14 results about "Methiodide" patented technology

The invention discloses a synthesis method of a high-abundance C-13 ethylene oxide compound, which comprises the following steps: (1) carrying out reaction on 13CH3I and diphenyl sulfide to obtain [13C] diphenylmethyl iodide; and (2) reacting the [13C] diphenylmethyl iodide with a carbonyl compound to obtain the high-abundance [13C] ethylene oxide compound. Diphenyl sulfide is adopted to replace dimethyl sulfide, the obtained [13C] methyl diphenyl sulfonium iodide avoids C-13 loss in the subsequent reaction process, and the abundance of C-13 is effectively improved.

The invention belongs to the technical field of material synthesis, and particularly relates to calcium dodecahydrododecaborate as well as a synthesis method and application thereof. According to the synthesis method of calcium dodecahydrododecaborate provided by the invention, calcium hydride CaH2, a borane dimethyl sulfide complex and an ether mixed organic solvent react in a reaction kettle to obtain a product, and monoethylene glycol dimethyl ether and tetrahydrofuran cyclic ether are compounded to obtain the ether mixed organic solvent; according to the method, the yield and purity of the product calcium dodecahydrododecaborate are improved, meanwhile, deionized water is used for carrying out solvent exchange on the product and drying is carried out, the purity of the product calcium dodecahydrododecaborate is further improved, efficient synthesis of calcium dodecahydrododecaborate is achieved, industrial preparation is facilitated, high-purity calcium dodecahydrododecaborate is provided, and the method is suitable for industrial production. The method is expected to meet the requirement of solid electrolyte battery commercialization on electrolyte, and solves the technical problem of lack of an efficient synthesis process of calcium dodecahydrododecaborate at present.

The invention discloses a Karl Fischer moisture determination method for sulfur-containing organic compounds, and belongs to the technical field of chemical analysis. The method comprises the following steps: adding absolute methanol, imidazole and an inhibitor (selected from N-substituted maleimide or acrylate compounds) into a titration system, then adding a sample, and titrating with a pyridine-containing Karl-Fischer reagent to the end point. The inhibitor can effectively capture reducing sulfur species and eliminate interference of the reducing sulfur species on iodine. Experiments show that for sulfur-containing samples such as 2, 2-dimethylthiopropane, dimethyl sulfide, dimethyl disulfide and the like, the deviation reduction rate of the method is more than 60% compared with that of a traditional method; the method is easy and convenient to operate, high in accuracy and suitable for moisture analysis of sulfur-containing organic matter in the fields of petrifaction, pharmacy and the like.

The invention discloses a room-temperature rapid preparation method of light metal hydroboron, and relates to the technical field of hydrogen storage materials. The method specifically comprises the following steps that S1, metal hydride is subjected to ball milling pretreatment according to a certain ball-to-material ratio; s2, mixing the pretreated metal hydride and dimethyl sulfide borane in a flask, then adding a solvent, and carrying out ultrasonic-assisted reaction; and S3, transferring the solid product into a tubular furnace, and carrying out vacuum drying to obtain the metal borohydride. The method has the advantages of simple process, low price, one-step reaction and high safety; the yield is obviously improved, the reaction conditions are obviously reduced, the production efficiency is greatly improved, and the method has an industrialization prospect.

The invention provides a heterogeneous catalyst COFBMTD-PY as well as a preparation method and application thereof, belongs to the technical field of photocatalysts, and can solve the problems that the current thioether oxidation reaction needs to be operated under a high-temperature condition, the dosage of the catalyst is large, an additional cocatalyst is needed, and in the actual use process, most of the catalysts cannot be recycled and are not easy to recover, so that the cost is low, and the like. The loss of the catalyst is serious, and the reaction waste is increased. The heterogeneous catalyst COFBMTD-PY disclosed by the invention is constructed by taking 1, 3, 6, 8-tetra-(p-aminophenyl)-pyrene and 2 ', 5'-bis ((1H-imidazole-1-yl) methyl)-[1, 1 ': 4', 1 ''-terphenyl]-4, 4''-diformaldehyde as units, and the heterogeneous catalyst COFBMTD-PY has a structural formula shown in the specification. The heterogeneous catalyst COFBMTD-PY disclosed by the invention can be applied to catalysis of oxidation reaction of methyl thioether and derivatives thereof, and has the advantages that efficient conversion of thioether is realized, reaction selectivity is precisely regulated and controlled, sulfone generation caused by excessive oxidation is avoided, a cocatalyst or extra oxygen is not needed, and the catalyst can be repeatedly utilized.

