54 results about "Diaminomaleonitrile" patented technology

The invention discloses a preparation method of high-purity 4,5-dicyano-2-trifluoromethylimidazole and salts thereof. The preparation method comprises the following steps: placing diaminomaleonitrile, trifluoroacetic acid and phosphorus pentoxide at a molar ratio of 1:(1-10):(0.5-2) in a reactor, adding a solvent or not, reacting at a reaction temperature of 40-140 DEG C for a reaction time of 0.5-8 hours, after the reaction, evaporating to remove the solvent and residual trifluoroacetic acid to obtain an intermediate product 4,5-dicyano-2-trifluoromethyl-imidazole; purifying the intermediate product 4,5-dicyano-2-trifluoromethyl-imidazole; and reacting the purified 4,5-dicyano-2-trifluoromethyl-imidazole and salts or hydroxide of a metal element to obtain 4,5-dicyano-2-trifluoromethylimidazole salts. The preparation method has mild entire process conditions and relatively low device investment and is suitable for requirements of large-scale production.

The invention belongs to the technical field of preparation and application of compounds, and particularly relates to a coumarin dye-based ratio-type bi-functional fluorescent probe, as well as synthesis and application of same. In the invention, for the first time, a new-type coumarin fluorescent ratio-type probe is synthesized. The method includes the steps of: 1) dissolving 7-hydroxy-4-methyl coumarin and urotropine in glacial acetic acid, performing a reaction, adding concentrated hydrochloric acid to the mixture so that the mixture is reacted therewith; 2) performing purification and separation by column chromatography to obtain a product, coumaric aldehyde; 3) dissolving the coumaric aldehyde and diamino maleonitrile in acetonitrile, dropwise adding a less amount of concentrated hydrochloric acid, stirring the mixture at room temperature, and performing separation and purification to obtain a final target product. The ion probe can effectively and quickly recognize copper and hypochloric acid, is high in selectivity and ionic competitiveness, and can be used for recognition of related actual water samples.

The invention relates to a composite material of a lithium battery cathode. The composite material is prepared according to a method taking DAMN as a modifier during N doping of graphite oxide. SnCl4.5H2O is added in the N doping process, and a composite structure of carbon nitride and tin oxide is formed through high-temperature carbonization. The invention further provides a SnO2 / CxNy / GN composite material which is controllably prepared according to a one-step hydro thermal method and high in N content. The SnO2 / CxNy / GN composite material is high in electrochemical property while being used for preparing the lithium battery cathode; due to nano-dispersion of SnO2 particles, cross-linking polymerization between the surfaces of the SnO2 particles and N-doped graphene, and introduction of DAMN, not only is the conductibility of graphite oxide improved, but also more reaction active sites are provided for reaction with SnO2 nanocrystalline, and the SnO2 nano-particles are stably and uniformly dispersed in a lamella of carbon nitride and graphene.

The invention relates to a method for preparing an imidazole compound with the following formula: wherein Rf is a fluorinated alkyl group comprising between 1 and 5 carbon atoms, said method comprising: (a) the reaction of the diaminomaleonitrile with the following formula: with the compound with the following formula: wherein Y represents a chlorine atom or the OCORf group to form the salified amide compound with the following formula: at temperature Tau1, and (b) the dehydration of the salified amide compound with formula (IVa) and / or the corresponding amino (IVb) to form the imidazole compound with formula (III), at temperature T2 higher than T1.

The invention relates to a composite material for a lithium-sulfur battery positive electrode and a preparation method of the composite material. Prevulcanization polymerization reaction is performedon diaminomaleonitrile and sulfur under a high temperature, sulfur eight-ring is opened under the high temperature to form a free radial, cyan cyclotrimerization is catalyzed to form a covalent triazine framework, sulfur is fixed on a polymer framework in a C-S bond form, and more sulfur is loaded onto the covalent triazine framework by a melting method. The nitrogen atom-doped covalent triazine framework has favorable conductivity, and the conductivity of the sulfur positive electrode can be effectively improved; the damage of volume expansion and shrinkage of the sulfur positive electrode tothe positive electrode can be reduced during the charge-discharge process by the stable covalent triazine framework, the sulfur fixed in the material in a chemical bond form can be used for effectively preventing a shuttle effect of lithium polysulfide, and excellent cycle property and rate performance of the composite material when used for the lithium-sulfur battery can be shown.

