39results about "Hydroxylamine" patented technology

The invention discloses a preparation method of an ultra-pure hydroxylamine aqueous solution, and relates to the field of organic chemistry and chemical industry production. The method comprises the following steps: reacting electronic-grade hydroxylamine salt with organic alkali in a proper solvent to generate hydroxylamine, then separating and removing salt and unreacted hydroxylamine in a reaction solution through a mercaptopyridine ion exchange modified membrane, and finally concentrating the solution into 50wt% ultra-high-purity hydroxylamine aqueous solution by adopting reduced pressure evaporation or multi-effect evaporation. The process has the characteristics of high efficiency, environmental protection, simplicity and easiness in operation, effectively improves the purity, yield and separation efficiency of hydroxylamine, and meets the strict requirements of electronic grade hydroxylamine on purity and metal ion content.

The invention discloses a preparation method of a high-purity ultra-clean hydroxylamine aqueous solution. A four-stage purification process comprises the following steps: 1) low-temperature chelation-ceramic membrane metal removal; 2) molecular sieve membrane rectification decomposition prevention; 3) pulse electrodialysis reversal deep desalination; and 4) gradient filtration terminal refining. According to the preparation method of the high-purity ultra-clean hydroxylamine aqueous solution, a low-temperature molecular sieve membrane rectification technology is adopted, hydroxylamine liquid-phase thermal decomposition is avoided through a vapor phase separation mechanism, and the decomposition rate is reduced to 1t from 15% of a traditional process; the method comprises the following steps of: removing metal through chelation-electrodialysis synergistically, ensuring that Fe and Cu ion residues are less than or equal to 0.05 ppb through a thiosemicarbazide-bipolar membrane system, ensuring the nitrogen environment in the whole process, ensuring that the dissolved oxygen is less than or equal to 5ppb, replacing liquid phase distillation with molecular sieve membrane vapor phase separation, solving hydroxylamine liquid phase thermal decomposition, and breaking through the trace metal removal limit by combining thiosemicarbazide-bipolar membrane synergistically removing impurities. And then through nanoscale terminal filtration, the metal / particle control reaches ppb-level limit which is superior to the SEMI standard, and double spanning of quality and cost is realized.

The invention relates to a method for efficiently preparing hydroxylamine hydrochloride. The method comprises the following steps: mixing a diacetylmonoxime solution and a hydrochloric acid solution, pretreating through a pressurized nano-bubble fluidized bed, and carrying out reaction distillation under heating and pressurizing; after the reaction is finished, cooling reaction liquid, performing primary filtration and suction filtration through cross-flow filtration equipment, and collecting hydroxylamine hydrochloride crystals; and washing the crystal with absolute ethyl alcohol, recovering ethyl alcohol through cross-flow filtration equipment, and finally freeze-drying to obtain the high-purity hydroxylamine hydrochloride. The preparation method comprises the following steps: stirring quinoline-8-yl acrylate, tributyltin acrylate, 4-vinyl benzocyclobutene, ethanol and benzoyl peroxide to obtain a mixed solution; immersing the PTFE membrane subjected to low-temperature plasma pretreatment into the mixed solution, and then carrying out ultrasonic cleaning and vacuum drying to obtain a polymer modified PTFE membrane; the hydroxylamine hydrochloride prepared by the method disclosed by the invention has relatively high purity and yield, and meanwhile, the content of heavy metal ions and the content of water are effectively reduced.

The invention discloses a preparation method of an electronic-grade hydroxylamine aqueous solution, and relates to the field of chemical preparation. The preparation method comprises the following steps: reacting electronic-grade ammonia water or organic alkali with electronic-grade hydroxylamine salt to generate a hydroxylamine aqueous solution; and after the reaction, separating through a POSS (Polyhedral Oligomeric Silsesquioxane) nano blending modified membrane, and removing salt, impurities and unreacted raw materials to obtain a high-purity hydroxylamine aqueous solution. And concentrating the solution into a 50% hydroxylamine aqueous solution by adopting a low-temperature vacuum concentration technology. The method can effectively remove metal ions and inorganic impurities, and ensures that the final product is high in purity and meets the electronic grade requirement.

