This invention relates to a method for preparing a hydrogenation palladium or carbon catalyst. The catalyst uses the particles or shaping active carbon as the carrier, loading active componentmetal Pd, wherein the Pd content is 0.2-5wt%. The preparing method comprises the following steps: a) acid cleaning the carrier active carbon; then flushing with water until neutral; drying; b) preparing Pd solution with water-soluble Pd compound and a complex builder; using Pd solution to immerse or spray the carrier active carbon, loading the Pd compound on the active carbon and then getting the catalyst prosoma, wherein the Pd compound content is 15-20wt% computed by Pd, the molecular ratio of complex builder and Pd is (0.01-1):1, the complex builder is any one from 8-bioquin, 2,3,4-trihydroxy-4-sulfonic acidazobenzene, ortho phenanthroline, o-aminophenol, o-hydroxybenzoic acidsodium or salicylaldehyde benzaldoxime; c) aging the catalyst prosoma, then deacidizing and getting the catalyst.
The invention discloses a method for preparing a single-molecular magnet [Dy2(saph)2(NO3)2(CH3OH)4] and relates to a method for preparing a single-molecular magnet. The invention aims at solving the problems that the synthetic method of the conventional rare earth complex single-molecular magnet is low in yield and the synthetic method of the complex is complicated. The method comprises the following steps: dissolving o-aminophenol salicylaldehyde in acetonitrile, thereby obtaining a solution A; dissolving dysprosiumnitrate in methanol, thereby obtaining a solution B; mixing the solution A and the solution B, adding a triethylamine solution into the mixed solution, stirring under room temperature condition, thereby obtaining a preform; and volatilizing a solvent out of the preform, thereby obtaining the complex. The [Dy2(saph)2(NO3)2(CH3OH)4] prepared by the method disclosed by the invention is a single-molecular magnet with good ferromagnetic properties, the yield of the preparation method disclosed by the invention is high and is over 52.84 percent, and the synthetic method of the single-molecular magnet is simple and high in repeatability. The invention belongs to the field of preparation of single-molecular magnets.
This is a kind of producing method of catalyst used for refining coarse terephthalic acid (CTA). The catalyst makes grains or molding active carbon as carrier, the content of loading active componentmetal Pd is 0.2 - 4wt%. It orderly includes: have acid wash to carrier active carbon; wash carrier active carbon with water to neutral; have soakage with watery solution containing nitriteion to carrier active carbon; dry carrier active carbon to get rid of water; prepare Pd solution with water-soluble Pd compound, a kind of complexing agent and water to infuse or insufflate the carrier active carbon; the content of Pd compound in the Pd solution counted by Pd is 15 - 20wt%; the mol proportion of complexing agent and Pd is (0.01 - 1) : 1, the complexing agent is got from anyone of 8-hydroxyquinoline, 2, 3, 4-trihydroxyl-4-sulfonic azobenzol, o-phenanthroline, o-Aminophenol, o-hydroxybenzoic sodium or o-hydroxybenzaldehyde oxime; after aginged, have deoxidizing treatment with reducing agent to get activator products.
The invention belongs to the technical field of water treatment, and particularly relates to a cubic nano ceriumoxide (CeO2) and application thereof as a mimic oxidase in degrading o-aminophenol. In the CeO2 preparation process, Ce(NO3)3.6H2O is used as a cerium source, urea is used as a precipitant, and CTAB (cetyltrimethylammonium bromide) is used as a surfactant. A precursor is firstly prepared, and the precursor is calcined to obtain the CeO2. Compared with the natural oxidase, the ceriumoxide provided by the invention has the advantages of high stability, low denaturation tendency, wide application range and high reutilization ratio, is easy for storage and transportation, also has high-efficiency oxidase catalytic activity, and thus, can well substitute the existing natural oxidase. When the cerium oxide provided by the invention is used in degrading o-aminophenol, the maximum degradation rate can reach 70% or above.
The invention discloses a preparation method of a single-molecular magnet [Dy2(saph)2Cl2].4CH3OH and relates to the preparation method of the single-molecular magnet [Dy2(saph)2Cl2].4CH3OH, which is used for solving the problems that an existing synthesis method for a rear-earth cluster compound single-molecular magnet is lower in yield, complex in synthesis method of a coordination compound and incapable of carrying out mass production. The preparation method comprises the following steps: I, dissolving o-aminophenol salicylaldehydeacetal into acetonitrile to obtain liquor A; dissolving dysprosiumchloride into methanol to obtain liquor B; mixing the liquor A with the liquor B, adding triethylamine with concentration of 0.001mol / L to obtain mixed liquor; II, stirring the mixed liquor obtained in the step I under the room temperature to obtain a preform; and III, volatilizing the preform in the solvent to obtain the single-molecular magnet [Dy2(saph)2Cl2].4CH3OH. The preparation method disclosed by the invention is simple, and high in yield which reaches over 45.76%. The preparation method disclosed by the invention is applied to the field of preparing the single-molecular magnets.
