35results about How to "The reaction process is safe and controllable" patented technology

The invention discloses a preparation method of methyl 3-methoxyacrylate. The preparation method comprises the steps: taking saturated monocarboxylic ester as a raw material and saturated carboxylic ester as an auxiliary material, and introducing formyl by utilizing methyl formate under the action of a catalyst; carrying out aldol condensation reaction with methanol under the condition that the ionic liquid is used as a catalyst, to obtain methyl 3,3-dimethoxypropionate; after the reaction is completed, separating methanol under reduced pressure, after separation is completed, increasing the temperature to 80-150 DEG C, carrying out an elimination reaction to remove one molecule of methanol on methyl 3,3-dimethoxypropionate, and thus obtaining methyl 3-methoxyacrylate, wherein methyl formate can be replaced with CO, and the raw material cost is lower. The method has the advantages of simple operation, easily available raw materials, high conversion rate, safety, environmental protection and low cost, and can realize industrial production.

The invention relates to a preparation method of Pramiracetam sulfate. The preparation method comprises the steps of using N, N-diisopropylethanolamine as a starting raw material, and conducting chlorination and ammonolysis to obtain an intermediate N, N- diisopropylethylene diamine; then conducting acylation, substitution, salt forming and refining to obtain the Pramiracetam sulfate. The preparation method of the Pramiracetam sulfate has the characteristics that the reaction process is safe and controllable, the cost of used raw materials and solvent is low and the raw materials and the solvent are easy to obtain; organic solvent is very easy to recycle, the emission of organic matters is greatly reduced, and the environmental friendliness is improved; since the intermediate N-[(2-diisopropyl amino) ethyl]-chloroacetamide is not separated and purified, the reaction equipment is simplified, and the operation process is enabled to be more high-efficient.

The invention discloses a method for preparation of a ketone compound and its derivatives by means of a carboxylic acid compound and a carboxylic ester compound in the presence of alkali. The method has the characteristics of wide substrate adaptability, short reaction time, high yield and high atom economy. The use of Lewis acid and heavy metals is avoided, the experimental operation steps are simple, the corrosion to equipment is small, and the amount of ''three wastes'' is small, so that the method is conducive to further promotion and application and industrial production.

Acetylenic ketone compounds and a preparing method thereof are disclosed. The general formula of the acetylenic ketone compounds is shown as a formula (I) in the specification. The preparing method includes adding an aldehyde compound A and a high-valence iodoalkyne compound B into a reaction system comprising a copper / gold salt catalyst, a secondary amine catalyst, a ligand catalyst and an oxidant and reacting at a temperature ranging from -20 DEG C to 200 DEG C. The acetylenic ketone compounds have a typical acetylenic ketone structure, have similarity with other acetylenic ketone compounds, and can be used for development of medicine intermediates and preparation of functional materials. The preparing method is simple in process, low in reaction condition requirements, safe and controllable in reaction procedures, high in atom utilization rate, high in production efficiency, and low in environment pollution stress, and obviously reduces the production cost of the acetylenic ketone compounds provided by the invention.

The invention belongs to the technical field of capacitor dielectric materials, and particularly relates to nanocrystalline barium titanate ceramic and a preparation method thereof. The preparation method of the nanocrystalline barium titanate ceramic comprises the following steps of: mixing barium carbonate and titanium dioxide, and carrying out ball milling, sanding, drying, sieving and calcining to obtain the barium titanate ceramic. The preparation method of the nanocrystalline barium titanate ceramic comprises the following steps of: mixing and ball-milling barium carbonate and titanium dioxide to increase the sintering activity of barium carbonate and titanium dioxide; carrying out solid-phase synthesis by using a sanding method to obtain barium titanate nano-powder with relatively small particle size and high tetragonality; the barium titanate nano-powder is subjected to calcination treatment, and the obtained nanocrystalline barium titanate ceramic has a small grain size and ahigh dielectric constant and can meet the requirement that a capacitor contains 5-6 ceramic grains in each single dielectric medium when being used as a ceramic capacitor material.