A method for preparing a hydroxylamine aqueous solution by catalytic hydrolysis of cyclohexanone oxime belongs to the technical field of hydroxylamine aqueous solution preparation. Specifically, cyclohexanone oxime and deionized water are added to a hydrolysis kettle to completely dissolve the cyclohexanone oxime, and an appropriate amount of a bisphenol-based solid acid catalyst is added. The mixture is stirred, refluxed, and condensed to obtain a reaction solution containing hydroxylamine. An extractant is added to the reaction solution, and the organic phase in the reaction solution is separated to obtain cyclohexanone; the residual aqueous phase is centrifuged to obtain the product hydroxylamine aqueous solution and the bisphenol-based solid acid catalyst, respectively, and the catalyst is recovered and recycled. This method significantly improves the conversion rate of the catalytic hydrolysis of cyclohexanone oxime, has a simple process route, simple operation, mild reaction conditions, and low energy consumption, and is a green and environmentally friendly production process.

The invention discloses a method for co-production of 2, 4-dichloro-5-fluoroacetophenone and hydroxylamine hydrochloride, and belongs to the technical field of organic chemical industry, 2, 4-dichlorofluorobenzene is used as a raw material, alkylation and reaction with tert-butyl nitrite are performed to generate oxime, and then hydrochloric acid hydrolysis is performed to generate 2, 4-dichloro-5-fluoroacetophenone and hydroxylamine hydrochloride; according to the method, co-production of the 2, 4-dichloro-5-fluoroacetophenone and the hydroxylamine hydrochloride is innovatively realized, not only are high yield and high purity of the target product 2, 4-dichloro-5-fluoroacetophenone ensured, but also the nitrogen element in the reaction is recycled and converted into the hydroxylamine hydrochloride with high additional value, and the atom economy is remarkably improved; according to the method, the operation process is greatly simplified, the use of dangerous reagents is avoided, and the intrinsic safety and environmental friendliness of the process are improved from the source; the method is simple to operate, safe and environment-friendly, the production cost is effectively reduced, and the market competitiveness of the product is enhanced.

A method for preparing an aqueous hydroxylamine solution belongs to the technical field of hydroxylamine preparation. Specifically, the method comprises adding an aqueous hydroxylamine sulfate solution to a raw material supply chamber, adding an aqueous sodium hydroxide solution to an alkali supply chamber, adding weakly alkaline water to a desalting chamber, adding a sulfuric acid solution to a concentrating chamber, circulating the sodium hydroxide solution between the anodic and cathodic chambers, and performing electrodialysis at room temperature to prepare the aqueous hydroxylamine solution. Furthermore, a method for preparing a stabilizer is provided, which can improve the stability of the aqueous hydroxylamine solution and reduce the damage to the hydroxylamine by metal ions.

The invention relates to a method for preparing hydroxylamine hydrochloride through ketoxime hydrolysis, and belongs to the technical field of hydroxylamine hydrochloride. The method comprises the following steps: pretreating ketoxime and a hydrochloric acid solution through a pressurized nanobubble fluidized bed, heating, then carrying out reaction distillation, and continuously steaming out a byproduct ketone during the period; after the reaction is finished, freezing and separating out the mixed solution, and filtering through cross-flow filtering equipment to obtain hydroxylamine hydrochloride crystals; performing negative pressure distillation concentration and cold separation on the filtrate, and repeating for 3 times to obtain hydroxylamine hydrochloride crystals and crystallization mother liquor; the crystallization mother liquor is returned to the reaction kettle to continuously participate in the hydrolysis reaction; the filtering membrane for the cross-flow filtering equipment is subjected to plasma modification treatment. The hydroxylamine hydrochloride prepared by the method disclosed by the invention has relatively high purity and yield and low chromaticity.

The invention develops an axial weak coordination synthesis method for regulating and controlling a cobalt phthalocyanine molecular metal d band center based on a graphdiyne topological structure. The method is characterized in that a series of graphdiyne two-dimensional interfaces with different topological structures are obtained by regulating and controlling the arrangement and proportion of sp-and sp-hybridized carbon atoms, and the adsorption configuration of cobalt phthalocyanine molecules along the graphdiyne topological structure two-dimensional interfaces is regulated by utilizing the d-pi action between sp-carbon and a cobalt metal center. The weak coordination regulation effect of sp-carbon on the d band center of cobalt phthalocyanine metal is realized. In the process of preparing hydroxylamine from nitrate through electro-catalysis, the adsorption energy of hydroxylamine at the Co-N4 site is reduced through the axial weak coordination effect of sp-carbon; sp-carbon can be used as a transfer station for catalyzing nitrate to nitrite to assist the nitrite to be reduced into hydroxylamine at the cobalt phthalocyanine Co-N4 site, so that a full-chain series catalytic mechanism is formed.

