21 results about "Cyclododecanone" patented technology

The invention relates to a catalyst for preparing cyclododecanone through cyclododecanol dehydrogenation and a preparation method and application thereof. The catalyst component comprises copper, zinc, zirconium, sodium, calcium, aluminum and iron; the catalyst is prepared from the following components in percentage by mass in an oxide form: 40 to 65 weight percent of copper oxide, 10 to 21 weight percent of zinc oxide, 10 to 30 weight percent of zirconium oxide, 5 to 20 weight percent of sodium oxide, 1 to 5 weight percent of calcium oxide, 0.5 to 1.5 weight percent of aluminum oxide and 0.05 to 0.5 weight percent of iron oxide. In one embodiment, according to the preparation method of the catalyst provided by the invention, water vapor is added during roasting in a nitrogen environment, so that the release speed of carbon dioxide is controlled, and formation of carbon deposition in the roasting process is reduced. The catalyst can solve the problem of low selectivity caused by low dehydrogenation reaction conversion rate and many by-product cyclododecene, and has the characteristics of high strength, good hydrothermal resistance, long service life and the like.

The invention relates to the technical field of cyclododecanol production, in particular to a method for inhibiting by-product cyclododecane in a cyclododecanol hydrogenation preparation process, which comprises the following steps: mixing one or more of cyclododecanone, epoxy cyclododecane or epoxy cyclododecene as raw materials with a solvent to prepare a raw material solution; the raw material liquid is subjected to a hydrogenation reaction, cyclododecanol is prepared, and the water content in the raw material liquid is 3-15 wt%. By adopting the technical scheme provided by the invention, on the premise of not changing the catalyst and the reaction system, the water content in the raw material liquid is controlled to be 3-15wt%, so that the water content of the reaction system in the reaction process is in a proper range, the generation of a byproduct cyclododecane can be effectively inhibited, and the yield of cyclododecanol is obviously improved; and the yield of the byproduct cyclododecane is reduced, so that the heat load of the tower kettle of the light component removal tower can be reduced by 20-50%.

This invention discloses a method for preparing dodecanoic acid lactam, comprising an oximation reaction of cyclododecanone, a rearrangement reaction of cyclododecanone oxime, and extraction and purification. The oximation reaction of this invention uses a cobalt-based MOF catalyst, which has high catalytic activity and can significantly improve the conversion rate of the cyclododecanone oximation reaction, thereby improving the overall reaction efficiency, reducing the formation of by-products, and thus improving the purity of the target product. In the rearrangement reaction of cyclododecanone oxime, zirconium oxide sulfate is used as a catalyst. This catalyst has good catalytic performance under high temperature conditions and can effectively promote the rearrangement reaction. Simultaneously, the ionic liquid is used as a solvent, which not only has good solubility but is also environmentally friendly and easy to recycle, reducing production costs and environmental impact.

The present invention relates to a method for recovering and reusing a selective homogeneous hydrogenation catalyst. The present invention relates to a method for recovering a selective homogeneous hydrogenation catalyst from a second reaction resolution in which a synthesis of cyclododecene is completed after synthesizing the cyclododecene by selective hydrogenation of a first reaction solution containing cyclododecatriene, triphenylphosphine, formaldehyde, and ruthenium chloride, and the method includes: preparing the selective homogeneous hydrogenation catalyst from the triphenylphosphine, the formaldehyde, and the ruthenium chloride during the selective hydrogenation of the first reaction solution, and synthesizing the cyclododecene; mixing a solvent containing cyclododecanone with the first reaction solution; and recovering the selective homogeneous hydrogenation catalyst through evaporation separation from the second reaction solution in which the synthesis of the cyclododecene is completed.