The invention relates to a method for recovering a carbon-fiber enhanced epoxy resin composite material. In the existing method, the requirement for equipment is high and the recovery cost is large. The method comprises the following steps of: cutting materials needing to be decomposed into blocks with the volume being 5cm<3>, putting the blocks in a backflow device containing acid liquor, heating for 5-20 minutes at the temperature of boiling point, cleaning and carrying out vacuum drying; then putting the obtained mixture into a reaction kettle, adding an organic solvent and an oxidizing agent, firstly heating, then cooling to normal temperature, and obtaining a primary product; and after cleaning, putting a solid product in the primary product into industrial acetone solution for dipping, obtaining recovered carbon fiber and carrying out pressure-reduced distillation on a liquid product to obtain phenol and derivatives thereof. In the method, reaction under low temperature and low pressure is realized and has the advantages of moderate reaction condition, easy control of reaction, fewer side products, no pollution basically and no corrosion to equipment and the like, so that the method is a green recovering method.

The invention relates to a method for preparing a diamond-like film by virtue of high-power laser irradiation. According to the method for preparing the diamond-like film by virtue of the high-power laser irradiation, a graphite coating of a substrate immersed in a circulating aqueous solution is irradiated by adopting high-power pulse laser; after absorbing energy of the laser, graphite is quickly gasified and ionized to produce massive high-speed plasma and also produce an instantaneous high-temperature and high-pressure microcell on the surface of the substrate, then the surface of the substrate is cooled at a high speed; and under the extreme unbalanced condition, nucleation and growth of a diamond are realized, wherein one part of graphite is converted into diamond, and molecular-scale and atomic-scale diffusion is carried out on the surface layer of the substrate. By adopting the method for preparing the diamond-like film by virtue of high-power laser irradiation, the problems that reaction conditions are special, devices are difficult to operate and cost is high are solved, continuous synthesis of the diamond-like film under macroscopic, normal temperature and normal pressure conditions is innovatively realized, a thick diamond-like film is obtained, reaction time is short, and bonding strength between the diamond-like film and the substrate is high.

The invention discloses a method for effectively synthesizing a nitrile compound by reacting a copper salt, a ligand and a co-catalyst, a final oxidant such as with ammonia water under the mild condition in an alcohol and synthesizing multiple heterocyclic compounds with a one-pot method. In the method, the substrate adaptability is wide, the reaction time is short, the yield is high and the atom economy is high. Use of severe conditions, such as high temperature and high pressure and toxic starting materials is avoided; and the preparation method is simple in operation steps and less in corrosion on instruments, generates less waste gas, waste water and industrial residue, and is beneficial to further popularization and application, and industrial production.

The invention discloses diarylmethane compounds as well as a preparation method and application thereof. The diarylmethane compounds have a molecular structural general formula as defined by a generalformula (I) in the description. The preparation method of the diarylmethane compounds comprises the steps of adding a benzyl halogenated hydrocarbon compound A and an arylboronic acid B into a reaction system containing an organic small-molecular catalyst, an alkali reagent and a solvent, and performing a reaction to prepare the compounds. The diarylmethane compounds provided by the invention contain electron withdrawing groups and an electron-donating group substituted diarylmethane basic structure, and can be widely used for synthesis of pharmaceutical intermediates, particularly polysubstituted methane compounds, and preparation of functional materials; and the preparation method has a simple process and low requirements for reaction conditions, the reaction process is safe and controllable, the atomic utilization rate and production efficiency are high, the regioselectivity and stereoselectivity of the products are efficiently ensured, a frontier science small-molecule organocatalysis concept is introduced, and the method is friendly to the environment.

