21 results about "Chloromethyl methyl ether" patented technology

The invention discloses a synthetic method of a substituted trans-dicyclohexyl alkenyl liquid crystal monomer, which comprises the following steps: reacting 4, 4 '-dicyclohexyl ketone with chloromethyl ether phosphine salt and potassium tert-butoxide at-10 DEG C to 0 DEG C to form 4, 4'-dicyclohexyl diene methyl ether; reacting with hydroxylamine hydrochloride under the action of a first catalyst to generate 4, 4 '-dicyclohexyl dioxime; under the action of a second catalyst, carrying out unilateral deprotection to generate 4-oxime 4 '-dicyclohexylformaldehyde; the preparation method comprises the following steps: reacting 4-oxime with R1BrPPh3 and potassium tert-butoxide at the temperature of 10 DEG C below zero to 0 DEG C to obtain 4-oxime 4 '-dicyclohexyl alkyl ethylene; reacting with formic acid to generate 4-formaldehyde-4 '-dicyclohexyl alkyl ethylene; the substituted trans-dicyclohexyl alkene liquid crystal monomer is prepared by reacting the substituted dicyclohexyl alkene with R2BrPPh3 and potassium tert-butoxide at the temperature of-10 DEG C to 0 DEG C to obtain a cis-trans mixture and carrying out transposition. The method comprises seven steps of reaction, transposition and purification are not needed in the early stage, transposition crystallization is only needed in the last step, and the total yield can reach 70% or above. The raw materials are cheap, easily available and low in cost.

The utility model belongs to the technical field of chloromethyl methyl ether production, and particularly relates to a transmission debugging device for chloromethyl methyl ether production, which comprises a pair of reaction kettles, an air exhaust assembly is arranged between the pair of reaction kettles; a top cover is arranged at the top of the reaction kettle; a shell is arranged outside the reaction kettle; a heating pipe is fixedly connected to the middle of the side wall of the shell. An air outlet is formed in the middle of the side wall of the heating pipe; a vent hole is formed in the middle of the side wall of the shell; the vent hole and the air outlet hole are correspondingly arranged; through the arrangement, the temperatures for generating hydrogen chloride gas and chloromethyl methyl ether can be respectively debugged, and the excessively high temperature in the reaction kettle can cause the hydrogen chloride gas and chloromethyl methyl ether to decompose or deteriorate, so that the quality and stability of the generated hydrogen chloride gas and chloromethyl methyl ether are influenced; by adjusting the temperature, the original chemical properties of the product can be kept in the generation process, and meanwhile, the generation of impurities is reduced by adjusting the reaction temperature, so that the purity of the product is improved.

This application relates to the field of polymer materials, specifically disclosing a resin for removing nitrate nitrogen from high-concentration sulfate solutions and its preparation method. The preparation method includes the following steps: S1, dispersing an oil-phase solution containing styrene, divinylbenzene, a porogen, and an initiator in an aqueous solution, polymerizing, and then washing with a solvent to obtain porous polymer spheres; S2, subjecting the obtained porous polymer spheres to chloromethyl ether for chloromethylation treatment to obtain a pre-modified resin; S3, subjecting the pre-modified resin to an amination reaction with an amination reagent to obtain a nitrate-removed resin; the nitrate-removed resin has a pore size of 2-10 nm accounting for 50-90%; this application also discloses the nitrate-removed resin prepared by the above preparation method. This application has the characteristic of achieving the removal of nitrate nitrogen from high-concentration sulfate wastewater.

The invention relates to the technical field of hydrogen energy preparation and impurity removal, in particular to high-alkali-resistance ion exchange resin for hydrogen energy preparation and impurity removal, which is prepared from the following raw materials: styrene, divinylbenzene, a pore-foaming agent, an initiator, an inorganic modifier, chloromethyl ether, an amination reagent and a polymerization inhibitor. The inorganic modifier is SiO2 (silicon dioxide) nano particles or TiO2 (titanium dioxide) nano particles modified by gamma-aminopropyl triethoxy silane; the amination reagent is N, N-dimethyl cyclohexylamine. Through an inorganic and organic synergistic modification strategy and optimized selection of an amination reagent with better alkali resistance, activity attenuation and structural deterioration of functional groups of the resin in a high-alkali environment are effectively inhibited, capacity loss of the resin in long-term operation is remarkably reduced, the service life of the resin is greatly prolonged, and the service life of the resin is prolonged. The long-term operation requirement of a high-alkali working condition in a hydrogen energy preparation process can be fully met, the resin replacement frequency is reduced, and the process operation cost is reduced.

