21 results about "Potassium borohydride" patented technology

The invention discloses a preparation method of 3-quinuclidinone hydrochloride, which comprises the following steps: carrying out temperature control reaction on 4-picolinic acid and chloroacetic acid under alkaline water conditions to obtain an aqueous solution of a compound a, and directly entering the next reaction without post-treatment after the reaction is finished; adding a reducing agent alkaline water system into the aqueous solution of the compound a, controlling the temperature to react, controlling the temperature to adjust the pH value to 5-5.5 after the reaction is finished, extracting with n-butyl alcohol, and drying to obtain an n-butyl alcohol solution of a compound b, and directly entering the next reaction step; wherein the reducing agent is one of sodium borohydride and potassium borohydride; dropwise adding thionyl chloride into an n-butyl alcohol solution of the compound b, controlling the temperature to react after dropwise adding is ended, and concentrating to remove the solvent and unreacted thionyl chloride after the reaction is ended, so as to obtain a compound c; carrying out Dieckmann condensation reaction on the compound c at controlled temperature under the condition of organic alkali by using toluene as a solvent, carrying out hydrochloric acid quenching reaction after the reaction is finished, and directly carrying out next-step reaction after extracting and removing impurities from a water phase containing a hydrochloride solution of a compound d by using toluene; and carrying out a decarboxylation reaction on the compound d in a hydrochloric acid aqueous solution at controlled temperature, after the reaction is finished, adjusting the pH value to 10-13, extracting, and salifying to obtain a target compound TM, namely 3-quinuclidinone hydrochloride. The preparation method of 3-quinuclidinone hydrochloride provided by the invention has the advantages of economical and easily available raw materials, mild reaction conditions, efficient reaction, simple operation and low cost, and is suitable for industrial application.

The invention provides a preparation method and application of a cobalt-based super-crosslinked polymer-based porous material for wastewater purification. According to the preparation method of the cobalt-based super-crosslinked polymer, sodium borohydride / potassium borohydride is used as a reducing agent to reduce cobalt nitrate, so that cobalt is loaded on the surface of the super-crosslinked polymer to obtain a composite material of the super-crosslinked polymer and transition metal, namely a catalytic oxidation method is introduced on the basis of adsorption, PMS is activated through the transition metal to generate free radicals, and the cobalt-based super-crosslinked polymer is obtained. The removal effect of the super-crosslinked polymer on the anion organic pollutant brilliant blue is further improved. The invention verifies that the cobalt-based super-crosslinked polymer has good adsorption and degradation properties on various pollutants. The invention researches the application of the adsorption-degradation system of the cobalt-based super-crosslinked polymer in the actual water body, and the experimental result shows that the adsorption-degradation system has a good removal effect on the anion organic pollutants and has the potential of removing the anion organic pollutants in the actual water environment.

The application is a kind of continuous preparation method and application of core-shell type reduced Cu-based catalyst. The method uses membrane dispersion micro-reactor technology, adopts liquid phase chemical reduction method with potassium borohydride-hydrazine hydrate as double reducing agent, continuously prepares reduced Cu-based nanoscale catalyst, does not need high temperature calcination and hydrogen reduction, can be directly used as active catalyst for catalytic reaction, and realizes green and efficient preparation. The catalyst prepared by the application is used in the reaction of preparing N-butyl-2,2,6,6-tetramethyl-4-piperidinamine from 2,2,6,6-tetramethyl-4-piperidinone and n-butylamine through reductive amination, and excellent catalytic activity and stability are shown.

The present application belongs to the technical field of wastewater treatment, and particularly relates to a method for removing total nitrogen in wastewater. Iron salt and carbon material containing hydroxyl and carbonyl are added into water, and then potassium borohydride is added, and the obtained mixture is freeze-dried under argon protection atmosphere to obtain iron-carbon filler; the iron-carbon filler is added into wastewater, the wastewater is adjusted to be weakly acidic, and stirring reaction is carried out for 0.5-1.5 h to obtain reduced effluent; persulfate is added into the reduced effluent, the wastewater is adjusted to be alkaline, and stirring reaction is carried out for 0.5-1.5 h, and then solid-liquid separation is carried out, and the obtained supernatant is treated effluent. The present application can remove total nitrogen in wastewater only by using iron-carbon filler and persulfate at normal temperature and pressure, and has the advantages of fast conversion rate, strong anti-interference ability, no secondary pollution and the like compared with traditional chemical oxidation-reduction technology; the reaction has wide original sources, low price, simple operation, and is environment-friendly, and has obvious economic and environmental benefits.

