34 results about "Synthesis methods" patented technology

The invention discloses a synthesis method for terpolymer block silicone oil. The synthesis method is characterized by comprising the steps of: (A) adding 100 parts by weight of dimethyl cyclosiloxane or octamethyl cyclotetrasiloxane, 4 parts by weight of epoxy-terminated disiloxane and 15 parts by weight of dimethylacetamide, raising the temperature to 70-80 DEG C, adding 0.02-0.1 part by weight of base catalyst, raising the temperature to 110-120 DEG C, reacting for 3-4 hours, slowly opening vacuum, extracting solvents and low molecular weight matters, continuously raising the temperature to 140-145 DEG C, maintaining the temperature and the vacuum for 2 hours, so as to obtain epoxy silicone oil; and (B) adding 80-100 parts by weight of epoxy-terminated silicone oil, 6-30 parts by weight of polyether polyol and 150 parts by weight of isopropyl alcohol, carrying out backflow reaction for 6-15 hours at 80-86 DEG C, and decompressing and removing the isopropyl alcohol or adding a propylene glycol displacement solvent, so as to obtain amino polyether block silicone oil. By utilizing the terpolymer block silicone oil disclosed by the invention, the fabric has good hand feel, namely fluffy feel and smooth feel, cannot be yellowed or is slightly yellowed.

Highly luminescent nanostructures, particularly highly luminescent quantum dots, comprising a nanocrystal core and thick shells of ZnSe and ZnS, are provided. The nanostructures may have one or more gradient ZnSe_xS_1-x monolayers between the ZnSe and ZnS shells, wherein the value of x decreases gradually from the interior to the exterior of the nanostructure. Also provided are methods of preparing the nanostructures comprising a high temperature synthesis method. The thick shell nanostructures of the present invention display increased stability and are able to maintain high levels of photoluminescent intensity over long periods of time. Also provided are nanostructures with increased blue light absorption.

The invention relates to a fluorosilicon waterproof oil repellent, and a synthesis method and application thereof. The synthesis method comprises the following steps: (1) mixing sodium borohydride, a simple substance iodine and 1/4 of perfluorinated polyether; slowly and dropwisely adding the rest 3/4 of perfluorinated polyether into the mixed solution, and reacting to obtain perfluorinated polyether methanol; (2) continuing adding bromopropylene and potassium carbonate, and reacting to obtain allyl perfluorinated polyether; and (3) mixing the allyl perfluorinated polyether, alkoxy silane and a platinum catalyst, and reacting to obtain the target product trialkoxysilylpropyl perfluorinated polyether. The fluorosilicon waterproof oil repellent is applicable to various glass panels, can easily form a film on the premise of ensuring the laminating effect, can obviously increase the scratch resistance of the protective film, and enables the protective film to have the waterproof, anti-fingerprint and oil-repellent functions. Besides, the film is very smooth, and thus, the fluorosilicon waterproof oil repellent has wide application prospects in high-end fields.

Provided is an auto-thermal evaporative liquid-phase synthesis method for cathode material for battery, comprising the following steps: (1) Adding a synthetic raw material of cathode material into a solvent to obtain a mixture A, the synthetic raw material of the cathode material containing lithium source, adding an accelerant into the mixture A, which makes the mixture A achieve a strong auto-thermal reaction to release heat to evaporate the solvent, and obtaining a solid precursor of the cathode material; (2) Drying the precursor, sintering in an atmosphere furnace and obtaining the cathode material. The method is simple in process, low in energy consumption, requirements for equipment and cost, and is applicable to industrial mass production and application. The cathode material obtained through the method is stability in batch, easy to process, low in internal resistance and high in capacity and has an excellent charging and discharging performance.

The present invention relates to a new process of synthesizing conductive polymers from monomers substituted with amine group. The process provides simple synthesizing steps for the conductive polymers without using other additives such as stabilizers or emulsifiers. The conductive polymers synthesized according to the present invention have highly enhanced solubility in common organic solvents and electrical conductivity compared to conventional conductive polymers. Therefore, the conductive polymers synthesized according to the present process can be utilized in applications that require high electrical conductivity, for example an electromagnetic interference shield or a transparent electrode of thin film, as well as in specific applications such as various conductive films, fibers, polymer blends, battery electrodes or conductive etch mask layers.

