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210results about "Halogenated hydrocarbon separation/purification" patented technology

Preparation method of chloromethyl styrene

The invention provides a method for preparing p-chloromethyl styrene, which comprises the following steps: (1) in the presence of a catalyst and an assistant, carrying out reaction on paraformaldehyde and hydrogen chloride to obtain a chloromethylation reagent; (2) reacting beta-halogenated ethyl benzene with the chloromethylation reagent obtained in the step (1) to obtain chloromethyl halogenated ethyl benzene; (3) adding an extracting agent into the chloromethyl halogenated ethylbenzene reaction liquid obtained in the step (2) for extraction to obtain an oil layer containing chloromethyl halogenated ethylbenzene and a water-containing acid layer, and crystallizing the oil layer to obtain purified p-chloromethyl halogenated ethylbenzene; and (4) in the presence of a solvent, carrying out elimination reaction on the purified p-chloromethyl halogenated ethyl benzene and alkali to obtain p-chloromethyl styrene.
Owner:JIANGSU YANGNONG CHEMICAL GROUP CO LTD

Beta-bromophenylethane rectification and purification process and system

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

Novel energy-saving environment-friendly refrigerant raw material preparation system

The invention relates to the technical field of refrigerant raw material preparation, and discloses a novel energy-saving environment-friendly refrigerant raw material preparation system which comprises a raw material preparation and supply unit, a reaction and separation unit and a refining unit which are connected in sequence, the reaction and separation unit comprises a mixer, a reflux device, a reactor, a cooling separation device, a membrane type absorption device and a tail gas tower which are connected in sequence; the refining unit comprises an azeotropic tower, a rectifying tower I and a rectifying tower II which are connected in sequence, and is used for performing dehydration, deacidification and rectifying purification on the separated crude chlorinated liquid to obtain a high-purity carbon tetrachloride product; by optimizing the technological process of the raw material preparation and supply unit, the reaction and separation unit and the refining unit, efficient, environment-friendly and energy-saving production of carbon tetrachloride is realized; the problem that the production raw material carbon tetrachloride of the fourth-generation refrigerant is insufficient is solved, the production cost is reduced, and the production efficiency is improved.
Owner:CHONGQING HAORAN ENERGY SAVING & ENVIRONMENTAL PROTECTION TECH CONSULTING SERVICE CO LTD

Dehydrohalogenation process

The invention provides a reactor comprising a reaction chamber having a catalytic surface in contact with reactants in said chamber; and a source for passing electrical current through said catalytic surface. The reactor can be used for dehydrohalogentation reactions, such as dehydrochlorination of HCFC-244bb to HFO-1234yf, and for reactions where zero valent metals are employed for catalysis. The invention further provides a process to prepare HFO-1234yf from HCFC-244bb using an electrically heated reaction chamber.
Owner:SOLSTICE ADVANCED MATERIALS US INC

Storage method for fluoro-2-butene

PendingJP2026063371APackaging corrosive chemicalsHalogenated hydrocarbon separation/purification
This invention provides a method for storing fluoro-2-butene that minimizes the progression of isomerization reactions during storage. [Solution] General formula C4H x F y Fluoro-2-butene, represented by the general formula where x is between 0 and 7, y is between 1 and 8, and x+y is 8, may or may not contain at least one of chromium, molybdenum, iron, zinc, and aluminum as a metal impurity. This fluoro-2-butene is stored in a container with the sum of the concentrations of chromium, molybdenum, iron, zinc, and aluminum (in the case where it contains these impurities) being 1000 ppb by mass or less.
Owner:RESONAC CORP

Post-treatment method and system for chloromethane synthesis

The invention relates to a post-treatment method and system for chloromethane synthesis, and the post-treatment method comprises the following steps: cooling a chloromethane crude product prepared in a reaction stage through an economizer, and then carrying out gas-liquid separation in a gas-liquid separator, a connecting pipeline between the economizer and the gas-liquid separator is filled with a water flow which flows in a direction opposite to that of the material, so that the temperature of a gas-phase discharge hole in the top of the gas-liquid separator is controlled to be 90-120 DEG C; the separated liquid phase enters a hydrochloric acid buffer tank with a partition plate, and an oil phase and a water phase are separated out; and washing the separated gas phase with water by a water washing tower, and then drying to obtain a chloromethane product. The economizer, the gas-liquid separator with specific temperature control and the hydrochloric acid buffer tank with the partition plate are arranged between the reaction system and the water scrubber, so that three-phase separation of'oil phase silicide-water phase-gas phase 'is efficiently realized, and the oil phase silicide is separated from the chloromethane crude product and does not enter the water scrubber and other subsequent systems; therefore, the problem of pipeline blockage in a post-treatment system is solved.
Owner:JIANGXI BLUESTAR XINGHUO SILICONE CO LTD

