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800 results about "Vacuum distillation" patented technology

Vacuum distillation is a method of distillation performed under reduced pressure, which lowers the boiling point of most liquids. As with distillation, this technique separates compounds based on differences in boiling points. This technique is used when the boiling point of the desired compound is difficult to achieve, will cause the compound to decompose or simply to save energy in heating. A reduced pressure decreases the boiling point of compounds. The reduction in boiling point can be calculated using a temperature-pressure nomograph using the Clausius–Clapeyron relation.

A method for refining crude lithium

The present invention provides a method for refining crude lithium, and belongs to the technical field of metal purification. The present invention melts the crude lithium material and then performs a first static sedimentation to obtain a supernatant melt 1, a low-impurity crude lithium melt, and a high-impurity crude lithium melt from top to bottom; the supernatant melt 1 is subjected to vacuum distillation under the condition of electromagnetic stirring without a paddle to volatilize low-boiling impurities, and then subjected to a second static sedimentation to form a bottom lithium melt and a supernatant melt 2; the supernatant melt 2 is separated to obtain purified lithium. The present invention performs vacuum distillation under the condition of electromagnetic stirring without a paddle, which not only realizes dynamic distillation of materials, reduces the distillation temperature, and improves the direct recovery rate of lithium, but also prevents the occurrence of cold zones inside to cause condensation and reflux of Na and K, thereby reducing the distillation efficiency and preventing secondary contamination of the product.
Owner:KUNMING DIBOO TECH

A method for preparing 6N high-purity zinc

The invention discloses a method for preparing 6N high-purity zinc, comprising the following steps: S1, alkali dissolution: dissolving electro zinc with sodium hydroxide, filtering after the reaction is completed; S2, acidification: adding hydrochloric acid to the filtered solution for acidification; S3, evaporation concentration: putting the acidified solution into an evaporating kettle for evaporation concentration; S4, freezing crystallization: filtering and drying the concentrated solution after cooling in a freezing tank; S5, secondary dissolution: dissolving the dried zinc chloride solid in an ether solution at room temperature, filtering; S6, vacuum distillation: putting the filtered ether solution into a vacuum distillation device, S7, heating and decomposing; S8, vacuum distillation. This method can achieve the purpose of preparing 6N high-purity zinc from electro zinc, and realize the low-cost recycling of zinc resources; at the same time, the alkali dissolution-acidification-ether secondary dissolution process can be used to effectively separate metals such as cadmium with a segregation coefficient close to 1 in zinc, which is convenient for the rear-end pyrometallurgical method to purify 6N high-purity zinc.
Owner:安徽铜冠产业技术研究院有限责任公司

Method for preparing 6N-grade high-purity zinc through twice vacuum distillation based on uniform temperature field

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.
Owner:LIUZHOU HUAXI COLORED DESIGN & RESEARCH INSTITUTE CO LTD

Dibutyl adipate as well as preparation method and application thereof

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.
Owner:SHANGHAI DONGGENG CHEM TECH CO LTD +1

Resource regeneration method of waste lubricating oil

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.
Owner:HUBEI ANNAIJI ENVIRONMENTAL PROTECTION TECH CO LTD

Dew point corrosion high-risk area prediction method suitable for atmospheric and vacuum distillation unit

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.
Owner:HEFEI GENERAL MACHINERY RES INST +2

Preparation method and system of high-purity metal rubidium or cesium

The invention provides a preparation method and system of high-purity metal rubidium or cesium, the method comprises the following steps: taking metal rubidium or cesium as a raw material, taking molten metal Ag as an extraction medium, utilizing the characteristics that Na, Li and K have certain solubility in metal Ag and rubidium and cesium are insoluble in Ag, reducing the content of impurities Na, Li and K in the metal raw material rubidium or cesium, and then carrying out vacuum distillation to obtain the high-purity metal rubidium or cesium. According to the method, purification and impurity removal are conducted on the metal rubidium or cesium through melt extraction, the metal raw material rubidium or cesium can be treated to prepare the high-purity metal rubidium or cesium product, the purification rate of Na and Li is 80% or above, the purification rate of K is 50% or above, the purity of the prepared high-purity rubidium is 99.90% or above, the purity of the prepared high-purity cesium is 99.95% or above, the yield is 95% or above, the technological process is short, equipment is simple, and the method is suitable for industrial production. The problems of low efficiency and unobvious impurity removal effect of traditional distillation are solved.
Owner:ZIJIN MINING RENEWABLE ENERGY & ADVANCED MATERIALS (CHANGSHA) CO LTD

