24 results about "Ethyl iodide" patented technology

The invention discloses a polymer sealing ring and a preparation method thereof, and relates to the technical field of polymer materials. The high-temperature-resistant fluororubber sealing gasket is prepared from the following raw materials in percentage by mass: 30 to 50 percent of fluorinated modified silicone rubber, 15 to 25 percent of fluororubber, 7.2 to 16.4 percent of hybrid white carbon black, 2.5 to 6 percent of hydroxyl silicone oil, 8 to 11 percent of plasma fluorinated modified aluminum oxide, 4 to 8 percent of carbon black, 0.8 to 1.4 percent of palm wax, 0.8 to 1.4 percent of internal release agent, 1 to 2 percent of vulcanizing agent, 3 to 5 percent of triallyl isocyanurate and 0.5 to 1 percent of anti-aging agent. The fluorinated modified silicone rubber is prepared by grafting C2-18-perfluoroalkyl iodoethane on a silicone rubber side chain, so that the low temperature resistance of the silicone rubber is effectively improved, and the phenomenon that methyl vinyl silicone rubber is easy to crystallize at low temperature is successfully inhibited; the sealing ring material has good performance at high and low temperatures, and the use temperature range of the sealing ring material is effectively improved.

The application discloses an organic compound biological probe and a preparation method and application thereof, and belongs to the field of fluorescent probes. The structural formula of the organic compound biological probe is as follows, and the preparation method comprises the following steps: adding 2,4-dihydroxybenzaldehyde and anhydrous potassium carbonate into anhydrous acetonitrile or DMF, then dropwise adding 1,4-dibromobutane to obtain a colorless oily compound 1 through reflux reaction; dissolving the compound 1 and triphenylphosphine in anhydrous acetonitrile to obtain a solid compound 2 through reflux reaction; dissolving 1,1,2-trimethyl-1H-benzo[e]indole and iodoethane in anhydrous acetonitrile to obtain a compound 3 through reflux; dissolving the compound 3 and the compound 2 in anhydrous ethanol, adding piperidine, and then performing reflux reaction and purification to obtain the organic compound biological probe. The organic compound biological probe can self-assemble into nanoparticles with a size of about 1.6 nm in water, has strong anti-photobleaching ability, and integrates red light and near-infrared dual-channel imaging, pH detection, mitochondrion targeting and chemotherapy.

The application discloses a preparation method of triethyl indium, and relates to the technical field of metal organic source synthesis, wherein a commonly used indium source is mainly trimethyl indium; the trimethyl indium is in a solid state at normal temperature, and is easy to cause the solid indium source to be easy to be hardened and to have excessive residues; when the solid indium source is used in a machine, the concentration output stability is worse than that of a liquid source; the liquid indium source will become an important indium source in the future; the operation method of the triethyl indium in preparation is more complicated; and the purity of the triethyl indium prepared by purification cannot reach a better ideal state. In the application, n-butyllithium and ethyl iodide are reacted under the protection of inert gas, then the reaction product is reacted with indium chloride to generate triethyl indium; the whole operation is simple, raw materials are easy to obtain, and the product has high purity; under the protection of inert gas, the interference of other solution reagents in the preparation process is reduced; therefore, high-quality triethyl indium raw materials can be purified and processed.

The invention discloses an organic compound biological probe and a preparation method and application thereof, wherein the organic compound biological probe is In-AIE, and the method comprises: dissolving rutin in acetonitrile, and then adding 4-formyl pyridine and n-tributylphosphine for reflux reaction to obtain compound 1; dissolving 1,1,2-trimethyl-1H-benzo[e]indole and iodoethane in anhydrous acetonitrile for reflux to obtain compound 2; adding 2,4-dihydroxybenzaldehyde and anhydrous potassium carbonate to anhydrous acetonitrile and then dropping 1,4-dibromobutane for reflux reaction to obtain colorless oily compound 3; dissolving compound 2 and compound 3 in anhydrous ethanol for reflux reaction to obtain solid compound 4; dissolving compound 1 and compound 4 in anhydrous acetonitrile for reflux reaction and then purifying to obtain solid In-AIE. It can quickly enter cells within 1 min, has strong anti-photobleaching ability, and integrates multi-channel imaging, pH detection, mitochondrial targeting and photodynamic therapy.

