61results about "Amino compound purification/separation" patented technology

The application discloses a device and method for preparing tert-butylamine by directly ammoniating isobutene, which comprises sequentially connected raw material preparation unit, reaction separation unit, rectification separation unit and circulating recovery unit; the raw material preparation unit is used for storing, mixing and heating raw materials; the reaction separation unit is used for pressurizing reaction of the raw materials in the raw material preparation unit and gas-liquid separation of products; the rectification separation unit is used for rectification separation of liquid-phase products separated by the reaction separation unit and recovery of part of unreacted raw materials; and the circulating recovery unit is used for rectification recovery of part of raw materials of gas-phase products separated by the reaction separation unit. The application has the characteristics of low overall equipment investment, high energy utilization rate, simple product separation and purification, perfect overall device design and small environmental pollution.

The present application relates to a kind of catalyst and its preparation method, the refining method of aniline, wherein the catalyst includes core and shell, the core includes acidic microporous-mesoporous composite molecular sieve and metal oxide loaded on the molecular sieve, the shell includes hydrophobic porous carrier layer and metal element loaded on the porous carrier layer.The catalyst of the present application can promote the conversion of cyclohexylamine and phenol in aniline into macromolecule, high-boiling substance, which can be quickly removed by simple rectification subsequently, finally realizing the synchronous efficient removal of phenol and cyclohexylamine, significantly improving the quality of aniline, while reducing the energy consumption of refining system and aniline loss, and no new impurities are introduced throughout.

A continuous recycling device of an organic base, including a first pump, a second pump, a third pump, a micro-mixer, a micro-channel reactor, a liquid-liquid separator and a continuous stirred tank. The third pump is configured to feed a first base-containing waste liquid to the micro-mixer. The first pump is configured to feed a solution of a second base to the micro-mixer. The micro-mixer is configured to mix the first base-containing waste liquid with the solution of the second base, and transfer the mixture to the micro-channel reactor. The liquid-liquid separator is configured to divide the reaction mixture into a top layer and a bottom layer. The continuous stirred tank is filled with a water-absorbing agent to absorb water in the top layer. A continuous recycling method using such device is also provided.

This invention relates to the field of recovered liquid treatment technology, and discloses a process for separating amines from NMP recovered liquid, comprising the following steps: Step S1: The NMP regenerated liquid is injected into a dehydration tower in a purification device for dehydration distillation; Step S2: The dehydrated NMP regenerated liquid is injected into a distillation device for secondary dehydration distillation; Step S3: The water and light components such as amines separated in the distillation device are collected using a side-collection method; the distillation device includes a distillation tower, which has multiple sets of packing materials fixedly installed inside and a feed pipe connected to the side of the distillation tower. The beneficial effects of this invention are: it allows the solution in the middle of the collection pan to enter the area between the two sets of separating rings in the side-collection pipe, reducing the probability of sediment and floating matter entering the side-collection pipe; simultaneously, the solution being extracted is in an isolated state, improving the purity of the extracted solution.

A low-carbon and environment-friendly method for synthesizing a primary amine from a halogenated hydrocarbon in the technical field of organic synthesis is provided. The method includes adding formaldehyde and ammonia in an alcohol solution at a ratio of 8 mol:8 mol for a full reaction, then adding 3 mol of the halogenated hydrocarbon at a suitable temperature, followed by a full reaction, and performing a series of post-treatment steps to obtain a target primary amine product with relatively high purity.

This invention discloses a method for preparing hexamethylenediamine, comprising the following steps: (1) under ammoniation reaction conditions, optionally in the presence of a solvent, subjecting hexanediol and ammonia to an ammoniation reaction to obtain an ammoniation reaction product; (2) separating and obtaining from the ammoniation reaction product a stream containing hexamethyleneimine and water, dehydrating the stream containing hexamethyleneimine and water to obtain a dehydrated stream containing hexamethyleneimine, and returning at least part of the dehydrated stream containing hexamethyleneimine as a circulating stream to the step (1), wherein a water content in the dehydrated stream containing hexamethyleneimine is less than 3 wt %, preferably less than 1.5 wt %. The invention can not only improve the yield of hexamethylenediamine but can also prolong the service life of the catalyst.