The invention relates to the technical field of organic compound synthesis, and provides a chiral phosphorus-sulfur compound and a Michael addition method thereof. The Michael addition method of the chiral phosphorus-sulfur compound comprises the following steps: respectively providing a phosphorus-sulfur compound A and a nitroolefin compound B with the following structures: A: B: adding the phosphorus-sulfur compound A and the nitroolefin compound B into a reaction system containing an N-heterocyclic carbene catalyst, a proton additive, an alkali reagent and a water absorption additive; performing a reaction under the condition that the temperature is -80 - 25 DEG C to obtain the chiral beta-nitro phosphorus-sulfur compound shown as the following structural general formula (I), thereby completing the Michael addition of the chiral phosphorus-sulfur compound.

The invention discloses a novel green synthesis method of tanshinone IIA sodium sulfonate, which comprises the following step: directly carrying out a sulfonation reaction on tanshinone IIA by adopting safe, stable and cheap sodium hydrogen sulfate in the presence of a catalyst to obtain tanshinone IIA sodium sulfonate. Compared with the existing method, the method has the advantages that a targetproduct can be obtained through a one-step reaction; strong corrosive sulfonation reagents such as concentrated sulfuric acid and pyridine sulfur trioxide and a large amount of saturated salt water and sodium carbonate needed by subsequent salt forming are avoided. The method has the advantages that the production process is simple and convenient, the efficiency is high, and reagents can be recycled, so that the production cost of the tanshinone IIA sodium sulfonate is obviously reduced, the environmental pollution pressure is greatly relieved, and the method has a great industrial productionvalue.

The invention discloses 1,2,3,4-tetrahydronaphthalene compound and a preparation method and application thereof. The 1,2,3,4-tetrahydronaphthalene compound has a molecular structural formula shown asformula (I) that is shown in the description. The preparation method of the 1,2,3,4-tetrahydronaphthalene compound comprises steps, such as subjecting styrene compound A, olefine compound B, a visiblelight catalyst, a cocatalyst and a solvent to reacting. The 1,2,3,4-tetrahydronaphthalene compound has a tetrahydronaphthalene basic framework containing electron-withdrawing group and electron-donating group substations, and is widely applicable to the preparation of functional materials and the synthesis of pharmaceutical intermediates, especially polycyclic-structure compounds. The preparationmethod herein is simple and has low reaction condition requirements, the reaction process has good safety and controllability, atom utilization rate and production efficiency are high, regio-and stereo-selectivity of products is effectively ensured, and the products have no pollution.

The invention relates to the technical field of waterborne polyurethane resin, in particular to a high-solid-content self-extinction waterborne polyurethane dispersion and a preparation method thereof. The high-solid-content self-extinction waterborne polyurethane dispersion comprises the following raw materials in percentage by weight: 15-40% of polymer polyol, 10-30% of isocyanate, 0.1-3% of a first chain extender, 0.3-15% of a second chain extender, 0.01-0.2% of a catalyst, 5-30% of an organic solvent and the balance of water, wherein the first chain extender is a dihydroxy sulfonic acid amine salt compound. According to the invention, 1, 2-dihydroxy-propanesulfonic acid amine salt is adopted as a preparation raw material of polyurethane, and acts together with substances such as specific polymer polyol, so that the solid content of the waterborne polyurethane is remarkably increased, and the production, storage and transportation costs are low; and the low-boiling-point organic solvent is adopted for smooth reaction, the problems of high danger coefficient and the like caused by introduction of a high-boiling-point solvent are avoided, the whole process is simple and convenient, the reaction process is safe, and the high-solid-content self-extinction waterborne polyurethane dispersion is suitable for being widely popularized in the field of waterborne polyurethane.

The invention provides a preparation method and application of anhydrous peroxycarboxylic acid. The preparation method comprises the following steps: carrying out reduced pressure dehydration and pre-concentration on low-concentration hydrogen peroxide, adding a catalyst a and a catalyst b, adding carboxylic acid, and carrying out electrolytic oxidation reaction to synthesize the anhydrous peroxycarboxylic acid. According to the method, the oxidation reaction effect is enhanced through the synergistic effect of electrons and metal salt, no pollution is caused, the requirement of green synthetic chemistry is met, and the prepared peroxycarboxylic acid does not contain water and can be used for preparing epsilon-caprolactone.