This is a kind of producing method of catalyst used for refining coarse terephthalic acid (CTA). The catalyst makes grains or molding active carbon as carrier, the content of loading active componentmetal Pd is 0.2 - 4wt%. It orderly includes: have acid wash to carrier active carbon; wash carrier active carbon with water to neutral; have soakage with watery solution containing nitriteion to carrier active carbon; dry carrier active carbon to get rid of water; prepare Pd solution with water-soluble Pd compound, a kind of complexing agent and water to infuse or insufflate the carrier active carbon; the content of Pd compound in the Pd solution counted by Pd is 15 - 20wt%; the mol proportion of complexing agent and Pd is (0.01 - 1) : 1, the complexing agent is got from anyone of 8-hydroxyquinoline, 2, 3, 4-trihydroxyl-4-sulfonic azobenzol, o-phenanthroline, o-Aminophenol, o-hydroxybenzoic sodium or o-hydroxybenzaldehyde oxime; after aginged, have deoxidizing treatment with reducing agent to get activator products.
The invention relates to the field of fluorescent probe compounds and discloses an iron ion fluorescent probe compound as well as a preparation method and application thereof. The fluorescent probe compound has the advantages of high luminous intensity, high sensitivity and wide pH adaptability. The fluorescent probe compound disclosed by the invention is a triphenylamineSchiff base type derivative with the chemical name of 2-hydroxyl-N-imidogenaniline-5-N,N-diphenylaniline. The invention further discloses the preparation method of the fluorescent probe compound, comprising the following steps: (a) taking ortho-aminophenol and 4-diphenylaminobenzaldehyde to react in an organic solvent to obtain a reaction solution; and (b) carrying out post-treatment on the reaction solution to obtain the fluorescent probe compound. The invention further discloses application of the fluorescent probe compound to detection of Fe<3+> ions.
The invention discloses a method for preparing diindolyl methane derivatives. The method comprises the following step: with titanocene dichloride and a ligand as catalysts, reacting indole and aldehyde to obtain the diindolyl methane derivative under an alkaline condition, wherein the ligand can be 8-hydroxyquinoline, catechol and o-aminophenol and the alkali is aniline, pyridine, pyrrole or triethylamine. The method is easy to operate, the reaction is high-efficiency and mild, the catalysts are low in price, non-toxic, stable to air and water, and substrate applicability is good; therefore, the method can be widely applied to preparation of diindolyl methane derivatives.
The invention discloses an aluminum ion fluorescent probe and a preparation method thereof. The method comprises the following steps: synthesizing 7-hydroxycoumarin-8-aldehyde by taking hexamethylenetetramine, 7-hydroxycoumarin and glacial acetic acid, and synthesizing the aluminum ion fluorescent probe by utilizing 7-hydroxycoumarin-8-aldehyde and ortho-aminophenol. The structure of the aluminumion fluorescent probe is represented by a nuclear magnetic spectrum and a mass spectrum; the spectral quality of the fluorescent probe is analyzed through an ultraviolet spectrum and a fluorescent spectrum; the result indicates that the fluorescent probe has high selectivity and is not interfered by other co-existing ions when identifying aluminum ions; and the probe generates coordination interaction with the aluminum ions according to the ratio of 1:1 and the reaction has reversibility. Therefore, the fluorescent probe can be applied to detection on the aluminum ions well.
This is a kind of producing method of catalyst used for refining coarse terephthalic acid (CTA). The catalyst makes grains or molding active carbon as carrier, the content of loading active componentmetal Pd is 0.2 - 4wt%. It orderly includes: have acid wash to carrier active carbon; wash carrier active carbon with water to neutral; have soakage with watery solution containing nitriteion to carrier active carbon; dry carrier active carbon to get rid of water; prepare Pd solution with water-soluble Pd compound, a kind of complexing agent and water to infuse or insufflate the carrier active carbon; the content of Pd compound in the Pd solution counted by Pd is 15 - 20wt%; the mol proportion of complexing agent and Pd is (0.01 - 1) : 1, the complexing agent is got from anyone of 8-hydroxyquinoline, 2, 3, 4-trihydroxyl-4-sulfonic azobenzol, o-phenanthroline, o-Aminophenol, o-hydroxybenzoic sodium or o-hydroxybenzaldehyde oxime; after aginged, have deoxidizing treatment with reducing agent to get activator products.