The invention provides a method for removing aluminum from rare earth leaching liquid, and relates to the technical field of metal extraction technologies. A method for removing aluminum from rare earth leachate comprises the following steps that S1, styrene and divinylbenzene are mixed, then a pore-foaming agent is added, and an organic phase is obtained after stirring; s2, dissolving polyvinyl alcohol in deionized water, and stirring until the polyvinyl alcohol is completely dissolved to obtain a water phase; s3, slowly adding the organic phase into the water phase, stirring to form a stable suspension, and transferring the stable suspension to a reaction kettle; s4, introducing nitrogen into the reaction kettle, heating, and polymerizing to obtain resin white balls; and S5, mixing the resin white balls with chloromethyl ether. The D290 resin is matched with the 5-sulfosalicylic acid for use, so that the separation difficulty of the complex is reduced. According to the novel technology, efficient aluminum removal can be achieved under the mild condition, rare earth loss is reduced, and the technology is environmentally friendly; through complexing condition optimization, adsorption process design and gradient regeneration technology, directional removal of aluminum ions and cyclic utilization of resin are realized.

The present invention relates to a type of perfluorocationic resin and anion exchange membrane and membrane electrode synthesized based on Aza-Michael addition reaction, wherein the perfluorocationic resin structure includes an A (tetrafluoroethylene structure) unit and a B (perfluorocationic) structural unit, and the B unit contains a perfluoroether group and a cationic group, wherein the cationic group is a group having at least one (-C-C-) group and one or more or connected groups in the structure. No catalyst and highly toxic reagent chloromethyl ether are required during the reaction process of the method provided by the present invention, the reaction conditions are mild, the degree of reaction can be effectively controlled, the molecular weight of the connecting chain segment in the obtained resin repeating unit is low, and the ion exchange capacity is high. The structural advantages of the perfluorocationic resin are retained in the obtained perfluorocationic resin chemical structure, and it has super stability under alkaline conditions, and can effectively improve the service life of the anion exchange membrane and membrane electrode prepared with the perfluorocationic polymer.

The invention discloses a recovery method of sevoflurane water-alcohol mother liquor, and belongs to the technical field of medicines. The method comprises the following steps: adding perlite into sevoflurane water-alcohol mother liquor, removing fluorine ions to obtain a fluoride-free water-alcohol solution, carrying out reduced pressure distillation on the solution to remove water, adding an inert organic solvent, recovering solid which is high-purity metal chloride, carrying out reduced pressure recovery on liquid which is the organic solvent, and recovering the residual solvent which is a high-boiling-point alcohol solvent; the sevoflurane water-alcohol mother liquor is a water phase obtained by adding water into a reaction solution of chloromethyl ether and alkali metal fluoride in a high-boiling-point alcohol solvent and carrying out phase splitting. Particularly, a reaction product metal chloride and high-boiling-point alcohol in the reaction are recycled. The benefit maximization of the sevoflurane process is realized, the three wastes are reasonably treated, and the comprehensive utilization of resources is realized.

The invention discloses a preparation method of polyphenylene sulfide based chelate fibers. The preparation method comprises the following steps: adding polyphenylene sulfide fibers into a reactor, adding a solvent for full swelling, then adding a cross-linking agent and a catalyst for reaction, and treating the obtained product to obtain cross-linked PPS fibers; adding the cross-linked PPS fiber into a solvent for swelling, then adding a nitration reagent for reaction, and treating a product after the reaction to obtain modified nitrocellulose PPS-NO2; the modified nitrocellulose PPS-NO2 is added into a solvent for swelling, then a reducing agent is added for a reduction reaction, a product obtained after the reaction is treated, and amino polyphenylene sulfide fiber PPS-NH2 is obtained; and adding the amino polyphenylene sulfide fiber PPS-NH2 into a solvent, and then adding a functional monomer to carry out grafting reaction, thereby obtaining the product polyphenylene sulfide-based chelate fiber. By utilizing the method to prepare the chelating functional fiber, the use defect of strong cancerogenic substances such as chloromethyl ether in the prior art can be effectively avoided. Meanwhile, the polyphenylene sulfide-based chelate fiber prepared by the method has relatively good stability and acid and alkali resistance.