The invention relates to a method for preparing a diamond-like film by virtue of high-power laser irradiation. According to the method for preparing the diamond-like film by virtue of the high-power laser irradiation, a graphite coating of a substrate immersed in a circulating aqueous solution is irradiated by adopting high-power pulse laser; after absorbing energy of the laser, graphite is quickly gasified and ionized to produce massive high-speed plasma and also produce an instantaneous high-temperature and high-pressure microcell on the surface of the substrate, then the surface of the substrate is cooled at a high speed; and under the extreme unbalanced condition, nucleation and growth of a diamond are realized, wherein one part of graphite is converted into diamond, and molecular-scale and atomic-scale diffusion is carried out on the surface layer of the substrate. By adopting the method for preparing the diamond-like film by virtue of high-power laser irradiation, the problems that reaction conditions are special, devices are difficult to operate and cost is high are solved, continuous synthesis of the diamond-like film under macroscopic, normal temperature and normal pressure conditions is innovatively realized, a thick diamond-like film is obtained, reaction time is short, and bonding strength between the diamond-like film and the substrate is high.

The invention discloses a method for preparing alkyl aluminoxane by using a microreactor. The continuous flow chemical reaction system includes a fluid delivery section, a microdisperser section, a microreactor section, and a collection and purification section. On the one hand, the dispersion size of water in the inert continuous phase is reduced through the microdisperser, the contact mode between the reactants is changed in the form of micro droplets, and it is fed into the continuous stirring reactor through multi-stage feeding to prevent excessive hydrolysis. Thereby reducing or avoiding the generation of solid by-products. On the other hand, the method uses a miniature continuous stirred reactor instead of a traditional microchannel reactor, reducing the risk of pipeline blockage. Aluminum alkyls and water react in a nearly equimolar ratio in a continuous stirred reactor to produce alkylaluminoxanes. The invention is simple and feasible, the reaction process is safe and controllable, the high-efficiency heat transfer and mass transfer characteristics ensure good heat removal and reaction performance, effectively reduce the excessive reaction and incomplete reaction, and the target product reaches a high yield and active.

The invention relates to a method for synthesizing NiO nanocube particles through a milisecond pulsed laser. The method realizes the preparation of lots of NiO nanocube particles under a room temperature condition; and the prepared products have high purity. The method comprises the steps of taking micron-level metallic nickel powder as a raw material, and dispersing the micron-order metallic nickel powder in a deionized water to form a mixture; using a submerged pump to enable the metallic nickel powder and water mixture to ceaselessly circulate; using the milisecond pulsed laser to bombard a circulating deionized water medium containing the metallic nickel powder; and purifying the product bombarded by the milisecond pulsed laser to obtain the NiO nanocube particles. The method realizes the synthesis of the NiO nanocube particles at normal temperature and pressures, and the NiO nanocube particles with higher purity are obtained at high efficiency by adopting the method.

The invention relates to a preparation process of glucosamine sulfate. The preparation process comprises the following steps of (1) uniformly stirring glucosamine hydrochloride and monohydric alcohol to obtain an alcoholic solution of glucosamine hydrochloride for later use; (2) adding an alkaline neutralizer into the alcoholic solution, adding a silver sulfate solution after the reaction is finished, stirring, standing, and carrying out solid-liquid separation on the reaction system; and (3) adjusting the liquid separated in the step (2) to be acidic, then distilling to obtain glucosamine sulfate, and recovering the distilled solvent. Silver sulfate is adopted to fix chloride ions in glucosamine hydrochloride in a monohydric alcohol system in a silver precipitation mode; compared with traditional adsorption, extraction and other methods, the method is efficient and rapid, more importantly, the chloride ions in glucosamine hydrochloride can be thoroughly removed; and the obtained silver precipitate is easy to separate and recover and can be used as an industrial by-product, and no extra solid waste is generated.