Device and method for treating hexafluoropropylene coarse pyrolysis gas in hexafluoropropylene preparation process

The invention discloses a device and a method for treating hexafluoropropylene coarse pyrolysis gas in a hexafluoropropylene preparation process, a quench cooler (1) is sequentially communicated with a carbon powder filter (2) and an external shell I (6), a spiral guide plate I (7) in the external shell I (6) is communicated with the external shell I (6), the spiral guide plate I (7) is communicated with a deacidification treatment unit (28), and the deacidification treatment unit (28) is communicated with a deacidification treatment unit (28). The deacidification treatment unit (28) is communicated with the gas outlet I (9) through a drainage pipe I (10), the dry-type deacidification device (3) is communicated with the external shell II (11), the spiral guide plate II (13) is communicated with the external shell II (11), the spiral guide plate II (13) is communicated with the dehydration treatment unit (29), the dehydration treatment unit (29) is communicated with the gas outlet II (24) through a drainage pipe II (14), and the dry-type deacidification device (3) is communicated with the gas outlet II (24) through a drainage pipe II (14). And the outer shell II (11) is communicated with the film coating powder remover (5). According to the invention, the hexafluoropropylene crude pyrolysis gas is effectively treated and collected.
Owner:TAIXING MEILAN NEW MATERIALS CO LTD

A methyl chloride cooling recovery system and a methyl chloride cooling recovery method

The present application belongs to the field of chemical production, and particularly relates to a chloromethane cooling and recycling system and a chloromethane cooling and recycling method. The chloromethane cooling and recycling system comprises a first condenser, a second condenser, a third condenser and a chloromethane recycling tank. The shell side inlet of the second condenser is connected with the tube side outlet of the third condenser, and the tube side inlet of the third condenser is used for passing in liquid chloromethane. The present application uses the vaporization endothermic principle of liquid chloromethane to cool and recycle chloromethane, and is good in economy. Moreover, since the to-be-cooled substance and the refrigerant are both chloromethane, even if mutual leakage occurs in the heat exchange process, the quality of the recycled chloromethane will not be affected and the loss of raw materials will not be caused.
Owner:ZHEJIANG XINAN CHEM IND GRP CO LTD +2

Method for reducing 1,1,1,2,2-pentafluoropropane (hfc-245cb) in a process for producing trans-1,3,3,3-tetrafluoropropene (hfo-1234ze(e))

A method for reducing 1,1,1,2,2-pentafiuoropropane (HFC-245cb) in a trans-1,3,3,3-tetrafluoropropene (HFO-1234ze(E)) manufacturing process including catalyst conditioning, temperature reduction, and contact time reduction. The method includes dehydrofluorinating 1,1,1,3,3-pentafluoropropane (HFC-245fa) with a catalyst mixture to produce a product mixture with HFO-1234ze(E) and HFC-245cb, and either incorporating a conditioned catalyst, using a lower temperature for the dehydrofluorination, or reducing the contact time for the dehydrofluorination to reduce the formation of HFC-245cb.
Owner:SOLSTICE ADVANCED MATERIALS US INC

Synthesis of 3-chloropropynyl and p-chlorobenzaldehyde

The present application relates to the technical field of fine chemical product synthesis, and in particular to a synthesis method of 3-chloropropynyl co-production of p-chlorobenzaldehyde, which comprises the following steps: mixing propargyl alcohol, a solvent, an ionic liquid catalyst, a cocatalyst DMF and a polymerization inhibitor p-tert-butyl catechol, heating and slowly adding p-chlorobenzylidene dichloride dropwise into the mixture, collecting the generated 3-chloropropynyl crude product at the tail gas outlet, cooling after the reaction is completed, and sequentially reducing pressure rectification of 3-chloropropynyl, the remaining propargyl alcohol and the solvent, and p-chlorobenzaldehyde product through a rectification tower. The present application solves the problems of using toxic and hazardous chemicals chlorinating agent in the production of existing 3-chloropropynyl, and generating a large amount of toxic waste acid gas or low-value byproducts, and the problem of low utilization rate of chlorine atom in the existing direct hydrolysis method of p-chlorobenzaldehyde, and reduces environmental pollution.
Owner:CHENGWU CHENHUI ENVIRONMENTAL PROTECTION TECH CO LTD

