32 results about "Disulfur dioxide" patented technology

The present application relates to a kind of catalyst for preparing ethylene sulfite, the preparation method of ethylene sulfite, the catalyst includes organic aluminum compound and amine, the molar ratio of the organic aluminum compound and the amine is 1-5:1.The preparation method of ethylene sulfite includes the reaction of contacting ethylene oxide with sulfur dioxide in the presence of the catalyst.The quaternary ammonium salt in the catalyst of the present application and trialkylaluminum are excited by phase transfer and coordination, etc.Effect, monomer ring-opening of ethylene oxide, promote SO2 and ethylene oxide to react to generate ethylene sulfite, and then high-purity ethylene sulfite is prepared with high yield.

The invention belongs to the field of chemical reagent moisture detection, and particularly relates to a coulometry Karl Fischer reagent for aldehyde ketone moisture detection and a preparation method of the coulometry Karl Fischer reagent. The coulometry Karl Fischer reagent for aldehyde ketone moisture detection is prepared from the following components in parts by weight: 1 to 15 percent of imidazole, 1 to 15 percent of 2-methylimidazole, 25 to 70 percent of ethylene glycol monomethyl ether, 5 to 30 percent of trichloromethane, 2 to 30 percent of trifluoroethanol, 2 to 10 percent of sulfur dioxide, 1 to 10 percent of methyl iodide, 0.1 to 5 percent of tetrabutylammonium iodide and 0.1 to 5 percent of iodine. The method does not contain hydroxyl compounds, effectively inhibits the generation of side reactions in detection, ensures the detection accuracy, and improves the product stability and effectively shortens the instrument equilibrium time by adding iodomethane and tetrabutylammonium iodide.

The application belongs to the technical field of chondroitin sulfate preparation, and particularly relates to application and application method of liquid sulfur dioxide in preparation of chondroitin sulfate or chondroitin sulfate salt. In the application, liquid sulfur dioxide is used as a solvent to perform sulfonation modification treatment on unsulfated chondroitin, on the one hand, the use of traditional high-boiling organic reagents is avoided, the difficulty of three-waste treatment is reduced, and the process is more green and environmentally friendly; on the other hand, the post-treatment operation of the sulfonation reaction is simpler, and sulfur dioxide can be removed from the system by only temperature control or pressure adjustment, so that solvent residues possibly existing in the final product are avoided, and the product is safer. In addition, by adjusting the key conditions of the sulfonation reaction, the proportion of chondroitin sulfate with 6 independent sulfation in the disaccharide unit of the sulfonation product is 70% to 90%, the reaction is stable and reliable, and the sulfonation rate is high.

The application provides a novel ratio near-infrared fluorescent probe for detecting sulfur dioxide, a preparation method and application of the fluorescent probe, the fluorescent probe is Cou-Oxo, the preparation method comprises the following steps: dissolving a compound Cou-CN and a compound 3 in toluene, adding piperidine to catalyze a reaction, refluxing at 114-116 DEG C under a nitrogen atmosphere for 4.8-5.2 hours, and after the reaction is completed, the fluorescent probe Cou-Oxo is obtained through purification.The ratio fluorescent probe has good light emitting characteristics, can effectively detect sulfur dioxide derivatives, has the potential of quantitative detection, and the lower limit of detection is 0.942 muM.The ratio fluorescent probe has a fast response to the detection of sulfur dioxide derivatives, has good light emitting characteristics and stability, and can detect HSO3 ‑ in a physiological pH range of 7-9; the ratio fluorescent probe has lower biological toxicity and is suitable for cell imaging.