Preparation method of soybean oil base polyhydric alcohol

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.
Owner:YIWU QUANCE NEW MATERIAL CO LTD

Molecular atmospheric and vacuum corrosion simulation method and device

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.
Owner:SYSPETRO TECH CO LTD

Preparation method of 5N high-purity antimony

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.
Owner:XIKUANG SHANXING ANTIMONY CO LTD

Method for preparing rosuvastatin calcium intermediate

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.
Owner:JIANGSU FURUI KANGTAI PHARM CO LTD

A device and method for preparing high-purity metal by vacuum distillation and bidirectional step condensation

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.
Owner:CENT SOUTH UNIV

Method for separating and purifying levoglucosenone from bio-oil

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.
Owner:NORTH CHINA ELECTRIC POWER UNIV

Lithium sulfide and preparation method thereof

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.
Owner:ZHANGJIAGANG HUASHENG CHEM CO LTD

Recovery method of photoresist stripping waste liquid

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.
Owner:ANQING XINXIANGRUI CHEM CO LTD

Preparation method and device of 2-phenylimidazoline and obtained product

The invention relates to a preparation method and device of 2-phenylimidazoline and an obtained product. The method comprises the following steps: adding benzonitrile, ethidene diamine and a catalyst into a reaction kettle, heating the reaction kettle to a reaction temperature in an inert gas atmosphere, starting a reaction, timing from 80 DEG C when the temperature is automatically increased to 155-180 DEG C, preferably 160-170 DEG C and is not increased any more, and reacting for 4-12 hours, preferably about 5-10 hours, after the reaction is finished, carrying out vacuum distillation on the reaction kettle, the product is obtained from the bottom of the reaction kettle (1), the material ratio is that the molar ratio of benzonitrile to ethylenediamine is 1: (1.03-1.20), and the molar ratio of the addition amount of the catalyst to ethylenediamine is (0.004-0.01): 1. The cyanobenzene is almost completely converted, the conversion rate is greater than 99.9%, and the residual quantity of cyanobenzene in the product is less than 0.01%, which is far superior to that of the existing production process.
Owner:HUNAN ZHONGCHUANG CHEM

Method for efficiently removing impurity lead in bismuth

The invention discloses a method for efficiently removing impurity lead in bismuth, and belongs to the technical field of non-ferrous metal refining. The method comprises the working procedures of material mixing, smelting and distillation, wherein crude bismuth and a vulcanizing agent are evenly mixed according to the mass ratio of 1000: (1-10) and then placed in a smelting container. Placing the smelting container in a smelting furnace for negative pressure smelting, and then placing a smelting product in a vacuum furnace for vacuum distillation. Lead sulfide is volatilized and enriched in the condensate, and bismuth is not volatilized, so that refined bismuth is obtained. According to the method, the vulcanizing agent reacts with the impurity lead to generate lead sulfide, the volatility of the lead sulfide is remarkably different from that of bismuth, the separation efficiency is improved, the separation process is simplified, the impurity lead in the crude bismuth can be efficiently removed, the content of lead in the obtained refined bismuth is smaller than or equal to 1 ppm, the additional value of the refined bismuth is high, the production process is simple, and the method is suitable for industrial production. High popularization and application values are realized.
Owner:KUNMING METALLURGY INST

Method for purifying p-dioxanone by coupling vacuum rectification with melt crystallization

The invention discloses a method for purifying p-dioxanone by coupling vacuum distillation with melt crystallization, which comprises the following steps: removing light and heavy impurity components contained in a crude product of p-dioxanone by vacuum distillation, and carrying out melt crystallization, sweating and filtering on the p-dioxanone subjected to vacuum distillation purification to obtain the p-dioxanone. High-purity p-dioxanone is obtained, and uncrystallized mother liquor is returned to the step of vacuum rectification.
Owner:CHINA PETROLEUM & CHEMICAL CORP +1

Method for preparing metallic titanium through two-step electrolysis in halide molten salt

