898 results about "Carbonylation" patented technology

The invention relates to a method for synthesizing a high-value product by using refinery furnace gas, which comprises the following steps: purifying refinery crude furnace gas, feeding the purified refinery crude furnace gas into a chemical looping three-stage normal-pressure reactor, respectively obtaining near-pure carbon dioxide, nitrogen and hydrogen products in each stage of flow, and adjusting a gas framework by using the near-pure hydrogen product obtained by reforming coke oven gas as a supplementary hydrogen source, after reaching the standard of the mixed raw material, pressurizing and feeding into a synthesizer, and carrying out gas-liquid separation to obtain a methanol or ammonia product. The method solves the problem that carbon dioxide and nitrogen cannot be utilized when the traditional refinery furnace gas replaces coal-based carbon monoxide to synthesize high-value products through chemical carbonylation; part of coke oven process tail end product coke oven gas is consumed, and the defect that a cheap hydrogen source needs to be supplemented due to unmatched raw material structures in the technological process is overcome; and the tail gas and low-grade heat recycling process in each stage of production process is also optimized, and near-zero emission in the life cycle and gradient utilization of chemical energy are realized.

The invention belongs to the field of iron high-valued treatment and tailing reduction, and relates to an iron high-valued treatment and tailing reduction recovery method for multi-source neodymium iron boron secondary resources. In order to solve the problems of iron tailing treatment and high-value utilization of iron elements in the secondary resource recovery process of the neodymium iron boron waste, the invention develops a new process of'oxidizing roasting, carbonylation method iron extraction and wet process rare earth recovery ', so that effective extraction of rare earth elements is realized, high-value recovery of iron is promoted, and the generation amount of tailings is reduced. According to the technology, 60%-86% of iron elements in the neodymium iron boron magnetic material waste can be prepared into pentacarbonyl iron with the high additional value, then pentacarbonyl iron can be pyrolyzed to prepare a carbonyl iron powder product, the amount of iron tailings obtained after rare earth leaching is 350-600 kg / t of raw materials, and the output of the iron tailings is only 40%-60% of iron tailings generated after rare earth magnetic materials are recycled through a conventional roasting-hydrochloric acid optimal solution method. The new process can provide powerful guarantee for efficient and high-value utilization of neodymium iron boron waste and tailing reduction.

The invention provides a separation method of a catalyst for preparing butyraldehyde through propylene carbonylation, and relates to the technical field of chemical synthesis. The separation method comprises the following steps: carrying out flash evaporation separation and low-pressure evaporator evaporation on a material obtained by carrying out a propylene carbonylation reaction on propylene and synthesis gas as raw materials, obtaining a gas-phase material from a collecting tank of a low-pressure evaporator, and outputting a liquid-phase catalyst solution; the gas-phase material is subjected to condensation and gas-liquid separation, crude butyraldehyde is output, and obtained non-condensable gas returns to a liquid distribution chamber of the low-pressure evaporator; wherein the catalyst is acetylacetone triphenyl phosphorus silicification carbonyl rhodium, and the operation temperature of the low-pressure evaporator is 85-95 DEG C. By controlling the circulating air volume and the evaporation temperature, high-temperature deactivation of the catalyst is prevented, the service life of the catalyst is prolonged, and the process cost is reduced; the process flow is simplified, and the method is suitable for large-scale process production.

The invention discloses a short c-axis flaky mordenite molecular sieve as well as a preparation method and application thereof, and belongs to the technical field of molecular sieves. The chemical composition of the short c-axis flaky mordenite molecular sieve is Ra.Mb. (SixAly) O2, r is a template agent tetraethylammonium ion; a is the mole number of R in each mole of (SixAly) O2, and a is more than or equal to 0.02 and less than or equal to 0.04; m is an alkali metal ion; b is the mole number of M in each mole of (SixAly) O2, and b is more than or equal to 0.02 and less than or equal to 0.06; x is the mole fraction of Si in each mole of (SixAly) O2, and x is more than or equal to 0.9 and less than or equal to 0.97; y is the mole fraction of Al in each mole of (SixAly) O2, y is more than or equal to 0.03 and less than or equal to 0.1, and x + y is equal to 1; and the dimension thickness of the stone molecular sieve in the c-axis direction is 20-80 nanometers. The molecular sieve shows excellent catalytic performance in a catalytic reaction for preparing methyl acetate through dimethyl ether carbonylation.