The application provides a synthesis method of 2-(3-hydroxypropyl)-cyclododecanone, which is as follows: under the action of an alkali catalyst, cyclododecanone and epichlorohydrin are reacted to obtain 2-epoxypropylcyclododecanone, and then hydrogen reduction is carried out to obtain 2-(3-hydroxypropyl)-cyclododecanone. The synthesis route is novel, the reagent such as epichlorohydrin is used for alkylation reaction, the epoxypropyl group can be introduced at the 2 position of cyclododecanone with high efficiency, compared with the alkylation reagents such as allyl alcohol and allyl acetate used in the traditional process, the method does not need a free radical initiator, and the monoalkylated product can be obtained with high selectivity, without double alkylation, multiple alkylation by-products, and the reaction yield is significantly improved. Secondly, the hydrogenation method can selectively obtain 2-(3-hydroxypropyl)-cyclododecanone, the reaction yield is high, and the selectivity is good. The method has good application prospect.

The present invention relates to a method for preparing hydrocarbon double acids using a cyclic hydrocarbon oxidation catalyst, wherein adipic acid and dodecanedioic acid may be produced with high yield while solving the problem of environmental pollution, the adipic acid and the dodecanedioic acid being prepared by using an oxidation reaction of a cyclohexane-cyclohexanone mixture and an oxidation reaction of a cyclododecane-cyclododecanone mixture, respectively, in the presence of a vanadium phosphate oxide-based catalyst and / or a cobalt-manganese oxide-based catalyst.

The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of cyclododecanone oxime. The preparation method of cyclododecanone oxime provided by the invention comprises the following steps: taking cyclododecanone and hydroxylamine salt as raw materials, and carrying out oximation reaction under the protection of polyphosphate to obtain a cyclododecanone oxime product, wherein the mass ratio of the polyphosphate to the cyclododecanone is (0.0001: 1)-(0.001: 1). According to the application, polyphosphate is used as a hydroxylamine protective agent, and compared with the prior art, the hydroxylamine decomposition rate can be remarkably reduced to be within 0.09%. Besides, a homogeneous reaction system is used, so that the reaction rate can be greatly increased, and the reaction time can be shortened to be within 1 hour; according to the method, the cyclododecanone oxime product is obtained through cooling crystallization, and oil-water two-phase separation and solvent removal after the reaction in a traditional oil-water two-phase reaction system are not needed, so that the process route is greatly simplified, and the production efficiency is improved.

The invention relates to a method for preparing cyclododecanone oxime, which comprises the following steps: S1, in the presence of a molecular sieve catalyst, carrying out hydrolysis reaction on an oxime compound and water to obtain a hydrolysis reaction product, and carrying out solid-liquid separation on the hydrolysis reaction product to obtain a solid-phase hydroxylamine molecular sieve and a liquid-phase product; and S2, mixing the solid-phase hydroxylamine molecular sieve, cyclododecanone and an optional solvent, and carrying out an oxime exchange reaction. According to the method provided by the invention, the problems that the catalyst and the reaction liquid are difficult to separate and the catalyst cannot be recycled can be effectively solved, the separation and purification process of the product and the reaction liquid in the oxime exchange reaction is effectively simplified, and a relatively high raw material conversion rate can be realized in a reaction system with relatively small dosage of cyclododecanone. In addition, the method disclosed by the invention is simple to operate and mild in condition, can realize continuous feeding and continuous reaction to generate hydroxylamine, and has a relatively good application prospect.

The application discloses a cyclododecanone oximation method, which adopts cyclododecanone and hydroxylamine salt to react, adopts alcohol ether phosphate as a reaction surfactant, and adopts hydroxamic acid as a metal ion chelating agent, so that the reaction rate of cyclododecanone oximation can be effectively improved, and the utilization rate of hydroxylamine can be improved.

This invention relates to the field of organic synthesis technology, and discloses a copper-based catalyst, its preparation method, and a method for catalyzing the preparation of cyclododecanol from cyclododecanol into cyclododecanone. The preparation method of the copper-based catalyst includes the following steps: preparing a catalyst with a specific surface area of ​​200-250 m² / g. 2 / g Al2O3-SiO2 composite support; copper source and rare earth oxide additives were loaded onto the Al2O3-SiO2 composite support, dried and calcined to obtain catalyst precursor; the catalyst precursor was reduced to prepare Cu + A copper-based catalyst with a molar ratio of 1.8 to 2.5:1 to elemental copper. This invention can control the Cu content in the copper-based catalyst. + The molar ratio with elemental copper allows the catalyst's activity state to be adjusted according to different production needs, thereby enabling flexible control of the reaction rate, improving process adaptability and operational stability; at the same time, it helps to suppress side reactions and improve the selectivity and purity of cyclododecanone.

