalyst layer;Reaction temperature is 20-80 ℃, normal pressure, feed liquid is the mixture of dimethylamine piperidine, hydrogen peroxide and deionized water, oxidation is carried out on the catalyst layer of continuous flow packed bed adiabatic reactor to make dimethylamine piperidine into dimethylamine piperidine oxy group, realize the continuous preparation of dimethylamine piperidine oxy group;The obtained reaction liquid is quenched, then filtered to remove solid particle quenching agent, vacuum distillation to remove water and vacuum rectification treatment obtain high-purity dimethylamine piperidine oxy group;The process scheme overcomes the series of deficiencies in the previous preparation process, such as complicated steps, low product purity, low production capacity in unit production time, realizes the continuous preparation of high-purity dimethylamine piperidine oxy group, with the characteristics of efficient, safe, green manufacturing.

The application belongs to the technical field of oil and gas field development, and particularly relates to a temperature-resistant and salt-resistant foaming agent for drilling and a synthesis method thereof. The synthesis method is as follows: diphenylamine-4-sodium sulfonate, isopropyl alcohol and 1,3-dibromopropane are added into a four-necked flask, stirred, heated and refluxed to obtain a mixed solution; 90-95wt% of isopropyl alcohol in the mixed solution is distilled off under reduced pressure, distilled water is added, and the whole is transferred into a separatory funnel, fully shaken, separated, and a small amount of oil phase is discarded; the pH is adjusted to 2-3, a precipitate is separated out, suction filtration is performed, and an intermediate is obtained; the intermediate is transferred into a four-necked flask with isopropyl alcohol, sodium bromoethyl sulfonate is added, the pH is adjusted to 7-8, and the product solution is obtained by heating and refluxing; the product is obtained by vacuum distillation, recrystallization and drying. The foaming agent for drilling has the advantages of good temperature resistance, salt resistance and salinity resistance.

The utility model discloses a device for extracting iris root oil by vacuum distillation, which belongs to the technical field of vacuum distillation extraction and comprises a distillation kettle, a top cover is arranged at the upper end of the distillation kettle, and a support frame is arranged on the top cover. Through the oil-water separation device, oil-water separation can be carried out at the first time by utilizing the oil-water separation device after condensation and liquefaction of an extracted substance, the process can be realized without an additional device, the whole extraction process is simplified, a lifting structure is arranged on an end cover, and when the amount of essential oil and water is changed, the lifting structure is arranged on the end cover; the lifting structure can rapidly adjust the height of the oil suction pipe, it is guaranteed that the tail end of the oil suction pipe is located in essential oil all the time, normal operation of oil-water separation work is guaranteed, the servo motor, the lead screw, the movable sleeve and other structures are adopted, adjustment is flexible and convenient, adjustment at any position can be achieved in the stroke, and the oil-water separation efficiency is improved. And the screw rod and the movable sleeve have a self-locking effect, so that the stability of the adjusted oil suction pipe can be guaranteed.

The invention belongs to the field of organic synthesis, and particularly relates to a method for preparing trimesoyl chloride in an immobilized catalysis mode. An immobilized catalyst is used as an acyl chloride reaction catalyst, thionyl chloride and benzene tricarboxylic acid are used as raw materials, and direct boiling reflux reaction is performed under the condition of not introducing other solvents; after the reaction is finished, filtering out the catalyst, and terminating the reaction; and then carrying out reduced pressure distillation to remove excessive reactant thionyl chloride, and then carrying out vacuum distillation to obtain the product trimesoyl chloride. By adopting the immobilized catalyst and taking the raw material as the reaction solvent, the method has the characteristics of mild reaction, simple process, high reaction speed, high product purity, high product yield and the like. And the immobilized catalyst and the reactant thionyl chloride can be recycled, so that the cost is saved, the reaction tail gas is easy to treat, the environmental pollution is not easily caused, and the method is suitable for industrial production. The final product is trimesoyl chloride, the purity can reach 99.2% or above, and the yield reaches 92% or above.

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.

The invention discloses a low-oxygen-content barium fluoride continuous vacuum distillation purification device and method, and relates to the technical field of barium fluoride purification, the device comprises a vacuum tower, the top surface of the vacuum tower is hermetically connected with a sealing cover, the center position of the top surface of the sealing cover is provided with a vacuumizing mechanism, and the inner side of the sealing cover is provided with a continuous feeding mechanism; a heating mechanism is arranged in the middle of the inner cavity of the vacuum tower; the vacuum pumping mechanism is arranged and used for controlling the continuous feeding mechanism and the heating mechanism while keeping the vacuum degree of the vacuum tower, so that the continuous feeding mechanism controls the continuous feeding speed of barium fluoride based on the barium fluoride distillation and purification speed of the heating mechanism, and the feeding accuracy of barium fluoride is guaranteed.

The utility model discloses a coking anti-blocking mechanism for a second-line distillation outlet of reduced pressure distillation, and particularly relates to the technical field of distillation kettles, the coking anti-blocking mechanism comprises a distillation kettle, a first distillation port and a second distillation port are respectively arranged on the distillation kettle, and a mounting groove is arranged in the second distillation port. A plurality of heating pieces which are arranged in a linear array are arranged in the mounting groove, an outlet pipe is arranged on the second distillation opening, and a plurality of guide grooves which are arranged in a linear array are formed in the outlet pipe. According to the distillation kettle provided by the utility model, exhaust and liquid discharge are realized through the first distillation port and the second distillation port on the distillation kettle, installation of a plurality of heating elements is realized through the installation groove of the second distillation port, liquid discharge is realized through the outlet pipe on the second distillation port, and liquid is guided through a plurality of guide grooves on the outlet pipe; the liquid flow rate is increased.

This invention provides a method for preparing high-purity imidazole ionic liquids, comprising the following steps: S1: 1-Ethyl-3-methylimidazolium chloride, sodium trifluoromethanesulfonate or sodium bis(trifluoromethanesulfonyl)imide, and glycerol solvent are added sequentially to a reactor, followed by stirring and reaction; S2: After the reaction is completed, stirring is turned off, and the resulting crude 1-ethyl-3-methylimidazolium ionic liquid and glycerol mixture are filtered and collected in a separator, with sodium chloride retained in the reactor and subsequently discharged; S3: Pure water is added to the separator, and the separator is stirred for a certain period of time before settling and separation; S4: The two phases in the separator are separated by a separator and then enter their respective purification devices; S5: The crude 1-ethyl-3-methylimidazolium ionic liquid is dehydrated by vacuum distillation to obtain the product; S6: The water and glycerol mixture is distilled under reduced pressure to obtain a reusable aqueous phase and a glycerol phase. This invention yields a product with a purity of over 99.5%; the solvents glycerol and water are reused after distillation. This method is simple, has a yield of over 94%, and is easy to implement in large-scale production.