The invention discloses a novel phosphoric acid purifier and a preparation method thereof. The novel phosphoric acid purifier comprises the following mass percentages of hydrosulfate 34-40.0%, sodium carbonate 21-24%, sulfate 3%, sulfur dioxide about 1%, and the balance water. A method for preparing a novel phosphoric acid purifier comprises the following steps: step 1: adding a measured amount of sodium thiosulfate to a reactor, heating and dissolving it; step 2: adding a measured amount of catalyst and an organic flocculant to prepare it under a temperature of 60°C-80°C. Sodium thiosulfate is used to replace sodium sulfide, sodium thiosulfate is used as a basic raw material, sodium thiosulfate is modified, and a suitable catalyst is added to increase the decomposition rate of S2-, so as to reduce the arsenic ions in a high arsenic-containing phosphoric acid solution from 60ppm to below 0.5ppm, thereby achieving the purpose of phosphoric acid dearsenicization.

The application discloses a method for continuously preparing high-purity sulfolane, and belongs to the technical field of organic synthesis. By introducing a solvent and a stable free radical type polymerization inhibitor, the self-polymerization of butadiene is effectively inhibited. By adopting a cooling crystallization mode to remove sulfur dioxide, the thermal decomposition of sulfolene sulfone is avoided, high yield and high purity are realized, the service life of a hydrogenation catalyst is not affected, and the catalyst can be completely reused. The cooling crystallization also realizes the separation of the polymerization inhibitor and sulfolene sulfone. The polymerization inhibitor is dissolved in the solvent and recycled, and does not enter the hydrogenation system, so that the final sulfolane product has a purity of above 99.9% and has no chromaticity problem. The process saves energy consumption, the solvent has wide universality, operation is simple, the process is safe and environment-friendly, easy to scale up, and meets the green production requirements.

The invention relates to a method for manufacturing sulphuric acid, which involves converting sulphur dioxide SO2 into sulphur trioxide SO3, by injecting gaseous sulphur dioxide into a converter (1) inside which at least one mass (2) of a catalyst for the conversion is present, and according to which, during phases in which the injection of the gaseous sulphur dioxide is stopped, the space inside the converter (1) is heated in such a way as to maintain a minimum temperature of 200° C., and preferably 250° C., within each catalyst mass (2), characterized by the fact that the stopping of the injection of the sulphur dioxide is slaved to the starting of the heating, and vice versa.

The invention discloses a preparation method of light-mediated aryl / heteroaryl sulfonamide and derivatives thereof, the reaction route is shown in the following formula, and the reaction comprises the following steps: (1) under the irradiation of blue light, reacting carboxylic acid active ester shown in the formula I with a sulfur dioxide source under the catalysis of a photocatalyst; and (2) acidifying the reaction product obtained in the step (1) to obtain the aryl / heteroaryl sulfonamide product as shown in the formula II. The method for catalyzing the reaction of the carboxylic acid active ester and the sulfur dioxide source under the action of the photocatalyst and the blue light to obtain the corresponding sulfonamide derivative has the advantages of simple reaction process operation, mild reaction conditions, recoverable raw materials, strong compatibility and adaptability, and wide substrate range and universality. # imgabs0 #

A method can include: introducing sulfur dioxide in an anolyte flow path of an electrolyzer; optionally, introducing water in the catholyte flow path of the electrolyzer; operating the electrolyzer; optionally: processing the products; and optionally: using the products. In some variants of the method, the amount of water introduced can be balanced such as to achieve a target sulfuric acid concentration.

The utility model belongs to the technical field of sulfuryl fluoride preparation equipment, and particularly relates to a reactor for preparing sulfuryl fluoride, which comprises a bottom frame, an outer barrel fixedly connected to the top of the bottom frame, a reaction barrel fixedly connected to the inside of the outer barrel, a bearing fixedly connected to the inner side of the reaction barrel, and a rotating frame fixedly connected to the inner side of the bearing. The rotating shaft drives the inner ring to rotate so as to drive the connecting rods to enable the outer ring to drive the spiral columns to rotate, the spiral columns are rotated by starting the motor, and the upper and lower adjacent spiral columns are arranged in a staggered manner, so that potassium fluoride particles attached to the outer sides of the spiral columns can be in full contact with sulfur dioxide and fluorine gas, and the reaction is more thorough; therefore, the preparation efficiency is improved.