The invention discloses a method for synthesizing red fluorogold nano-clusters through photoinduction and application thereof and belongs to the technical field of fluorogold nano-clusters. The methodcomprises the following steps: under a room temprature condition, adding mono(6-mercapto-6-deoxy)-beta-cyclodextrin into chloroauric acid and reacting at a stirring speed of 550 to 600 rmp until a solution becomes colorless, so as to obtain a solution A; slowly adding silver nitrate into the solution A and reacting at the stirring speed of 550 to 600 rmp for 9 to 10 min; then adding lipoic acid to obtain a mixed system B; reacting at the stirring speed of 550 to 600 rmp for 9 to 10 min; then regulating the pH (Potential of Hydrogen) of the solution to 3.5 to 4.5 by adopting hydrochloric acid,so as to obtain a solution B; putting the solution B under LED (Light Emitting Diode) lamplight and reacting for 85 to 90 min, so as to obtain a light yellow solution, i.e., the red fluorogold nano-clusters Au(0)@Au(I)-6-SH-beta-CD. According to the method disclosed by the invention, a photo-reduction method takes mercapto-beta cyclodextrin as a coating agent to synthesize gold nano-clusters; anda synthesis method is simple and can be used for selectively detecting silver ions.

The invention relates to a preparation method of diphenyl ether dianhydride and isomers thereof, which is characterized in that the preparation method comprises the following steps of: adding solvent and monochlorophthalic anhydride into a reactor with a drying and distilling device, increasing temperature for reflux for a certain period under the protection of N2, adding alkali metal salt and catalysts, conducting reflux reaction for a certain period, decreasing the temperature, conducting filtration to obtain crude products, adding cyanophenyl and the crude products prepared through the reaction into the clean reactor with the drying and distilling device, increasing the temperature for reflux for a certain period under the protection of N2, decreasing the temperature, conducting filtration and drying to obtain the diphenyl ether dianhydride and the isomers thereof. The preparation method provided by the invention has the advantages that the synthesis method of the diphenyl ether dianhydride is widened, the preparation process of the diphenyl ether dianhydride is simplified, the environmental pollution is reduced and a new method is provided for the industrial production of the diphenyl ether dianhydride.

The invention relates to a zinc oxide-based nano-drug composition, and a preparation method and an application thereof. The preparation method of the composition comprises the following steps: 1, mixing a sodium hydroxide and/or potassium hydroxide-alcohol solution and a zinc acetate-alcohol solution to obtain a zinc oxide colloid reaction solution; 2, taking the zinc acetate-alcohol solution, simultaneously or successively adding the zinc acetate-alcohol solution and the drug molecule-containing sodium hydroxide and/or potassium hydroxide-alcohol solution to the zinc oxide colloid reaction solution obtained in step 1; and 3, centrifuging a mixed solution obtained in step 2, removing the obtained supernatant, washing the obtained material, purifying the washed material, and drying the purified material to prepare the composition. Zinc oxide is compounded with the drug through directly using the self properties of zinc oxide and the drug, and no polymer is introduced, so the synthesis method is simple and effective. The prepared composition has good dispersibility, the hydrodynamic size is 40-90nm, and the composition has the characteristics of high bioavailability, low toxicity and degradability.

Embodiments of the invention provide a picture synthesis method and apparatus. The method specifically comprises the steps of adding to-be-synthesized sub-pictures to a sub-picture directory in response to an addition instruction for the to-be-synthesized sub-pictures, thereby obtaining sub-pictures in the sub-picture directory; performing synthesis according to the sub-pictures in the sub-picture directory to obtain a corresponding first target picture; determining a storage path of the first target picture; and generating a Less file corresponding to the first target picture according to synthesis information corresponding to the sub-pictures in the sub-picture directory and the storage path of the first target picture. According to the method and the apparatus provided by the embodiments of the invention, the update of the first target picture can be realized through the update of the sub-picture directory, so that the convenience and update efficiency of the update process of the first target picture can be improved and the manpower cost required for updating the first target picture can be reduced.