The invention belongs to the technical field of dimethyl sulfoxide production, and particularly relates to a technology for producing dimethyl sulfoxide through dimethyl sulfide oxidation. According to the process, dimethyl sulfide is taken as a raw material, dimethyl sulfoxide is taken as a solvent, hydrogen peroxide is taken as an oxidizing agent, a micro-channel reactor is utilized to strengthen a reaction process, and the dimethyl sulfoxide is continuously produced under the conditions of low temperature and low system pressure. According to the method, the conversion rate of the raw materials is increased, the reaction conditions are mild, the reaction time is short, the reaction safety is high, post-treatment of a product after reaction is simple, and continuous production can be realized.

3-chloro-2-methyl phenyl dimethyl sulfide is a key intermediate for synthesizing tembotrions, and the target product 3-chloro-2-methyl phenyl dimethyl sulfide is finally synthesized by taking 3-chloro-2-methylaniline and sodium methyl mercaptide as raw materials through diazotization and methyl mercaptan. In order to solve the danger problem existing in the diazotization production process, the invention provides a production process for continuous production of 3-chloro-2-methylphenyldimethyl sulfide in the micro-channel reactor, and the production process has the advantages that compared with a traditional reaction kettle, the micro-channel reactor is provided with a reaction channel with a small diameter, so that the yield of 3-chloro-2-methylphenyldimethyl sulfide is increased; and the catalyst has the advantages of large specific surface area, large volume ratio, high mass transfer and heat transfer efficiency, good operability, no obvious amplification effect and the like. Particularly, the risk of over-temperature explosion in the diazotization reaction process is greatly reduced due to the efficient heat transfer efficiency and the tiny material holding amount of the microreactor.

This invention relates to a method for the electrocatalytic oxidation of anisole to anisole sulfoxide using iron-based complexes, belonging to the fields of homogeneous catalysts and electrocatalytic oxidation technology. The invention utilizes an iron-based complex formed by coordination between a tetraamide macrocyclic ligand (TAML-H4) and metallic iron as a homogeneous molecular catalyst, with water as the sole oxygen source, to construct an electrocatalytic anisole oxidation system. Through the synergistic effect of the catalyst and water, a proton-coupled electron transfer and single-electron oxidation process occurs at the anolyte, resulting in the loss of two electrons and two protons to generate a high-valence iron-oxygen active intermediate [Fe]. Ⅴ (O)(TAML)] – This invention achieves highly efficient and selective oxidation of anisole, generating the high-value-added product benzyl sulfoxide at the anode. It eliminates the need for additional strong oxidants, employs mild reaction conditions, boasts high atom economy, and is environmentally friendly, making it suitable for the green conversion of sulfides in the synthesis of fine chemicals. This provides a feasible pathway for the industrial production of sulfoxide compounds.

This invention relates to a photocurable composition comprising: cyanoacrylate A selected from the group consisting of n-hexyl cyanoacrylate, n-heptyl cyanoacrylate, n-octyl cyanoacrylate, and mixtures thereof; a free radical photoinitiator; a metallocene compound; compound B selected from the group consisting of boron trifluoride, boron trifluoride diethyl ether, boron trifluoride dihydrate, boron trifluoride ethanol, boron trifluoride methanol, boron trifluoride acetic acid, boron trifluoride butyl ether, boron trifluoride butanol, boron trifluoride propanol, boron trifluoride dimethyl sulfide, boron trifluoride acetonitrile, boron trifluoride tetrahydrofuran, and boron trifluoride isopropanol; and optionally a free radical polymerization inhibitor, provided that when the photocurable composition contains a free radical polymerization inhibitor, its weight content is 0.04 wt.% or less; wherein the molar content of compound B is greater than or equal to 0.141 mmol per 1 kg of composition; and wherein the molar ratio of metallocene compound / compound B ranges from 2 to 8.