A method for co-producing caprolactam and hydroxylamine sulfate comprises: (1) ammoximation reaction: ketone, ammonia and hydrogen peroxide are reacted at a certain temperature under the action of a titanium silicon catalyst to produce an oxime solution; (2) hydrolysis reaction: caprolactam sulfate is added with an appropriate amount of desalted water, stirred, and the hydrolysis temperature is controlled to carry out a hydrolysis reaction to obtain a hydrolysis reactant caprolactam sulfuric acid solution; (3) co-production reaction of caprolactam and hydroxylamine sulfate: oxime solution is added to step (3), and the reaction is carried out at a certain temperature and pressure to obtain caprolactam and hydroxylamine sulfate solution; (4) physical separation: the reactants in step (3) are separated into layers, the upper layer is a light phase, which is an organic solvent containing caprolactam, and the lower layer is a heavy phase, which is an aqueous phase containing hydroxylamine salt; (5) the organic solvent containing ketone is returned to step (1) for ammoximation reaction, or after the solvent is removed, it is returned to step (1) for ammoximation reaction; the lower layer is subjected to sedimentation, centrifugal separation, and drying to obtain a crude caprolactam solution and hydroxylamine sulfate salt. The invention has the advantages of simple process, combining the production of caprolactam with the production of hydroxylamine salt, reducing the by-product of ammonium sulfate, and producing caprolactam and hydroxylamine salt at the same time.

A method for preparing a hydroxylamine aqueous solution by catalytic hydrolysis of butanone oxime belongs to the technical field of hydroxylamine preparation. The present invention uses low-temperature catalytic hydrolysis of butanone oxime and extraction and separation to obtain a hydroxylamine aqueous solution; the catalyst undergoes a sulfhydryl addition reaction with vinylguanamine and 4-allylcatechol through a macroporous styrene thiol resin to obtain a guanidine resin, which is then sulfonated to obtain a guanidine solid acid catalyst. The guanidine solid acid catalyst has higher acid strength and stronger catalytic activity, can more effectively promote the hydrolysis of butanone oxime, can significantly increase the hydrolysis rate and conversion rate of butanone oxime, and has good economic benefits.

The application discloses a method for synthesizing electronic-grade hydroxylamine salt based on high-purity butanone oxime and electronic-grade acid, and relates to the field of chemical synthesis. Specifically, high-purity butanone oxime is reacted with electronic-grade inorganic acid to generate hydroxylamine salt and butanone; after butanone is evaporated under reduced pressure, the water solution is concentrated and cooled to crystallize; then, vacuum heat treatment is performed, and small molecular impurities are removed through membrane separation of a thienyl carboxylic acid plasma grafting modified membrane, so that electronic-grade hydroxylamine salt is obtained. The method has high efficiency and is easy to popularize on an industrial scale.

The application discloses a process and system for preparing hydroxylamine nitrate, wherein the process for preparing hydroxylamine nitrate comprises the following steps: obtaining modified nano-metal cation resin by loading nano-metal oxide on an acidic cation resin to form the modified nano-metal cation resin; and preparing hydroxylamine nitrate solution by filling the modified nano-metal cation resin into an ion exchange column, obtaining hydroxylamine hydrochloride solution, adding the hydroxylamine hydrochloride solution into the ion exchange column to adsorb the hydroxylamine hydrochloride by the modified nano-metal cation resin, removing the adsorbed chloride ions by water washing, and desorbing the hydroxylamine in the modified nano-metal cation resin by using nitric acid solution to obtain the hydroxylamine nitrate solution. The modified nano-metal cation resin is applied in the process for preparing hydroxylamine nitrate by ion exchange with hydroxylamine hydrochloride solution as raw material, so that the selection performance and adsorption performance of the cation resin can be effectively improved, and the adsorption capacity and conversion efficiency of the cation resin are effectively improved.

The application discloses a preparation method of electronic-grade hydroxylamine aqueous solution and relates to the field of chemical preparation. Electronic-grade ammonia water or an organic base is reacted with electronic-grade hydroxylamine salt to generate hydroxylamine aqueous solution. After the reaction, the hydroxylamine aqueous solution is separated through a POSS nano-blended modification membrane to remove salt, impurities and unreacted raw materials, so that high-purity hydroxylamine aqueous solution is obtained. The solution is concentrated to 50% hydroxylamine aqueous solution through a low-temperature vacuum concentration technology. The method can effectively remove metal ions and inorganic impurities, and ensure that the purity of the final product is high and meets the electronic-grade requirement.