System and method for recovering methane chloride from methyl chlorosilane synthesis tail gas

The invention provides a system and method for recycling methane chloride from methyl chlorosilane synthesis tail gas. According to the method, 85%-90% of methane chloride in the methyl chlorosilane synthesis tail gas is recycled in a three-stage sectional type condensation mode. 90-95% of residual methane chloride is recovered through directional absorption of dichloromethane; and finally, residual methane chloride is recovered in a decompression analysis and reflux impurity removal mode, the total recovery rate of methane chloride is larger than or equal to 99%, the purity of methane chloride is larger than or equal to 99.5%, waste of methane chloride is greatly reduced, high recovery of methane chloride is achieved, and methane chloride can be directly reused in a methyl chlorosilane synthesis reaction.
Owner:LUXI CHEM GRP CO LTD

Method for purifying photoacid generator containing metal ion impurities based on crystallization process

The invention relates to a method for purifying a photoacid generator containing metal ion impurities based on a crystallization method. The light purification method comprises the following steps: (a) dissolving a photoacid generator crude product in a first solvent to form a supersaturated solution; (b) crystallizing the photoacid generator; (c) separating the photoacid generator crystals; and optionally (d) washing the separated photoacid generator crystal with a second solvent. The invention also relates to the high-purity photoacid generator prepared by the method and a photoresist containing the high-purity photoacid generator. According to the method, the photoacid generator containing metal ion impurities can be efficiently purified at low cost.
Owner:张江国家实验室

Composite stabilizers for 2-bromo-3,3,3-trifluoropropene and methods of use thereof

The present application relates to a composite stabilizer of 2-bromo-3,3,3-trifluoropropene and its use method, the composite stabilizer comprises: a phenolic compound, a phosphite or thioester compound, an acid binding agent, the molar ratio of the amount of the three substances is 1:0.1~6:0.1~6, and the mass ratio of the amount and 2-bromo-3,3,3-trifluoropropene is 0.001~1.0:100. Through the interaction between the above stabilizer components, the rectification process of the product can effectively inhibit the deterioration problems such as the increase of acid value, the color change to yellow and the decrease of purity of 2-bromo-3,3,3-trifluoropropene, provide excellent long-term stability, facilitate its production, transportation and storage, and ensure its smooth application in the field of new fire extinguishing agent, organic synthesis and the like.
Owner:NEWERA CHEM SHANDONG CO LTD +1

Gas separation method

The purpose of the present disclosure is to provide a novel separation method for separating refrigerant gas. This gas separation method comprises: a first step in which a raw material gas containing at least a refrigerant gas A and a refrigerant gas B is supplied to a first module to obtain a first separation gas and a first holding gas that differ in composition from the raw material gas; and a second step in which the first separation gas is supplied to a second module to obtain a second separation gas and a second holding gas that differ in composition from the first separation gas. The first module and / or the second module includes a molecular sieve membrane.
Owner:DAIKIN INDUSTRIES LTD

Environment-friendly refrigerant, preparation method and recovery system thereof

The invention relates to the technical field of refrigerants, and particularly provides an environment-friendly refrigerant and a preparation method and a recovery system thereof. In order to solve the problems that a traditional refrigerant is high in global warming potential (GWP), large in degradation energy consumption and not matched with a novel catalyst, the refrigerant is hydrofluoroolefin containing beta-position C = C double bonds, the molecular general formula is CF3CF = CHR (R is H or F), the molecular size is smaller than or equal to 0.8 nm, and the refrigerant is specially designed for being matched with a mesoporous structure of a TNT-120 titanium dioxide nanotube, and adsorption-mass transfer optimization and photo-thermal synergistic degradation synergism are achieved. And a closed-loop solution from production to scrapping is provided for the novel refrigerant. The recycling system adopts a catalytic reactor of which the inner wall is loaded with a titanium dioxide nano coating, and the refrigerant is efficiently degraded under the conditions of low temperature (25-240 DEG C) and low light intensity (0.5-3W / cm < 2 >). The refrigerant has a GWPlt (GWPlt); the refrigerant has the advantages of being good in heat stability, low in degradation energy consumption, environmentally friendly in the whole life cycle and the like, is suitable for replacing a high-GWP refrigerant and meets the requirement for green refrigeration.
Owner:ANHUI ZHONGKE DULING COMMERCIAL APPLIANCE CO LTD

