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92 results about "Ethyl iodide" patented technology
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Ethyl iodide (also iodoethane) is a colorless flammable chemical compound. It has the chemical formula C₂H₅I and is prepared by heating ethanol with iodine and phosphorus. On contact with air, especially on the effect of light, it decomposes and turns yellow or reddish from dissolved iodine.
Preparation method of fluorine-silicon surfactant
ActiveCN102070662ARaw materials are easy to getSmooth responseGroup 4/14 element organic compoundsTransportation and packagingSolventMethanol
The invention discloses a preparation method of a fluorine-silicon surfactant. The method comprises the following steps of: continually dripping 13 to 18 weight parts of trichlorosilane into 44 to 65 weight parts of perfluor alkyl ethylene or perfluor alkyl ethyl iodide serving as a raw material in the presence of 0.1 to 1.0 weight part of noble metal catalyst so as to obtain an intermediate product; and adding 14.8 to 20 weight parts of high-boiling-point solvent into the intermediate product, continuously dripping 10 to 16.35 weight parts of methanol or ethanol for reacting, decompressing and rectifying so as to obtain a target product. In the method, raw materials are readily available, byproduct is not produced, a reaction in an entire synthesis process is stable, process control is stable, safety, low cost and easy separation are realized, the yield of a final fluorine-silicon surfactant is over 95 percent, and the purity of the surfactant is over 98 percent. Due to the presence of a siloxane active group, the fluorine-silicon surfactant can react with and be tightly combined with substances with a hydroxy functional group, such as glass and the like, so that the surface of the fluorine-silicon surfactant has high waterproofness, oil resistance and soil resistance, surface tension is less than 17.6 dynes per meter, and light transmittance is over 99.9 percent.
Owner:JINZHOU DPF TH CHEM CO LTD
Hyperbranched polyamide modified chitosan quaternary ammonium salt microsphere for wastewater treatment and preparation method and application thereof
ActiveCN105669986ALarge specific surface areaImprove adsorption capacityOther chemical processesWater contaminantsEthylenediamineQuaternary ammonium cation
The invention provides hyperbranched polyamide modified chitosan quaternary ammonium salt which is obtained through the reaction of hyperbranched polyamide, chitosan and alkyl halide.The hyperbranched polyamide is prepared from trimesoyl chloride and ethylenediamine through a solution polymerization method.The alkyl halide comprises methyl iodide, ethyl iodide, methyl bromide or ethyl bromide.The microsphere prepared from the quaternary ammonium salt is applied to treatment of methyl orange wastewater, the final dye removal rate can reach 99.67%, the microsphere is renewable, and the preparation process is simple and free of pollution.
Owner:ZHANJIANG JIALI GLOVE PRODS
Method for preparing and purifying water-soluble cyanine dye (Cy5.5)
ActiveCN102010614AEasy to operateLow costMethine/polymethine dyesMethyl groupThin layer chromatogram
The invention discloses a method for preparing and purifying a water-soluble cyanine dye (Cy5.5), which comprises the following steps of: reacting 1,3-disulfonic acid-6-naphthylhydrazine serving as an initiative raw material with methyl isopropyl ketone to generate 1,1,2-trimethyl-benzindole-1,3-disulphonate; reacting the 1,1,2-trimethyl-benzo-indole-1,3-disulfonate with ethyl iodide and 6-bromocaproic acid respectively to generate N-ethyl-2,3,3-trimethyl-benzindole-5,7-disulphonate (product 1) and N-(epsilon-carboxy-pentyl)-2,3,3-trimethyl-benzindole-5,7-disulphonate (product 2); reacting the product 1 with beta-anilino-acraldehyde-anil-hydrochloride and then directly reacting the product 1 with the product 2 to prepare the Cy5.5; and preparing a thin layer chromatogram, and repeatedly purifying and separating the Cy5.5 to obtain a pure product of the Cy5.5. The method is easy and convenient to operate and has a high yield, the product does not need expensive high performance liquid chromatography (HPLC) (C-18 reverse column) for separation, and the method has great significance for meeting requirements of domestic autonomous production.