The invention discloses a preparation method of a hydroxylamine aqueous solution applicable to the field of semiconductors, which comprises the following steps: (1) adding an inorganic alkali aqueous solution into a hydroxylamine salt aqueous solution until the pH value of the hydroxylamine salt aqueous solution reaches 9-11 to obtain a hydroxylamine aqueous solution crude product; (2) adding an organic solvent into the hydroxylamine aqueous solution crude product, so that the solubility of a salt-containing component is changed, further crystallizing and separating out, and carrying out solid-liquid separation to remove a salt-containing solid, so as to obtain a desalted hydroxylamine solution; (3) carrying out reduced pressure distillation on the desalted hydroxylamine solution to remove the organic solvent, and increasing the concentration of hydroxylamine by azeotropy of the organic solvent and water to obtain a hydroxylamine aqueous solution without the organic solvent; and (4) purifying the hydroxylamine aqueous solution from which the organic solvent is removed through ion exchange resin, and removing trace metal ion impurities and anion impurities in the solution to obtain the hydroxylamine aqueous solution applicable to the semiconductor field.

A hydroxylamine free base, and a preparation method and reaction system therefor. The reaction system comprises a rectification column (1), a heating device (2), and a condensation device (3). A catalyst loading section (11) is provided in the rectification column (1), a hydrogen peroxide feed port (12) is provided on a side wall of the rectification column (1) above the catalyst loading section, and an ammonia feed port (13) is provided on the side wall of the rectification column (1) below the catalyst loading section (11). The heating device (2) is used for heating the reboiler of the rectification column (1); the condensation device (3) communicates with the top of the rectification column (1) and is used for condensing steam flowing out of the top of the rectification column (1) and for controlling the reflux ratio of the rectification column (1).

The invention belongs to the technical field of oil field fracturing tracer, and discloses a long-acting coating tracer agent for monitoring multi-stage fracturing and preparation and application of the long-acting coating tracer agent. The 15 long-acting coating tracers are hydrochloro hydroxylamine praseodymium, hydrochloro hydroxylamine neodymium, hydrochloro hydroxylamine samarium, hydrochloro hydroxylamine europium, hydrochloro hydroxylamine gadolinium, hydrochloro hydroxylamine terbium, hydrochloro hydroxylamine dysprosium, hydrochloro hydroxylamine holmium, hydrochloro hydroxylamine erbium, hydrochloro hydroxylamine thulium, hydrochloro hydroxylamine ytterbium, hydrochloro hydroxylamine lutetium, hydrochloro hydroxylamine lanthanum, hydrochloro hydroxylamine cerium and hydrochloro hydroxylamine yttrium; under-well production data of more than three years can be continuously obtained, materials are brought to the stratum along with fracturing, special construction operation is not needed, sampling is only needed at a well mouth, well shut-in is not needed, and quantitative and long-term capacity monitoring of each section of the horizontal well is achieved.

The application relates to a hydroxylamine aqueous solution purification process based on the combination of ion exchange membranes and adsorption resins, and relates to the hydroxylamine preparation technical field. Impurity-containing hydroxylamine aqueous solution is removed of impurities by passing through a strong-acid cation exchange resin column and a strong-alkali anion exchange resin column; the ion-exchanged hydroxylamine solution is filtered through a benzocyclobutene high-temperature sintering modified membrane to further improve the purity of the solution; the solution filtered through the modified membrane is introduced into an ion exchange membrane electrodialysis device for deep impurity removal; the benzocyclobutene high-temperature sintering modified membrane is prepared by using alumina ceramic powder, titanium dioxide, 4-vinyl benzocyclobutene, dibenzoyl peroxide and polyvinyl alcohol adhesive; the application can significantly reduce the impurity content and realize efficient separation and purification of hydroxylamine.