The invention relates to a Schiff base multifunctional fluorescence probe, and a preparation method and application thereof. The structure of the fluorescence probe is shown as a formula shown as the accompanying drawing. According to the preparation method, dimethylamino acraldehyde and diaminomaleonitrile are dissolved into an alcoholic solution to be prepared into a mixed solution; concentrated hydrochloric acid is added into the mixed solution; reaction is performed for 5 to 7h at 70 to 80 DEG C; precipitation, filtration and washing are performed; then, recrystallization is performed to obtain a purified product. The Schiff base multifunctional fluorescence probe has the advantages that the fluorescence probe is a Schiff base compound and comprises imine bonds and amino groups; the good selectivity is realized on Cu<2+> and PO4<3-> recognition; when the fluorescence probe acts with other common metal ions or anions, the fluorescence signals are not basically changed; the anti-interference capability is high; good sensing properties are realized; the detection limit is low; meanwhile, the preparation process of the fluorescence probe is simple; the operability is high.

The invention discloses a rhodamine B derivatives-based multi-channel fluorescent probe, a preparation method and application thereof. The chemical formula of the fluorescent probe is C34H34N8O2; thepreparation method includes steps of preparing a compound A by mixing rhodamine B and hydrazine hydrate in accordance with a molar ratio of (0.25-1):1; then preparing a compound B by mixing the compound A and glyoxal in accordance with the molar ratio of (0.25-1):1; dissolving the compound B and diaminomaleonitrile in anhydrous ethanol in accordance with the molar ratio of (0.25-1):1; adding 2-3 drops of glacial acetic acid and preparing the multi-channel fluorescent probe through stirring, refluxing, distillation and separation. The fluorescent probe is applied to detection of trivalent metalion and Hg<2+> ion. Furthermore, the invention has the significant advantage that the fluorescent probe can enhance recognition of Fe<3+>, Cr<3+>, Al<3+> and Hg<2+> fluorescence in identical solventenvironment, with high detection sensitivity.

The invention discloses a preparation method of high-purity 4,5-dicyano-2-trifluoromethylimidazole and salts thereof. The preparation method comprises the following steps: placing diaminomaleonitrile, trifluoroacetic acid and phosphorus pentoxide at a molar ratio of 1:(1-10):(0.5-2) in a reactor, adding a solvent or not, reacting at a reaction temperature of 40-140 DEG C for a reaction time of 0.5-8 hours, after the reaction, evaporating to remove the solvent and residual trifluoroacetic acid to obtain an intermediate product 4,5-dicyano-2-trifluoromethyl-imidazole; purifying the intermediate product 4,5-dicyano-2-trifluoromethyl-imidazole; and reacting the purified 4,5-dicyano-2-trifluoromethyl-imidazole and salts or hydroxide of a metal element to obtain 4,5-dicyano-2-trifluoromethylimidazole salts. The preparation method has mild entire process conditions and relatively low device investment and is suitable for requirements of large-scale production.

The invention relates to an amidoxime-group-modified cyclodextrin / sodium alginate gel ball composite adsorption material which is prepared by combining amidoximated diaminomaleonitrile with an oxygen-containing functional group of sodium alginate and an oxygen-containing functional group of cyclodextrin, so that on the one hand, amidoxime groups are introduced, adsorption sites in gel are increased, and selective adsorption capacity of composite material to hexavalent uranium is greatly enhanced; on the other hand, the sodium alginate and the cyclodextrin enhance the mechanical properties of the material and obtain stronger mechanical properties, so that the material has good mechanical properties, can be repeatedly used for multiple times, is easy to separate from water, and adsorption sites in the composite aerogel are also increased; the composite adsorption material is used for enriching hexavalent uranium, is high in enrichment rate and short in adsorption time, is not influencedby seawater salinity, can be repeatedly used, is easily separated from a water body, and is easy to recover and recycle.

The invention discloses a diaminomaleonitrile derivative being characterized in that a structural formula is represented as the formula (I). The invention also discloses a preparation method and an application of the diaminomaleonitrile derivative. A chemical sensor prepared from the diaminomaleonitrile derivative is sensitive in response to mercury ion, is good in selectivity, is high in recognizing intensity and is free of interference of foreign metal ions. Meanwhile, fluorescence of the sensor appears in a visible region when the sensor detects the mercury ion so that existence of the mercury ion can be detected just by naked eyes in a colorimetric analysis manner. The method is high in practical value and has a huge application prospect in quick and simple detection of the mercury ion.

A method for preparing an imidazole compound with the following formula: wherein Rf is a fluorinated alkyl group comprising between 1 and 5 carbon atoms, said method including: (a) the reaction of the diaminomaleonitrile with the following formula: with the compound with the following formula: wherein Y represents a chlorine atom or the OCORf group to form the salified amide compound with the following formula: at temperature T1, and (b) the dehydration of the salified amide compound with formula (IVa) and / or the corresponding amino (IVb) to form the imidazole compound with formula (III), at temperature T2 higher than T1.