The invention relates to the technical field of carbonylation, and discloses a phosphine nitrogen compound and a metal complex as well as a preparation method, a composition and application thereof and a carbonylation reaction method. Wherein the phosphine-nitrogen compound has a chemical structure as shown in a formula (II), and the metal complex prepared from the phosphine-nitrogen compound has the characteristics of high catalytic activity, good thermal stability, difficulty in inactivation and high product selectivity in catalytic carbonylation reaction. # imgabs0 #

The invention discloses a method for recovering platinum and palladium from high-cobalt nickel-containing carbonylation slag, and relates to the technical field of non-ferrous metal carbonylation metallurgy, the method comprises the following steps: S1, hydrogen reduction and activation; s2, feeding into a high-pressure carbonylation reactor; and S3, efficient carbonylation. According to the method, the carbonylation slag is subjected to hydrogen reduction activation treatment, nickel protoxide and cobalt oxide are changed into simple substance nickel, the simple substance nickel is fed into a carbonylation reactor for carbonylation under the protection of reducing gas or inert gas after activation treatment, 95% of Ni, 85% of Fe and 80% of Co are carbonylated to enter a gas phase after carbonylation, bonding of cobalt and a platinum solid solution is broken through carbonylation, and the nickel-cobalt-cobalt-cobalt-cobalt alloy is obtained. Nickel protoxide is difficult to dissolve in various strong acids and oxidizing acids, and a foundation is laid for further separation of base metals and non-metallic element sulfur from precious metals to produce high-grade platinum concentrate.

The invention discloses a small-grain mordenite molecular sieve as well as a preparation method and application thereof, a crystallization process is directionally controlled by adopting a sectional regulation and control crystallization method, so that the morphology and acid distribution of the molecular sieve are regulated and controlled, and the synthesis method is simple in process and suitable for large-scale industrial production; the grain diameter of the small-grain mordenite molecular sieve obtained by the method disclosed by the invention is 15-300nm; the B acid center of the 8-membered ring pore channel accounts for gt of the total B acid center; the catalyst is used for the carbonylation reaction of dimethyl ether, and has good activity and stability.

The invention relates to a multifunctional tandem catalytic process for directly preparing methyl acetate / ethanol from synthesis gas. According to the process, a novel catalyst for preparing dimethyl ether from synthesis gas is prepared by adopting an impregnation method, and after the catalyst is sequentially connected with a dimethyl ether carbonylation catalyst and a hydrogenation catalyst in series, efficient directional synthesis of methyl acetate and ethanol is realized in a double-bed or three-bed sequential filling form. According to the invention, high CO conversion per pass, high methyl acetate selectivity and low acetic acid selectivity can be realized, and the problems of corrosion and difficult conversion of a subsequent hydrogenation system are effectively avoided; the multifunctional catalytic system provided by the invention is simple in preparation method and easy to realize industrial large-scale production.

The invention discloses a green and efficient carbonyl alkylation pyrrolo [1, 2-a] indole synthesis method, and relates to the technical field of organic synthesis. An alpha-bromocarbonyl compound is used as a carbonyl alkyl source, Ir (ppy) 3 is used as a photosensitizer, potassium hydroxide is used as alkali, sodium dimethyl dithiocarbamate is used as an additive, acetonitrile is used as a solvent, a carbonyl alkylation / cyclization reaction of N-alkenyl substituted indole is realized under the condition of visible light, and corresponding carbonyl alkylation pyrrolo [1, 2-a] indole is obtained. The method is convenient to operate, green and efficient in reaction and wide in substrate applicability.

The invention discloses a non-noble metal catalyst, a preparation method thereof and application of the non-noble metal catalyst in preparation of acetic acid through methane oxidation, and belongs to the field of direct conversion and utilization of methane. The active metal of the catalyst is transition non-noble metal MnOx, and the carrier is an MFI type molecular sieve (ZSM-5). The catalyst can directly react methane and oxygen at low temperature to prepare acetic acid without adding a co-reducing agent and carbonylation raw materials (such as H2 and CO). The nanometer MnOx catalyst has the advantages of mild reaction conditions, high acetic acid selectivity and the like, the acetic acid selectivity can reach 81.8%, and the nanometer MnOx catalyst shows good recycling stability.