The utility model discloses a kind of tetraalkyl ammonium hydroxide recovery devices, it is related to tetraalkyl ammonium hydroxide recovery technical field, and wherein, tetraalkyl ammonium hydroxide recovery device includes adsorption unit and desorption unit, adsorption unit includes adsorption device, adsorption cavity of adsorption device is filled with adsorbent, liquid inlet line is used to introduce waste water and / or regenerating medium, liquid outlet line is used to discharge reclaimed water and / or tetraalkyl ammonium hydroxide solution, desorption unit includes desorption reagent line and / or desorption device;By adsorbent directly absorbing tetraalkyl ammonium hydroxide in waste water, the complexity of processing is reduced, the consumption of reagent is reduced, can be realized by desorption reagent or desorption device tetraalkyl ammonium hydroxide desorption, and the regeneration of adsorbent is realized, and after desorption, pure tetraalkyl ammonium hydroxide can be used for developing again by adjusting concentration and discharging reclaimed water, while realizing waste water purification, resource recovery and cost control.

The application discloses a method for recovering fluorine and triethylamine from fluorine-containing organic wastewater, and belongs to the technical field of fluoride preparation. The method adopts the synergistic effect of an organic phase of an extractant A and an extractant B under the condition that the pH is 0.5-4, realizes selective extraction of fluorine ions and inhibition of extraction of metal impurity cations under the premise that water-soluble triethylamine is not extracted through a one-step liquid-liquid extraction process, thereby realizing efficient and low-loss recovery of fluorine and triethylamine, and further preparing high-purity fluorides and triethylamine. The method has the advantages of short process, no need of complicated impurity removal process, high fluorine recovery rate, low production cost and the like.

This invention provides a method for removing phenol from crude aniline, the method comprising: step (1): feeding crude aniline and an aqueous solution of alkali metal hydroxide into a microreactor for contact reaction, controlling the flow rate of crude aniline and the aqueous solution of alkali metal hydroxide to make the molar ratio of alkali metal hydroxide to phenol in crude aniline 1:1-10:1, to obtain a reaction mixture; the concentration of the aqueous solution of alkali metal hydroxide is 0.1wt%-0.7wt%; step (2): transferring the obtained reaction mixture to a liquid-liquid separator to form an aniline organic phase and an inorganic phase rich in phenol salts, separating the aniline organic phase and the inorganic phase rich in phenol salts to obtain purified aniline; the method of this invention can effectively remove phenol from crude aniline, and the present invention can achieve a phenol removal rate of 99.7% using less alkali metal hydroxide.

The utility model relates to primary amine production technical field, concretely is primary amine rectification purification system. Primary amine rectification purification system, including storage tank, storage tank is connected with rectifying column through heat exchanger, and the bottom of rectifying column is connected with membrane evaporator through pipeline, and the inside of rectifying column is equipped with primary condenser, and rectifying column is connected with gas -liquid separation tank through secondary condenser. The system is through the additional membrane evaporator, and the liquid phase material of rectifying column bottom discharge is handled again. The unique structure design of membrane evaporator makes it can distribute liquid material into film shape evenly, greatly increases evaporation area, strengthens mass transfer process, further separates the primary amine and impurity remaining in liquid phase, significantly improves the purity of product, satisfies the strict requirement of high -end application field to primary amine high purity.

The present application relates to the technical field of energy saving of methylamine device, and discloses a waste heat recovery system and method of methylamine device.The waste heat recovery system of the methylamine device comprises a dehydration tower, a separation tank, a circulating pump, a heat pump, a separation tower and a concentration tower, and each device is connected through a pipeline to form a closed loop: the dehydration tower top steam outlet is connected with the separation tank inlet, the separation tank liquid phase outlet is connected with the dehydration tower heat exchange inlet through the circulating pump, the gas phase outlet is connected with the heat pump input end, and the heat pump output end is connected with the separation tower tower kettle and the concentration tower tower kettle respectively; the waste heat recovery method of the methylamine device is as follows: the dehydration tower top steam is recovered to the separation tank for gas-liquid separation, the liquid phase is continuously heat-absorbed through the circulating pump, the gas phase is transported to the tower kettle for heating after energy is improved through the heat pump, and the gas phase in the tower kettle is condensed and recycled, the present application fully recovers the waste heat at the top of the dehydration tower through closed loop operation, reduces the consumption of methylamine rectification steam, and realizes energy saving and consumption reduction.