The present application relates to a method for preparing sulfuryl fluoride, the method comprising: (1) providing a reaction stream comprising an organic base-hydrogen fluoride complex; (2) introducing sulfur dioxide and chlorine into the reaction stream comprising the organic base-hydrogen fluoride complex, and reacting to form a product stream comprising sulfuryl fluoride. The method described in the present application has mild reaction conditions, high product yield and purity, material recycling, less waste, etc., and is suitable for industrial production.

The present invention relates to a reducing scale inhibitor and a preparation method thereof, comprising the following components in mass percentages: thiourea dioxide 1-1.5%, sodium bisulfite or sodium metabisulfite 10-15%, urea 3-5%, sodium hexametaphosphate 10-20%, hydrolyzed maleic anhydride 8-10%, oxalic acid 5-10%, and the balance being water. The reducing scale inhibitor of the present invention can significantly reduce the ORP and residual chlorine in wastewater with only a small dosage, and at the same time has a good scale inhibition effect on calcium ions, iron ions, manganese ions, etc. in the wastewater.

A method for preparing cyano sulfonyl fluoride compounds is provided. Oxime ether compounds are used as free radical precursors, and under the condition of photocatalyst regulation, and in combination with the strategy of free radical sulfur dioxide insertion, the process involves photocatalytic oxidation, C—C bond cleavage rings, free radical SO2 insertion and fluorination to achieve cyano / fluorosulfonyl reaction of oxime ether, yielding cyano sulfonyl fluoride products.

The application discloses a synthesis method of a beta-fluorosulfonyl sulfone compound and application thereof, and belongs to the technical field of chemical synthesis and medicinal chemistry. The method comprises the following steps: under a protective atmosphere, potassium trifluoroborate compound, a photocatalyst, a sulfur dioxide source, a hydrogen source and ethylenesulfonyl fluoride are mixed in an organic solvent, and reaction is carried out under light irradiation to obtain the beta-fluorosulfonyl sulfone compound. The application can realize preparation of a series of beta-fluorosulfonyl sulfone compounds, provides a new synthesis method for synthesis of the beta-fluorosulfonyl sulfone compound, and sulfone groups and sulfonyl fluoride groups are part of the structures of various drug molecules, so that the application is expected to be widely applied in the fields of organic synthesis, drug development and polymer materials.

The invention relates to the technical field of chemical preparation, in particular to a production method and a production system of sodium sulfite, and discloses a production method of sodium sulfite, which comprises the following steps: introducing tail gas containing sulfur dioxide into the system, and then enabling the tail gas to enter a first-stage falling film absorption tower, a second-stage falling film absorption tower and a third-stage falling film absorption tower; the method comprises the following steps: carrying out circulating absorption by using a sodium hydroxide solution containing ethylene glycol, introducing a sodium sulfite solution into a neutralization kettle by using a primary circulating pump, adding liquid caustic soda to adjust the pH value of the sodium sulfite solution to 8-9, and carrying out reduced pressure concentration on water by using a falling-film evaporator to obtain a high-concentration ethylene glycol suspension containing sodium sulfite, introducing the high-concentration ethylene glycol suspension into a centrifugal machine, and ethylene glycol is recycled and reused, so that a sodium sulfite solid containing a trace amount of ethylene glycol is obtained. The problem that when sodium sulfite is prepared in winter in an existing method, the sodium sulfite solution is prone to crystallization, and consequently pipelines are blocked is solved, and the effects of preventing the sodium sulfite solution from crystallization in winter and avoiding pipeline blocking are achieved.

The invention discloses a synthesis method of 18F-labeled alkyl sulfonyl fluoride molecules based on hypervalent iodine (III) carboxylate, which comprises the following steps: in a solvent, in the presence of an 18F-fluorination reagent, a sulfur dioxide source and copper salt, carrying out a reaction shown as follows on a compound shown as a formula II to obtain a compound shown as a formula I, namely the 18F-labeled alkyl sulfonyl fluoride molecules # imgabs0, in which R is # imgabs1 # imgabs2 #, R1 is phenyl or cyano, R2 is phenyl or cyano, and R3 is phenyl or cyano; r1 is methyl, methoxy, nitro, methyl formate and bromine; and R2 is phenyl. The problem of limitation of an existing < 18 > F sulfonyl fluoride labeling method is solved, a novel method which is simple in reaction condition, efficient and good in substrate applicability is developed, synthesis of < 18 > F labeled alkyl sulfonyl fluoride is achieved, raw materials are easy to obtain, and operation is easy.

