55 results about "Tetrabutylammonium hydrogen sulfate" patented technology

The invention discloses a method for determining N-methylamino ammate in production of acesulfame. The method mainly comprises the steps of: (1) selecting an analytical chromatographic condition, an ODS column (4.6mm*25cm) or other equivalent chromatographic columns, wherein the wavelength is 250nm, the flow velocity is 1ml/min, the column temperature is 25 DEG C, and the sample amount is 20mu l; (2) preparing tetrabutylammonium hydrogen sulfate solution from deionized water until the molar concentration is 1.0-2.0mmol/L, and preparing a mobile phase from the prepared tetrabutylammonium hydrogen sulfate solution and chromatographic grade methanol according to the volume ratio of 60 to 40; (3) diluting the sample to be tested by an organic solvent according to the volume ratio until the concentration is 0.5-2.0%, so as to prepare a test solution; (4) absorbing the test solution by a microinjector, injecting into an efficient liquid chromatograph, and analyzing by an area external standard method; and (5) recording the content of the N-methylamino ammate in the sample to be tested. By adopting the method disclosed by the invention, the content of the N-methylamino ammate can be accurately and rapidly determined.

The present invention provides a detection method for sodium impurities in omeprazole. The method comprises the following steps: 1) adopting a high performance liquid chromatography, wherein chromatographic conditions comprise that: octadecylsilane chemically bonded silica gel is adopted as a filler, a phosphate buffer, a tetrabutylammonium hydrogen sulfate buffer and acetonitrile are mixed according to a volume ratio of 64:6:30 to be adopted as a mobile phase, and a detection wavelength is 280 nm; 2) preparing a system suitability test solution, wherein 10 ml of omeprazole is placed in a 50 ml volumetric flask, 5 ml of a mixing solution is added to the 50 ml volumetric flask, a shaking treatment is performed to dissolve, and the solution inside the 50 ml volumetric flask is diluted into 50 ml to obtain a mixed solution of omeprazole and an omeprazole sulfonylation compound, wherein the mixing solution is prepared by mixing a potassium permanganate solution with a mass content of 0.05% and acetonitrile according to a volume ratio of 1:1, and the resulting mixed solution is adopted as the system suitability test solution; and 3) measuring, wherein 10-20 mul of the system suitability test solution is taken and injected into the chromatograph, and the chromatogram is recorded. With the present invention, the impurities are effectively destroyed, the analysis is accurate, the system stability is good, the balance time is short, and the coat is low.

The invention discloses a preparation method of a 24-epibrassinolide intermediate, and belongs to the field of chemical synthesis, and the preparation method comprises the following steps: 1) taking ergosterol as an initial raw material, carrying out methanesulfonylation under the catalysis of tetrabutylammonium hydrogen sulfate to obtain a first-step product, namely an intermediate 1, filtering afirst-step reaction solution, and directly carrying out a next-step reaction on a filtrate; 2) adding water and potassium bicarbonate into the filtrate obtained in the step 1), carrying out heating reaction, and carrying out split-phase water removal, concentration, cooling and filtration to obtain an intermediate 2; 3) reacting the intermediate 2 with benzyl halide in the presence of an acid-binding agent to generate an etherification product; 4) reacting the etherification product with tetrabutylammonium bromide and tetrabutylammonium hydrogen persulfate to obtain an intermediate 3; compared with a traditional CrO3/pyridine oxidation method, the method has the advantages that the use of an oxidizing agent containing heavy metal chromium and having serious pollution to the environment isavoided, the reaction conditions are mild, the yield is high, the post-treatment is simple, the next step of reaction can be performed without refining, and the method is suitable for industrial production.

The invention discloses a tetrabutylammonium hydrogen sulfate buffer salt system for liquid chromatogram detection. A solvent is water, and a solute comprises tetrabutylammonium hydrogen sulfate and a buffer ion pair; the buffer ion pair is composed of monopotassium phosphate and phosphoric acid; and the solute also comprises a complexing agent which is optimized from dipotassium ethylene diamine tetraacetate. The tetrabutylammonium hydrogen sulfate buffer salt system provided by the invention is stable within 24h and is free of a turbid phenomenon. Taking moxifloxacin hydrochloride related substance analysis as an example, the chromatographic behaviors of the tetrabutylammonium hydrogen sulfate buffer system placed for 24h at room temperature and a newly prepared tetrabutylammonium hydrogen sulfate buffer system on a reversed phase column to moxifloxacin, N-methyl impurities, an impurity A, an impurity B, an impurity C, an impurity D and an impurity E are substantially resistant.

