24results 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 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.

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.

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.

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 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 relates to a method for preparing an electronic-grade hydroxylamine aqueous solution by using an industrial-grade 50% hydroxylamine aqueous solution as a raw material through a microfiltration, ion exchange and nanofiltration combined technology. The method comprises the following steps: firstly, removing suspended particles and colloidal substances by microfiltration pretreatment; removing ion impurities through a specially modified ion exchange resin combined bed; and finally, deeply purifying by utilizing a nanofiltration technology to obtain a high-purity product. The method is short in process route, safe to operate and low in cost, the electronic-grade hydroxylamine aqueous solution can be stably produced, the metal ion content is lower than 10 ppt, the particle size of particles is controlled to be larger than 0.1 micrometer and smaller than 50 particles / ml, the resistivity reaches 18.2 M omega.cm, and the industrial requirements of semiconductor manufacturing, integrated circuits and display panels are met.

A method for preparing an aqueous solution of hydroxylamine by thermal decomposition of hydroxylamine phosphate belongs to the field of hydroxylamine preparation technology. Specifically: hydroxylamine phosphate is added to a sublimation apparatus containing an acceptor. The apparatus is subjected to thermal decomposition under reduced pressure and increased temperature. The acceptor is rapidly cooled, and crystals of a specific shape, i.e., high-purity hydroxylamine crystals, are obtained by solidifying the crystals in the acceptor. The crystals are then dissolved in high-purity water to obtain an aqueous solution of hydroxylamine. In addition, a guanidine-stabilizing synergist is obtained by reacting the thiol group of tetramercaptoporphyrin with allylthiourea via a thiol-ene addition reaction. This synergist can inhibit the decomposition reaction of hydroxylamine through multiple pathways, thereby improving the stability of hydroxylamine.

The invention discloses hydroxylamine free alkali as well as a preparation method and a reaction system thereof. The reaction system comprises a rectifying tower, a heating device and a condensing device. A catalyst filling section is arranged in the rectifying tower, a hydrogen peroxide feeding hole is formed in the side wall of the rectifying tower above the catalyst filling section, and an ammonia feeding hole is formed in the side wall of the rectifying tower below the catalyst filling section; the heating device is used for heating a tower kettle of the rectifying tower; the condensing device is communicated with the top of the rectifying tower and is used for condensing steam flowing out of the top of the rectifying tower and controlling the reflux ratio of the rectifying tower. The rectifying tower is used for preparing free hydroxylamine through reaction of hydrogen peroxide and ammonia, the boiling point difference among water, ammonia and hydroxylamine is used, the reaction can be promoted, further reaction between hydrogen peroxide and hydroxylamine can be avoided, hydroxylamine decomposition reaction caused by metal in the catalyst can be avoided, the generated pure hydroxylamine is enriched in the tower kettle, and the purity of the hydroxylamine is improved. The purity and the yield of the free hydroxylamine are improved.