This invention provides a PVP-coated Cu-based electrocatalytic material, its preparation method, an electrode for electrocatalytic carbon dioxide reduction, and its application. Copper chloride dihydrate, polyvinylpyrrolidone (PVP), and dimethylformamide are mixed to obtain a mixture. Under a protective atmosphere and with stirring, potassium borohydride solution is added dropwise to the mixture, generating a precipitate. The precipitate is then centrifuged and dried to obtain the PVP-coated Cu-based electrocatalytic material. This invention introduces PVP, which has the advantages of low cost and wide availability. Cross-linked nanosheet-like copper-based catalytic materials are successfully prepared by reducing divalent copper ions with potassium borohydride solution. During the reduction process, 0.18–0.22 g of PVP (based on 2 mmol of copper) is introduced to coat the copper nanosheet structure, effectively regulating the valence state change of divalent copper ions during the reduction process, controlling it between monovalent and divalent copper, thus making it more favorable for the formation of C2 products.

The invention discloses a nitrogen-phosphorus-boron-iron co-doped coconut shell activated carbon carrier and a preparation method and application thereof, the method comprises the following steps: S1, crushing coconut shell activated carbon, and carrying out Ar / water vapor activation treatment to obtain pretreated activated carbon; s2, after the chitosan solution and the urea solution are mixed, phytic acid is added, the pH is adjusted to 5.5-6.0, stirring is conducted, and a wetting agent is obtained; s3, adding a wetting agent into the pretreated activated carbon, heating, stirring, filtering, washing, and drying in vacuum to obtain pre-activated activated carbon containing nitrogen and phosphorus; and S4, dissolving ammonium ferric citrate and sodium citrate in deionized water, adding ethylene glycol, stirring, then adding the pre-activated activated carbon containing nitrogen and phosphorus, heating, stirring again, then dropwise adding a potassium borohydride mixed solution, and roasting to obtain the nitrogen, phosphorus, boron and iron co-doped coconut shell activated carbon carrier. After the nitrogen-phosphorus-boron-iron co-doped coconut shell activated carbon carrier provided by the invention is loaded with the metal catalyst, the common problems of low conversion rate and poor selectivity in nitro hydrogenation reaction can be solved.

The invention discloses an efficient and safe microwave digestion-atomic fluorescence detection method for total selenium in soil, and belongs to the technical field of analytical chemistry and environmental detection.According to the method, the content of total selenium in selenium-rich soil is rapidly, accurately and safely measured by optimizing the sample weighing amount, the microwave digestion procedure and the detection conditions, and the detection accuracy is improved. The method comprises the following specific steps: weighing 0.1 g of an air-dried and sieved selenium-rich soil sample, adding 5mL of concentrated nitric acid, then carrying out a microwave digestion process of heating to 175 DEG C for 12 minutes and maintaining for 48 minutes, after digestion, adding 5mL of 6mol / L hydrochloric acid, carrying out acid removal reduction at 140 DEG C, fixing the volume to 15mL by using 5% diluted hydrochloric acid, and finally determining by using an atomic fluorescence spectrophotometer by using 5% hydrochloric acid as a carrier current and 1% potassium borohydride and 0.5% potassium hydroxide as reducing agents. According to the method, the use of dangerous reagents such as hydrofluoric acid and perchloric acid is avoided, the detection period is remarkably shortened, the linear range is 0-10 mu g / L, and the correlation coefficient is Rgt; the average recovery rate is up to 101.13%-101.51%, and the precision is RSDlt (Research Standard Defect); the requirements of rapid detection of the total selenium content of the selenium-rich soil, agricultural production and environmental evaluation are met.

The utility model provides a liquid chromatography-atomic fluorescence flow path analysis system, which relates to the technical field of chemical analysis, and comprises a mobile phase processing device, a sample online reaction device, a gas path device and a gas-liquid separation device, the sample online reaction device is used for carrying out separation, online ultraviolet digestion and hydride generation on a sample; according to the device, the mobile phase does not need to be degassed manually, an experimenter only needs to prepare the mobile phase and place a pipeline in a corresponding reagent bottle, and an instrument can perform online degassing on the mobile phase, so that the time required for preparing the mobile phase is saved, hydrogen is supplemented when a sample reacts with a reducing agent to generate gaseous hydride, the dosage of potassium borohydride is effectively reduced, and the production cost is reduced. While the physical health of experimenters is ensured and a friendly laboratory environment is provided, the influence of water vapor on a test result can be reduced, and the sensitivity and the stability of an instrument are improved.