Method and device for producing m-halogenated alkylbenzene through continuous reaction

The invention relates to a method and device for producing m-halogenated alkylbenzene through continuous reaction, and the method comprises the following steps: a reaction step: taking halogenated benzene and o-halogenated alkylbenzene and / or p-halogenated alkylbenzene as raw materials, and carrying out reaction in a reaction kettle under the catalysis of a catalyst; a washing step: washing the mixture obtained in the reaction step with water; a distillation step: distilling the mixture obtained in the water washing step, and refluxing the separated unreacted substances or byproducts to the reaction kettle; an adsorption step: carrying out molecular sieve adsorption on the remaining distillate after distillation in the distillation step, and separating a target product and a reaction by-product; and a refluxing step: refluxing the by-product separated by the molecular sieve into the reaction kettle. According to the method, halogenated alkylbenzene can be produced in a high-conversion-rate and environment-friendly manner.
Owner:江苏聚由新材料科技有限公司

Processes for the co-production of hfc-236ea, z-hfo-1225ye, e-hfo-1225ye, and hfo-1234yf

This application provides a process for co-producing HFC-236ea, Z-HFO-1225ye, E-HFO-1225ye, and HFO-1234yf, comprising: under a first catalyst, reacting hydrogen and HFO-1225ye to obtain a first reaction product stream; mixing the first reaction product stream with HFP and reacting it under a second catalyst to obtain a stream containing HFC-245eb and HFC-236ea; then separating the stream containing HFC-245eb and the stream containing HFC-236ea; under a third catalyst, reacting the stream containing HFC-236ea, washing with water, and extracting to obtain Z-HFO-1225ye and E-HFO-1225ye streams; under a fourth catalyst, reacting the stream containing HFC-245eb, washing with water, and separating to obtain the HFO-1234yf stream.
Owner:QUANZHOU YUJI ADVANCED MATERIALS CO LTD

Filtering device for rectifying and purifying chloroethane

The filter device comprises a fixed barrel, a delivery pump and a filter cartridge, the input end of the delivery pump is fixedly installed at one end of a connecting pipe, the other end of the connecting pipe is fixedly installed in one side of the fixed barrel, and the output end of the delivery pump is fixedly installed at one end of a delivery pipe. And the other end of the conveying pipe is fixedly mounted in one side of the purifying tower. By arranging the filter cartridge, impurities in a liquid mixture can be effectively filtered before the liquid mixture enters the purifying tower, the rectification effect is prevented from being influenced, and the filter cartridge is provided with the notch, the rubber gasket, the fixed block, the limiting clamping groove, the connecting block, the sliding groove, the spring, the sliding block, the limiting clamping block, the shifting block, the handle and the like; the sealing cover can be installed and fixed through the connection of the sealing cover, the rubber gasket and the notch and the connection of the limiting clamping block and the limiting clamping groove, the sealing cover is convenient to disassemble and assemble through the arrangement of a handle, a shifting block and the like, and the operation is more labor-saving compared with the operation of screwing the sealing cover.
Owner:JIANGSU YINZHU GRP HAIBAI TECH CO LTD

Kettle for dehydration and alcohol removal of dichloroethane

The utility model provides a kettle for dehydration and alcohol removal of dichloroethane, which comprises a reaction kettle, the reaction kettle comprises a kettle body, a stirring mechanism is fixedly arranged at the top of the kettle body, a stirring shaft is fixedly connected with a transmission mechanism through a support rod, the bottom of the transmission mechanism is fixedly connected with a mixing mechanism, the mixing mechanism comprises a connecting seat, a stirring rod and a hydraulic cylinder, the connecting seat is fixedly connected with the bottom of the enclosure, the top end of the stirring rod is rotatably connected with the interior of the connecting seat, and a plurality of uniformly distributed rod bodies are arranged on the stirring rod. The stirring mechanism and the mixing mechanism are arranged in the kettle body and are matched to realize full mixing, and the mixing mechanism can be folded after stirring, so that the mixing efficiency can be improved, the subsequent standing layering cannot be influenced, the production period of dichloroethane can be effectively shortened, the production efficiency is improved, and the production cost is reduced. The dichloroethane recovery solvent is subjected to washing alcohol removal treatment, and the yield of acylation reaction is better stabilized and improved, so that the solvent scrap consumption and the production cost are reduced.
Owner:DALIAN JIUXIN CROP SCI CO LTD