The application discloses a method for preparing dodecanolactam from cyclododecanone oxime, wherein the cyclododecanone oxime raw material is diluted, mixed with fluorocarbon auxiliary agent, preheated, and then reacted in a microchannel after passing through a dynamic mixer and entering the microchannel, and the reaction liquid is separated into dodecanolactam product after neutralization and water washing; the method can effectively enhance reaction conversion rate and selectivity, improve stability and safety of device operation, and improve product quality.

The application discloses a preparation method of high-purity cyclododecanone, and steps of the method comprise the following steps: 1) cyclododecanol is subjected to a dehydrogenation reaction under the action of a dehydrogenation catalyst to obtain a dehydrogenation reaction liquid rich in cyclododecanone; 2) the dehydrogenation reaction liquid is introduced into cyclopentyl methyl ether, cyclododecanone solid is precipitated, then solid-liquid separation is carried out, and the solid is subjected to vacuum rectification after being melted to obtain high-purity cyclododecanone. The method can prepare a cyclododecanone product with a purity of greater than or equal to 99.998%, impurities cyclododecane and cyclododecene can be controlled at an extremely low level, and the anti-yellowing capacity of the product is significantly enhanced.

The invention discloses a preparation method of a high-yield cyclopentadecanolide intermediate, and belongs to the technical field of fine chemical engineering and flavors and fragrances. According to the invention, cyclododecanone is used as a raw material, the cyclododecanone and allyl chloride which is easy to obtain the raw material are subjected to carbon group a-site substitution under an alkaline condition, then hydroxyl is introduced through hydroboration oxidation, and finally, cyclization is carried out under an acidic condition to obtain 16-oxabicyclo [10.4. 0] hexadecane-1 (12)-ene, allyl alcohol or tert-butyl propylene ether in the prior art is replaced by allyl chloride, so that the yield of 16-oxabicyclo [10.4. 0] hexadecane-1 (12)-ene is improved. The price is far lower than that of tert-butyl propylene ether and is cheaper than that of highly toxic allyl alcohol, so that the safety and environmental friendliness of the production process are improved; the reaction route is simple and efficient, raw material selection is specific, side reactions are reduced, and the total yield is remarkably increased; in conclusion, compared with the prior art, the synthesis method disclosed by the invention is low in raw material price, high in yield and simple in process route, realizes high-yield preparation of the cyclopentadecanolide key intermediate, and has a potential industrial application prospect.

The present invention relates to the field of chemical production technology, and specifically to a method for preparing a cyclopentadecalactone intermediate bicyclic olefin ether, comprising the following steps: (1) using cyclododecanone as a starting material, and subjecting it to a free radical addition reaction with a fatty acid allyl ester to obtain a cyclododecanone addition ester; and (2) subjecting the cyclododecanone addition ester to a one-step ring-closure reaction in an alcohol solvent under high-temperature acid catalysis to obtain the bicyclic olefin ether. The present invention shortens the three-step reaction of the existing process to two steps, reduces the labor intensity and energy consumption of production, and simultaneously reduces the production cost of the product while increasing production capacity. The present invention fundamentally eliminates the generation of high-salt wastewater, making the entire process more environmentally friendly. The present invention does not use highly toxic chemicals, making the production site safer and healthier. The crude bicyclic olefin ether obtained by the present invention can be directly used in the synthesis of cyclopentadecalactone without undergoing additional purification operations, without affecting product quality.

The application discloses a preparation method of dodecene oxide and cyclododecanone. The application provides a preparation method of dodecene oxide as shown in formula B, which comprises the following steps: performing hydrogenation reaction on a compound as shown in formula A in the presence of a catalyst to obtain a compound as shown in formula B; and the catalyst is selected from any one of the following schemes: scheme one: the catalyst is a palladium catalyst and an amine compound; and scheme two: the catalyst is a palladium complex containing an amine compound. The preparation method of dodecene oxide provided by the application does not generate alcohol by-products. The dodecene oxide prepared by the application can be used to efficiently prepare high-purity cyclododecanone.