This application relates to the technical field of carbon capture, and specifically discloses a preparation process of an amine solution purification resin for a carbon capture system. The preparation process includes the following steps: S1: Mix styrene, divinylbenzene, acrylate, initiator, porogen, dispersant and water evenly, raise the temperature for reaction, cool down, perform solid-liquid separation, extract the porogen, and wash to obtain polystyrene microspheres; S2: Mix the polystyrene microspheres, chloromethyl methyl ether, Lewis acid catalyst and solvent evenly, raise the temperature for reaction, cool down, perform solid-liquid separation, and wash to obtain chloromethylated polystyrene microspheres; S3: Mix the chloromethylated polystyrene microspheres, triethylenetetramine, tetrabutylammonium bromide, antioxidant and ethanol evenly, raise the temperature for reaction, cool down, perform solid-liquid separation, wash, perform plasma treatment, soak in a silane coupling agent solution, perform solid-liquid separation, and wash to obtain the product. The purification resin prepared in this application has a good removal effect on heat stable salts in amine solution.

The application relates to the technical field of iron phosphate preparation, in particular to a high-purity iron phosphate material and a preparation method thereof. The preparation method of the high-purity iron phosphate material provided by the application comprises the following steps: mixing polystyrene microspheres, chloromethyl methyl ether, a first catalyst and an organic solvent to obtain primary modified polystyrene microspheres; mixing the primary modified polystyrene microspheres, aminomethyl phosphonic acid, a second catalyst, a cocatalyst and an organic solvent to obtain secondary modified polystyrene microspheres; mixing an iron source solution and a phosphorus source solution, then adding the secondary modified polystyrene microspheres to carry out reaction, and baking to obtain the high-purity iron phosphate material. The iron phosphate material obtained by the method has low impurity content and high tap density, and the preparation method is relatively simple, low in energy consumption and convenient to operate.

The invention provides an anionic membrane as well as a preparation method and application thereof. The preparation method of the anionic membrane comprises the following steps: S1, prepolymerization: dissolving a first unsaturated monomer containing a halogen group, a second unsaturated monomer and an initiator in an organic solvent, and carrying out polymerization reaction after dissolving to obtain a membrane casting solution; s2, curing: coating a supporting base material with the membrane casting solution, and curing to form a membrane; s3, functional modification: transferring a membrane into an organic amine solution for soaking after the membrane is completely cured to form a membrane, and fully reacting to obtain a functional modified anionic membrane; the molar ratio of the first unsaturated monomer to the second unsaturated monomer is 1: (0.03-0.10). According to the preparation method, the use of high-carcinogenicity chemicals such as chloromethyl methyl ether is avoided, the green production of the high-performance anion membrane is realized, the accurate regulation and control of the physical and chemical properties of the anion membrane are also realized, and higher current efficiency and lower unit energy consumption are obtained when the anion membrane is applied to the salt concentration test of electrodialysis.

This invention discloses a method for preparing polyphenylene sulfide (PPS)-based chelated fibers. PPS fibers are added to a reactor, and a solvent is added to allow them to swell fully. A crosslinking agent and a catalyst are then added to carry out the reaction. The resulting product is treated to obtain crosslinked PPS fibers. The crosslinked PPS fibers are then added to a solvent to swell, followed by the addition of a nitrifying agent to carry out the reaction. The product is then treated to obtain modified nitrated fiber PPS-NO2. The modified nitrated fiber PPS-NO2 is then added to a solvent to swell, followed by the addition of a reducing agent to carry out a reduction reaction. The product is then treated to obtain amino-based PPS-NH2. The amino-based PPS-NH2 is then added to a solvent, followed by the addition of a functional monomer to carry out a grafting reaction, yielding the product, polyphenylene sulfide-based chelated fibers. Using this invention to prepare chelated functional fibers effectively avoids the drawbacks of using highly carcinogenic substances such as chloromethyl ether in existing technologies. Furthermore, the polyphenylene sulfide-based chelated fibers prepared by this invention exhibit good stability and acid and alkali resistance.