The invention relates to the technical field of organic synthetic chemistry, and particularly relates to a beta-carbonyl chiral amino compound and a preparation method thereof. The molecular structural general formula of the beta-sulfonyl chiral amino compound is shown in the formula I in the description, wherein different kinds of functional group substituents are introduced into R1, R2, FG1 andFG2 in the formula I, so that various types of beta-sulfonyl chiral amino compounds are achieved. In addition, the functional group on nitrogen in the formula I can be removed to become an exposed amino group. Therefore, a research basis is provided for screening useful molecules.

The invention discloses a chiral 1,2-diamine compound and a preparation method and application thereof. The molecular structure general formula of the chiral 1,2-diamine compound is shown as the general formula (I) in the specification. The preparation method of the chiral 1,2-diamine compound comprises the steps that an amine compound A and a nitroolefin compound B are added to a reaction system containing an n-heterocyclic carbine catalyst, an alkali reagent, a proton additive and a dewatering reagent for reacting and other steps. The chiral 1,2-diamine compound comprises chiral quaternary carbon atoms containing electrondrawing groups and amino groups, and can be widely used for synthesizing drug intermediates, especially heterocyclic ring structure compounds, and preparing functional materials. The preparation method is simple in process and low in requirement for reaction conditions, the reaction process is safe and controllable, the atom utilization rate and production efficiency are high, meanwhile, the enantioselectivity of products is efficiently guaranteed, and the environment pollution pressure of the methodology is low through the introduction of the small organic molecule asymmetric catalysis concept.

The invention discloses a method for effectively synthesizing a nitrile compound by reacting a copper salt, a ligand and a co-catalyst, a final oxidant such as with ammonia water under the mild condition in an alcohol and synthesizing multiple heterocyclic compounds with a one-pot method. In the method, the substrate adaptability is wide, the reaction time is short, the yield is high and the atom economy is high. Use of severe conditions, such as high temperature and high pressure and toxic starting materials is avoided; and the preparation method is simple in operation steps and less in corrosion on instruments, generates less waste gas, waste water and industrial residue, and is beneficial to further popularization and application, and industrial production.

The invention discloses an alpha-tetra-substituted chiral acetyenic ketone compound, as well as a preparation method and application thereof. The molecular structural general formula of the alpha- tetra-substituted chiral acetyenic ketone compound is as shown in general formula (I) in the specification. The preparation method comprises the following steps: adding a diyne enamine compound A into areaction system containing a functionalized reagent B, a chiral phosphoric acid catalyst and a base reagent to react, and the like. The alpha-tetra-substituted chiral acetyenic ketone compound can bewidely applied to preparation of medicinal intermediates since massive chiral compounds with a special ring structure are obtained by simple chemical transformation. The preparation method is simple in process and low in requirement for reaction conditions, has safe and controllable reaction process, high atom utilization and high production efficiency, can efficiently ensure the enantioselectivity of products, and has small environmental pollution pressure by introducing the concept of organic small-molecular asymmetric catalysis.

The invention discloses a preparation method of an iron-aluminum-chromium filter material, and relates to the field of material processing and manufacturing. The problems that an existing filtering material is complex in preparation process and high in cost, and potential safety hazards exist in the preparation process are solved. The preparation method comprises the steps that iron powder with the particle size ranging from 75 micrometers to 750 micrometers, aluminum powder with the particle size ranging from 5 micrometers to 40 micrometers and chromium powder with the particle size ranging from 50 micrometers to 180 micrometers are stirred in a ball mill for 120 minutes, an initial ingredient is obtained, in the initial ingredient, the atom percentage content of the iron powder ranges from 65% to 70%, the atom percentage content of the aluminum powder ranges from 23% to 25%, and the atom percentage content of the chromium powder ranges from 2% to 5%; the initial ingredient is placed in a cold isostatic press to be pressed into a pressed blank, and the pressing pressure ranges from 200 Mpa to 260 Mpa; the pressed blank is placed in a sintering furnace filled with hydrogen to be subjected to in-situ reaction sintering, heat preservation is conducted for 2-3 h, the filtering material is obtained, and the temperature in the sintering furnace ranges from 1200 DEG C to 1300 DEG C during in-situ reaction sintering.