The invention discloses a detection method for determining a degradation impurity dimethylamino formic acid in neostigmine methylsulfate, the detection method is carried out by using a high performance liquid chromatograph, a mobile phase is composed of a mobile phase A and a mobile phase B, and isocratic elution is adopted; the isocratic elution is adopted, the total volume of the mobile phase is 100%, the volume of the mobile phase A is 26%-30%, and the volume of the mobile phase B is 74%-70%; the detection method is carried out by using a high performance liquid chromatograph, a chromatographic column adopts acrylic acid amine bonded silica gel as a filling agent, and a mobile phase is composed of a phosphate buffer solution and acetonitrile. According to structural characteristics of products and properties of compounds, chromatographic conditions are optimized, so that a blank solvent and other components in a test sample have no interference on measurement of dimethylamino formic acid, detection specificity, sensitivity and accuracy are improved, and medicine quality is controlled more strictly.

The application discloses a method for synthesizing benzyl sulfoxide by selectively oxidizing benzyl sulfide, belongs to the technical field of fine organic synthesis, and can solve the problems of a long synthesis process, complex catalyst preparation and long reaction time in the synthesis of benzyl sulfoxide at present. The method uses benzyl sulfide as raw material, uses ozone as an oxidant, introduces tert-butyl alcohol as an inhibitor to control the reaction process, and uses ethyl acetate as a reaction solvent, and benzyl sulfoxide is prepared through selective oxidation. The innovative process has the advantages of mild process conditions, environmental friendliness, no need to add any catalyst and high product yield. The method has great potential and value in the industrial application field.

The invention provides a low-byproduct methyl mercaptan synthesis process. The byproduct of dimethyl sulfide is inevitably generated in the process of generating methyl mercaptan from hydrogen sulfide and methanol. The method comprises the following steps: filling a thioether conversion catalyst at the front end, introducing methyl sulfide with a large proportion of hydrogen sulfide ratio, connecting a multi-stage methyl mercaptan synthesizer in series at the rear end, supplementing and introducing methanol, reacting excessive hydrogen sulfide at the front end with methanol to generate methyl mercaptan, gradually heating the multi-stage methyl mercaptan synthesizer from front to back, filling a high-selectivity catalyst in the methyl mercaptan synthesizer at the front end, the last-stage methyl mercaptan synthesizer is filled with a high-conversion-rate catalyst, hydrogen sulfide is slightly insufficient, and hydrogen sulfide is basically consumed. According to the designed methyl mercaptan synthesis process, the byproduct of dimethyl sulfide is reduced, the amount of tail gas is reduced, compression and recycling of hydrogen sulfide are avoided, gas-liquid entrainment is reduced while energy consumption is reduced, condensation of the product is facilitated, and the yield of methyl mercaptan is increased.

The invention relates to a preparation method of a modified gamma-Al2O3 catalyst and a synthesis method for converting dimethyl sulfide into methyl mercaptan. The catalyst is prepared by adopting an equivalent-volume impregnation method, taking VIB, VIIB, VIII and IIB group metal oxides as active components, taking alkali metal, lanthanide series metal and nonmetal oxides as assistants, loading the active components and the assistants on a gamma-Al2O3 carrier treated by organic phosphonic acid (HEDP (hydroxyethylidene diphosphonic acid) and ATMP (amino trimethylene phosphonic acid)), enabling the metal loading capacity to be 0.5-20wt%, drying and roasting. According to the catalyst, the dimethyl sulfide conversion rate (greater than or equal to 60%) and the methyl mercaptan selectivity (greater than or equal to 95%) are remarkably improved through the synergistic effect of acidic site regulation and metal active components. The invention also discloses the optimal process conditions of the catalytic reaction: the reaction temperature is 230-400 DEG C, the pressure is 0-5.0 MPa, the air speed is 50-150h <-1 >, and the molar ratio of H2S to dimethyl sulfide is 1-8. The technology solves the problem of high-value utilization of dimethyl sulfide byproducts, has the characteristics of carbon deposition resistance, sulfur deposition resistance and high stability, and is suitable for industrial production.