The invention discloses a pyridazino quinoxaline diamine Schiff base cobalt ion fluorescent probe and a preparation method thereof. The preparation method comprises the following steps: taking a camphor derivative camphorquinone as a raw material, and carrying out cyclization reaction on the camphor derivative camphorquinone and 2, 3-diaminomaleonitrile to obtain 5, 9, 9-trimethyl-5, 6, 7, 8-tetrahydro-5, 8-bridge methylene quinoline-2, 3-dicarbonitrile; carrying out condensation cyclization with hydrazine hydrate to obtain 6, 11, 11-trimethyl-6, 7, 8, 9-tetrahydro-6, 9-bridged methylene pyridazino [4, 5-b] quinoxaline-1, 4-diamine; carrying out condensation reaction with 2-hydroxyl-1-naphthaldehyde to obtain 6, 11, 11-trimethyl-6, 7, 8, 9-tetrahydro-6, 9-bridge methylene pyridazino [4, 5-b] quinoxaline-1, 4-diamine condensed 2-hydroxyl-1-naphthaldehyde bis-schiff base. The compound can be quickly and specifically complexed with Co < 2 + > at room temperature, so that orange-yellow fluorescence of a solution is quenched, the color of the solution is changed from orange red to dark red under sunlight, and the compound can be used as a fluorescent probe for detecting cobalt ions andhas a good application prospect.

The invention discloses a method for detecting trace iron ions at high sensitivity, which comprises the steps of: searching a proper medium condition of diaminomaleonitrile (DAMN); measuring fluorescence intensities of a coordination compound, the coordination compound and a medium, and the coordination compound and the medium and metal ions; determining hypersensitivity or quenching effect generated by metal ions to the fluorescence of the coordination compound; measuring a linear relation between the concentration of the metal ions and a quenching value; and measuring the content of the metal ions in food. By using characteristic of quenching generated by the iron ions to the fluorescence of the DAMN and the linear relation formed between the fluorescence quenching value (delta F) and the concentration of the iron ions, the method is further used for measuring the content of iron in foods of infant rice flour, milk powder and the like, wherein the detection limit of the iron is 1.5 mu g.L<-1>, and the relative standard deviation is 0.17 percent. Compared with the prior art, the method has the advantages of good selectivity, high sensitivity, simple and convenient use, and the like.

The invention relates to a near infrared fluorescent dye THX-Ba for mitochondrial localization and a preparation method and an application thereof. The dye has the structural formula (I) and has stable pH fluorescence opening effect in water phases under different pH conditions, and prepared diaminomaleonitrile condensation derivatives can be used for hypochloric acid detection. The fluorescent dye has the following advantages: the fluorescent dye has the properties of stability to pH, large Stokes displacement (116 nm), good light stability, good water solubility, good cell membrane permeability and excellent mitochondrial localization performance, aldehyde and carboxyl groups of the fluorescent dye can be easily modified to generate biologically related tracers, and derivatives obtainedafter the aldehyde groups are condensated with diaminomaleonitrile have remarkable selective recognition performance for hypochloric acid and are excellent mitochondrial localization near infrared fluorescence probes for selective hypochloric acid detection.

The invention discloses a method for synthesizing 4-(1-hydroxyl-1-methylethyl)-2-propyl iminazole-5-carboxylic ethyl ester, which comprises the steps of: using trimethyl orthobutyrate and diaminomaleonitrile as raw materials, and performing backflow reaction to prepare an imidic acid ester intermediate in presence of alcohols solvents; adding active carbon, continuously performing backflow for 1 hour, and filtering while the mixture is hot; cooling the filtrate to 0-15 DEG C, and introducing ammonia to prepare 2-propyl iminazole-4,5-dinitrile; adding the 2-propyl iminazole-4,5-dinitrile to a mixed solution of hydrochloric acid and ethanol and esterfying in backflow state to prepare 2-propyl iminazole-4,5-diethyl dicarboxylate; and performing reaction of 2-propyl iminazole-4,5-diethyl dicarboxylate and a Grignard reagent to prepare the 4-(1-hydroxyl-1-methylethyl)-2-propyl iminazole-5-carboxylic ethyl ester. By adopting the synthesizing method, the total yield of the synthesized 4-(1-hydroxyl-1-methylethyl)-2-propyl iminazole-5-carboxylic ethyl ester is 81% which is obviously superior to the total yield (55%) of the traditional references; and the invention has the advantages of concise process and low cost and is suitable for industrial production.