The invention discloses a preparation method of a ligand, a fluorescent probe, and a preparation method and an application of the fluorescent probe. The ligand is DATP, and is obtained by reacting a compound 1, NaN3, tetrabutylammonium hydrogen sulfate, bis(2-pyridylmethyl)amine, propargyl bromide, CuI, and a CH2Cl2 and CF3COOH mixed solvent. The fluorescent probe adopts DATP and Ni<2+> as cores,Eu<3+> and Ni<2+> are linked with the ligand through a Ni-N coordination bond, and Tb<3+> is linked with the ligand trough Tb-O and Tb-N coordination bonds. The fluorescent probe of the invention is prepared with DATP as the core, and a Eu<3+>/Tb<3+> complex can be used in time-resolved fluorescence detection to effectively eliminate interference from samples and short-lived fluorescence such as scattered light, so the prepared fluorescent probe has the advantages of good water solubility, extremely high sensitivity, excellent selectivity to histidine, simple preparation method and mild conditions, and is suitable for detecting histidine in biological systems.

The invention discloses a method for measuring sodium sulfite content through high performance liquid chromatography. The method uses octadecylsilane chemically bonded silica as a filling agent, and uses tetrabutylammonium hydrogen sulfate-added phosphate buffer solution-methanol as mobile phases, wherein the volume ratio of the buffer solution to the methanol is 90: 10 to 70: 30; the detection wavelength is 214+/-5nm; and the flow rate is 0.5 to 1.2ml/min. By adopting the method, the sulfite ion can be effectively separated from other similar ions, and the sulfite ion can be accurately quantified. The method is high in specificity, excellent in precision, high in accuracy, and capable of quickly and accurately measuring the sodium sulfite content.

The invention relates to a method for synthesizing benzyl alkyl disulfide. Thiourea and benzyl thiocyanate taken as sulfur sources, alkyl halide taken as a raw material, potassium iodide and tetrabutylammonium hydrogen sulfate taken as catalysts, potassium phosphate taken as alkali react in water to obtain an asymmetric benzyl alkyl disulfide compound. According to the method, sulfur alcohol with pungent smell is prevented from being used as a sulfur source, and a microwave reaction technology and a one-pot method are adopted, so that the purposes of green and environmental protection can be achieved, the operational program is simplified, and the costs of synthesis and large-scale production are further reduced.

The invention provides a method for detecting related substances in a ketoconazole sample, a method for preparing compound ketoconazole cream or compound ketoconazole hair lotion and a preparation containing ketoconazole. The method for detecting the related substances in the ketoconazole sample comprises steps as follows: the related substances in the ketoconazole sample are detected with HPLC (high-performance liquid chromatography), loperamide hydrochloride is adopted as a reference substance, a flowing phase A is a tetrabutylammonium hydrogen sulfate solution with the concentration being 0.34w/v%, and a flowing phase B is acetonitrile. With the adoption of the detection method, the related substances in the ketoconazole sample can be effectively detected.

The invention discloses a 1-amino-3-alkyl-1, 2, 3-triazole nitrate compound and its synthesis. The synthesis method consists of: taking glyoxal and hydrazine hydrate as materials to react to obtain glyoxal bishydrazone; taking water as a solvent, adding the glyoxal bishydrazone and a catalyst to react so as to obtain 1-amino-1, 2, 3-triazole; then adopting water as the solvent, in the presence of a phase transfer catalyst tetrabutylammonium chloride or tetrabutylammonium hydrogen sulfate, adding a alkylation reagent dropwisely to undergo reaction to obtain 1-amino-3-alkyl-1, 2, 3-triazole bromide; and finally using water as the solvent, and adding silver nitrate to undergo reaction, thus obtaining the 1-amino-3-alkyl-1, 2, 3-triazole nitrate. The compound 1-amino-3-alkyl-1, 2, 3-triazole nitrate provided in the invention is an energetic surfactant. Adding of the energetic surfactant into mixed explosives can enhance the physicochemical properties and dispersion performance, etc., and has little influence on the overall energy of the mixed explosives. The synthesis process involved in the invention is carried out in a solvent-free condition or in a water solution, the cost is low, and the environmental pollution is small, thus meeting the dual development needs of environment and economy.