The invention relates to a beta-carboline compound and a synthesizing method and application thereof, and belongs to the technical field of medicines. The structure of the compound is shown in a formula I. Being proved by preliminary experiment, the beta-carboline compound has the advantages that the activity of resisting renal fibrosis in vitro is obvious, and the good potential medical value is realized; the beta-carboline compound can be applied to prepare various types of medicines for resisting renal fibrosis and chronic renal diseases. The formula I is shown in the description.

The invention relates to a synthesis method of an asymmetric azoxybenzene compound. According to the synthesis method, in an organic solvent, silver oxide is taken as the only promoter to carry out dehydrogenation condensation reactions. According to the synthesis method, aromatic amines and nitrosobenzene are taken as raw materials, and high efficient and selective synthesis is carried out undermild conditions to obtain the asymmetric azoxybenzene compound, which has a wide application range. The used promoter is commercial silver oxide, the synthesis raw materials are cheap and easily available; after reactions, silver oxide is converted into silver, which can be recovered and reused; the synthesis method is environment friendly, and compared with the prior art, the synthesis method ismore practical, is worthy to popularize, and is sustainable.

The invention discloses a method for synthesizing 2, 3-dichloropyridine (III). The method comprises that 1) pyridine (I) as a main starting raw material and chlorine undergo a full reaction in water or vapor as a reaction medium in the presence of a chlorination inducer to produce a pyridine chloride (II) as the next reaction raw material, and 2) the pyridine chloride (II) as a reaction raw material contacts with hydrogen and undergoes a catalytic hydrogenation reduction reaction in water or vapor as a reaction medium in the presence of an acid-binding agent and a catalyst to produce 2, 3-dichloropyridine (III) having purity of 99% or more, wherein the catalyst is a nanometer IrO2-ZnO-MnO2 composite catalyst. The reaction equation is shown in the description and n is 2-5. The method has the advantages of high reaction conversion rate, high selectivity, stable product quality, simple processes and low cost and solves the problem that the existing synthesis method produces 2, 3-dichloropyridine (III) having unstable quality and satisfying the quality standards after multiple rectification processes.

The invention relates to a catalyst for preparing acrylic acid by oxidation of acrylic aldehyde, a preparation method of the catalyst, and a synthesis method of acrylic acid, and is used for mainly solving the problem of not high selectivity of an acrylic acid catalyst in the prior art. The technical problem is better solved through adopting the technical scheme that the acrylic acid catalyst contains an active component represented by the following general formula of Mo12VaCubXcYdZeKfOj, wherein X is at least one selected from W, Cr and Sn, Y is at least one selected from Fe, Bi, Co, Ni, Sb, Zr and Sr, and Z is at least one selected from lanthanide elements. The acrylic acid catalyst can be used in industrial production of acrylic aldehyde oxidation production of acrylic acid.

The invention discloses a synthesis method of EPS-RB nanometer particles for photodynamic bacterium resistance. Lactobacillus plantarum exopolysaccharides EPS, rose-bengal RB, 1-(3-dimethylaminopropyl)-3-ethylenediamine hydrochloride EDC-HCl and N-hydroxysuccinimide NHS are used as raw materials; reaction is performed in dimethyl sulfoxide DMSO to obtain compounds EPS-RB; the compounds EPS-RB aresubjected to self assembly to form spherical nanometer particles in a water solution; a good photodynamic bacterium resistance effect is achieved. The compound can realize the self aggregation in thesolution to form nanometer particles; the nanometer particles generates singlet oxygen higher than free RB under the light illumination condition, so that the photodynamic bacterium resistance on escherichia coli and staphylococcus aureus is superior to that of the free RB. The concentration required by EPS-RB nanometer particles for completely killing escherichia coli and staphylococcus aureus isrespectively 8mu M and 500nM; the concentration required by the free RB is respectively 16 mu M and 1000nM.

The invention discloses selenium-substituted benzodipyrene imide and synthesis method as well as application to a solar battery. The synthesis method is characterized in that: perylenetetracarboxydianhydride is taken as a raw material for preparing anhydride perylene bisimide dimer anhydride through butyl tetracarboxy perylene; different alkyl chain-substituted and selenium-substituted benzodipyrene imide can be prepared easily and simply through an anhydride intermediate. The acceptor molecule has superior photoelectric property, can be applied to organic solar battery, and has simple requirement on device structure, and the photoelectric conversion efficiency under the condition of no optimizing manners such as solvent additive, thermal annealing and the like can reach up to 5.17 percent.