The invention discloses a preparation method of a hydroxy ketone compound based on electrosynthesis and the hydroxy ketone compound prepared by the preparation method, and belongs to the technical field of preparation of hydroxy ketone compounds. The preparation method of the hydroxyl ketone compound based on electrosynthesis comprises the following steps: in a protective atmosphere, in an organic solvent, taking an epoxy compound as shown in a formula 1, an aryl iodide as shown in a formula 2 and a carbon monoxide source as reaction raw materials, and under an electrochemical condition and the action of an accelerant and a metal catalyst, carrying out electrosynthesis on the reaction raw materials to obtain the hydroxyl ketone compound based on electrosynthesis. Carrying out electroreduction carbonylation reaction to obtain a hydroxy ketone compound as shown in a formula 3; the reaction process is shown as a reaction formula (1). According to the method, metal powder is prevented from being used as a reducing agent, the operation method is simple and convenient, and the safety is good. # imgabs0 #

The invention belongs to the technical field of synthesis of organic chemical products through olefin carbonylation, and particularly relates to a catalyst system for ethylene carbonylation reaction. The catalyst system includes a palladium salt, one or more phosphine ligands, and one or more phosphorus (P)-containing compounds as stabilizers; the molar ratio of the palladium to the phosphine ligand to the stabilizer is 1: (1-6): (60-1000). According to the method, the phosphorus (P)-containing compound serving as the stabilizer is introduced to replace the sulfonic acid, direct use and supplement of the sulfonic acid are avoided, the catalytic activity and stability of a catalyst system can be improved, the equipment and process requirements can be reduced, and the method has a good application prospect.

The application discloses a radial flow fixed bed catalytic reactor for CO carbonylation coupling to generate oxalate, which comprises a cylindrical container composed of an upper head, a cylindrical barrel and a lower head from top to bottom in sequence, and the cylindrical container is externally provided with a reaction gas feeding port, a reaction gas discharging port, a heat exchange medium inlet, a heat exchange medium outlet, a catalyst feeding port and a catalyst discharging port; a catalytic bed is divided into an adiabatic zone and a heat exchange zone from inside to outside, and the heat exchange zone is provided with multiple groups of concentric circular arranged heat exchange pipes which are arranged in two rows as a group. The radial flow fixed bed catalytic reactor for CO carbonylation coupling to generate oxalate has the characteristics of uniform axial distribution of reaction gas, reasonable bed temperature distribution, high catalyst utilization rate and small reactor pressure drop, and is suitable for the reaction of carbonylation coupling to generate ester and is also suitable for other exothermic gas-solid phase catalytic reactions.

The invention discloses a key intermediate for synthesizing a bryochratoxin compound and a method for synthesizing the bryochratoxin compound, and belongs to the field of chemical synthesis.The synthesis method of the key intermediate comprises the steps that a compound shown in the formula (III) is dissolved in a reaction solvent, then Lewis acid is added for an intramolecular Prins cyclization reaction, and the compound shown in the formula (III) is obtained. Obtaining a compound as shown in a formula (IV); then carrying out iodination and carbonylation reactions of exocyclic double bonds of the B ring to convert the olefin into an olefine acid ester compound; after the key common intermediates are obtained, grass moss 1, 7 and 9 and grass moss 9-N3 analogues can be respectively synthesized, so that divergent synthesis of the grass moss analogues is realized; according to the invention, through an esterification reaction of C1 carboxyl and C25 hydroxyl, acetalation of C15 aldehyde group is carried out at the same time, and then through a closed-loop strategy of constructing a macrolide skeleton through gem-bisilicon-mediated intra-molecular stereoselective Prins cyclization, specific selective construction of the cis-Z type of the B ring in the carex 1 is realized.

The invention provides a method for removing metal impurity ions in a carbonylation synthesis acetic acid catalyst solution and filtering equipment thereof, and belongs to the technical field of metal impurity ion removal in the carbonylation synthesis acetic acid catalyst solution. Comprising the following steps: S1, carrying out preliminary adsorption on heavy metal ion impurities through strong-acid ion exchange resin, S2, carrying out circulating filtration adsorption through a filter assembly, and guiding the adsorbed carbonylation synthesis acetic acid catalyst solution into a cooling chamber, S3, pouring clear water into a processing barrel, and carrying out treatment for 2-3 hours. And the cleaned water-liquid mixture is subjected to centralized adsorption treatment through the magnetic adsorption rod. By arranging the cleaning assembly, the cleaning effect on the inner face and the outer face of the metal filter plate is achieved, the filter assembly does not need to be detached and cleaned independently, the cleaning effect on residual heavy metal ion impurities is further improved, and meanwhile the cleaning efficiency of the filter assembly is improved.