The invention discloses a fermentation type seaweed granular fertilizer and a fermentation method thereof, and belongs to the technical field of biological fertilizers, plant active substances of enzymolysis seaweed active powder, grain byproducts and organic nutrition of soybean meal are fused, after microbial fermentation, nutrition release is more balanced, robust growth of crops can be promoted, and the yield and quality can be improved; seaweed residues are secondarily utilized through an enzymolysis technology, macromolecular substances are degraded into micromolecular active components through alginate lyase and cellulase, enzymolysis seaweed active powder is prepared, the nutritive value of seaweed is excavated to the maximum extent, the cost of raw materials is reduced, nano zeolite serves as a carrier of microelements, iron ions are reduced and stabilized through potassium borohydride, and then iron ions are reduced and stabilized through potassium borohydride; and then the nitrohumic acid is used for chelating elements such as zinc, iron and boron, and the adsorption performance of the nano zeolite is combined, so that the double stability of the chelated trace elements and the porous carrier is realized.

The invention relates to a production method for improving photo-thermal stability of a chloromethyl ethyl ether industrial product, and belongs to the technical field of chloromethyl ethyl ether processing.The preparation of an intermediate 1 comprises the steps that 80-120 mL of ethyl alcohol, 20-25 g of 3, 5-di-tert-butyl-4-hydroxybenzaldehyde and 6-10 g of n-butylamine are added into a 250 mL four-opening bottle provided with a backflow water diversion device, the temperature is increased to 60 DEG C, a reaction is carried out for 1 h, and an intermediate 2 is obtained; cooling to 0 DEG C by adopting an ice salt bath, adding 1-3g of potassium borohydride in batches, keeping the temperature at 0 DEG C, continuing to react for 0.5 hour, and adding a 5% citric acid aqueous solution to adjust the pH value to 2.0-3.0; the special photo-thermal stabilizer is synthesized and compounded with the epoxidized soybean oil, a single stabilizer and a special formula free of chloromethyl ether are generally adopted in the traditional method, the photo-thermal stabilizer containing the hindered phenol and piperazine structure is synthesized by the method, synergistic protection of light shielding, thermal stability and acid capture is achieved after compounding, and the product performance is remarkably improved; and the purity retention rate is 95-97% after 168h of ultraviolet aging.

The application relates to the field of photocatalysis, in particular to a composite material for photocatalytic degradation of PFOA and a preparation method thereof. The composite material comprises the following steps: step one: using titanium foil as an anode and a nickel sheet as a cathode, carrying out anodic oxidation, and then annealing to obtain TiO2-NT; step two: first, acid pickling TiO2-NT, and then preparing TiO2-NT suspension liquid; adding chloroplatinic acid, a dispersing agent and potassium borohydride into the TiO2-NT suspension liquid to prepare a Pt / TiO2-NT composite material; step three: coating ammonium perrhenate on the Pt / TiO2-NT composite material, and then sintering, repeating 1-2 times to obtain a modified Pt / TiO2-NT composite material; and step four: preparing a MIP-Pt / TiO2-NT composite material through a molecular imprinting technology.

The application relates to the technical field of cement grinding aids, and particularly discloses a high-efficiency composite Portland cement clinker grinding aid and application thereof. The grinding aid comprises separated A liquid and B liquid. The A liquid comprises a mixed solution of ethylene glycol and water and dihydrogen iron phosphate, wherein the volume ratio of the ethylene glycol to the water is 3-3.7:1, and the dihydrogen iron phosphate in the mixed solution is in a saturated state. The B liquid comprises a sodium borohydride and / or potassium borohydride solution, a polycarboxylic acid water reducing agent and modified magnesium oxide powder. The mass fraction of the sodium borohydride and / or potassium borohydride solution is 3-5%, the mass fraction of the polycarboxylic acid water reducing agent in the B liquid is 12-17%, and the content of the modified magnesium oxide powder is 4.5-7 g / L. The above grinding aid can effectively eliminate the electrostatic effect of cement particles, reduce the re-agglomeration between the particles, improve the dispersity of the cement clinker particles, and thus improve the grinding efficiency.