Owner:TIANJIN SUNGENE BIOTECH
S-1-(4-ethoxybenzyl)-3-azapentane-1,5 diamine preparation method
ActiveCN101007775AImprove securityHigh yieldOrganic compound preparationCarboxylic acid amides preparationLithium hydroxideOrganic synthesis
The invention discloses a making method of S-1-(4-ethoxy benzyl)-3-aza pantane-1, 5 diamine in the organic synthetic technical domain, which comprises the following steps: 1reacting L-tyrosine alkyl ester protected by amino and ethyl iodide catalyzed by anhydrous carbonate alkali to produce L-tyrosine alkyl ester protected by O-ethyl-amino; 2. reacting L-tyrosine alkyl ester protected by O-ethyl-amino and anhydrous ethanediamine to do ester exchange to produce O-ethyl-L-tyrosinamide protected by N-(2-amino ethyl)-amino; 3. stripping protecting group of amino through trifluoroacetic acid; 4. using aluminium lithium hydroxide to reduce; obtaining the product. The invention reduces technical difficulty with mild reacting condition, which can prepare key intermediate of Gadoxetic acid disodium (Gd-EOB-DTPA).
Owner:CHIA TAI TIANQING PHARMA GRP CO LTD
Process for preparing diethyl zinc
InactiveCN1827623ASimple production processReduce manufacturing costZinc organic compoundsZinc alloysCopper
The invention relates to a method for preparation of compounds and especially to a method for preparation of zinc diethyl. The preparation technology of the said method includes the following steps: a. adding powdered copper-zinc alloy into a reactor with an agitator, of which the powdered copper-zinc alloy occupies 8-12 % of the reactor, replacing the air in the reactor with inert gas, afterwards, beginning to stir; b. heating the temperature of the reactor to 40-150 DEG C while stirring, simultaneously, dripping iodoethane and bromoethane, after the reaction is initiated, gradually dripping bromoethane continuously, and controlling the temperature at 40-100 DEG C to stably reflux the reactants; c.after the reflux, controlling the temperature of the reactor at 100-120 DEG C, continuously stirring the reactants for 0.5-2 hours, and then beginning to distill in reduced pressure state to obtain high-purity zinc diethyl. The technical project of this invention is characterized in that it is of simple process, low cost, and high yield rate and purity of the obtained product.
Owner:INNER MONGOLIA MENG XI HIGH TECH GRP CO LTD
Preparation method and application of ratiometric fluorescent probe for detecting hydrazine
ActiveCN108982447AReduce consumptionImprove detection accuracyOrganic chemistryColor/spectral properties measurementsCyclohexanoneSodium acetate
The invention relates to a preparation method and application of a ratiometric fluorescent probe for detecting hydrazine. The preparation comprises the steps that phosphorus oxychloride is dissolved in dichloromethane, the mixture is slowly dropped into N,N-dimethylformamide, and after the dropwise addition is finished, cyclohexanone is added for reaction so as to obtain a compound 1; then, benzoindoles and iodoethane are dissolved in acetonitrile for heating and refluxing reaction so as to obtain a compound 2; the compound 1 and the compound 2 are subjected to heating and refluxing by takingmethylbenzene and n-butyl alcohol as solvents so as to obtain a fluorescent probe compound 3; the compound 3 is dissolved in anhydrous N,N-dimethylformamide, and sodium acetate is added for reaction under the protection condition of nitrogen so as to generate a compound 4; and the compound 4 is dissolved in anhydrous dichloromethane containing acetyl chloride, triethylamine is added for reaction for 4 hours at normal temperature under the protection of the nitrogen so as to generate the probe Ben-Cy1. ccording to the preparation method and application of the ratiometric fluorescent probe, theprobe works in a near-infrared region, is suitable for qualitative and quantitative analysis, low biotoxicity and high selectivity in biological samples and can be applied to the related fields of analytical chemistry, life organic analytical chemistry and the like.