The invention belongs to the field of organic synthesis and in particular relates to a synthesis method of a polysubstituted isoindoline derivative. The synthesis method comprises the following steps:after sufficiently mixing arylchloride, o-aminophenol, olefin with an electron withdrawing group, a catalyst, an additive, an oxidant, an alkali and a solvent, raising temperature and reacting; after reaction is finished, carrying out post-treatment to obtain a target product.
The invention relates to a chlortetracycline (CTC) molecularly imprinted (MIP) affinity membrane sensor and a preparation method thereof. The specific affinity membrane is formed based on an electropolymerization method, and CTC as a template molecule and o-aminophenol (OAP) as a functional monomer form a molecularly imprinted polymer membrane on the surface of a glassy carbonelectrode by an electrochemistry method. CTC contains a phenolic hydroxyl group, an enol group and a dimethylamino group and the hydroxyl group in the OAP structure can be used as a latent coordination site so that OAP amino group, and phenolic hydroxyl group and enol group of CTC undergo intermolecular hydrogen bond interaction. OAP hydroxyl group and CTC dimethylamino group undergo a reaction so that multiple binding sites between OAP and CTC exist and the prepared molecularly imprinted polymer has very high CTC selectivity and bonding capability. The sensor can be used for on-site fast detection, does not need specimen pre-treatment, and has a low cost, simple processes and high sensitivity. The sensor has a detection linear range of 20-610nM and sensitivity of 15nM.
The invention provides a fluorescent probe for detecting peroxynitrite. The probe has a general structure formula Ia or Ib. The probe is prepared by: (1) stirring R4-substituted o-aminothiophenol or R4-substituted o-aminophenol and R1 / R2-substituted benzaldehyde in a methanol solution at a room temperature for two hours to obtain Ia; and (2) performing oxidative condensation of R4-substituted o-aminothiophenol or o-aminophenol and R2-substituted o-hydroxybenzaldehyde to obtain a benzothiazole or benzoxazole intermediate, coupling triflate converted by the phenolic hydroxyl group of the intermediate and R3-substituted p-hydroxybenzene tert-butyldimethylsilylester / p-aminobenzene tert-butyldimethylsilylester, and performing methylation of anilinenitrogen atoms and hydroxy elimination of silylester protecting group to obtain Ib. The fluorescent probe provided in the invention can have fast specific reaction with peroxynitrite to generate a product with strong fluorescence, so that specific detection of peroxynitrite is realized. The general structure formula of the probe in the invention is shown in the description.
A high-efficiency energy-saving diesel fuel additive is prepared from the following raw materials in parts by weight: 4-8 parts of sodium carboxymethylcellulose, 2-7 parts of 2-methyl cellosolve, 4-6 parts of tritolyl phosphate, 5-8 parts of calciumperoxide, 20-26 parts of ethyl alcohol, 5-7 parts of ferrocene, 3-7 parts of petroleumether, 5-7 parts of zincprimary alcohol dialkyl thiophosphate, 4-6 parts of graphite, 5-7 parts of N,N-disulfoxide salicyl propanediamine, 4-7 parts of isobutanol, 8-12 parts of ethelene glycol alkyl monophenyl ether, 3-7 parts of 3-hydroxybutyraldehyde, 4-8 parts of cyclopentane, 2-6 parts of triethyl orthoacetate, 4-7parts of ortho aminophenol, 2-4 parts of a modified additive and 4-6 parts of spermine. The high-efficiency energy-saving diesel fuel additive has the benefits that the utilization ratio of diesel oil is improved, an excellent protective effect is played for a fuel oilsystem, the heat efficiency is improved, the oil consumption is effectively reduced, and an efficient energy-saving effect can be played.
Disclosed is a 3-substituted nalidixic acid analog compound and its preparation method and uses in pharmacy, wherein the compound has antineoplastic activity and a general formula (I) with the 3-position substituted by benzimidazole and benzothiazole, the preparation process of the compound comprises condensing various substituted naphthyridine ketone-3-formylic acid, o-phenylenediamine, o-aminophenol, o-aminobenzenethiol and into polyphosphoric acids. The compound can be used in preparing anti-cancer medicaments.