The invention relates to plug-in agricultural solid hydrogen supply equipment and a continuous hydrogen supply method, the plug-in agricultural solid hydrogen supply equipment comprises a hydrogen supply container and a solid hydrogen storage material, the hydrogen supply container comprises a containing cavity, a liquid inlet and an exhaust hole, the liquid inlet and the exhaust hole are communicated with the containing cavity, and the solid hydrogen storage material is contained in the containing cavity of the hydrogen supply container; the hydrogen supply container is inserted into the agricultural substrate, liquid and the solid hydrogen storage material in the containing cavity are controlled to react to release hydrogen by regulating and controlling liquid inlet parameters of the liquid inlet, and hydrogen overflows to the agricultural substrate from the exhaust hole; the solid hydrogen storage material comprises at least one of magnesium hydride, calcium hydride, potassium hydride, ammonia borane, potassium borohydride, magnesium borohydride and calcium borohydride. By adjusting the liquid inlet parameters of the liquid inlet, such as liquid inlet material composition, liquid inlet amount, liquid inlet speed, liquid inlet pH value and the like, the process of supplying hydrogen to the agricultural substrate is simply and conveniently controlled, and the problems that hydrogen supply is not uniform, unstable, difficult to continue and the like are solved.

The invention discloses a method for prolonging the service life of a three-position valve on an atomic luminoscope at a relatively low temperature, relates to the technical field of analytical instruments, and aims to solve the problem of liquid leakage caused by a gap generated by the difference of thermal expansion coefficients of a valve core and a valve body of the three-position valve in a low-temperature environment by adopting a thermal compensation sealing technology. The valve element is expanded through heating to compensate the gap, and the sealing performance is recovered. The method specifically comprises two modes of directly heating the valve element or indirectly heating the current-carrying liquid and the reducing agent flowing through the valve element. Constant-temperature hot air is adopted for direct heating, and hydrochloric acid current-carrying liquid and a potassium borohydride reducing agent containing potassium hydroxide are preheated and then introduced into the valve body through indirect heating. The leakage three-position valve can stop leakage immediately, the recovery degree of the liquid suction amount of the injector is high, the stability of the correlation coefficient of the standard curve is improved, the service life is prolonged, the cost of spare parts is saved, the analysis efficiency and economic benefits are remarkably improved, existing instruments do not need to be transformed, and operation is easy, convenient and safe.

The invention provides a synthesis method of 4, 4 '-(2-pyridylmethyl) bisphenol, which comprises the following steps: (1) 2-pyridine formyl chloride hydrochloride and phenyl ether are subjected to Friedel-Crafts acylation to obtain a compound II; (2) obtaining a compound III from the compound II under the action of a reducing agent sodium borohydride or potassium borohydride; (3) performing Friedel-Crafts alkylation on the compound III and phenol to obtain a compound IV; and (4) carrying out dealkylation on the compound IV in a reducing agent hydrobromic acid or hydroiodic acid to obtain the compound I 4, 4 '(2-pyridylmethyl) bisphenol. The method has the advantages of high yield, mild reaction conditions, few byproducts and simple process, and has high industrial application value.

The application discloses a kind of solid hydrogen storage materials and preparation method thereof.The material is dense solid composite, by hydrogen production agent, non-noble metal boride catalyst and composite lithium cobalt oxide carrier is formed by pressure molding, and water can be supplied hydrogen.Hydrogen production agent is based on sodium borohydride or potassium borohydride;The carrier is modified composite lithium cobalt oxide, and has carrier and catalytic function.This application eliminates liquid solvent and porous support structure, builds synergistic catalytic system, to improve mass and volume hydrogen storage density, and ensure stable hydrogen production rate.Preparation method only involves solid phase mechanical mixing and pressing molding, and process is simple, suitable for large-scale production.The material has the characteristics of portable, safe, and can be used as an ideal hydrogen source, applied to hydrogen fuel cell and other fields.

This invention discloses a method for preparing flake potassium cyanate. Urea and potassium borohydride are ground in an agate mortar at a mass ratio of 1:0.10–0.12 for 30–60 minutes to obtain a first substance. The first substance is then spread evenly in a covered crucible and placed in the center of a muffle furnace. A solid-state melting method is used to ensure a complete reaction. The muffle furnace is heated from room temperature at a rate of 3–5 °C per minute. ‑1 The mixture was heated at a rapid rate until it reached 500–600°C, and held for 120 minutes to obtain a second substance. After the reaction was complete, the second substance was allowed to cool naturally, then washed with anhydrous ethanol, centrifuged, dried, and cooled to room temperature to obtain flake potassium cyanate. This invention proposes a novel method for preparing flake potassium cyanate using a solid-state melting method. The process for preparing flake potassium cyanate is simple, completed in one step, and has good application prospects.