Owner:QUFU NORMAL UNIV
Intermediate for preparing obeticholic acid, preparation method of intermediate and preparation of obeticholic acid
The invention relates to the technical field of medicine, and particularly relates to a intermediate for preparing obeticholic acid, a preparation method of the intermediate and a preparation of obeticholic acid. A route is provided to take acetaldehyde as electrophilic reagent, compared with a method of introducing ethenyl and ethyl iodide through an aldol condensation reaction, the yield is sharply improved; cyclohexylamine salt is refined to form a compound (V), the product quality can be sharply improved; double bonds are hydrogenated and then carbonyl is reduced so that ethenyl can be reduced, and by controlling appropriate temperature, by-products of deethylation can be sharply reduced. The method is mild, green and environmentally friendly, besides, the yield is higher than an existing preparation method, the route reaction condition is economical and effective, and suitable for industrial production on a large scale.
Owner:CHANGZHOU PHARMA FACTORY
Laser processing method and equipment
InactiveCN1460892AAvoid damageImprove securitySemiconductor/solid-state device manufacturingOriginals for photomechanical treatmentLaser processingMachined surface
Owner:V TECH CO LTD
Laser machining method and apparatus
InactiveUS6926801B2Improve security levelLow costSemiconductor/solid-state device manufacturingOriginals for photomechanical treatmentMachined surfaceOptoelectronics
In a laser machining method for removing remaining defects on a photomask, there has been problems to be resolved that damage is formed at the portion of the substrate where the defect has been removed, thus resulting in degraded quality of machining. In a laser machining method for removing remaining defects on a photomask by a method of laser machining, the remaining defects are removed by using a configuration in which irradiation with a laser beam is performed from below with a to-be-machined surface directed downward, and irradiation with a laser beam in an atmosphere containing a halogenated hydrocarbon gas (as an example, ethyl iodide).
Owner:LASERFRONT TECH
Preparation method of perfluoroalkyl ethyl alcohol
The invention discloses a method for preparing perfluoroalkyl ethyl alcohol with perfluoroalkyl ethyl iodide, which comprises the following steps: (a) fuming sulphuric acid and the perfluoroalkyl ethyl iodide are mixed at 55-75DEG C, thus obtaining premixed reactants; (b) the premixed reactants are heated to 130DEG C at most to ensure the fuming sulphuric acid to react with the premixed reactants of the perfluoroalkyl ethyl iodide, thus forming sulfate; and (c) hydrolysis is carried out and the perfluoroalkyl ethyl alcohol is separated.
Owner:SHANGHAI 3F NEW MATERIAL
Visual organic molecular fluorescence probe on basis of cyanine and method for preparing visual organic molecular fluorescence probe
InactiveCN107903257ARealize qualitative detectionEasy to operateOrganic chemistryFluorescence/phosphorescenceBromoacetic acidFluorophore
The invention belongs to the technical field of fluorescence spectrum detection and analysis, and particularly relates to a visual organic molecular fluorescence probe on the basis of cyanine and a method for preparing the visual organic molecular fluorescence probe. The visual organic molecular fluorescence probe comprises a cyanine fluorophore and benzothiazole groups. The method includes stepsof (1), dropwise adding phosphoryl chloride into N, N'-dimethylformamide to obtain mixtures, then adding the mixtures into bromoacetic acid and carrying out reaction to obtain products II; (2), carrying out reaction on 2, 3, 3'-trimethyl indole and ethyl iodide to obtain products III; (3), dropwise adding piperidine into the products II and the products III and carrying out reaction to obtain products IV; (4), carrying out reaction on the products IV and aminothiophenol at the room temperature to obtain the visual organic molecular fluorescence probe. The visual organic molecular fluorescenceprobe and the method have the advantages that obvious color change of the visual organic molecular fluorescence probe can be seen in natural light or ultraviolet lamps, linear relations between the fluorescence intensity and peroxynitrite negative ions are established, and accordingly the peroxynitrite negative ions can be qualitatively and quantitatively detected; the visual organic molecular fluorescence probe is good in selectivity and high in sensitivity, detection methods are easy to implement, and obvious effects can be realized.