The invention provides a preparation method of a 3-methylene cyclobutyl derivative, which takes a propylene derivative and propadiene as initial raw materials, adopts a continuous flow chemical technology, and solves the problem that a reaction channel is blocked by propylene derivative polymerization while ensuring the product conversion rate by screening process conditions such as a polymerization inhibitor and a reaction solvent. Reaction is safe and controllable, equipment cost is low, and the method is suitable for industrial production.

The invention discloses a controllable preparation method of alkylaluminoxane, which comprises the following steps: step S1, finely dispersing the reaction water to below 10 microns through a dispersion release device; step S2, controlling the release of the dispersed reaction water process, input it into the reaction system to contact with the alkylaluminum solution to obtain the alkylaluminoxane solution. The method can realize sufficient dispersion of water in the reaction system, greatly reduces the possibility of excessive hydrolysis reaction, and the production process is safe and controllable.

The invention provides a preparation method of 2-(2-(2-aminoethoxy) ethoxy) acetic acid, and belongs to the field of pharmacy. The method comprises the following steps of: (1) taking a compound A0 and Bn2NH as raw materials to react to prepare a compound A1; (2) taking the compound A1 and an oxidizing agent as raw materials to react to prepare a compound A2; (3) taking the compound A2 and hydrogen as raw materials to react to prepare a compound A3; and (4) taking the compound A3 and fluorenylmethoxycarbonyl succinimide as raw materials to react to prepare the 2-(2-(2-amino ethyoxyl) ethyoxyl) acetic acid. Compared with a preparation method in the prior art, the preparation method disclosed by the invention avoids the use of a dangerous raw material NaH, and is mild in reaction condition, safe and controllable in reaction process, high in product yield and purity and suitable for industrial production.

The invention discloses a diyne enamine compound, a preparation method and application thereof. The general molecular structure formula of the diyne enamine compound of the present invention is described in the general formula (I) in the description. The preparation method of the diacetylene amine compound comprises the steps of adding a secondary amine A and a gold catalyst into a reaction system containing an electrophile compound B, a pyridine ligand C and an acetylenic compound D for reaction. The diyne enamine compound of the present invention contains a highly conjugated enamine structure skeleton, which is convenient for further functionalization, and can be widely used in the synthesis and preparation of pharmaceutical intermediates, especially polycyclic compounds. The preparation method has simple process, low requirements on reaction conditions, safe and controllable reaction process, high atom utilization rate and production efficiency, and at the same time, the regio and stereoselectivity of the product can be efficiently guaranteed, and the introduction of the concept of organometallic catalysis makes the methodological Environmental pollution pressure is small.

The invention discloses an α-tetrasubstituted chiral acetylene compound, a preparation method and application thereof. The general molecular structure formula of the α-tetrasubstituted chiral ynone compound of the present invention is described in the general formula (I) in the description. The preparation method of the α-tetrasubstituted chiral ynone compound comprises the steps of adding the diacetylene enamine compound A into a reaction system containing a functional group reagent B, a chiral phosphoric acid catalyst and an alkaline reagent for reaction. The α-tetrasubstituted chiral acetylenone compound of the present invention can obtain a large number of chiral compounds with special ring structures through simple chemical transformation, and is widely used in the preparation of pharmaceutical intermediates. Its preparation method has simple process, low requirements on reaction conditions, safe and controllable reaction process, high atom utilization rate and production efficiency, and at the same time efficiently guarantees the enantioselectivity of the product, and the introduction of the concept of asymmetric catalysis of organic small molecules makes the method The environmental pollution pressure of the school is small.