A process for preparing 2-alkylimidazole-4,5-dicarboxylic acid includes such steps as putting 2-alkyl benzimidazole in solvent, and oxidizing loop-opening reaction under existence of catalyst and oxidant.

The invention discloses a covalent organic framework material, a preparation method and an application thereof. The preparation method comprises the following steps: refluxing hexaketocyclohexane octahydrate and diaminomaleonitrile; filtering out a black suspension while a solution is hot; washing by using hot AcOH; obtaining a black solid, and suspending the black solid in 30wt% HNO3; carrying out heating treatment to obtain a dark brown suspension; and pouring the hot dark brown suspension into ice water, filtering the suspension to obtain black solid HAT-CN, and carbonizing HAT-CN under protection of nitrogen or an inert gas to prepare the covalent organic framework material COF-CN. A first specific discharge capacity of the prepared electrode material reaches 1695mAh / g under current density of 0.01 V-3V and 100mA / g; and a discharge capacity is 708mAh / g after 50 cycles.

The invention provides a tetraphenyl ethylene-diaminomaleonitrile derivative which has a structure in a formula (I) and provides a novel compound, namely the tetraphenyl ethylene-diaminomaleonitrile derivative. The tetraphenyl ethylene-diaminomaleonitrile derivative has the structure as shown in the formula (I), and the molecular formula is C31H22N4. The tetraphenyl ethylene-diaminomaleonitrile derivative has a typical AIE effect, is high in luminous intensity in water, sensitive in response to Hg<2+>, good in selectivity and high in specificity, is almost not disturbed by hetero-metal ions, and is an ideal sensing molecule for quickly detecting Hg<2+> in water. Furthermore, the preparation method is simple, feasible, mild in condition and suitable for industrialized application. The formula is as shown in the specification.

The invention relates to an amidoxime group-containing three-dimensional cyclodextrin / graphene aerogel composite adsorbing material and a preparation method and application thereof. According to the preparation method, amidoximation diaminomaleonitrile is combined with an oxygen-containing functional group of graphene oxide and an oxygen-containing functional group of cyclodextrin, on one hand, anamidoxime group is introduced, the selective adsorption capacity of the composite material on hexavalent uranium is greatly enhanced, on the other hand, amidoximated diaminomaleonitrile is rich in amino groups, the graphene oxide can react with an oxygen-containing group on a graphene oxide sheet layer and an oxygen-containing group on carboxymethyl-beta-cyclodextrin, according to the preparationmethod, the graphene aerogel serves as a carrier, amidoxime groups are crosslinked to the graphene aerogel, the crosslinking degree of the aerogel is increased, formation of the aerogel is facilitated, meanwhile, the specific surface area of the composite material is greatly increased, the material is endowed with high adsorption capacity, the enrichment rate is high when the composite material is used for enriching hexavalent uranium, and the adsorption time is short.

The invention discloses an environment-friendly printing ink. The printing ink comprises the following components in parts by weight: 20-30 parts of polymerizable water-soluble hyperbranched polyamide, 20-30 parts of diaminomaleonitrile / 2,2'- [1,4-phenylene bis(oxymethylene)]diethylene oxide polycondensate, 1-3 parts of tetramethyl tetravinyl cyclotetrasiloxane, 0.5-1 part of water-based photoinitiator, 0.5-1 part of dispersing agent, 0.2-0.6 part of defoaming agent, 10-13 parts of water-based pigment, 1-4 parts of emulsifying agent and 20-30 parts of deionized water. The invention also discloses a preparation method of the environment-friendly ink. The environment-friendly ink disclosed by the invention has the advantages of good adhesive force, friction resistance, good solvent resistance, high curing speed, good performance stability, good flexibility, and safety and environmental protection in use.

The invention discloses a tanshinone benzimidazole fluorescent probe for detecting ClO <-> ions as well as a preparation method and application of the tanshinone benzimidazole fluorescent probe, and belongs to the technical field of fine organic synthesis. 4-(1, 6, 6-trimethyl-7, 8, 9, 12-tetrahydro-6H-furan [2 ', 3': 1, 2] phenanthro [3, 4-d] imidazole-11-yl) benzaldehyde is prepared through direct condensation reaction of tanshinone IIa with terephthalaldehyde and ammonium acetate, then the 4-(1, 6, 6-trimethyl-7, 8, 9, 12-tetrahydro-6H-furan [2 ', 3': 1, 2] phenanthro [3, 4-d] imidazole-11-yl) benzaldehyde reacts with 2, 3-diamino-2-butene dinitrile to synthesize 2-amino-3-(((E)-4-(1, 6, 6-trimethyl-7, 8, 9, 12-tetrahydro-6H-furan [2 ', 3': 1, 2] The compound is (2R, 3R, 4R, 4R, 4d) imidazole-11-yl) benzylidene) amino) maleic nitrile. Benzimidazolyl and diaminomaleonitrile Schiff base groups are introduced into the probe, the probe can selectively react with ClO <->, fluorescence is enhanced, and the detection result is accurate.