Owner:NORTH CHINA ELECTRIC POWER UNIV (BAODING)
Method for preparing perfluoroalkyl ethanol
InactiveCN107324973ASimple processLow costOrganic compound preparationHydroxy compound preparationGreeningTower
The invention discloses a method for preparing perfluoroalkyl ethanol. The method comprises the following steps: enabling perfluoroalkyl ethyl iodide, a mixed solvent and water to react, and separating and purifying the obtained mixture containing perfluoroalkyl ethanol, by-product olefins, solvent salt and water, thereby obtaining the perfluoroalkyl ethanol product, wherein the separation and purification comprise the following steps: (1) adding a mixture containing perfluoroalkyl ethanol, by-product olefins, solvent salt and water into a rectifying tower for performing reduced pressure distillation, controlling the vacuum degree to be -0.91 to -0.96MPa so as to obtain distillate containing perfluoroalkyl ethanol, by-product olefins and water and bottom liquid, performing strong base treatment on the bottom liquid, and filtering to obtain the recycled mixed solvent; and (2) performing azeotropic distillation on the distillate, thereby obtaining the mixed solution of the by-product olefins and water and the product perfluoroalkyl ethanol. The method disclosed by the invention has the advantages of simplicity in process, greening, environment friendliness, convenience, high efficiency and low cost.
Owner:JUHUA GROUP TECH CENT
A method for increasing the yield of fluorine-containing alkyl ethanol
InactiveCN102276415AHigh yieldLow costOrganic compound preparationHydroxy compound preparationOleumSulfite salt
Owner:山东中氟化工科技有限公司
Method for preparing perfluoro alkyl ethylene
InactiveCN101565350AEasy to separateLow investment costPreparation by hydrogen halide split-offSolventPressure reduction
The invention relates to a method for preparing perfluoro alkyl ethylene. The method comprises the following steps that: in a container provided with a mechanical stirrer, a condenser and a heating system, a solution of organic alkali and perfluoro alkyl ethyl iodide which is more than stoichiometric amount are mixed; the mixing solution is catalyzed by adding a catalyst and then subjected to heating backflow to generate the perfluoro alkyl ethylene; and the solvent and the perfluoro alkyl ethylene with higher purity are separated in modes of normal pressure rectification and pressure reduction rectification respectively. The method has the advantages that: the preparation method is simple, and the reaction is quick; the obtained product is easily separated and high in purity; the solvent can be recycled; and the use equipment is simple, so that the costs on energy and equipment investment are saved.
Owner:山东中氟化工科技有限公司
Organic phosphine-containing polymer carrier loaded Rh-based catalyst, preparation and applications thereof
InactiveCN111111775AHigh activityImprove stabilityOrganic-compounds/hydrides/coordination-complexes catalystsCatalyst activation/preparationPolymer sciencePropanoic acid
The invention provides a large-surface-area hierarchical-pore-structure organic phosphine-containing polymer loaded Rh-based catalyst for preparing ethyl propionate and propionic acid through ethanolheterogeneous carbonylation, and a preparation method thereof. The catalyst is mainly composed of a main active component and a carrier, wherein the main active component is an Rh metal complex, the content of the Rh metal complex is 0.01-5.0% of the weight of the catalyst, the organic phosphine-containing polymer carrier is generated by selecting an organic salt monomer containing vinyl phosphineand adopting a solvothermal method through self-polymerization or mixed polymerization. Through strong ionic bond action between a metal complex and the quaternary phosphonium salt in a polymer carrier skeleton, an Rh metal component is highly dispersed in the polymer carrier in a monatomic form, and in a fixed bed reactor, CH3CH2OH / CO can be converted into ethyl propionate with high activity andhigh selectivity at a certain temperature and pressure under the action of the catalyst and an iodoethane cocatalyst.
Owner:DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
Liquid phase reaction process of methyl acetate and CO to produce acetic anhydride and its catalyst preparing process
ActiveCN1986053AHigh activityImprove stabilityMolecular sieve catalystsCarboxylic acid anhydrides preparationAcetic anhydrideHigh heat
The present invention is the preparation process of acetic anhydride through liquid phase reaction of methyl acetate and CO and the preparation process of its catalyst. The catalyst has Rh-Pd complex with Rh / Pd weight ratio of 4-5 as the active component in 2.0-5.0 wt%, ethyl iodide or methyl bromide as co-catalyst in 0.5-9.5 wt%, and carrier of ZSM or MCM molecular sieve in 30.0-40.0 wt%. The catalyst is prepared through dissolving soluble compound of the catalyst and co-catalyst to obtain solution, soaking the carrier inside the solution, high temperature roasting at 500.0-600.0 deg.c for 1.0-1.5. The catalyst is used in preparing acetic anhydride through liquid phase reaction of methyl acetate and CO and can result in high methyl acetate converting rate and acetic anhydride yield. The present invention provides one new industrial production way.