The invention discloses a preparation method of a special monomer perfluoro (3-oxapent-4-ene) sulfonyl fluoride (PFSAF) for perfluorosulfonic acid resin, belongs to the technical field of special fluorine material synthesis, and is characterized in that a specific preparation system is utilized, fluorosulfonyl ethyl oxatetrafluoroiodoethane (II) is used as a raw material, and different organic metal reagents are used for preparing the special monomer perfluoro (3-oxapent-4-ene) sulfonyl fluoride (PFSAF) for the perfluorosulfonic acid resin, so that the special monomer perfluoro (3-oxapent-4-ene) sulfonyl fluoride (PFSAF) is obtained. The one-step removal of iodine and fluorine is realized to construct a perfluoroalkenyl functional group, and the synthesis of the special monomer (PFSAF, I) of the perfluorosulfonic acid resin exchange membrane is completed. Compared with the existing synthesis method, the method has the advantages of short steps, cheap and easily available reagents and high yield, has the potential of large-scale engineering preparation, and provides a solid foundation for low-cost development of the perfluorosulfonic acid proton exchange membrane.

The invention discloses a synthesis method of N-ethyl-3-chloro-4-iodo-pyrazole, which comprises the following steps: reacting pyrazole with an acetylation reagent to generate N-acetyl pyrazole; the method comprises the following steps: reacting N-acetylpyrazole with a chlorination reagent in the presence of alkali and an activating agent to generate N-acetyl-3-chloropyrazole; the preparation method comprises the following steps: enabling N-acetyl-3-chloropyrazole to react with an iodination reagent, so as to generate N-acetyl-3-chloro-4-iodinated pyrazole; the preparation method comprises the following steps: enabling N-acetyl-3-chloro-4-iodine pyrazole to react with a reducing agent, so as to generate N-ethyl-3-chloro-4-iodine-pyrazole. By adopting an acetyl protection / reduction innovative strategy, a high-crisis diazotization process and a difficult-to-control iodoethane alkylation reaction are avoided, efficient and high-selectivity synthesis of N-ethyl-3-chloro-4-iodo-pyrazole by taking cheap pyrazole as a raw material is realized, the whole reaction route is simple and safe, the product purity and yield are remarkably improved, and the method is suitable for industrial production. And the method is more suitable for industrial large-scale production.

This invention belongs to the field of detection technology, specifically relating to a method for preparing a fluorescent probe for viscosity detection, comprising: dissolving 4-methoxysalicylaldehyde, acrolein, and potassium carbonate in 1,4-dioxane to obtain product 1; dissolving 1,1,2-trimethylbenzo[e]indole and iodoethane in anhydrous ethanol to obtain product 2; dissolving product 1 and product 2 in anhydrous ethanol, adding piperidine, and obtaining the fluorescent probe MCC-ETB under nitrogen protection; and dissolving the fluorescent probe MCC-ETB in DMSO to prepare a mother liquor. The fluorescent probe of this invention can achieve viscosity detection, has a simple synthesis route, and requires convenient detection equipment and methods. It can be applied to electrolyte solutions with complex solvent systems, enabling qualitative and quantitative detection of electrolyte viscosity changes.

The invention provides a novel organic synthesis fluorescent probe as well as a preparation method and application thereof, and the method comprises the following steps: carrying out a palladium-catalyzed cross-coupling reaction on 3, 6-dibromo-9-phenylcarbazole and 4-vinylpyridine to generate a compound Ph-BPV-Cz, and introducing iodoethane through a quaternization reaction to obtain the novel organic synthesis fluorescent probe. Key structural units such as carbazole, pyridine and vinyl are ingeniously fused in a molecular skeleton of the probe, so that the probe has excellent optical properties, good chemical stability, rich reaction activity and modifiability. Through the synergistic effect of the structural units, the probe can be specifically combined with RNA, and the obvious change of the fluorescence characteristic of the probe is triggered, so that the probe can be used for RNA detection. Besides, PCz-ViPy-Et-PCz effectively enhances the chimeric ability with a DNA double-helix groove by virtue of the synergistic effect of a rigid carbazole skeleton and a pyridinium group, so that specific recognition and fluorescence response to a DNA sequence are realized, and the probe can be used for DNA detection.

The invention discloses plant-based hairline cream and a preparation method thereof, and relates to the technical field of cosmetics. When the plant-based hairline cream is prepared, black sesame is cleaned and crushed, and then the crushed black sesame reacts with a sodium hydroxide solution and a hydrochloric acid solution in sequence to obtain black sesame pigment; coating the nanometer perlite powder loaded with the black sesame pigment with ethyl orthosilicate to obtain silicon dioxide coated nanometer perlite powder; the preparation method comprises the following steps: sequentially reacting carboxymethyl cellulose with 2-iodoethane-1-amine and imidazole-4-methyl formate to obtain imidazolium salt cellulose; and finally emulsifying glycerol, sodium hyaluronate, 1, 3-butanediol, vitamin E, sweet almond oil, imidazolium salt cellulose and liquid paraffin, uniformly mixing with the silicon dioxide coated nano perlite powder, and standing to prepare the plant-based hairline cream. The plant-based hairline cream prepared by the invention has excellent makeup holding capacity, moisturizing capacity and antibacterial capacity.