The application provides a method for preparing a perovskite film by reducing the surface energy of PbI2 by using aryl amidine hydrochloride, the perovskite film and application. The method comprises the following steps: preparing a PbI2 solution modified by aryl amidine hydrochloride and coating on the surface of a substrate, annealing to obtain a PbI2 film, then coating a cation solution on the surface of the PbI2 film, and annealing to obtain a perovskite film. By using 2-phenoxyethyl amidine hydrochloride, the surface energy of the PbI2 film is effectively reduced, and the PbI2 porous channel is successfully constructed, so that the cation solution can fully diffuse in the PbI2 film, the solid-liquid interface reaction between PbI2 and the cation is promoted, the problem of PbI2 residue is solved, and the high-quality preparation of the perovskite film is ensured. The perovskite solar cell device prepared by using the perovskite film has obviously improved open-circuit voltage, fill factor and photoelectric conversion efficiency, and has excellent photoelectric performance.

A method of making 1,5 pentanediamine (a.k.a. PDA, pentamethyldiamine, PMDA and cadaverine) by decarboxylation of lysine using lysine decarboxylase in the presence of sulfate, or more preferably phosphate anion salts of lysine is described. The process works at high pHs at which the decarboxylase does not function using HCL salts of lysine and at substrate concentrations not achievable with lysine HCL at the ordinary pH optima of the carboxylase. In addition, a chromatographic process for purifying the PDA from lysine and the conjugate anions of the lysine salt is described that is applicable as a general process for purifying any diamine from a product mixture comprising amino and / or carboxylic acids along with their conjugate anions, which method uses a strong anion exchange resin as the stationary phase. The method does not utilize any organic solvent and is shown to be economical and efficient for industrial scale isolation of diamines from complex mixtures containing amino and / or carboxylic acids and conjugate anions from the amine salts.

The present invention relates to a method for producing ethyleneamines from a mixture containing water (H2O), ethylenediamine (EDA), and N-methylethylenediamine (NMEDA), comprising: (i) providing a feed stream containing EDA, NMEDA, and water; and (ii) separating the feed stream provided in step (i) in one or more distillation columns into a. fraction A containing water and NMEDA, wherein the weight ratio of water to NMEDA in fraction A is greater than 100:1; b. fraction B containing water, NMEDA, and EDA, wherein the weight ratio of water to NMEDA is in the range of 1:100 to 100:1; and c. fraction C containing water and EDA, wherein the weight ratio of EDA to water is greater than 5:1).

A method of purifying ethylenediamine includes the steps as follows. A phenyl compound is added into an ethylenediamine mixture solution, so as to obtain a mixture to be distilled, wherein the ethylenediamine mixture solution includes at least one of a first organic amine compound with a boiling point higher than ethylenediamine and a second organic amine compound with a boiling point lower than ethylenediamine, and the phenyl compound, ethylenediamine and water form an azeotrope. The mixture to be distilled is distilled under a distillation pressure, so as to obtain a low boiling point mixture, wherein the distillation pressure equals to or is smaller than a normal pressure. The low boiling point mixture is phase-separated and water is removed, so as to obtain a purified ethylenediamine product. A purity of the purified ethylenediamine product is larger than 99.5%.

A method for recovering raw and auxiliary materials in the production of lithium bis(fluorosulfonyl)imide is described. The method includes one or more different recovery sections A, B, C, D and / or E, corresponding to the recovery and post-treatment of the raw and auxiliary materials such as triethylamine, a fluoride ion, an ester solvent, and a crystallization liquid respectively used in the production of lithium bis(fluorosulfonyl)imide. The method for recovering raw and auxiliary materials of the present application enables the production of lithium bis(fluorosulfonyl)imide to have significantly improved economic efficiency and environmental protection.

This invention belongs to the field of chemical synthesis technology, specifically relating to a tetramethylammonium chloride synthesis apparatus. It includes a reaction vessel, a condenser layer, a water pump, a stirring mechanism, and a condenser tube. The reaction vessel includes a lid and a vessel body, which are detachably and fixedly connected. The lid has an air inlet and a liquid inlet, while the vessel body has a liquid outlet. The condenser layer covers the outer perimeter of the vessel body and has a water inlet and a water outlet. One end of the water pump is connected to the water inlet, and the other end is connected to the water outlet. The stirring mechanism is used to stir the liquid inside the reaction vessel and works in conjunction with the reaction vessel. The condenser tube is located inside the vessel body and communicates with the condenser layer; the condenser tube is a condenser tube with good thermal conductivity. This solution solves the problem that scale easily forms inside the condenser layer on the outside of the reaction vessel, preventing the internal temperature of the reaction vessel from decreasing.