Owner:山东华鲁恒升集团德化设计研究有限公司 +1
Preparation method of lubricating oil containing fluorine
The invention relates to a preparation method of lubricating oil containing fluorine, comprising the following steps: taking 34-72 parts by weight of perfluoro alkyl iodide or perfluoro alkyl ethyl iodide and 5-13 parts by weight of olefine monomer as main ingredients, adding 0.8-1.5 parts by weight of initiator, and carrying out synthetic reaction at the temperature of 40-120 DEG C for 0.5-4 hours; adding 1-12 parts by weight of catalyst, 30-65 parts by weight of acetic acid and 38-75 parts by weight of alcohol solvent after reaction, and reacting continuously at the temperature of 40-120 DEG C for 1-4 hours; filtering, removing the solvent, washing and dewatering, thus obtaining the fluorine containing lubricating oil. Compared with perfluoropolyether, the invention has the advantages that process is simple, service time is long, cost is reduced by 30%, thermal stability is good, viscosity thereof is slightly changed at the temperature of 220-280 DEG C, mechanical abrasion is reduced by more than 90%, cost performance is high, no pollution is produced, adaptive limit temperature range is wide, the adaptive limit temperate ranges from minus 40 to 280 DEG C, and the lubricating oil containing fluorine has small possibility of oxidation, thus being applicable to inflammable and explosive places, and the obtained fluorine containing lubricating oil can save fuel oil by more than12%, thus achieving obvious energy conservation effect.
Owner:JINZHOU DPF TH CHEM CO LTD
Preparation method for acyclic compound used as foaming agent
InactiveCN103819314ANot effectivelyHigh purityFlotationEther preparation by ester reactionsDialysis membranes1-Propanol
The invention belongs to the technical field of a mineral flotation preparation and discloses a method and approach for preparing a novel foaming agent. The method for preparing the foaming agent comprises the following eight steps in all (di-propoxy-ethoxy propanol is used as an example): 1, performing the reaction on dipropylene glycol and sodium hydride to generate sodium dipropylene glycol; 2, performing the reaction on 1-propanol and sodium hydride to generate 1-sodium propoxide; 3, performing the reaction on 2-diiodoethane and 1-sodium propoxide to generate 1-(2-iodoethoxy) propane; 4, performing the reaction on the sodium dipropylene glycol and the 1-(2-iodoethoxy) propane to generate a compound using the di-propoxy-ethoxy propanol as a main body; 5, removing a residual tetrahydrofuran solvent; 6, carrying out impurity removal and purification on the product by using a dialysis membrane; 7, carrying out concentration on the product; 8, purifying the product to obtain the di-propoxy-ethoxy-propanol with the purity of 99.96 percent. Compared with other commercial foaming agents widely and industrially applied, the foaming agent prepared through the method disclosed by the invention has relatively obvious advantages and characteristics on the aspects of fluid dynamics parameters and related flotation performance.
Owner:张炜
Perfluoroalkyl ethanol preparation method
InactiveCN103772150AHigh yieldMild conditionsOxygen-containing compound preparationOrganic compound preparationDistillationCarboxylic salt
The invention discloses a perfluoroalkyl ethanol preparation method. The method comprises the following steps: 1, adding perfluoroalkyl ethyl iodide carboxylate and an alcoholic solvent into a pressure-resistant reaction vessel, carrying out stirring heating for an esterification reaction for 3-48h, cooling the above obtained reaction liquid to room temperature, filtering out a generated iodized salt precipitate, distilling the obtained filtrate to recover the alcoholic solvent, and carrying out reduced pressure distillation to obtain perfluoroalkyl ethyl acrylate; and 2, mixing perfluoroalkyl ethyl acrylate, an alkali and an alcohol-water solvent, stirring at room temperature for 3-48h, carrying out reduced pressure distillation to remove the alcohol-water solvent, adding water and ether to the obtained residues, separating the obtained ether layer, extracting the obtained water layer with ether, drying the obtained ether layer mixture by anhydrous sodium sulfate, filtering, distilling the obtained filtrate to recover ether, and carrying out reduced pressure distillation of the residues to obtain highly-pure perfluoroalkyl ethanol. The method is economic, safe and environmentally-friendly.