The invention discloses a preparation method and application of a binder-free self-forming MOR molecular sieve. The preparation method comprises the following steps: mixing sodium hydroxide, alkaline silica sol and an aluminum source, stirring and aging to form gel, transferring the gel into a hydrothermal kettle, sealing, and carrying out crystallization reaction at 170 DEG C for 5 days to obtain the formed centimeter-level MOR molecular sieve after crystallization. When the catalyst is used for a reaction for preparing methyl acetate through dimethyl ether carbonylation, compared with a commercial MOR, the catalyst has a higher dimethyl ether conversion rate. According to the method, the centimeter-level formed MOR molecular sieve is directly prepared by a one-pot method, a simple amplification experiment is carried out, an expensive and toxic organic template agent is not used in the whole synthesis process, and an additional binder is not needed, so that environmental protection is facilitated, the production cost can be reduced, and the method is suitable for industrial production.

The invention provides a method for preparing dicarboxylate by palladium-double ligand tandem catalysis of carbonylation of 1, 3-conjugated diene, and the method comprises the following steps: adding 1, 3-conjugated diene into a reaction solution containing a palladium cation source, a first ligand monodentate phosphine ligand L1, a second ligand bidentate phosphine ligand L2, an anion source and alcohol, then adding a carbonyl source, and reacting to obtain the dicarboxylate. The dicarboxylic acid ester is obtained. According to the invention, a tandem catalysis strategy is adopted, two ligands of monodentate phosphine and bidentate phosphine are introduced at the same time, a palladium catalysis tandem system is constructed, the dicarboxylate is directly prepared from 1, 3-conjugated diene by a one-pot method, the dosage of the expensive bidentate phosphine ligand is effectively reduced under the same catalysis efficiency, and the use of organic strong acid as an auxiliary agent can be avoided; and the requirement on the material of the reactor is reduced.

The invention relates to the technical field of recycling of cast nickel-based high-temperature alloy return scraps, and particularly discloses a method for extracting valuable metals in high-temperature alloy return scraps through carbonylation metallurgy. Comprising the steps of sulfuration smelting of the return scrap, carbonylation nickel extraction of the return scrap, chlorination of the material after nickel extraction, and graded carbonylation tungsten, chromium and molybdenum extraction, and nickel, chromium, tungsten and molybdenum in the cast nickel-based high-temperature alloy return scrap can be prepared into high-purity metal products by utilizing the characteristic of high selectivity of the carbonylation process. The nickel-based high-temperature alloy tailings can be directly sold as products in the forms of nickel carbonyl, chromium carbonyl, tungsten carbonyl and molybdenum carbonyl, meanwhile, the enrichment of rare and precious metals in the nickel-based high-temperature alloy tailings is realized, CO gas and chlorine gas used in the extraction process can be recycled, and the process can ensure the product quality while saving the cost, and is suitable for industrial production. And the method has huge economic benefits and relatively high popularization and implementation values.

The invention belongs to the technical field of organic synthesis, and discloses a 5-hydroxybenzofuran derivative and a preparation method thereof. The structural formula of the 5-hydroxybenzofuran derivative is as shown in formula (I), and R1, R2 and R3 are respectively C1-C20 alkyl, ester group, carbonyl, nitro and the like, and C5-C30 aryl or heteroaromatic ring group. Based on indirect oxidation and coupling cyclization strategies, a beta-dicarbonyl compound and hydroquinone which are simple and easy to obtain are used as substrate raw materials, and various 5-hydroxybenzofuran derivatives with different substituent groups are constructed in combination with an oxidizing agent and a catalyst. The 5-hydroxybenzofuran derivative disclosed by the invention is expected to obtain an excellent application prospect in later modification and development of new drugs and novel materials. # imgabs0 #