Method for reducing risk of burning and explosion in deoxygenation process of oxygen-containing gas

A method for reducing the risk of burning and explosion in a deoxygenation process of an oxygen-containing gas includes multiple steps. According to this method, in the presence of a gaseous alkane, hydrogen reacts with an oxygen-containing gas from which an unsaturated hydrocarbon has been removed. The oxygen-containing gas contains the oxygen and the unsaturated hydrocarbon, and the content of the oxygen in the oxygen-containing gas is greater than 0.5% by volume. A gaseous alkane is introduced to reduce the risk of burning and explosion of a mixed gas. A hydrocatalytic reaction is carried out to promote oxygen in the mixed gas to react with hydrogen to produce water, which removes oxygen from the oxygen-containing gas and also effectively inhibits carbon deposition on the surface of a catalyst and the production of a carbon oxide, which enhances the toleration for fluctuation of the oxygen content in a raw gas.
Owner:CHINA PETROLEUM & CHEMICAL CORP +1

Directional synthesis process of electronic-grade hexafluoroethane based on composite catalyst

The invention relates to the technical field of electronic-grade fluorine-containing special gas synthesis, in particular to an electronic-grade hexafluoroethane directional synthesis process based on a composite catalyst, which comprises the following steps: S1, carrying out reflux treatment on activated carbon by hydrofluoric acid-nitric acid mixed liquor, sequentially loading aluminum trichloride, cesium fluoride, lanthanum oxide and graphene quantum dots, and roasting in a nitrogen atmosphere to prepare the composite catalyst; s2, mixing tetrafluoroethylene and hydrogen fluoride in proportion, dehydrating through a molecular sieve, and removing impurities through a nano-zinc oxide coating purification tower; s3, introducing the raw materials into a fixed bed with a guide plate, and carrying out segmented temperature control reaction under the adjustment of a composite catalyst and perfluorohexane; and S4, condensing, alkali-washing and drying the reaction product, and rectifying in a rectifying tower to obtain the electronic-grade hexafluoroethane. And S5, adsorbing the rectification tail gas by a composite adsorbent, and resolving and recycling the raw materials for pretreatment. The process improves the selectivity and purity of hexafluoroethane, prolongs the service life of the catalyst, is good in regeneration effect, reduces energy consumption and raw material loss, reduces wastewater discharge, and meets the requirements of the semiconductor industry.
Owner:HEFEI JINSHI CHEMICAL CO LTD

Method for preparing 2-bromoheptafluoropropane through photothermal conversion

The invention relates to the technical field of preparation of fluorine-containing organic intermediates, in particular to a method for preparing 2-bromoheptafluoropropane through photothermal conversion. The method comprises the following steps: respectively vaporizing, mixing and preheating heptafluoropropane and bromine, introducing into a photo-thermal reactor, carrying out bromination reaction to obtain mixed gas containing 2-bromoheptafluoropropane, introducing the mixed gas containing 2-bromoheptafluoropropane into a fluorine removal device containing silicon dioxide, carrying out fluorine removal reaction, washing with water, carrying out alkali washing, dehydrating, compressing, condensing, carrying out two-stage rectification, and drying to obtain 2-bromoheptafluoropropane. The high-purity 2-bromoheptafluoropropane is obtained. According to the method, hydrogen fluoride is removed from the mixed gas containing 2-bromoheptafluoropropane through a fluorine removal reaction, hydrogen bromide is removed through water washing, alkali washing and dehydration, impurities are removed through secondary rectification, finally, the high-purity 2-bromoheptafluoropropane product is obtained through drying and dehydration, and the purity of the product is up to 99.91-99.98%.
Owner:SHANDONG HAIHUA GRP CO LTD +1