Owner:JIANGSU LEE & MAN CHEM
Method for carrying out catalytic synthesis on arene 2,2,2-trifluoro-ethyl sulfide through copper
The invention discloses a method for carrying out catalytic synthesis on arene 2,2,2-trifluoro-ethyl sulfide through copper. The method includes the steps that copper iodide is adopted as a catalyst, diimine is adopted as a bidentate ligand, arene halogen, powdered sulfur and 2,2,2-trifluoro-ethyl iodide are adopted as reactants, sodium borohydride is adopted as a reducing agent, stirring is conducted for 1-24 hours at the temperature of 80 DEG C to 95 DEG C in an N,N-dimethyl formamide solvent, aftertreatment is conducted on reaction liquid after the reaction is completed, and the arene 2,2,2-trifluoro-ethyl sulfide compound is obtained. The synthesis method has the advantages that the catalyst is low in price, easy to obtain and low in toxicity, the raw materials are easy to obtain, operation is easy and convenient, and the universality of functional groups is good.
Owner:FUZHOU UNIV
Preparation process of diethyl zinc
A process for preparing diethyl zinc includes such steps as activating and drying Zn powder, adding it along with cuporous iodide and a quarter of the mixture of iodoethane and bromoethane into reactor, adding finished diethyl zinc as trigger, heating, adding rest of said mixture, heating, stirring while reacting, vacuum distilling and collecting product at a temp lower than -35 deg.C.
Owner:大连保税区科利德化工科技开发有限公司
Fiber material folding iodine adsorber
PendingCN110575730ASo as not to damageReduce weightGas treatmentDispersed particle separationFiberCarbon fibers
The invention relates to a fiber material folding iodine adsorber comprising an adsorber housing; an air inlet and an air outlet are respectively formed in two sides of the adsorber shell; a fiber material folding type filter element is arranged in an inner cavity of the adsorber shell; the fiber material folding type filter element comprises an adsorption layer formed by overlapping a plurality of layers of fiber material filter paper; filter paper is folded into a snake-bellied shape, two ends of the filter paper are bonded and sealed by a resin glue, and the adsorption layer is reinforced and supported by a supporting plate. During use, gas enters from the air inlet and penetrates through the adsorption layer, radioactive iodine in the gas is adsorbed through the adsorption layer, and the adsorbed and purified gas flows out from the air outlet. The adsorption layer is made of a porous carbon fiber filter paper material, the adsorption layer is soaked in a solution formed by triethylene diamine or potassium iodide alone or in a mixed mode according to a certain proportion, the adsorption layer has the capacity of adsorbing radioactive iodine (elemental iodine, inorganic iodide, methyl iodide, ethyl iodide and the like), and the porous carbon fiber filter paper material is light in weight and facilitates waste treatment.
Owner:CHINA INST FOR RADIATION PROTECTION
Synthetic method of N-(1H,1H,2H,2H-perfluorinated octyl) acrylamide
InactiveCN106278921AReduce usagePromote safe productionOrganic compound preparationCarboxylic acid amides preparationOrganic solventHydrogen
The invention discloses a synthetic method of N-(1H,1H,2H,2H-perfluorinated octyl) acrylamide. The method includes the steps that 1H,1H,2H,2H-perfluorinated hexyl ethyl iodide, sodium azide and organic solvent are mixed to react, water is added after the reaction is finished, the mixture is still standing and layered, and the organic layer is washed to obtain 1H,1H,2H,2H-perfluorinated octyl azide; under the action of Pd / C catalyst, hydrogen is used for hydrogenation reduction, and 1H,1H,2H,2H-perfluorinated octylamine is obtained through filtration and concentration; 1H,1H,2H,2H-perfluorinated octylamine, triethylamine and acryloyl chloride react in solvent at room temperature, after reaction is finished, the N-(1H,1H,2H,2H-perfluorinated octyl) acrylamide product is obtained through washing, concentration and reduced pressure distillation. The possibility of explosion in the production process is avoided, and the synthetic method has the advantages of being simple in process, safe in production, high in yield and easy to industrialize.