The application relates to the technical field of pharmaceutical chemistry, and discloses a flurbiprofen ester enantiomer prodrug compound, a preparation method thereof, a pharmaceutical composition and purposes, the compound is (R)-AF377 or (S)-AF377, is formed by covalently connecting a carboxyl of (R)-flurbiprofen, (S)-flurbiprofen and a phenolic hydroxyl of acetaminophen through an ester bond, corresponding chiral carbons are R configuration and S configuration respectively, and structures are shown in formula (I) and formula (II). The application further provides a preparation method of the compound, a pharmaceutical composition containing the compound and purposes of the compound in pain, inflammation or fever treatment. The compound has high optical purity, releases an active ingredient in the liver, (S)-AF377 has synergistic anti-inflammatory analgesic activity, (R)-AF377 has independent analgesic activity, can reduce side effects of single drug use, improves bioavailability, and provides a new drug selection for treatment of mild to moderate inflammatory pain.

The application provides a synthesis process of polyethylene polyamine and belongs to the technical field of polyethylene polyamine.The synthesis process comprises a reaction unit, a circulation unit, a deamination unit and a refining unit; fresh EDA, circulating EDA and circulating DETA are mixed in the reaction unit, the temperature is increased from 60-65 DEG C to 76-80 DEG C, and heating is carried out to 155-165 DEG C to enter a reactor; when entering the reactor, the flow rate of EDA is 8487-9381 kg / h, the flow rate of DETA is 2829-3127 kg / h, hydrogen is heated to 155-165 DEG C to enter the reactor, the flow rate of hydrogen is 220-260 kg / h, an amination reaction is carried out, the reaction temperature is 155-165 DEG C, the reaction pressure is 17.5-18.5 MPa, and the reactor is provided with a catalyst; by using the synthesis process, the raw material cost is reduced, ethylenediamine and diethylenetriamine are recycled, the purity of polyethylene polyamine is improved, and the production level of fresh ethylenediamine and fresh diethylenetriamine is reached.

The invention provides a deuterated methylamine hydrochloride green synthesis method based on a continuous flow technology, which seamlessly integrates photocatalytic nitrification, catalytic hydrogenation and online acidification salification into a continuous and compact technological process through the continuous flow technology. And one-stop continuous synthesis from a gaseous raw material to a high-purity product is realized under a mild condition. Inert C-D bonds in deuterated methane can be efficiently activated at near room temperature in the core photocatalytic nitration step, and compared with a traditional high-temperature and high-pressure process, energy consumption is greatly reduced; the deuterated methane is used as a raw material, the use of a highly toxic reagent is avoided from the source, a continuous flow reaction system is combined with integrated water electrolysis for hydrogen production, the liquid holdup is small, and the intrinsic safety is high; meanwhile, a new way is provided for high-value utilization of deuterated methane, and the iron-based photocatalyst is low in cost and environmentally friendly and has good recycling potential.

The utility model relates to chemical solid -liquid separation device technical field, specifically a kind of multi-stage solid-liquid separation device of m-phenylenediamine crude product, including catalyst settling kettle, the lateral wall of catalyst settling kettle is equipped with first flow rate control valve;In the process that m-phenylenediamine carries out multi-stage separation, it sequentially passes through catalyst settling kettle, first flow rate control valve, first pump body, primary membrane filter kettle, second flow rate control valve, secondary membrane filter kettle and the pipeline intercommunication structure of second pump body and obtains m-phenylenediamine purified liquid to carry out multi-stage solid-liquid separation, in the process of separation, the flow rate of each pipeline is controlled by first flow rate control valve, second flow rate control valve and third flow rate control valve, to balance the air pressure balance between each kettle, reduce the situation that flow rate reduces even counterflow because of pressure problem occurs.