This invention discloses a method for synthesizing N-amino-3-azabicyclooctane hydrochloride, relating to the field of fine chemical synthesis. The method begins with cyclohexanone to construct 2-formamide-cyclohexanone, followed by chlorination at 0°C to 5°C, and then a ring-condensation rearrangement reaction in methanol at 10°C to 15°C for 10 hours to construct a cyclopentanediimide precursor skeleton. Next, in a zinc chloride and potassium borohydride reduction system, a first reduction salting reaction is performed under reflux with a gradient temperature increase up to 100°C to obtain 3-azabicyclooctane hydrochloride. Finally, a second reduction salting reaction involving nitrosation and zinc powder is carried out sequentially. This invention effectively suppresses side reactions such as ring-opening by precisely controlling the temperature, timing, and feed gradient of the rearrangement and ring-condensation steps, significantly improving the conversion rate of the target skeleton and the purity of the final product.

This invention proposes an online monitoring method for total arsenic in water, comprising the following steps: mixing a water sample with a potassium persulfate aqueous solution and heating to digest it, oxidizing all forms of arsenic to pentavalent arsenic; adding sulfuric acid and tartaric acid to the digestion solution to adjust the pH to 12, and adding ascorbic acid and potassium iodide to complex copper ions, adding potassium borohydride to generate arsine, and purging with air to remove the arsine; introducing the arsine into an iodine and potassium iodide aqueous solution to oxidize it to arsenate, then adding ammonium molybdate to generate arsine molybdenum heteropolyacid, and again adding ascorbic acid and potassium iodide to reduce it to molybdenum blue; measuring the absorbance and plotting a standard curve to calculate the total arsenic content. By using an iodine-potassium iodide solution as the arsine absorption solution, the absorption efficiency and stability are superior to conventional acidic potassium permanganate solution; simultaneously, tartaric acid masks antimony ions, and ascorbic acid and potassium iodide synergistically complex copper ions, effectively eliminating Sb. 3+ / Cu 2+ Interference can be eliminated to achieve accurate online monitoring of total arsenic in water.

The present application relates to a kind of synthesis methods of reducing ambrox, comprising the following steps: ambrinol is dissolved in organic solvent, then adding catalyst aluminum trichloride, quaternary ammonium salt catalyst, then stirring condition is at least divided into 3 times and adds potassium borohydride, control reaction liquid temperature is 20-25 degrees Celsius, the total consumption time of first feeding to reaction end of potassium borohydride is 2-5h, reaction generates reducing ambrox, obtains the reaction liquid containing reducing ambrox;Dilute sulfuric acid is added to the reaction liquid containing reducing ambrox, adjusts the pH of reaction liquid to 3-4, keep 1h, then drop alkali solution, adjust the pH of reaction liquid to 5.2-7.5, keep 1h, filter, filtrate is placed and is layered, organic solvent layer is concentrated to dryness under reduced pressure and obtains reducing ambrox product.The present application process condition is mild, yield is high, product purity is good, raw material cost is low, pollution is small, easy to industrialization.

The invention provides a preparation process of super ambrota ether, and relates to the technical field of perfume production, and the preparation process comprises the following preparation steps: mixing palladium carbon powder and absolute ethyl alcohol, introducing nitrogen and carrying out ultrasonic oscillation, adding polyethyleneimine, heating and filtering to obtain core-shell particles; mixing and heating the core-shell particles, potassium borohydride and a citric acid solution, filtering and drying to obtain a composite reducing agent; the method comprises the following steps: mixing sclareolide, a composite reducing agent and tetrahydrofuran, exhausting, heating, cooling, filtering, adding n-hexane, standing, taking an upper oil phase, and distilling to obtain sclarediol; the method comprises the following steps: mixing sclarediol, methylbenzene and an acid catalyst, heating and refluxing, filtering, cooling and washing, standing and layering, separating out an upper organic phase, drying and filtering to obtain a prefabricated crude product; mixing and heating the prefabricated crude product and absolute ethyl alcohol, cooling and recrystallizing, filtering and separating, washing and drying to obtain the super ambrota ether. According to the method, the yield of the super ambrota ether can be improved, and the recovery of reaction raw materials is also realized.