The invention relates to a preparation method and application of a conjugated organic framework/perfluorinated sulfonic acid resin composite proton exchange membrane, belonging to the field of proton exchange membrane fuel cells. The invention aims to solve the technical problems of low proton conductivity and low mechanical property of existing perfluorosulfonic acid proton exchange membranes. The preparation method comprises the following steps: 1, dissolving phosphonitrilic chloride trimer and melamine in an organic solvent, then adding triethylamine and tetrabutylammonium hydrogen sulfate, and carrying out a reflux reaction to obtain COF; step 2, ultrasonically dispersing COF in N-methyl pyrrolidone, and then adding perfluorinated sulfonic acid resin powder to obtain an emulsion; and 3, blade-coating a glass plate with the emulsion, and carrying out post-treatment to obtain the COF/perfluorinated sulfonic acid resin composite proton exchange membrane. The proton exchange membrane is used for preparing a fuel cell or a water electrolysis device. The method is simple and rapid in process and low in raw material price, the obtained composite membrane is uniform and good in interfacial compatibility, and the proton conductivity and the mechanical performance of the perfluorosulfonic acid proton exchange membrane can be improved at the same time.

The invention discloses a method for rapidly extracting benzo[a]pyrene in food. The method comprises the following steps: drying food, and crushing the food by a homogeneous disperser and performing homogenization to obtain a sample for standby; adding a component A, a component B and distilled water in a centrifuge tube in order, uniformly mixing the materials and performing centrifugation for 3-10 min at 3000-8000 r/min so that a super molecular solvent phase and a water phase are in an up-down structure, removing the water phase at a lower layer, and keeping an upper layer super molecular solvent; wherein the mass ratio of the component A to the component B to distilled water is 1:0.2-0.4:5-10, the component A is at least one of tetrabutyl ammonium hydroxide, tetrabutylammonium bromideand tetrabutylammonium hydrogen sulfate, the component B is at least one of heptanol, octanol and nonanol, mixing the sample in the step a) and the super molecular solvent in the step b) and performing ultrasonic processing for 5-20 min under 20-40 KHz, then passing the mixed liquor through an organic filter membrane with 0.45 [mu]m, and taking the filter membrane liquid.

The invention provides a pentafluorophenol preparation method, which comprises: using hexafluorobenzene and potassium hydroxide as raw materials, adding an appropriate amount of tetrabutylammonium hydrogen sulfate, N-sulfopropyl-3-methylpyridine triflate, N-methyl-2-[(2-methylphenoxy)acetyl]hydrazinium methylthioamide and 2,2,6,6-tetramethylpiperidine-oxynitride to a tert-butyl alcohol aqueous solution with a mass fraction of 80-85%, heating to achieve a slight boiling state, carrying out a reflux reaction for 2-3 h, adding an appropriate amount of water, distilling to recover the tert-butyl alcohol solvent, adjusting the PH value of the remaining aqueous solution by using refined hydrochloric acid to 9-10, adsorbing with a functionalized D101 macroporous adsorption resin, acidifying with refined hydrochloric acid to achieve the PH value of 1-2, layering, distilling the upper layer water phase until no oily substance exists, collecting the distilled product, combining the collected product and the lower layer oil phase, rectifying, collecting the distillate at the temperature of 142-144 DEG C, and cooling to a room temperature to obtain the colorless and transparent crystal pentafluorophenol. According to the present invention, the preparation method has advantages of simple and reasonable process, less side reactions, high reaction yield and high product purity, and can meet the quality requirements for the preparation of the high-quality liquid crystal materials and drugs.