The application discloses a preparation method of ultrahigh-purity hydroxylamine aqueous solution and relates to the field of organic chemistry and chemical production. The method comprises the following steps: reacting electronic-grade hydroxylamine salt and an organic base in a proper solvent to generate hydroxylamine, then removing salt and unreacted hydroxylamine in the reaction solution through a sulfhydryl pyridine ion exchange modified membrane, and finally concentrating the solution to 50wt% ultrahigh-purity hydroxylamine aqueous solution through vacuum evaporation or multi-effect evaporation. The process has the characteristics of high efficiency, environmental protection and simple operation, effectively improves the purity, yield and separation efficiency of hydroxylamine, and meets the strict requirements of electronic-grade hydroxylamine on purity and metal ion content.

The application discloses a kind of high-purity hydroxylamine free base aqueous solution's fast preparation method, comprising: to anion exchange resin is pickled-water washed-alkali washed-water washed operation, obtain the pretreated anion exchange resin;Make hydroxylamine salt aqueous solution flow through pretreated anion exchange resin, obtain high-purity hydroxylamine free base aqueous solution.The application uses hydroxylamine salt as raw material, is dissolved in water to prepare and form hydroxylamine salt aqueous solution, directly with salt solution low temperature through basic anion exchange resin, by hydroxylamine salt and anion exchange resin reaction, exchange, high yield, high-purity hydroxylamine free base aqueous solution is obtained in one step.The application method can quickly prepare and obtain high-purity hydroxylamine free base aqueous solution, with simple process flow, hydroxylamine free base monomer decomposition rate is low, hydroxylamine free base aqueous solution product metal ion, anion content is less and so on.

Provided are thermo-responsive nitric oxide (NO) releasing molecules ("donors") and their use with polymer delivery systems. The delivery systems may include devices that allow for delivery of a dose of NO for inhalation such as portable inhalation devices. The compositions and methods may be used in the treatment of pulmonary conditions such as pulmonary hypertension, acute pulmonary vasoconstriction, respiratory distress syndrome, pulmonary edema, sepsis, and asthma. In some aspects, the compositions and methods provide a portable NO delivery mechanism allowing safe and pure NO administration outside of as well as in hospital settings.

According to the invention, hydrogen-substituted graphdiyne (HsGDY) is used as a carrier of polyphthalocyanine iron (FePPc) molecules, ordered double acetylenic bonds of the hydrogen-substituted graphdiyne (HsGDY) are used as coordination sites, and the polymerization degree of FePPc growing along a HsGDY two-dimensional plane is controlled through d-pi interaction with Fe-N4 sites, so that the interlayer stacking behavior of the HsGDY is inhibited; therefore, the hydrogen-substituted graphdiyne-loaded small-size polyphthalocyanine iron (HsGDY and FePPc) composite nano array electrode with a high exposure degree and a stable electrochemical interface is formed. Key points are that the HsGDY can promote enrichment and conversion of nitrate radicals and electrons on an interface of the HsGDY and FePPc; the double acetylenic bond can be used as an active site for catalytic conversion of NO3 <-> to NO2 <->, and the conversion of NO2 <-> from a polyphthalocyanine iron Fe-N4 site to NH2OH is promoted; the double acetylenic bonds interact with d-pi of the Fe-N4 site, so that the adsorption energy of NH2OH at the Fe-N4 site can be reduced, the desorption of NH2OH is promoted, and the HsGDY-coated FePPc composite molecular catalyst with series catalytic action is obtained.

The invention provides a method for preparing and purifying an electronic-grade hydroxylamine solution, which is suitable for meeting the requirements of the fields of electronic chemicals, medicines and the like on an ultra-clean high-purity hydroxylamine solution. The method comprises the following steps: S1, carrying out multi-stage feeding synthesis and concentration reaction on hydroxylamine salt; s2, adding a chelating agent and pre-filtering; s3, the chelate resin and the mixed bed resin are connected in series for adsorption; and S4, terminal ultrafiltration. Compared with a traditional process, the method does not need to distill hydroxylamine for concentration, so that the risk of rapid and violent decomposition of hydroxylamine is avoided. The chelating agent can settle a large amount of metal impurities with low energy consumption, and can be used as a hydroxylamine stabilizer. The concentration of the electronic-grade hydroxylamine obtained by preparation and purification of hydroxylamine salt is 35-45%, and the metal ion content is 1t; the number of particles with the particle size of 5 ppb and 0.2 mu m is smaller than or equal to 50 pcs / mL.