The invention discloses a preparation method of fluoroether, an electrolyte, a battery and a power utilization device. The invention relates to the technical field of batteries, in particular to a preparation method of fluoroether, an electrolyte, a battery and a power utilization device. The preparation method of the fluoro-ether comprises the following steps: reacting a metal fluoride solution with a carbonyl compound and an alkyl compound to obtain the fluoro-ether, wherein the fluoroether has a simple structural formula as shown in a formula (I), and R1 is straight-chain or branched-chain alkane; r2 is fluoroalkane, wherein the number of fluorine atoms is 4. The invention provides a novel fluoro-ether synthesis route which can be carried out in a normal pressure environment, the process is simple, the post-treatment is simple, the yield of fluoro-ether is improved, side reactions are reduced, and the product is easy to separate.

The invention discloses a preparation method and application of an eight-membered ring aluminum-rich mordenite nanosheet. The preparation method comprises the following steps: respectively weighing a silicon source, inorganic alkali, an aluminum source, a template agent Te, water and a metal additive Me according to a molar ratio of 1: (0.1-0.3): (0.02-0.08): (0.1-0.3): (10-40): (0.01-0.1); mixing and stirring the raw materials in an ice-water bath to prepare initial gel; putting the initial gel into a hydrothermal reaction kettle, carrying out hydrothermal crystallization in a drying box, and then centrifuging, filtering and drying to obtain a sodium mordenite molecular sieve; roasting the sodium mordenite molecular sieve to remove the organic template agent; carrying out ammonium ion exchange on the roasted mordenite molecular sieve in a water bath kettle to obtain an ammonium type mordenite molecular sieve; carrying out roasting treatment on the ammonium type mordenite molecular sieve to obtain a hydrogen type octatomic ring aluminum-rich mordenite nanosheet; the eight-membered ring aluminum-rich mordenite nanosheet prepared by the preparation method disclosed by the invention can exert excellent performance in a reaction for preparing acetic acid or methyl acetate through carbonylation of methanol or dimethyl ether.

The invention relates to the technical field of drug synthesis, and discloses a preparation method of a lysine-specific demethylase 1 (LSD1) inhibitor key intermediate, and the preparation method of the intermediate comprises the following steps: step 1, esterification reaction: reacting a compound A with a symmetric carbonylation reagent X to generate an asymmetric carbonate compound B; step 2, amine-ester exchange reaction: exchanging ester groups in the compound B with amine groups in the compound C to generate an amide compound D; step 3, cyclization reaction: converting carbonyl in the compound D into epoxy substituent in the compound E; and 4, fluorination reaction: reacting the compound E with a fluorination reagent, and carrying out ring opening to generate a fluorine substituted compound F. The preparation method comprises the following steps: oxidizing a key intermediate of the LSD1 inhibitor, connecting the key intermediate with an amine fragment, and performing functional group modification to obtain the fluorine-substituted cyclopropylamine compound with LSD1 inhibitory activity, thereby achieving the beneficial effect that the fluorine-substituted cyclopropylamine compound with LSD1 inhibitory activity can be conveniently and quickly synthesized from the intermediate.

The invention discloses a method for extracting iron and nickel by comprehensively recycling nickel smelting slag through carbonylation metallurgy, which specifically comprises the following steps: 1) carrying out reduction treatment on the nickel smelting slag to obtain a metal alloy; (2) the metal alloy is subjected to powder processing, so that metal alloy powder is obtained; (3) the metal alloy powder is treated through a mineral processing technology, so that metal alloy concentrate and tailings are obtained; 4) activating the metal alloy concentrate to obtain activated metal alloy powder; (5) the activated metal alloy powder reacts with carbon monoxide in a pressurized container, and a nickel carbonyl, carbonyl iron and carbon monoxide mixture and carbonylation tailings are obtained; and 6) carrying out subsequent condensation-rectification-decomposition treatment on the mixture of carbonyl nickel, carbonyl iron and carbon monoxide to obtain carbonyl nickel powder, carbonyl iron powder and carbon monoxide. According to the method, the high-purity carbonyl nickel powder can be extracted from the stockpiled nickel smelting slag, and high-valued application of iron can be achieved.