The invention relates to the technical field of composite conductive adhesives, and discloses a nano-silver powder conductive adhesive with good conductivity. The nano-silver powder conductive adhesive includes the following raw materials in parts by weight: 100 parts of epoxy resin E-51 matrix resin, 98 parts of a curing agent, 0.67 part of a curing accelerator, a composite self-sintering surfactant composed of 1-3 parts of benzyltriethylammonium chloride and 1-4 parts of tetrabutylammonium hydrogen sulfate, 140-165 parts of a nano silver powder conductive filler, 1 part of a malonic acid conductive accelerator, 2 parts of a silane coupling agent, 1 part of an antioxidant and 2 parts of an antifoaming agent. The nano silver powder conductive adhesive solves the technical problem that the existing nano silver powder conductive adhesive has poor conductivity while meeting high-density connection.

The invention provides a peonile synthesis method. The peonile synthesis method includes that cyclohexanone and benzyl cyanide are subjected to reaction in an inorganic alkali solution under a catalytic action of tetrabutylammonium hydrogen sulfate. The peonile synthesis method has advantages of technical simplicity, mild reaction conditions, high reaction selectivity and high yield.

The invention relates to a method for detecting the dissolution rates of a glucosamine hydrochloride preparation. Isocratic elution is carried out by taking a monopotassium phosphate buffer solution-acetonitrile containing a positive ion pair reagent (tetrabutylammonium hydroxide, tetrabutylammonium hydrogen sulfate or tetrabutylammonium bromide) as a mixed mobile phase, and the proportion of the mixed mobile phase is optimized; during chromatographic analysis, the retention time of the main peak of the glucosamine hydrochloride on a chromatographic column (such as a C8 column) is prolonged, the main peak is prevented from being interfered by a dissolution medium and an auxiliary material solution, the reproducibility is good, and the sensitivity is high. By adopting the dissolution rate detection method provided by the invention, the requirement on a chromatographic column is low in the chromatographic analysis process, an amino column is not needed, a pre-column derivatization reaction is not needed, the method can adapt to the accurate determination of the dissolution rates of the glucosamine hydrochloride preparation in different dissolution media, the interference of a blank solvent and auxiliary materials is eliminated, and the method has the advantages of simple operation, high sensitivity, low cost, good reproducibility, high accuracy and wide application range.

The invention belongs to the field of organic substance content detection, and particularly relates to a method for detecting the content of 3, 3, 20, 20-bis(ethylenedioxy)-17alpha-hydroxy-19-norpregna-5(10),9(11)-diene in an ulipristal acetate intermediate I. The method comprises the following steps: preparing a test solution; preparing a reference substance solution of 3, 3, 20, 20-bis(ethylenedioxy)-17alpha-hydroxy-19-norpregna-5(10),9(11)-diene; wherein chromatographic conditions are shown as follows: octadecylsilane is used as a stationary phase, a mobile phase is selected for gradient elution, and the detection wavelength is 235 nm; wherein the mobile phase A is a tetrabutylammonium hydrogen sulfate solution with the mass concentration of 0.01%-0.1% or a lauryl sodium sulfate solution with the mass concentration of 0.01%-0.1%, and the mobile phase B is acetonitrile; determining the content. The detection result is accurate, and the detection method is efficient, quick and sensitive, so that the quality of the ulipristal acetate finished product is improved.

The invention relates to capturing and eliminating dry powder for efficiently removing hydrogen sulfide gas, and a preparation method thereof. A purpose of the present invention is mainly to solve theproblems of low hydrogen sulfide removal rate and easy secondary pollution in the prior art. According to the technical scheme, the capturing and eliminating dry powder comprises granular active carbon, a modifier, a promoter and an adjusting agent, wherein the modifier comprises a soluble iron salt, a soluble copper salt and a soluble zinc salt according to a mass ratio of 1-10:1-10:1-10, the promoter is at least one selected from tetrabutylammonium bromide, tetrabutylammonium chloride and tetrabutylammonium hydrogen sulfate, the adjusting agent is at least one selected from K2CO3, Na2CO3, KHCO3 and NaHCO3, and based on the amount of the dried granular active carbon, the adding amount of the modifier is 1-5%, the adding amount of the promoter is 0.01-0.1%, and the adding amount of the adjusting agent is 0.01-0.05%. With the technical scheme, the problem in the prior art is well solved. The capturing and eliminating dry powder of the present invention can be used for the capturing andeliminating of hydrogen sulfide gas.