The invention discloses a synthesis method of tonkinensine B shown in formula (III). The synthesis method comprises the steps as follows: cytisine shown in formula (I), maackiain shown in formula (II), formaldehyde and 4-dimethylaminopyridine are mixed in an organic solvent, the obtained mixture reacts at 85-95 DEG C for 2-3 h, a reaction solution is subjected to posttreatment, and the product tonkinensine B shown in the formula (III) is obtained. The preparation process method is simple, takes short time and is high in yield. Experiment results show that the yield can reach 73% or above withthe adoption of the synthesis method.

The invention discloses a synthesis method for a porous ZnCo2O4 nanosheet and a pseudo-cubic micro-nano structure. The synthesis method comprises the following steps: (1) weighing CTAB (CetyltrimethylAmmonium Bromide), and dissolving in the mixed solution of deionized water and ethylene glycol at a constant temperature to obtain settled solution; (2) weighing Zn(NO3)2.6H2O, Co(NO3)2.6H2O and ureaat the molar ratio of 1:2:15, dissolving in the solution obtained in (1), and fully stirring; (3) transferring the solution obtained in (2) to a polytetrafluoroethylene lining stainless steel reaction kettle, sealing, and reacting for 3-20h at the temperature of 100-180 DEG C; (4) after reaction is finished, naturally cooling to room temperature, carrying out centrifugation, respectively cleaningwith the deionized water and absolute ethyl alcohol for three times, and drying to obtain a Zn-Co precursor. According to the synthesis method, through the simple regulation and control of reaction parameters, the micro-nano structure of ZnCo2O4 of different morphologies can be obtained through synthesis.

The invention relates to a method for preparing cubic boron nitride (cBN) single crystal-film homogeneous P-N junction, and belongs to a method for preparing semiconductor components. The method comprises the steps of: synthesizing a semiconducting cBN single crystal with semiconductor characteristic and preparing a doped cBN film, wherein the cBN film has the semiconductor characteristic opposite to that of the cBN single crystal; the semiconducting cBN single crystal with the semiconductor characteristic is synthesized by a high-pressure direct synthesis method or a high-pressure re-diffusion method; and the doped cBN film is prepared by taking the semiconducting cBN single crystal with the semiconductor characteristic as a substrate and doping and growing a cBN film with a semiconductor type opposite to a substrate type by a vacuum vapor deposition method. The vacuum vapor deposition method is a vacuum physical vapor deposition method or a vacuum chemical vapor deposition method. The method has the advantages of reduction in processing difficulties, improvement on production efficiency, yield and the like and great improvement compared with the conventional technology for preparing a cBN homogeneous P-N junction by high-pressure systemization and re-growth processes.

The invention relates to an imidazolamide ligand and a nickel complex thereof as well as application of the nickel complex to polyisoprene synthesis and belongs to the field of novel compounds and organic synthesis. The complex is used in the polyisoprene synthesis, and a polyisoprene synthesis method comprises the following the steps: dissolving a co-catalyst, the imidazolimide nickel complex and an isoprene monomer in a solvent, stirring at a temperature of 25 DEG C under the condition of argon gas protection for reaction for 2-4 hours, separating and purifying to obtain a polyisoprene product. The polyisoprene synthesis method provided by the invention is efficient and environmentally-friendly and has high selectivity.

The invention discloses a fluorescence probe molecule as well as a preparation method and application thereof to hypochlorite ion detection. The fluorescence probe molecule is put into a testing sample with hypochlorite ions, whether the color of the testing sample is conspicuously changed or not can be detected, and in addition, the fluorescence probe molecule is good in selectivity upon hypochlorite ions and can stably respond to hypochlorous acid. The concentration of hypochlorite ions can be calculated by measuring fluorescence intensities at different wave sections, no complex physical orchemical method is implemented in the testing process, and the fluorescence probe molecule has the advantages of being simple to operate, rapid and efficient and high in sensitivity.