The invention relates to a selective hydrogenation reduction method of a non-conjugated ketene compound, which comprises the following steps: in a nitrogen atmosphere, mixing a ketene compound shown as a formula (I), a hydrogen source, a catalyst, a ligand, a reducing agent and an organic solvent, and stirring at room temperature for 8-24 hours to obtain a reaction solution; and performing column chromatography separation and purification on the reaction liquid to obtain the alkyl ketone compound as shown in the formula (II). According to the method, iodoethane or bromoethane is used as a hydrogen source, and compared with the prior art, the method has the advantages of higher yield, mild reaction conditions, good selectivity, no need of high-pressure hydrogen, no pungent smell and environmental protection.

The invention belongs to the field of fluorine chemical industry, and particularly relates to a synthesis method of 1, 1, 1, 2, 2, 5, 5, 6, 6, 6-decafluoro-3-hexene. The preparation method comprises the following steps: 1, carrying out addition reaction on pentafluoro halogenated hydrocarbon such as pentafluoro iodoethane or pentafluoro bromoethane serving as a raw material and ethylene, carrying out dehydrohalogenation to obtain 3, 3, 4, 4, 4-pentafluoro butene, carrying out addition reaction on the 3, 3, 4, 4, 4-pentafluoro butene and the pentafluoro halogenated hydrocarbon, and carrying out dehydrohalogenation to obtain 1, 1, 1, 2, 2, 5, 5, 6, 6, 6-decafluoro-3-hexene. And the other method comprises the following steps of: reacting pentafluoro halogenated hydrocarbon serving as a raw material with acetylene to obtain 3, 4-dibromo (diiodo)-1, 1, 1, 2, 2, 5, 5, 6, 6, 6-decafluoro-hexane, and removing bromine or iodine to obtain 1, 1, 1, 2, 2, 5, 5, 6, 6, 6-decafluoro-3-hexene. The synthesis method provided by the invention has the advantages of easily available raw materials, simple operation, convenient purification and easy large-scale production.

This invention belongs to the field of fine chemical engineering and organic synthesis technology, and relates to a method for preparing high-purity 1,1-difluoro-2-iodoethylene. The method includes: firstly, in an aprotic organic solvent, under controlled low-temperature conditions, allowing vinylidene fluoride to undergo an addition reaction with iodine monochloride to obtain the intermediate 1-chloro-1,1-difluoro-2-iodoethane; subsequently, the intermediate undergoes a controlled elimination reaction in an alkaline aqueous solution, and the product is immediately removed by reactive distillation, finally purified by distillation to obtain the target product. This invention effectively controls the thermal effect of the addition reaction by introducing a specific solvent, suppressing side reactions such as iodine radical coupling, and eliminating the need for expensive metal catalysts or phase transfer catalysts. The process is simple and safe to operate, with an intermediate separation yield of over 95%, high overall yield, and high product purity, making it suitable for large-scale industrial production.

The invention provides a high-sensitivity detection method for quinclorac in grains and honey. The high-sensitivity detection method comprises the following steps: S1, extracting; S2, deriving; S3, redissolving and on-machine analysis of GCMSMS (Gas Chromatography Mass Spectrometry) and LCMSMS (Liquid Chromatography Mass Spectrometry). According to the technical scheme, iodoethane is adopted to react with quinclorac under the alkaline condition to generate a new compound 3, 7-dichloro-8-quinoline carboxylic acid ethyl ester, the derivation reaction speed is high, and the reaction can be completed within 60 minutes; and the used derivatization reagent is safe to use and low in cost. According to the method, the derivative 3, 7-dichloro-8-quinoline carboxylic acid ethyl ester of quinclorac is quantitatively detected through GCMSMS, the sensitivity is high, the quantification limit is far lower than that in an existing literature method, and the harsh requirement of the market for quinclorac detection in food can be met.

The invention discloses design, synthesis and activity research of a fluorescent probe for in-situ detection of nitroreductase. The synthesis route of the fluorescent probe is as follows: # imgabs0 # aReagens and bonds: (i) Ethyl iode, KOH and DMF, and the temperature is 90 DEG C; (ii) MethylMagnesite chloride, NaI, THF (tetrahydrofuran), and the temperature is 55 DEG C; (iii) 4-nitrobenzyl bromide, K2CO3, DMF (Dimethyl Formamide), rt, K2CO3, K2CO3, DMF, rt and K2CO3; and (iv) n-Butanol, Toluene, and the temperature is 100 DEG C.