The invention discloses a method for synthesizing electronic-grade hydroxylamine salt based on high-purity diacetylmonoxime and electronic-grade acid, and relates to the field of chemical synthesis. The method specifically comprises the following steps: reacting high-purity diacetylmonoxime with electronic-grade inorganic acid to generate hydroxylamine salt and butanone; evaporating out butanone under reduced pressure, and cooling and crystallizing the concentrated water solution; and then carrying out vacuum heat treatment, and carrying out membrane separation through a thiophene carboxylic acid plasma grafting modified membrane to remove small molecular impurities so as to finally obtain the electronic-grade hydroxylamine salt. The method is high in energy efficiency and easy to industrially popularize on a large scale.

The invention relates to a hydroxylamine aqueous solution purification process based on combination of an ion exchange membrane and adsorption resin, and relates to the technical field of hydroxylamine preparation. A hydroxylamine aqueous solution containing impurities passes through a strong-acid cation exchange resin column and a strong-base anion exchange resin column, and the impurities are removed; the hydroxylamine solution subjected to ion exchange is filtered through a benzocyclobutene high-temperature sintering modified membrane, and the purity of the solution is further improved; introducing the solution filtered by the modified membrane into an ion exchange membrane electrodialysis device for deep impurity removal; the benzocyclobutene high-temperature sintering modified membrane is prepared from aluminum oxide ceramic powder, titanium dioxide, 4-vinyl benzocyclobutene, dibenzoyl peroxide and a polyvinyl alcohol binder. The method can significantly reduce the impurity content, and realizes efficient separation and purification of hydroxylamine.

The application discloses a method for preparing a hydroxylamine aqueous solution by a hydroxylamine salt neutralization method, and belongs to the technical field of hydroxylamine aqueous solution preparation. Specifically, a hydroxylamine salt is added into a reaction container, and is dissolved in a proper amount of deionized water; stirring is started under normal pressure; an alkali solution is added dropwise to perform a neutralization reaction; after the neutralization reaction is completed, the reaction solution is reduced-pressure filtered; a proper amount of a stabilizer is added into the filtrate; and then, reduced-pressure distillation is performed; and a distillate is the hydroxylamine aqueous solution. In the method, a pyrazolone type stabilizer is adopted, a mercapto imidazole sodium propyl sulfonate is introduced as a chelating agent, and a piperazine functional group is introduced, so that the stabilizing effect of the stabilizer can be effectively increased.

This invention discloses a process for preparing high-purity hydroxylamine by electromagnetic microwave-driven hydroxylamine salt pyrolysis and sublimation. The process specifically involves: adding a reducing boron salt to an aqueous solution of hydroxylamine salt; reducing metal ions in the hydroxylamine salt under microwave conditions; then adsorbing the metal ions through an electromagnetic field; concentrating, crystallizing, and centrifuging to obtain hydroxylamine salt with a metal impurity content of less than 100 ppb; subsequently, the hydroxylamine salt undergoes low-temperature pyrolysis and sublimation under vacuum and electromagnetic microwave action to obtain hydroxylamine crystals with a metal impurity content of less than 0.1 ppb, with a sublimation yield ≥85%. These hydroxylamine crystals are dissolved in ultrapure water to obtain an aqueous solution of hydroxylamine with a metal impurity content of less than 0.1 ppb. This invention utilizes the synergistic effect of microwaves and electromagnetic fields to generate hydroxylamine crystals through pyrolysis and sublimation at a relatively low reaction temperature with high selectivity, achieving safe and efficient results with a single-pass yield of not less than 85% from the electromagnetic microwave-driven pyrolysis and sublimation of hydroxylamine sulfate and hydroxylamine phosphate.

The invention discloses equipment and a method for producing a chemical product by taking industrial tail gas as a raw material, and relates to the technical field of chemical product production.The equipment for producing the chemical product by taking the industrial tail gas as the raw material comprises a mixing device, a decoloring device, a hydrolysis device and a distillation device, a stirring kettle is fixedly connected into the heating kettle; two backflow parts are arranged at the top of the stirring kettle; one end of each backflow part is communicated with the inner cavity of the stirring kettle. Through mutual cooperation of the adjusting piece, the rotating piece and other devices, the adjusting piece and the rotating piece are connected through the telescopic piece, on one hand, the position of the adjusting piece is limited through the telescopic piece, and the adjusting piece can rotate in the backflow groove conveniently; the adjusting part is controlled to rotate in the reflux tank according to the temperature of the solution to change the gas output and reflux quantity of the stirring kettle, so that the accurate control on the temperature of the solution is realized.