The invention relates to a method for continuously preparing ethylene sulfate, and belongs to the field of organic chemical industry. The method comprises the following steps: firstly, modifying titanium silicalite molecular sieve particles by adopting a silane coupling agent and nano aluminum trifluoride to obtain titanium silicalite molecular sieve particles with a hydrophobic acidic shell as a catalyst, filling the catalyst into a tower reactor, and adding ethylene oxide and sulfur dioxide into a first mixer and a first preheater; feeding into a tower type fixed bed reactor from the tower bottom under a certain pressure, and reacting under the catalysis of a catalyst hydrophobic acidic shell to obtain ethylene sulfite; hydrogen peroxide and chloroform enter the fixed bed tower reactor from the tower top after passing through a second mixer and a second preheater, and are subjected to oxidation reaction with ethylene sulfite to obtain ethylene sulfate. The ethylene sulfate is prepared in a continuous manner, so that the reaction time is shortened, and the production efficiency and the production safety are improved.

The application provides a kind of construction of indole derivative fluorescent probe for detecting viscosity and sulfur dioxide in vivo, and belongs to the field of biological detection.The fluorescent probe (denoted as BIC) of the application utilizes the strong nucleophilicity of sulfur dioxide, and realizes the specificity selection of sulfur dioxide by generating new product BIC-SO2 through Michael addition reaction with double bond in the structure of probe; in addition, benzene ring and indole in BIC structure can freely rotate in low viscosity environment, resulting in non-radiation consumption of excited state energy, showing very weak fluorescence; in high viscosity solution, the free rotation of probe is inhibited, resulting in the recovery and enhancement of probe fluorescence, showing very strong fluorescence. Therefore, the fluorescent probe of the application can simultaneously detect viscosity and sulfur dioxide in vivo.

The invention discloses a method for efficiently preparing methanesulfonic acid from methane, which comprises the following reaction processes: introducing methane, sulfur dioxide and oxygen into a fixed bed reactor filled with a catalyst, and carrying out gas-liquid separation on reaction components to obtain methanesulfonic acid, the catalyst is a supported catalyst comprising an active metal and a carrier; the active metal comprises at least one noble metal selected from palladium, platinum and iridium and at least one other metal selected from vanadium, molybdenum, iron and potassium. The method has the advantages of simple process, high product yield, mild reaction conditions, easiness in industrialization and the like.

The present application relates to a kind of nickel cobalt hydroxide mass promotion method, the present application directly uses sulfur dioxide and air oxidation after removing iron aluminum, manganese in the liquid after removing iron aluminum, directly convert into manganese dioxide and other manganese oxides, remove manganese first, save the cost of continuous reducing agent;After removing manganese, the liquid is treated to form conversion alkali crystal slurry, itself contains little manganese, and the insoluble and non-reactive manganese oxide caused by excessive alkali problem will not be brought, so that the manganese content in nickel cobalt hydroxide product is reduced, and the quality of nickel cobalt hydroxide product is improved.

The present invention relates to an arylsulfonyl fluoride and a preparation method using an aryliodonium salt as a raw material, comprising: mixing the aryliodonium salt, a sulfur dioxide source, a fluorine source, and a photosensitizer in an organic solvent in an inert gas atmosphere, and stirring the mixture for reaction under light conditions to obtain the arylsulfonyl fluoride; wherein the aryliodonium salt has the following structural formula: #imgabs0# wherein R 1 、R 2 wherein the anion X is H, alkyl, halide, methoxy, cyano, or trifluoromethyl, respectively; and the anion X is a hexafluorophosphate anion, a trifluoromethanesulfonate anion, or a p-toluenesulfonate anion, etc. Compared with the prior art, the present invention, based on a novel strategy of "free radical sulfur dioxide insertion fluorination," achieves efficient, metal-free photocatalytic synthesis of arylsulfonyl fluorides at room temperature. This method has the advantages of mild reaction conditions, simple operation, and good yields. It is also highly applicable to both symmetrical and asymmetrical aryliodonium salts, and the gram-scale reaction provides more possibilities for introducing sulfonyl fluoride groups into drug molecules.