The invention belongs to the technical field of thermosetting resin, and discloses benzoxazine monomer containing ethynyl groups and norbornene and a preparation method and application of the benzoxazine monomer. According to the preparation method, ortho-norbornene-functionalized phenol is firstly synthesized by using norbornene dianhydride and o-aminophenol, and then the benzoxazine monomer containing ethynyl groups and norbornene is prepared by using the ortho-norbornene-functionalized phenol, ethynyl-containing aniline and paraformaldehyde in a low-polarity solvent. In addition to curablecross-linking of oxazine rings, curing cross-linking can also be performed on carbon-carbon double bonds and ethynyl groups in norbornene groups; the curing temperature of the norbornene groups is reduced significantly through introduction of the ethynyl groups, and is reduced from 350 DEG C to 220 DEG C, so that the processability of the resin is improved; not only can a new variety be added to benzoxazine compounds, but also the thermodynamic properties of the resin material can be improved significantly by a multiple-crosslinked network system formed through curing of the resin; and the preparation method has the advantages of simpleness, high operability, high yield, low production cost and easy industrial production.
The invention discloses a method for synthesizing a benzoxazole compound by using nitration by-products of aromatic hydrocarbon and application of the benzoxazole compound. The method comprises the main process: performing step-by-step crystallization on nitration products of a 2,4-dinitrochlorobenzene production enterprise so as to obtain 2,4-dinitrochlorobenzene, 2,6-dinitrochlorobenzene (I) anda small amount of residues, adopting the obtained 2,6-dinitrochlorobenzene (I) as the main starting material, and performing hydrolysis, selective catalytic hydrogenation reduction, cyclization, halogenation, carbon-carbon coupling and other processes so as to synthesize the benzoxazole compound, wherein the obtained compound can be used as a main raw material to synthesize a series of chemical intermediates with important application, and the chemical intermediates include o-aminophenol, 2-amino-4-nitrophenol, 2-amino-5-nitrophenol and hydrochloride of o-aminophenol, 2-amino-4-nitrophenol, 2-amino-5-nitrophenol. Through the method, the industrial by-products are converted into high value-added aromatic aminophenol products, industrial hazardous waste of the 2,4-dinitrochlorobenzene production enterprise is reduced, the scope of products of the enterprise is widened, and the economic benefits of enterprise are increased.
The invention belongs to the field of chemical wastewater treatment and particularly relates to a method for treating o-nitrophenol production wastewater. For wastewater produced after o-nitrochlorobenzene is hydrolyzed to prepare o-nitrophenol, ethanol is adopted as a desorbent in the method; and under the premise of utilizing existing process equipment and basis procedures, valuable o-nitrophenol can be effectively recovered without the need of toxic / expensive chemical agents, special treatment equipment or extra energy consumption. On this basis, the method can achieve effective utilizationof an o-nitrophenol recovery product, improve the overall process efficiency for preparing the o-aminophenol and the recovery efficiency of salts and other by-products, and avoid secondary pollution.The invention further provides a method for producing o-aminophenol related to the aforementioned method for treating wastewater.
The invention provides Binol-diform-o-aminophenol type Schiff base, and a synthesis method and an application thereof, and relates to a 2,2'-dihydroxy-1,1'-dinaphthalene-3,3'-diformaldehyde-o-aminophenol type Schiff base, and a synthesis method and an application thereof. The invention aims to solve a problem that Schiff base prepared from 2-hydroxy-1-naphthaldehyde-o-aminophenol in a plane structure has no recognition capability on metals. The structure formula of the 2,2'-dihydroxy-1,1'-dinaphthalene-3,3'-diformaldehyde-o-aminophenol type Schiff base is represented as the description. The method includes the steps of: 1) preparing a crude product of the 2,2'-dihydroxy-1,1'-dinaphthalene-3,3'-diformaldehyde-o-aminophenol type Schiff base; and 2) concentrating the crude product, dissolvingthe crude product in methanol, performing suction filtration, and washing and drying the product to obtain a pure product. Compared with analogues having plane structures, the synthesized Schiff basehas significantly enhanced fluorescent recognition capability. The compound can be used for detecting cerium ions in trace amount.
The invention discloses 5-aryl-5H-dibenzo[b,f]azepine-10(11H) ketone compounds and a preparation method thereof. The preparation method comprises the following steps: reacting N-aryl-o-aminophenol compounds with o-bromophenylacetic acid compounds in the presence of an alkali, a catalyst and microwave to obtain a triarylamine intermediate substituted by carboxyl and hydroxyl; performing intramolecular acylation reaction and cyclization of the triarylamine intermediate in the presence of a catalyst to obtain the 5-aryl-5H-dibenzo[b,f] azepine-10(11H) ketone compounds. The method disclosed by the invention has the advantages of convenient and simple operation, short reaction time and convenient post treatment; and the ketone compounds are conveniently prepared by using simple raw materials, and therefore sustainable development and utilization can be achieved.