The invention belongs to the technical field of detection, and particularly relates to a preparation method of a fluorescence probe for detecting viscosity, which comprises the following steps: dissolving 4-methoxysalicylaldehyde, acrolein and potassium carbonate in 1, 4 dioxane to obtain a product 1; dissolving 1, 1, 2-trimethylbenzo [e] indole and iodoethane in absolute ethyl alcohol to obtain a product 2; dissolving the product 1 and the product 2 in absolute ethyl alcohol, adding piperidine, and obtaining the fluorescent probe MCC-ETB under the protection of nitrogen; the method comprises the following steps: dissolving a fluorescent probe MCC-ETB in DMSO to prepare a mother solution; the fluorescent probe provided by the invention can realize viscosity detection, is simple in synthetic route, simple and convenient in detection equipment and method, can be applied to an electrolyte solution with a complex solvent system, and can qualitatively and quantitatively detect the viscosity change of the electrolyte.

The present invention belongs to the field of organic synthesis, and relates to a method for synthesizing pentafluoroiodoethane by co-conversion iodination. It is obtained by reacting carboxylic acid, pentafluoroethane and iodine in a catalyst, oxygen or a mixed gas of oxygen and an inert gas; wherein the catalyst is an AB-type bifunctional catalyst loaded on a carrier, which can not only catalyze decarboxylation iodination reaction, but also catalyze dehydrogenation iodination reaction. The single-pass conversion rate of the present invention in terms of iodine atoms reaches more than 70%, and other high-value-added iodides can be flexibly produced as by-products by changing the raw materials; not only the raw materials are cheap and safe, and the sources are convenient, but also the reaction temperature is low and the catalyst life is long; and the product separation and purification is simple, the synthesis process is safe, and it is suitable for large-scale industrial production.

The invention relates to an antibacterial PE composite board and a preparation method thereof, and belongs to the technical field of polymer materials. The antibacterial PE composite board comprises, by weight, 100 parts of HDPE resin, 14-18 parts of LLDPE resin, 7.5-11 parts of antibacterial modified cellulose, 1.7-2.2 parts of lubricant and 0.15-0.2 parts of antioxidant. The antibacterial modified cellulose takes microfibrillated cellulose as a matrix, is oxidized by sodium periodate, and aldehyde groups are formed on cellulose molecules, namely, aldehyded fibers are obtained, and then amine-aldehyde condensation is carried out between aliphatic chain monoamine and the introduced aldehyde groups, and alkyl aliphatic chains are introduced into the side chains of cellulose macromolecules for modification, namely, alkylated fibers are obtained, and finally, quaternization treatment is carried out by ethyl iodide. The antibacterial modified cellulose reduces crack generation of a board under the action of external force deformation, and inhibits the reproduction of fungi invading the cracks, has good antibacterial effect, and enables the board to maintain stable mechanical properties.

The invention discloses a device and a method for preparing a narrow-distribution fluorine-containing surfactant by a VDF telomerization method, and belongs to the field of fluorine fine chemical engineering. The device comprises a VDF vaporization conveying system, a polymerization reaction system, a raw material metering system, a conveying system and a recovery system, triethylamine tri-hydrofluoride ionic liquid is adopted as a medium, the reaction temperature (80 + / -0.5 DEG C) and the raw material ratio (VDF: iodoethane = 12: 1 mol) are accurately regulated and controlled through microwaves, and efficient telomerization reaction is achieved. The polydispersity index (PDI) of the product is less than or equal to 1.2, the surface tension is as low as 18mN / m, the solvent recovery rate reaches 95%, the problems of wide product distribution and poor environmental protection property of the traditional process are solved, and the method is suitable for the field of high-end fine chemical engineering.

The present invention discloses a method for determining CO2 distribution in a porous medium when CO2 displaces natural gas, belonging to the field of rock physics and geophysical exploration technology, and comprising the following steps: S1, placing a porous medium core model in a holder, heating and pressurizing it to preset experimental conditions; S2, taking an initial image of the rock by X-CT scanning; S3, displacing CO2 extracted with iodine ethane indicator into the core, and taking a CT image of the rock after CO2 injection by X-CT scanning; S4, characterizing the distribution of CO2 based on the CT images of different CO2 injection amounts. When CO2 displaces natural gas or other gases, the distribution of CO2 can be accurately and quantitatively described by real-time monitoring of the distribution changes of CO2 in the core or simulated formation. This can make a scientific and accurate assessment of the CO2 displacement effect, and plays an important role in studying the laws of migration, storage, diffusion, etc. of CO2 plumes under formation conditions.