The invention provides a synthetic method of condensed epoxy glycoside, which comprises the following steps: mixing a 1, 3-dicarbonyl compound, alkali and a 2, 3-unsaturated glycosyl donor, adding an organic solvent for reaction, monitoring the reaction process by TLC (Thin Layer Chromatography), and terminating the reaction when the 2, 3-unsaturated glycosyl donor completely disappears, thereby obtaining the condensed epoxy glycoside. The alkali used in the method is DBU, so that a condensed epoxy glycoside product with high yield and high selectivity can be generated. According to the method, after condition screening, the high-yield and high-selectivity fused epoxy glycoside can be generated by only one-step reaction without using a noble metal catalyst and only using cheap alkali, and the commercial 1, 3-dicarbonyl compound and alkali are adopted as reaction conditions, so that the cost of generating oxygen glycoside is greatly reduced.

The utility model discloses a catalytic synthesis device for carbonylation synthesis of acetic anhydride, which belongs to the technical field of synthesis devices, and adopts the technical scheme that the catalytic synthesis device comprises a reaction kettle body and a purification mechanism, the top of the reaction kettle body is rotatably connected with an upper cover, and the top of the upper cover is bolted with a motor; the output end of the bottom of the motor is rotationally connected with a rotating rod, the reaction kettle body is arranged, the reaction kettle body can support and limit a catalyst, acetic anhydride, the upper cover and the discharging pipe, the upper cover can support and limit the motor and can seal or open the reaction kettle body, the motor can drive the rotating rod to rotate, and the rotating rod can drive the reaction kettle body to rotate. The rotating rod can drive the rotating shaft to rotate, the rotating shaft can drive the stirring blades to rotate, the stirring blades can fuse and stir a catalyst and acetic anhydride on the inner side of the reaction kettle body, and the exhaust pipe can guide carbon monoxide on the inner side of the reaction kettle body to the purification mechanism.

The invention relates to a synthesis method of 5, 5-disubstituted 2-isoxazoline, according to the method, oxime of a formula (II) and a carbonyl compound of a formula (I) react in the presence of a boron trifluoride complex and in the presence of an optional organic solvent or no solvent, the reaction conditions are mild, and the product yield is high.

The invention provides a synthesis method of alpha condensed ring C-glycoside, which comprises the following steps: mixing a catalyst, a ligand, an additive, a 1, 3-dicarbonyl compound and a 2, 3-unsaturated glycosyl donor, adding an organic solvent, reacting at room temperature, monitoring the reaction process by TLC (Thin Layer Chromatography), and terminating the reaction when the 1, 3-dicarbonyl compound completely disappears, thereby obtaining the alpha condensed ring C-glycoside. The catalyst Co (THMD) 3 used in the invention can catalytically generate a carbon glycoside product with high yield.

A process reacts olefins having 4 to 20 carbon atoms and the feed stream used, containing at least linear olefins and branched olefins, is distilled between two reaction steps and only the high-boiler phase obtained in this distillation is subjected to the second reaction, a heterogeneously catalysed hydroformylation, a homogeneously catalysed hydroformylation or a homogeneously catalysed alkoxycarbonylation.

The invention provides an energy-saving method and device for producing feed-grade propionic acid by using methanol carbonylation acetic acid waste liquid. The methanol carbonylation acetic acid waste liquid comprises the following components in percentage by mass: 40-80% of acetic acid, 20-60% of propionic acid and the balance of high-boiling residues, the method comprises the following steps: (1) evaporating the waste liquid by adopting a film evaporator with a scraper conical structure at the bottom to obtain a first gas phase and first kettle residues, controlling the evaporation rate to be 50-85% in the evaporation process, and keeping the first kettle residues in a flowing state; 2) directly feeding the first gas phase obtained in the step 1) into a recovery rectifying tower to obtain a second gas phase and crude propionic acid, and condensing the second gas phase to obtain acetic acid; 3, the crude propionic acid obtained in the step 2 passes through a resin tower, trace impurity metal ions are removed, and then the feed-grade propionic acid product is obtained.The method is simple in technological process, low in energy consumption and capable of running continuously, the content of the recycled propionic acid is larger than or equal to 99.5%, and the concentration of the impurity metal ions reaches the feed-grade standard.

The present invention relates to the field of organic synthesis, and more particularly to a method for the oxidation of allylic alcohols to α,β-unsaturated carbonyl compounds in the presence of a zirconium catalyst and a hydrogen acceptor.