The present invention provides a method for determining the water content in a radioactive suspension, comprising: taking the radioactive suspension and determining the mass of the radioactive suspension; adding the radioactive suspension to a Karl Fischer reagent, causing the water in the radioactive suspension to react with the Karl Fischer reagent and oxidizing iodine to iodide ions, wherein the Karl Fischer reagent at least comprises: iodine, sulfur dioxide, and pyridine; subjecting the iodide ions to electrolytic treatment to reduce the iodide ions to iodine and obtaining the amount of electricity consumed when reducing the iodide ions; and calculating the water content in the radioactive suspension according to the mass of the radioactive suspension and the amount of electricity consumed when reducing the iodide ions. The solution of the present invention can quickly and accurately determine the water content in the radioactive suspension.

The application provides a method for preparing sulfinic acid compounds, sulfinic acid salt compounds, sulfonic acid salt compounds and sulfonyl compounds through sulfinylation, comprising the following steps: under the conditions of a protective atmosphere and light, performing a sulfinylation reaction on an alkyl compound and a sulfur dioxide donor under the condition of a catalyst to obtain an alkyl sulfinic acid compound. The main catalyst comprises a metal salt, and the metal elements in the metal salt comprise one or more of Fe, Cu and Ce; the cocatalyst comprises one or more of chlorosilane, a tetraalkylammonium chloride, an alkali metal chloride and hydrochloric acid. The method in the application has high catalytic efficiency (TON>350000, TOF>50000 / h), high selectivity (the conversion selectivity of sulfinic acid is >99%), high conversion rate (sulfinic acid is close to complete conversion), and is low in cost, high in atomic economy, basically free of waste in the production process, and green, low-carbon and environmentally friendly.

The present application relates to a catalyst for preparing ethylene sulfite, the catalyst comprising a hydrocarbyl borane and a nitrogen-containing organic compound, the molar ratio of the hydrocarbyl borane and the nitrogen-containing organic compound being 0.1-0.5:1. The present application also relates to a method for preparing ethylene sulfite, the method comprising: contacting ethylene oxide with sulfur dioxide in the presence of the catalyst described in the present application. The catalyst of the present application can well catalyze the synthesis of ethylene sulfite, the preparation process conditions are easy to control, and high-purity ethylene sulfite can be prepared at a high yield.

A method can include: introducing sulfur dioxide in an anolyte flow path of an electrolyzer; optionally, introducing water in the catholyte flow path of the electrolyzer; operating the electrolyzer; optionally: processing the products; and optionally: using the products. In some variants of the method, the amount of water introduced can be balanced such as to achieve a target sulfuric acid concentration.

The present invention belongs to the technical field of organic synthesis, and particularly relates to a method for efficiently preparing sulfonyl fluorides. The steps of this method are as follows: Step 1: Under a nitrogen atmosphere and at room temperature, electrochemically electrolyze a reaction mixture formed by trimethyl quaternary ammonium salt, a sulfur dioxide source, a fluorine source, an electrolyte, and a solvent using a constant voltage until the reaction is complete; Step 2: Wash and dry the organic phase, and perform vacuum distillation; Purify to obtain the sulfonyl fluoride compound. The present invention utilizes the electrochemical cathodic reduction of trimethyl quaternary ammonium salt to generate aryl or alkyl radicals; and then reacts with the SO2 source to generate aryl or alkyl sulfur dioxide radicals. These radicals can continue to be oxidized at the anode to generate aryl or alkyl sulfur dioxide cations, which then react with fluoride ions to obtain the target product. This reaction has no intermediate links and is simple and convenient to operate. The synthesis of the target product by an electrochemical method broadens the synthesis methods of sulfonyl fluorides.