The invention relates to a method for preparing cyclododecanone oxime, which comprises the following steps: in the presence of a solid acid catalyst, cyclododecanone, an oxime compound and an optional solvent are mixed for oxime exchange reaction, and the solvent is a non-acidic solvent. According to the method disclosed by the invention, the oxime in the oxime compound is replaced by cyclododecanone under the action of the solid acid catalyst instead of using a liquid acid catalyst, so that the problems that the liquid acid catalyst is difficult to separate from the reaction liquid, the catalyst cannot be repeatedly used and the like are solved; the separation and purification process of the product and the reaction liquid in the oxime exchange reaction process is effectively simplified, and the method is a continuous and green production process and has a better application prospect.

The present invention relates to cyclododecanone and a preparation method therefor. According to the present invention, a cyclododecanone preparation method capable of achieving a high conversion rate and minimizing unreacted materials and the production of reaction byproducts can be provided. In addition, the present invention implements a high conversion rate and selectivity despite a simplified process, and thus can be helpfully utilized in economical laurolactam production methods that are easy to mass-produce commercially. According to the present invention, the proportions of cyclododecanol, cyclododecadiol, and the like, obtained as reaction byproducts, in the final product can be drastically reduced, and cyclododecanone can be produced at a high conversion rate.

The application provides a catalyst, a preparation method thereof and application of the catalyst in cyclododecanone synthesis. The application uses modified Cu-Zn-Si as a catalyst, and cyclododecanol as a raw material to prepare cyclododecanone through a dehydrogenation reaction. The combination of pyridine thione compounds and fluorine pyrimidine compounds is used as a modifier of the Cu-Zn-Si catalyst, which can significantly reduce the occurrence of a side reaction of cyclododecanol dehydration to generate cyclododecene, improve the selectivity of cyclododecanone, and make the selectivity of cyclododecanone greater than or equal to 99.5%, and the content of cyclododecene in the product less than or equal to 0.3%.

The present application relates to a kind of preparation methods of cyclododecanone. The method is from cyclododecanone, first cyclododecanone and methyl vinyl ketone are carried out cycloaddition under the catalysis of Lewis acid to generate spiro lactone, then, under the condition of metal catalyst, hydrogenation ring-opening rearrangement cyclododecanone generates cyclododecanone. The two-step reaction designed in the present application uses one-pot method, and no other any solvent is used in the synthesis process, no waste water is generated, safe and environmentally friendly, and the product yield is as high as 95% or more.

The application provides a method for synthesizing 2-(3-hydroxypropyl)cyclododecanone, which comprises the following steps: taking cyclododecanone as a starting material, synthesizing cyclododecanone diallyl acetal with diallyl acetal, and then obtaining 2-(3-hydroxypropyl)cyclododecanone through a cleavage reaction. The addition of palladium metal compounds in the reaction process effectively reduces the addition products of cyclododecanone and multiple allyl alcohols, and the coupling products of cyclododecanone itself, so that the effect of inhibiting side reactions is achieved. 2-(3-hydroxypropyl)cyclododecanone is an important intermediate for synthesizing cyclopentadecanolide, solves the problem of limited raw materials in the synthesis route of the musk cyclopentadecanolide, and has the advantages of high atom utilization rate and low raw material cost.

The invention relates to the technical field of cyclododecanone oxime preparation, and discloses a preparation method of cyclododecanone oxime. The invention relates to a cyclododecanone oxime preparation method, which comprises: in the presence of a solid acid catalyst and an ammonium salt auxiliary agent, carrying out an oxime exchange reaction on reaction raw materials such as cyclododecanone and an oxime compound to obtain cyclododecanone oxime, the ratio of pyridine infrared B acid to L acid at 350 DEG C of the solid acid catalyst is (0.5-2.5): 1. According to the method, the conversion rate of the raw materials and the selectivity of the target product can be improved, meanwhile, the solid acid serves as the catalyst, the preparation process is clean, economical efficiency is good, and the method has good industrialization prospects and has huge potential in development of environment-friendly processes and promotion of sustainable development.