Owner:JUHUA GROUP TECH CENT
Environment-friendly preparation process for synthesizing perfluoroalkyl alcohol by solvent method
ActiveCN106495985ALow investment costSimple processOrganic compound preparationHydroxy compound preparationAlcoholGas phase
The invention discloses an environment-friendly preparation process for synthesizing perfluoroalkyl alcohol by a solvent method. The environment-friendly preparation process comprises the following steps: adding perfluoroalkyl ethyl iodide, a mixed solvent and water in a stirring reaction kettle, wherein the molar ratio of the water and the perfluoroalkyl ethyl iodide is 4-10:1, and the weight ratio of the mixed solvent and the perfluoroalkyl ethyl iodide is 3-10:1; in the temperature of 140-160 DEG C, reacting for 10-20 hours under the normal pressure backflow state; and washing layering, rectifying, and dehydrating the reaction liquid, and obtaining a product. After the end of the reaction, the gas phase detection analysis is performed to the product, the percent conversion of the perfluoroalkyl ethyl iodide is more than 98%, the selectivity of the perfluoroalkyl alcohol is more than 95%, and the yield of the perfluoroalkyl alcohol is more than 90%. The environment-friendly preparation process has the advantages of small device investment cost, simple process, low cost, safety and environment friendliness.
Owner:JUHUA GROUP TECH CENT
Processes for producing acetic acid from a reaction medium having low ethyl iodide content
ActiveUS20160137575A1Reduce concentrationStay focusedOrganic compound preparationChemical recyclingIodineMethyl acetate
A process for producing high purity acetic acid from a carbonylation reaction, wherein the carbonylation reaction is carried out while maintaining a low ethyl iodide content in the reaction medium. The ethyl iodide concentration may be maintained by removing acetaldehyde from the reaction medium and / or by adjusting at least one A) hydrogen partial pressure in the reactor, B) methyl acetate concentration of the reaction medium; and / or C) methyl iodide concentration of the reaction medium.
Owner:CELANESE INT CORP
Preparation method and application of a ratiometric fluorescent probe for detecting hydrazine
ActiveCN108982447BReduce consumptionImprove detection accuracyOrganic chemistryColor/spectral properties measurementsCyclohexanoneSodium acetate
The invention relates to a preparation method and application of a ratiometric fluorescent probe for detecting hydrazine. The preparation comprises the steps that phosphorus oxychloride is dissolved in dichloromethane, the mixture is slowly dropped into N,N-dimethylformamide, and after the dropwise addition is finished, cyclohexanone is added for reaction so as to obtain a compound 1; then, benzoindoles and iodoethane are dissolved in acetonitrile for heating and refluxing reaction so as to obtain a compound 2; the compound 1 and the compound 2 are subjected to heating and refluxing by takingmethylbenzene and n-butyl alcohol as solvents so as to obtain a fluorescent probe compound 3; the compound 3 is dissolved in anhydrous N,N-dimethylformamide, and sodium acetate is added for reaction under the protection condition of nitrogen so as to generate a compound 4; and the compound 4 is dissolved in anhydrous dichloromethane containing acetyl chloride, triethylamine is added for reaction for 4 hours at normal temperature under the protection of the nitrogen so as to generate the probe Ben-Cy1. ccording to the preparation method and application of the ratiometric fluorescent probe, theprobe works in a near-infrared region, is suitable for qualitative and quantitative analysis, low biotoxicity and high selectivity in biological samples and can be applied to the related fields of analytical chemistry, life organic analytical chemistry and the like.