The utility model belongs to the field of chloromethyl methyl ether raw material conveying devices, and particularly relates to a raw material conveying device for chloromethyl methyl ether manufacturing. A methanol inlet and a formaldehyde inlet are fixedly connected to the side wall of the bottom end of the reaction furnace; a hydrogen chloride input pipe is fixedly connected to the side surface of the case; a gas channel corresponding to the hydrogen chloride input pipe is formed in the case; methyl alcohol is introduced into the reaction furnace from the methyl alcohol inlet, formaldehyde is introduced into the reaction furnace from the formaldehyde inlet, after the methyl alcohol and the formaldehyde are fully mixed, an internal air pump of the hydrogen chloride gas conversion box is driven immediately, and a hydrogen chloride solution is introduced into the machine box through the hydrogen chloride input pipe, so that hydrogen chloride gas passes through a mixed solution of formaldehyde and methyl alcohol from bottom to top; finally carrying out reaction; the methanol inlet and the formaldehyde inlet are oppositely arranged, so that the mixing rate of formaldehyde and methanol is increased, hydrogen chloride gas passes through a solution from bottom to top through the hydrogen chloride input pipe on the side wall of the case, and the reaction rate of raw materials is increased.

The invention discloses an electromagnetic shielding fabric and a preparation method thereof, and relates to the technical field of textile fabrics. When the electromagnetic shielding fabric is prepared, 3, 9-dichloro-2, 4, 8, 10-tetraoxa-3, 9-diphosphospiro [5.5] undecane-3, 9-dioxide and formic acid are subjected to a reaction, then the reaction product and tetramethyl divinyl disiloxane are polymerized, and a phosphorus-silicon synergistic flame retardant is prepared; the preparation method comprises the following steps: polymerizing carbazole and N-vinyl carbazole, and depositing on magnesium hydroxide to prepare polycarbazole coated magnesium hydroxide; the preparation method comprises the following steps: sequentially reacting 3-allyl-2-hydroxybenzaldehyde with tyrosine and dimethyl tin chloride to prepare an organic tin antibacterial agent; reacting polystyrene with chloromethyl methyl ether and an organic tin antibacterial agent in sequence to prepare modified polystyrene; preparing a spinning solution from the modified polystyrene, the polycarbazole coated magnesium hydroxide and the phosphorus-silicon synergistic flame retardant, and performing wet spinning and spinning by a spinning machine to obtain the electromagnetic shielding fabric. The electromagnetic shielding fabric prepared by the invention has excellent electromagnetic shielding, antibacterial, flame-retardant and mechanical properties.

The invention relates to a preparation method of a [18F] fluoroestradiol precursor compound, which is characterized in that chloromethyl methyl ether used in the fifth step in the synthesis process of the existing [18F] fluoroestradiol precursor compound in the market is replaced by bromomethyl methyl ether with lower toxicity. The problem of purchasing highly toxic chloromethyl methyl ether in the synthesis process is successfully solved, the harm of highly toxic product residues brought into human bodies is also solved, and meanwhile, the pollution to the environment in the compound synthesis process is also reduced.

The invention provides a preparation method of macroporous resin for recovering noble metals, which belongs to the technical field of resin synthesis, and comprises the following steps: preparing hexahydropyridine by pyridine catalytic hydrogenation; rectifying the hexahydropyridine to obtain high-purity hexahydropyridine; preparing macroporous white balls by taking styrene, divinylbenzene, a pore-foaming agent, an initiator and a dispersing agent as raw materials; eluting the macroporous white balls to form holes; carrying out chloromethylation reaction on the macroporous white balls subjected to elution pore forming and chloromethyl ether; and carrying out amination reaction on the chloromethylated macroporous white balls and high-purity hexahydropyridine to obtain the macroporous resin. According to the preparation method of the macroporous resin for recovering the precious metal, the prepared macroporous resin is excellent in adsorption performance and long in service life under the conditions of high acid and strong oxidants.