Method of purifying methyl fluoride by removing dimethyl ether

A method and system for purifying methyl fluoride (MeF) by removing dimethyl ether (Me2O) using a lithium salt sorbent, such as LiFSI or LiTFSI, are disclosed. Contaminated MeF is contacted with the sorbent, which preferentially adsorbs Me2O due to strong Lewis acid-base interactions, yielding purified MeF. The process may involve flowing through a sorbent bed, cryogenic collection, temperature differentials, or pumping, with optional multiple cycles for enhanced purity. This approach provides superior efficiency and purity compared to conventional methods, with experimental reductions up to 80% in Me2O content. Alternative salts and porous supports are also provided.
Owner:SOUTH 8 TECHNOLOGIES INC

Hexachloroethane crude product alkali washing kettle with good sealing performance

A kettle cover is arranged at the top end of a kettle body, a plurality of second connecting plates are arranged on the periphery of the kettle cover, the second connecting plates correspond to first connecting plates of the kettle body in a one-to-one mode and are connected with the first connecting plates of the kettle body in a fastening mode, and an inwards-concave surrounding plate is arranged at the bottom of the kettle cover and connected with the inner wall of the kettle body. An annular groove is formed in the outer edge of the inwards-concave surrounding plate, a sealing ring is arranged in the annular groove formed in the inwards-concave surrounding plate, the sealing ring is pressed on the inner wall of the kettle body and the inner wall of the kettle cover, a plurality of first reinforcing plates are evenly arranged on the sealing ring in the radial direction, the bottoms of the first reinforcing plates are connected with the inner wall of the inwards-concave surrounding plate, and a stirring paddle is arranged in the kettle body. Meanwhile, a plurality of first reinforcing plates are arranged in the kettle cover, and the bottoms of the first reinforcing plates are supported on the concave coaming, so that the supporting performance of the kettle cover and the concave coaming is greatly improved, leakage caused by deformation of the kettle cover or the concave coaming in the long-term use process is avoided, and the service life is prolonged.
Owner:NANTONG DONGGANG DRAINAGE CO LTD

Separation system and separation method of dichloromethane, ethanol and methanol aqueous solution multi-element azeotropic system

The invention discloses a separation system and a separation method of a dichloromethane, ethanol and methanol aqueous solution multi-element azeotropic system. The separation system comprises three stages of rectifying towers connected in series; a reflux pipeline with a condenser is connected to a tower top extraction port of each stage of rectifying tower, and the reflux pipeline corresponding to the first stage of rectifying tower is also connected with a mixer for mixing tower top extraction substances of the first stage of rectifying tower with water and a phase splitter for separating oil and water in the mixer; a water phase outlet of the phase splitter and a tower kettle extraction opening of the first-stage rectifying tower are respectively connected with a feeding opening of the second-stage rectifying tower; a methanol extraction opening is formed in the side line of the second-stage rectifying tower; a tower kettle extraction opening of the second-stage rectifying tower is connected with a feeding opening of the third-stage rectifying tower; and a device for separating ethanol and water is connected to a tower top extraction port of the third-stage rectifying tower. The method provided by the invention can effectively separate the dichloromethane, ethanol and methanol aqueous solution multi-element azeotropic system, and the obtained dichloromethane, ethanol and methanol products have high purity.
Owner:CHINA ELECTRONICS SYST ENG NO 2 CONSTR

Preparation method of tert-butyl lithium

The invention relates to the technical field of tert-butyllithium preparation, in particular to a tert-butyllithium preparation method which comprises the following steps: preparing raw materials, dissolving lithium and washing oil, mixing the raw materials to start reaction, dropwise adding a modifier, carrying out heat preservation treatment, cooling, settling and taking clear liquid. According to the method, trace impurities on the surface of lithium are removed in the pretreatment link, the PVP coating can block contact of water, oxygen and lithium in a long-acting mode, lithium is prevented from going bad in the earlier stage of storage and reaction, and meanwhile the compatibility of lithium and organic solvents such as n-pentane is enhanced; the interference of impurities on the reaction can be eliminated in a high-purity state of the chlorinated tert-butane, byproducts such as lithium tert-butoxide are prevented from being generated, the moisture in the system is strictly limited by deep dehydration, a stable anhydrous environment is provided for synthesis of the tert-butyllithium, and the reaction efficiency is guaranteed; the operation of deep dehydration and impurity removal by activated aluminum oxide creates a high-cleanliness solvent system for the reaction, avoids the action of water and polar impurities with tert-butyllithium or reaction intermediates, and prevents product decomposition or impurity generation.
Owner:SHANGYU HUALUN CHEM