The invention relates to the technical field of preparation of tetrabutylammonium hydrogen sulfate and particularly relates to a system and a method for preparing high-purity tetrabutylammonium hydrogen sulfate through an electrolysis process. The system comprises an electrolyte supply system, an electrolytic tank and a gasification system, wherein an outlet of the electrolyte supply system is connected with an electrolyte inlet of the electrolytic tank; a cathode hydrogen outlet of the electrolytic tank is connected with an inlet of the gasification system; the electrolyte supply system comprises a reaction kettle; the reaction kettle is connected with an iodobutane adding device and a tributylamine adding device. Through the system and the method, tetrabutylammonium hydrogen sulfate is prepared by the electrolysis process; the system and the method are green and environmentally friendly and are low in pollution; the prepared tetrabutylammonium hydrogen sulfate is high in yield and purity; meanwhile, the preparation process is simple and is suitable for large-scale production of middle and small-sized enterprises.

The invention discloses a method for preparing a polycarboxylate superplasticizer macromonomer by using a waste lithium battery, namely, a preparation and synthesis method of allyl polyethylene glycol monomethyl ether. The method is characterized by comprising the steps of making polyethylene glycol monomethyl ether react with chloropropene at a temperature of 60 DEG C for 4-5 hours under the conditions that metal lithium extracted from the recovered waste lithium battery is used as a catalyst, tetrabutylammonium hydrogen sulfate is used as a phase transfer catalyst and an atmosphere is protected by an inert gas, and continuously cooling at a temperature of 50 DEG C for 1 hour to discharge the polycarboxylate superplasticizer macromonomer. According to the method, lithium in the recovered waste lithium battery is used as the catalyst, so that the resource is favorably recycled. Compared with a conventional direct esterification method, the method has the advantages that the reaction can be performed at a relatively low temperature of 50-60 DEG C and a normal pressure, the requirement for equipment is relatively low, the retention rate of generated double bonds is high, and the generated allyl ether bonds are more stable than allyl ester bonds and are difficult to hydrolyze. The method is relatively high in reaction conversion rate, free from waste emission in a preparation process, and low in production cost.

The method comprises the following steps: (1) taking a graphite sheet A as a positive electrode, a platinum electrode as a negative electrode and a sulfate solution B as an electrolyte, and keeping for 0.3-3 hours under the direct current voltage of 1-5V; (2) the electrolyte is replaced with a weakly alkaline electrolyte C, the voltage is adjusted to be 5-30 V, electrification continues to be conducted for 0.5-5 h, a precipitate D is obtained, and the weakly alkaline electrolyte is obtained by adjusting the pH value of the sulfate solution to be 8-14 through tetrabutylammonium hydrogen sulfate; (3) dissolving the precipitate D obtained in the step (2) in an organic solvent, and performing ultrasonic treatment to obtain a solution E; centrifuging the solution E, and performing suction filtration and cleaning on the supernatant with deionized water to obtain a separated solid; and (4) drying the solid separated in the step (3) to obtain the high-purity graphene. The obtained graphene has a low degree of oxidation, a small number of layers and a large size.

The invention belongs to the field of chemical plating and particularly relates to a chemical nickel-tin-tungsten-phosphorus-plating amorphous multifunctional alloy plating solution and plating thereof. The chemical nickel-tin-tungsten-phosphorus-plating amorphous multifunctional alloy plating solution comprises following components: NiSO4.6H2O.NaH2PO2.H2O.SnCl4.3H2O, tungsten salt, NSWP synergist, complex carboxylic acid complexant, amidogen catalyzed complexant, a surface active agent and water; and the NSWP synergist is composed of ammonium sulfate, ammonium chloride, ammonium acetate, tetrabutylammonium hydrogen sulfate, sodium fluoride, sulfated castor oil and the like. The plating solution is very high in stability and very large in deposition velocity; and pinhole defects caused bythe plating solution are prevented, the plating solution can be attached to a base material better, and the plating is not prone to falling off. The invention further provides the plating of the plating solution. The plating is high in abrasion resistance, tenacity and ductility, and the resistance to corrosion of hydrogen sulfide, chloride and carbon dioxide is improved.