The invention relates to a drying method of an imidazolyl fluorine-containing lithium salt. The method comprises the following steps: (1) adding diaminomaleonitrile and perfluorinated anhydride into a reaction container, adding a solvent into the container, carrying out a stirring reaction, and after the diaminomaleonitrile is completely reacted, evaporating to remove the reaction solvent and a byproduct to obtain an intermediate product 2-perfluoroalkyl-4, 5-dicyanoimidazole; (2) carrying out a reaction on 2-perfluoroalkyl-4, 5-dicyanoimidazole and a metal salt or hydroxide aqueous phase suspension until the system is neutral to obtain a 2-perfluoroalkyl-4, 5-dicyanoimidazole salt; (3) decolorizing the 2-perfluoroalkyl-4, 5-dicyanoimidazolium salt in pure water by using activated carbon, filtering, and recrystallizing in pure water; (4) rinsing the 2-perfluoroalkyl-4, 5-dicyanoimidazolium salt obtained in the step (3) by using a solvent with water; and (5) filtering the rinsed 2-perfluoroalkyl-4, 5-dicyanoimidazole salt, and carrying out vacuum drying on the filtered 2-perfluoroalkyl-4, 5-dicyanoimidazole salt to obtain a finished product of the 2-perfluoroalkyl-4, 5-dicyanoimidazole lithium salt. According to the invention, the generation of reaction byproducts can be effectively avoided, and the subsequent vacuum drying effect is improved.

The invention discloses a synthesis method based on diaminomaleonitrile asymmetric Schiff base. The asymmetric Schiff base synthesis method, namely an acyl chloride occupation method, is efficient, simple and wide in application and is explored by virtue of high acyl chloride reaction activity. The preparation method of the base comprises the following steps: enabling reaction of diaminomaleonitrile and acetyl chloride in an ice water bath to obtain a monoacetylated product Ac-DAMN, and then enabling a condensation reaction with salicylaldehyde to obtain an asymmetric Schiff base ligand; enabling reaction of the ligand and Zn(NO3)2*6H2O in a methanol solution to obtain a coordination crystal. The method is simple in reaction, mild in condition, easy to operate and high in product yield, and is a novel technology for designing and synthesizing the asymmetric Schiff base through the acyl chloride occupation method and further synthesizing the asymmetric Schiff base complex.

The invention discloses a method for continuously preparing 2-trifluoromethyl-4, 5-dicyanoimidazole lithium salt, and a reaction device and belongs to the field of preparation of 2-trifluoromethyl-4, 5-dicyanoimidazole lithium salt. The method comprises the following steps of: generating 2-trifluoromethyl-4, 5-dicyanoimidazole from trifluoroacetic anhydride and diaminomaleonitrile; and making the 2-trifluoromethyl-4, 5-dicyanoimidazole to react with lithium carbonate so as to generate the 2-trifluoromethyl-4, 5-dicyanoimidazole lithium salt. In order to overcome the defects in existing intermittent reaction, the invention provides the method for preparing the 2-trifluoromethyl-4, 5-dicyanoimidazole lithium salt and the reaction equipment, the method can be used for continuous production and has relatively high efficiency.

The invention discloses an industrial production method of 4-amino-5-imidazolecarboxamide, belonging to the technical field of organic synthesis. The industrial production method comprises the following steps: S1, reacting diaminomaleonitrile with formamide under the action of phosphorus oxychloride to generate an intermediate 1; and S2, subjecting the intermediate 1 to a ring closing reaction under an alkaline condition so as to generate 4-amino-5-imidazolecarboxamide. The method has the advantages of simple raw materials, low price, short reaction steps, short production period, simple operation and easy realization of industrial production, avoids the generation of cyano-containing wastewater, nitrogen-containing wastewater and the like in traditional synthesis methods, causes very small environmental protection pressure, and realizes preparation of the high-quality 4-amino-5-imidazolecarboxamide only through two reactions.