The invention belongs to the technical field of anti-cancer drugs, and particularly discloses an isopentenyl flavonoid compound and a preparation method and application thereof.The isopentenyl flavonoid compound is of a structure shown in the formula (1), and according to the method, firstly, chloromethyl methyl ether is used for reacting 2, 4, 6-trihydroxyacetophenone with 2, 4, 6-trihydroxyacetophenone to obtain 2, 4, 6-trihydroxyacetophenone; the preparation method comprises the following steps: protecting hydroxyl at the position 4 by using a reaction solvent, then carrying out a substitution reaction on isopentenyl bromide and the product, then carrying out a microwave reaction by using N, N-diethyl aniline as a solvent to generate Claisen rearrangement, then carrying out a Claisen-Schmidt reaction with corresponding aldehyde to generate chalcone, and finally carrying out ring closing by using iodine and carrying out deprotection by using hydrochloric acid to obtain the chalcone. And preparing to obtain the compound. The compound disclosed by the invention is novel in structure, relatively good in activity and small in toxicity, has relatively good anti-tumor activity as an inhibitor, has relatively good inhibitory activity on various tumor cells including colorectal cancer, breast cancer, lung cancer, liver cancer and the like, can be applied to preparation of anti-tumor drugs, and has wide application prospects. Good application prospects are realized in the anti-tumor aspect.

The present application relates to a method for preparing a large-capacity adsorption resin for water treatment, comprising the following steps: S1: uniformly mixing a monomer formulation and an aqueous phase mixture, heating, and keeping the temperature to react, to obtain a polymer; S2: washing the polymer with water, washing with an organic solvent, and drying and sieving the powder to obtain an intermediate product; S3: uniformly mixing the intermediate product, monochloromethyl ether, sulfuric acid, and a catalyst, heating, keeping the temperature to react, cooling, washing with an organic solvent, distilling, adding liquid alkali, adjusting the pH, stirring, filtering, and obtaining chloromethylated beads; S4: dripping trimethylamine solution, dimethylamine solution, tri-n-butylamine, polyethylene polyamine, pyridineamine, methylal, and urotropine into the chloromethylated beads, heating, keeping the temperature to react, filtering, and distilling to obtain quaternized beads; S5: washing the quaternized beads with water, converting with hydrochloric acid, filtering, washing with water, and drying to obtain a large-capacity adsorption resin. The adsorption resin in the present application has high cleanliness, large adsorption capacity and strength, and is suitable for water treatment.

The invention relates to the technical field of carbon capture, and particularly discloses a preparation process of amine liquid purification resin for a carbon capture system.The preparation process comprises the following steps that S1, styrene, divinylbenzene, acrylate, an initiator, a pore-foaming agent, a dispersing agent and water are mixed to be uniform, heating reaction, cooling and solid-liquid separation are conducted, the pore-foaming agent is extracted, washing and drying are conducted, and an amine liquid purification resin is obtained; the polystyrene microspheres are obtained; s2, uniformly mixing the polystyrene microspheres, chloromethyl methyl ether, a Lewis acid catalyst and a solvent, carrying out heating reaction, cooling, carrying out solid-liquid separation, and washing to obtain chloromethylated polystyrene microspheres; and S3, uniformly mixing chloromethylated polystyrene microspheres, triethylene tetramine, tetrabutylammonium bromide, an antioxidant and ethanol, carrying out heating reaction, cooling, solid-liquid separation, washing and plasma treatment, soaking in a silane coupling agent solution, carrying out solid-liquid separation, and washing to obtain the product. The purification resin prepared by the invention has a relatively good removal effect on heat-stable salts in the amine liquid.

The application discloses a preparation method of a novel MOM-protected C3 side chain of cefodizime, and belongs to the technical field of pharmaceutical synthesis intermediates. The method is as follows: 2-chloro-3,4-dihydroxybenzaldehyde is used as raw material, and chloromethyl methyl ether (MOMCl) or bromomethyl methyl ether (MOMBr) is used to protect two phenolic hydroxyl groups. After the aldehyde group is oxidized into a carboxylic acid by using a Pinnick method, the carboxylic acid is condensed with 2-chloroethylamine to obtain an amide, and finally, the amide is reacted with tetrahydropyrrole to obtain the target product: 2-chloro-3,4-bis(methoxymethoxy)-(2-(pyrrol-1-yl)ethyl)benzamide. N The application has mild reaction conditions and simple operation, and is suitable for industrialized production of cefodizime.