The invention relates to a method for preparing metallic titanium through two-step electrolysis in halide molten salt, and belongs to the technical field of metallurgy. The method comprises the following steps: by taking fluorine-chloride mixed molten salt as primary electrolytic molten salt, adding TiO2 into the fluorine-chloride mixed molten salt, uniformly mixing, heating the fluorine-chloride mixed molten salt containing TiO2 to the electrolytic temperature of 650-850 DEG C in an inert atmosphere, inserting a cathode and an anode, carrying out primary molten salt electrolysis, taking out a cathode product, and carrying out secondary electrolytic treatment on the cathode product to obtain the TiO2 / TiO2 composite material. Performing vacuum distillation or washing on the cathode product to remove impurities, and drying to remove attached electrolyte to obtain a primary electrolytic product crude titanium; the method comprises the following steps: by taking primary electrolysis product crude titanium as a soluble anode, high-purity metal titanium as a cathode and chloride molten salt as secondary electrolysis molten salt, heating the chloride molten salt to the electrolysis temperature of 550-750 DEG C in an inert atmosphere, inserting the cathode and the anode, performing electrolytic refining, and washing the electrolysis product with diluted hydrochloric acid and deionized water to remove impurities, thereby obtaining the low-oxygen metal titanium powder. A low-melting-point molten salt system is adopted in two-step electrolysis, and energy consumption can be effectively reduced.
Owner:KUNMING UNIV OF SCI & TECH

Low-temperature vacuum distillation equipment convenient for material separation

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.
Owner:JIANGSU BLUE SOURCE ENVIRONMENTAL PROTECTION TECH CO LTD

Method for preparing high-purity indium based on ultrasonic vacuum distillation-electromagnetic pulse zone melting

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.
Owner:SICHUAN UNIV

Vacuum distillation-zone melting impurity removal device and method for low-melting-point metal

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.
Owner:XIAN RARE METAL MATERIALS RES INST CO LTD

Lining high-vacuum regulating valve

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.
Owner:HANGZHOU LIANGSHENG ELECTRIC CO LTD

Preparation method of bis (trifluoromethylsulfonyl) imide salt

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.
Owner:HENAN FLUORINE BASED NEW MATERIAL TECH CO LTD

A method for preparing high-purity metallic bismuth

The present invention relates to a method for preparing high-purity metallic bismuth, and relates to the technical field of non-ferrous metal metallurgy. The preparation method comprises the following steps: (1) in an inert atmosphere, a bismuth-containing raw material, phosphorus pentoxide and sulfate accounting for 1 / 3 to 1 / 2 of the total amount of sulfate are melted to obtain a product, and then the product is skimmed to remove the generated phosphate scum to obtain metallic bismuth with a purity of 4N; (2) the metallic bismuth obtained by skimming in step (1) is ground and sieved, and then mixed with sulfate accounting for 1 / 2 to 2 / 3 of the total amount of sulfate and subjected to two-stage vacuum distillation; (3) while performing two-stage vacuum distillation in step (2), graded condensation is performed to obtain high-purity metallic bismuth with a purity of 5N. Compared with traditional vacuum distillation and zone smelting processes, the present invention has the advantages of good purification effect, high impurity removal efficiency, etc., and has good application prospects.
Owner:安徽铜冠产业技术研究院有限责任公司

Preparation method of polyoxyethylene ether surfactant with piperazine group

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.
Owner:JIANGSU STERRIC CHEM IND

Continuous production process of cationic etherifying agent

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.
Owner:DONGYING ZEAO CHEM CO LTD

Green synthesis method of high-purity hexafluoropropylene tripolymer

The invention discloses a green synthesis method of a high-purity hexafluoropropylene tripolymer, and relates to the technical field of hexafluoropropylene tripolymer preparation. The preparation method comprises the following specific steps: adding a hexafluoropropylene monomer into a reaction kettle, cooling the reaction kettle to a reaction temperature, slowly adding a high-activity catalyst, simultaneously starting stirring, and maintaining the reaction temperature and pressure; after the reaction time is up, cooling the reaction system, terminating the reaction, filtering and recovering the high-activity catalyst, and carrying out vacuum distillation to separate unreacted hexafluoropropylene monomers and byproducts, so as to obtain a hexafluoropropylene tripolymer crude product; and further purifying the hexafluoropropylene tripolymer crude product through column chromatography to obtain the high-purity hexafluoropropylene tripolymer. Due to the special structure and functional groups of the catalyst, the selectivity of a reaction product and the conversion rate of raw materials can be improved, and the high-purity hexafluoropropylene tripolymer can be prepared.
Owner:INNER MONGOLIA FLUORINE TECH CO LTD

Method for separating and refining fusel oil in Fischer-Tropsch synthesis

PendingCN120204746AVacuum condensationOrganic compound preparationPropanolFusel alcohol
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.
Owner:JIANGSU XUYI HIGH TECH CO LTD