The invention discloses a method for preparing N,N-diethyl-3-pyridine carboxamide. The method comprises the following steps: adding nicotinic acid and dichloromethane into a reaction bottle and dropwise adding oxalyl chloride at the temperature of 0 DEG C; after oxalyl chloride is added dropwise, stirring and reacting at the temperature of 0 DEG C for 0.5-1 hour and reacting at room temperature for 4-6 hours; after the reaction is ended, dropwise adding a sodium hydroxide solution for regulating the pH value of the reaction solution to 7, slowly dropwise adding diethylamine at the temperature of 5 DEG C below zero to 10 DEG C; after diethylamine is added dropwise, reacting at the room temperature for 6-8 hours; after the reaction is finished, adding a sodium carbonate solution, stirring, standing for layering, removing the lower water layer, drying the organic layer, thereby obtaining a crude product of N,N-diethyl-3-pyridine carboxamide; adding the crude product of N,N-diethyl-3-pyridine carboxamide into dichloromethane, discoloring, oxidizing, removing dichloromethane, performing reduced-pressure distillation, thereby obtaining the finished product of N,N-diethyl-3-pyridine carboxamide. The method is low in equipment requirement, slight in environmental pollution and low in danger coefficient and is a synthesis method which is environment-friendly and very suitable for industrial production.

The invention relates to a novel green and practical synthesis method of a N,N-dimethyl pyridine compound. The reaction method is characterized in that common inorganic alkaline and water are respectively used as an accelerant and a reaction solvent; under the mild condition and in air, 2-halogenated pyridine derivatives and N,N-dimethylformamide compounds can be smoothly promoted to selectively perform dehalogenation amination reaction to generate corresponding N,N-dimethyl pyridine derivatives. The direct amination reaction of cheap and easy-to-obtain inorganic alkaline promoted 2-halogenated pyridine compounds and N,N-disubstituted methylformamide compounds is innovatively realized for the first time; the limitation that a metallic catalyst needs to be used by a traditional method is overcome; a bran-new strategy is provided for laboratory preparation and industrial production of the N,N-dimethyl pyridine compound.

The invention discloses a synthesis method of an indole-2,3-dione compound. The method comprises the following steps that a raw material as shown in a formula I is added into a Schlenk reactor, then acatalyst bis(acetonitrile)dichloropalladium (PdCl2(CH3CN)2), an oxidizing agent silver acetate (AgOAc) and a solvent methylbenzene are added, reaction is carried out under an oxygen atmosphere at 120-150 DEG C for 8-36 hours, a TLC board is used for monitoring the reaction, and after the reaction is carried out completely, the indole-2,3-dione compound as shown in a formula II is obtained throughpost-treatment.

The invention relates to a synthesis method for organically synthesizing an intermediate N-allylthiourea. The synthesis method mainly comprises: adding 4-5 mol urea, 3 mol allyl alcohol, 12 L of a potassium bromide solution and 1.5 mol alumina powder in a reaction container, controlling the stirring speed at 90-110 rpm, heating the solution to a temperature of 80-90 DEG C, maintaining for 100-130min, carrying out pressure reducing distillation, cooling the solution to a temperature of 10-15 DEG C, precipitating to obtain a crystal, washing with an ether solution, washing with a dimethylaminesolution, re-crystallizing in a methanol solution, and dewatering with a dewatering agent to obtain the finished product N-allylthiourea.

The invention discloses a preparation method of a hindered phenol antioxidant 1019. The method comprises the following steps: dissolving 3-(3, 5-dibutyl-4-hydroxyphenyl) propionyl chloride into an organic solvent; adding the solution obtained from the former step into a mixed solution prepared from propane diamine, inorganic base and water by an agitating manner; controlling the temperature of the reaction system under adding to 0 to 50 DEG C; further reacting at the temperature of 0 to 50 DEG C after adding until reaching the end of reaction; heating to reach the temperature of 50 to 80 DEG C after reaction; separating out a lower water phase; washing an organic phase at two to three times through water until the pH of the washing water is 6 to 7; cooling; crystallizing; filtering; drying to obtain the target product, namely, N, N'-bi-(3-(3,5-di-butyl-4-hydroxyphenyl) propionyl) propane diamine. Compared with the existing synthesis method, the preparation method has the advantages that the yield is high, conditions of reaction are mild, the operation is simple, the product is easily separated and purified, and the quality is high; the preparation method is suitable for industrial production.