The application provides a high-sensitivity detection method for quinclorac in grains and honey, comprising S1 extraction, S2 derivatization, S3 redissolution and GCMSMS and LCMSMS on-machine analysis. Through the technical scheme of the application, the application adopts iodine ethane to react with quinclorac under alkaline conditions to generate a new compound 3,7-dichloro-8-quinoline carboxylic acid ethyl ester; the derivatization reaction speed is fast, and the reaction can be completed in 60 minutes; the used derivatization reagent is safe and low in cost. The application quantitatively detects the derivatization product 3,7-dichloro-8-quinoline carboxylic acid ethyl ester of quinclorac by GCMSMS, is high in sensitivity, far lower in quantitative limit than the quantitative limit in the prior art method, and can meet the stringent requirements of the market on the detection of quinclorac in food.

A composition includes particular amounts of a first solvent selected from benzaldehyde, 1,3-dioxolane, tetrahydropy-ran, 4-picoline, ethyl benzoate, methyl benzoate, or a combination thereof; a second solvent selected from cyclic ketones, aliphatic ketones, methyl acetate, dimethyl carbonate, tert-butyl acetate, propylene carbonate, PCBTF, ethyl acetate, 1,2-butylene oxide, anisole, dimethyl acetamide (DMA), pyridine, dimethyl maleate, dimethyl sulfide, triethyl phosphate, pyrrolidine, 1-vinyl-2-pyrrolidinone, 2-pyrrolidinone, thioacetic acid, N, N diethyl formamide, n-methyl pyrrole, 2-methyl pyrazine, ethyl iodide, dimethyl sulfoxide (DMSO), or a combination thereof. The solvent composition can be particularly useful in adhesive formulations such as solvent cements.

The invention relates to a method for co-producing chlorosilane and iodoethane. The method comprises the following steps: enabling tert-butyl dimethyl ethyoxyl silane (dimethyl vinyl ethyoxyl silane or tert-butyl diphenyl ethyoxyl silane) and thionyl chloride to enter a micro-channel reactor at the same time to react; rectifying the reaction liquid to obtain tert-butyl dimethyl chlorosilane (dimethyl vinyl chlorosilane or tert-butyl diphenyl chlorosilane) and diethyl sulfite; the method comprises the following steps: putting magnesium iodide into a reaction container, adding water to prepare a solution, starting stirring, and heating; slowly dropwise adding the byproduct diethyl sulfite; and after dropwise adding, reacting to obtain iodoethane.

The invention relates to an antioxidant lubricating oil composition and a preparation method thereof, and belongs to the technical field of lubricating oil. The composition is prepared from the following components in percentage by weight: 3.8 to 4.4 percent of an extreme pressure anti-wear agent, 2.5 to 3.0 percent of a clearing agent, 2.2 to 2.8 percent of an oily additive, 0.75 to 0.92 percent of a modified antioxidant, 1.7 to 2.1 percent of an ashless dispersant, 0.4 to 0.5 percent of an anti-rust agent, 3.5 to 4.2 percent of a viscosity index improver and the balance of polyol ester base oil, the modified antioxidant is a compound with a three-branch naphthylamine structure and a central quaternary ammonium structure formed by click addition of triallylamine and 4-chlorobenzyl mercaptan, quaternization of iodoethane and substitution of 2-naphthylamine, the modified antioxidant has good antioxidant capacity at high temperature, and meanwhile, the oil sludge amount of the lubricating oil at high temperature is effectively reduced.

The invention relates to a preparation method of high-purity diiodosilane, and belongs to the technical field of preparation of organosilicon compounds. The preparation method comprises the following steps: adding iodoethane, bis (diethylamino) silane and a solvent into a three-neck flask, and carrying out stirring reaction under the protection of argon; in the reaction process, yellow white precipitate is slowly generated, and a yellow reaction product is finally obtained; filtering the yellow product through a filter column to obtain colorless transparent liquid and yellowish white solid tetraethylammonium iodide; carrying out atmospheric distillation on the obtained colorless transparent liquid; carrying out adsorption refining on the residual reaction liquid, adding a polystyrene-based complexing active agent, filtering, and carrying out reduced pressure rectification on the filtrate to obtain diiodosilane; the polystyrene-based complexing active agent is prepared from styrene, allylidene triphenylphosphine, trans-2-butene-1, 4-dicarboxylic acid, divinyl benzene, water, potassium persulfate and gelatin; the purity of the prepared diiodosilane reaches 99.5% or above, and the purity grade of metal ions reaches 6N grade.