The invention provides a method for detecting the content of water in 2, 3, 4-trihydroxy benzophenone 1, 2-diazido naphthoquinone-5-sulfonate, which comprises the following steps: pretreating a sample by using an external dissolution method, measuring the content of water in 2, 3, 4-trihydroxy benzophenone 1, 2-diazido naphthoquinone-5-sulfonate by using a Karl Fischer Coulomb method, and measuring the content of water in 2, 3, 4-trihydroxy benzophenone 1, 2-diazido naphthoquinone-5-sulfonate by using a Karl Fischer Coulomb method. The Karl-Fischer reagent comprises the following components in percentage by mass: 70% of methanol, 10% of diethanol amine, 10% of imidazole, 5% of sulfur dioxide and 5% of hydriodic acid, a sample needs to be pretreated by an external dissolution method before moisture detection, the moisture content m1 of the measured sample, the moisture content m2 of a blank solvent, the weight x1 of the solvent and the weight x2 of the sample are recorded and measured respectively, correction is performed by using a correction formula, and the content of the sample is measured. Finally, the moisture determination of the 2, 3, 4-trihydroxy benzophenone 1, 2-diazido naphthoquinone-5-sulfonate is realized.

A first method for determining moisture content in a sample includes the steps of providing a reagent comprising sulfur dioxide or a derivative thereof; a base; optionally a hydrogen halide or a hydrogen halide donor; a solvent; and a sulfonic acid; and titrating the sample with the reagent. A second method for determining moisture content in a sample includes the steps of providing the reagent described above, mixing the sample with the reagent; and adding an iodine source to the sample and / or the reagent. The reagent can alternatively consist essentially of sulfur dioxide or a derivative thereof; imidazole and / or a derivative thereof; optionally a hydrogen halide or a hydrogen halide donor; acetonitrile; methanesulfonic acid; and methanol and / or ethanol.

The invention discloses a system and a method for producing ammonium sulfite by using electrolytic manganese ammonium sulfate double salt, which are characterized in that the calcination effect is improved through the pretreatment of drying, crushing and the like, and the ammonium sulfate is finally converted into sulfur dioxide through the calcination in an oxygen-free environment to prepare the ammonium sulfite. The difference is that a direct blending and calcining mode is adopted for treatment at home and abroad, but the method cannot be popularized and applied technically and economically, after ammonium sulfate in the ammonium sulfate double salt is decomposed, a high-value ammonium sulfite product can be produced by adopting the mode, and the method is high in technical feasibility and low in cost. And the residual high-manganese-content substance can be used for producing electrolytic manganese metal by an electrolytic manganese system, so that certain economic benefits can be generated, and huge environmental protection benefits and safety guarantee are achieved.

The invention is directed toward the production of 3-methylsulfolene using isoprene and can be used in the chemical and petrochemical industry. A process of producing 3-methylsulfolene using isoprene comprises reacting isoprene with sulfur dioxide in a cyclization reaction in the presence of an isoprene polymerization inhibitor and a tenfold excess of solvent relative to the amount of 3-methylsulfolene produced, at a temperature of 60-80°C and a pressure of 1.0 MPa for 1-2 hours, and subsequently purifying and drying the 3-methylsulfolene. The process is carried out in a plant for producing 3-methylsulfolene which consists of a batch reaction apparatus having an agitator and a heat exchange jacket, a fractionating column, pumps, feedstock tanks, final product tanks, intermediate tanks, a sulfur oxidation unit, a filter unit, and a unit of heat exchangers that are interconnected by a system of pipes with shutoff valves. The process of producing 3-methylsulfolene provides a high yield of high-purity target product, prevents large losses of solvent and enables more efficient use of sulfur, and can be used for industrial-scale production with the aid of the proposed plant, which provides for efficient production of 3-methylsulfolene.