This application discloses a method and apparatus for producing bio-based pentanediamine. The method includes: using pentanediamine fermentation broth and / or its treated broth as raw materials, decarbonizing the raw materials to obtain a decarbonized liquid, then subjecting the decarbonized liquid to alkaline hydrolysis to obtain an alkaline hydrolysate; extracting the alkaline hydrolysate using an extractant and an auxiliary agent, collecting the oil phase to obtain an extract; removing light components from the extract, then separating pentanediamine and the extractant by distillation to obtain high-purity pentanediamine; and passing the raffinate through a crystallization evaporation system to obtain crystalline salt and organic fertilizer. This application enables the continuous industrial production of pentanediamine. Extraction with a multi-component extractant and auxiliary agent transfers pentanediamine to the oil phase, and controls emulsification and entrainment in the oil phase, preventing salt from entering the oil phase and avoiding salt precipitation during subsequent refining processes that could cause equipment and pipeline blockage. High-purity pentanediamine is obtained by distillation of the oil phase, avoiding the enormous energy consumption of traditional water concentration methods.

This invention discloses a method for preparing m-phenylenediamine, relating to the field of fine chemical hydrogenation synthesis technology. The method involves preparing a homogeneous feed solution by mixing pretreated isophthalonitrile and anhydrous methanol. A modified Raney Ni catalyst is added to the homogeneous feed solution for low-pressure hydrogenation. The modified Raney Ni catalyst is then separated from the homogeneous feed solution after the low-pressure hydrogenation reaction to obtain a crude m-phenylenediamine solution. The crude m-phenylenediamine solution is then purified by distillation after removing methanol to obtain m-phenylenediamine. The entire process is continuous, and the obtained m-phenylenediamine yield is ≥98.5%, purity is ≥99.5%, and moisture content is ≤0.1%. The modified Raney Ni catalyst is a Mo-Co dual-auxiliary modified Raney Ni catalyst, which can be reused to reduce costs.

A kind of for dichloroethane initial distillation device, including vertical cylinder and the base of cylinder bottom setting, gas outlet is provided in the center of cylinder top end head, the cylinder below heat exchange cavity is divided into intercommunication reaction cavity by multiple layers of grid plate, the cylinder in each layer grid plate top is filled with packing respectively, the cylinder in the topmost packing top is provided with feeding distributor, the cylinder in feeding distributor top is provided with feeding pipe in communication with outside, the heat exchanger of multiple heat exchange pipes is communicated with the top of reaction cavity by passing through heat exchange cavity, the cylinder in discharge elbow top is fixedly connected with gas phase inlet pipe.This utility model can make dichloroethane be enriched to a certain extent, can separate out most of the impurities with the dichloroethane boiling point difference larger, reduce the material complexity and processing capacity of subsequent rectification etc separation equipment, improve the efficiency and economy of entire production process, provide more favorable conditions for subsequent rectification etc operation of further purifying dichloroethane.

The application belongs to the technical field of organic afterglow crystal materials, and particularly relates to a host-guest type organic long afterglow crystal material and a preparation method and application thereof. The host-guest type organic long afterglow crystal material provided by the application ingeniously selects electron-rich diphenylamine material which is easy to crystallize and cheap and easy to obtain as a host material, and simultaneously introduces an electron-rich aniline derivative of the same type which is similar in structure and cheap and easy to obtain as a guest, thereby constructing a series of crystal materials with regular structures, and obtaining a series of new long afterglow light-emitting materials with adjustable colors (from yellow to green). The afterglow time of the material is more than 2s, the material has good afterglow light-emitting performance, and has good environmental stability to water and oxygen, thereby showing the application potential of the material in the fields of information encryption and anti-counterfeiting, and being capable of providing a theoretical basis and a material basis for practical applications such as data encryption and anti-counterfeiting.

The application discloses aniline production preparation system, including new hydrogen tank, first reactor and second reactor, the first inlet of first reactor is communicated with new hydrogen tank through first pipeline, first pipeline is equipped with first hydrogen gas mixing tank and first vaporizer in turn away from new hydrogen tank, first vaporizer is used for input nitrobenzene; first reactor is used for input catalyst; the first inlet of second reactor is communicated with new hydrogen tank through second pipeline, second pipeline is equipped with second hydrogen gas mixing tank and second vaporizer in turn away from new hydrogen tank, second vaporizer is used for input nitrobenzene; second reactor is used for input catalyst. The application can reduce hydrogen storage in the field, reduce equipment floor area, improve production safety, reduce cost.

This invention discloses a method for the distillation purification of m-phenylenediamine, relating to the field of fine chemical purification technology, comprising the following steps: S1, feeding crude m-phenylenediamine into a deammoniation and light-light ... m-Phenylenediamine products fully meet the usage requirements of high-end applications such as nylon MXD6 and high-end epoxy curing agents, and can be applied directly without additional treatment.