Owner:QUFU NORMAL UNIV
Method for measuring ethoxy content of ethyl cellulose by using headspace gas chromatography
InactiveCN102183592AImprove continuityHigh sensitivityComponent separationInternal standardAdipic acid
The invention relates to a method for measuring ethoxy content of ethyl cellulose by using headspace gas chromatography. The measuring method comprises the following steps of: hydrolyzing the ethyl cellulose by hydroiodic acid in the presence of an adipic acid catalyst under high-temperature closed conditions, wherein the ethoxy of the ethyl cellulose is converted into iodoethane, o-xylene is used as an absorbent, and the hydrolysis reaction of the ethyl cellulose is complete due to the actions of the catalyst and the absorbent; selecting toluene as internal standard solution, selecting the iodoethane as standard sample solution, performing headspace sampling, and performing gas chromatography; and calculating the ethoxy content of the sample according to the peak areas of the internal standard solution and the standard sample solution. The method is superior to a common chemical titration method, and has the characteristics of short analysis time, simple operation, high accuracy and the like.
Owner:SOUTH CHINA UNIV OF TECH
Asymmetric squarylium cyanine colorimetric probe for identifying copper ions and application of asymmetric squarylium cyanine colorimetric probe
ActiveCN114315691AGood optical performanceHigh sensitivityOrganic chemistryMaterial analysis by observing effect on chemical indicatorEthyl groupTrimethyl benzene
The invention relates to an asymmetric squarylium cyanine colorimetric probe for identifying copper ions and application of the asymmetric squarylium cyanine colorimetric probe, and a preparation method of the asymmetric squarylium cyanine colorimetric probe comprises the following steps: synthesizing 3-ethyl-1, 1, 2-trimethyl-1H-benzo [e] indole from 1, 1, 2-trimethyl-1H-benzo [e] indole and iodoethane, synthesizing diethoxy squaric acid from squaric acid and ethanol, and synthesizing diethoxy squaric acid from 3-ethyl-1, 1, 2-trimethyl-1H-benzo [e] indole and 3-ethyl-1, 1, 2-trimethyl-1H-benzo [e] indole. The preparation method comprises the following steps: synthesizing 3-ethyl-1, 1, 2-trimethyl-1H-benzo [e] indole squaric acid hemicyanine from 3-ethyl-1, 1, 2-trimethyl-1H-benzo [e] indole, and synthesizing asymmetric double-square acid cyanine from the 3-ethyl-1, 1, 2-trimethyl-1H-benzo [e] indole squaric acid hemicyanine and 3-diethylaminophenol for selective recognition and detection of copper ions. The asymmetric squarylium cyanine chemical sensor has the beneficial effects that the asymmetric squarylium cyanine chemical sensor has the characteristics of good optical performance and high sensitivity. When the copper ions are detected and identified, the color of the solution is obviously changed, so that colorimetric detection is facilitated.
Owner:CHANGZHOU UNIV
Method for synthesizing aromatic hydrocarbon/alkane 2,2,2-trifluoroethyl selenium ether through copper catalysis and application of aromatic hydrocarbon/alkane 2,2,2-trifluoroethyl selenium ether to insecticides
ActiveCN109232343AGood adaptabilityThe reaction is easy to operateBiocideOrganic chemistrySolventChemistry
The invention relates to the field of crop pest insecticides and particularly relates to a method for synthesizing aromatic hydrocarbon / alkane 2,2,2-trifluoroethyl selenium ether through copper catalysis and application of an aromatic hydrocarbon / alkane 2,2,2-trifluoroethyl selenium ether compound to insecticides. The method comprises the following steps: taking cuprous iodide as a catalyst, taking diimine as a bidentate ligand, taking aromatic hydrocarbon / alkane halogen, selenium powder and 2,2,2-trifluoroiodoethane as reactants, taking sodium borohydride as a reducing agent, stirring for 1-24 hours under 95-110 DEG C in a N,N-dimethylformamide solvent, then carrying out post-treatment on reaction liquid after the reaction is ended to obtain a 2,2,2-trifluoroethyl selenium ether compound.The synthesis method has the advantages that the catalyst is cheap and easily available and is low in toxicity, the raw materials are easily available, the operation is simple and convenient, the functional group universality is high and the like; the fluorine-containing compound has high activity on plutella xylostella, tetranychus cinnabrinus and the like; the death rate of pests under the dosage of 600 mg / L of the fluorine-containing compound reaches up to 100%; the fluorine-containing compound can be used as a novel and efficient fluorine-containing insecticide.
Owner:FUZHOU UNIVERSITY
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