16 results about "Chloromethyl Ether" patented technology

The invention relates to the technical field of chemical reaction equipment, and discloses a reaction device and method for synthesizing free radicals from chloromethyl ethyl ether, the reaction device comprises a support, the inner wall of the support is rotatably connected with a shell, the top of the shell is connected with a first feeding port in a penetrating mode, and when a driving rod rotates, the driving rod drives a second gear ring and a first circular ring to rotate through a gear; due to the fact that the diameter of a first gear ring and the diameter of a second gear ring are different, the rotating speed difference exists between a first circular ring and a driving rod, metal particles enter the inner wall of the driving rod through a second feeding port, and the rotating speed difference exists between the driving rod and the first circular ring, it can be regarded that an auger rotates on the inner wall of the driving rod, and the rotating auger drives the metal particles to flow upwards; flowing metal particles flow out from the discharging port, so that the metal particles precipitated at the bottom of the reaction kettle can flow from bottom to top, and the situation that ethanol is differentiated from part of solution due to the fact that the metal particles at the bottom are heated too high is effectively prevented.

The invention relates to the technical field of adsorption materials, in particular to modified adsorption resin for a high-impurity n-heptane raw material and a purification method of the modified adsorption resin. The resin is prepared from the following raw materials: polystyrene-divinylbenzene resin microspheres, chloromethyl ether, 1, 3, 5, 7-tetra (4-chloromethylphenyl) adamantane, 2-methylimidazole and the like. During preparation, polystyrene-divinylbenzene resin microspheres are subjected to chloromethylation to introduce active sites, adamantine crosslinking to construct rigid pore channels, and imidazolyl functionalization to introduce specific adsorption sites. During purification, dynamic adsorption is performed after pretreatment of two stages of adsorption columns, mild regeneration is performed by using an ethanol-acetone mixed solution, isoparaffin, aromatic hydrocarbon and oxygen-containing compounds can be synchronously removed, high-purity n-heptane is obtained, the resin regeneration performance is excellent, and the whole process is easy to industrialize.

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 a production method for improving photo-thermal stability of a chloromethyl ethyl ether industrial product, and belongs to the technical field of chloromethyl ethyl ether processing.The preparation of an intermediate 1 comprises the steps that 80-120 mL of ethyl alcohol, 20-25 g of 3, 5-di-tert-butyl-4-hydroxybenzaldehyde and 6-10 g of n-butylamine are added into a 250 mL four-opening bottle provided with a backflow water diversion device, the temperature is increased to 60 DEG C, a reaction is carried out for 1 h, and an intermediate 2 is obtained; cooling to 0 DEG C by adopting an ice salt bath, adding 1-3g of potassium borohydride in batches, keeping the temperature at 0 DEG C, continuing to react for 0.5 hour, and adding a 5% citric acid aqueous solution to adjust the pH value to 2.0-3.0; the special photo-thermal stabilizer is synthesized and compounded with the epoxidized soybean oil, a single stabilizer and a special formula free of chloromethyl ether are generally adopted in the traditional method, the photo-thermal stabilizer containing the hindered phenol and piperazine structure is synthesized by the method, synergistic protection of light shielding, thermal stability and acid capture is achieved after compounding, and the product performance is remarkably improved; and the purity retention rate is 95-97% after 168h of ultraviolet aging.

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 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.

A preparation method of the adsorbent resin comprises the following steps: S1, dispersing an oil-phase monomer, a pore-foaming agent and an initiator in a water-phase solution, and heating and stirring for reaction; s2, adding the polymeric microspheres into dichloroethane, heating, stirring and swelling, then adding chloromethyl ether and zinc chloride, and heating for reaction; s3, adding the chloromethylated microspheres into a solvent, stirring and swelling, dropwise adding ethanolamine, and heating and stirring for reaction; s4, introducing nitrogen, adding dichloroethane into the intermediate product, stirring for swelling, adding a catalyst, and heating and stirring for reaction; s5, performing Soxhlet extraction and vacuum drying on the post-crosslinked resin to obtain the hypercrosslinked adsorption resin. The adsorbent resin provided by the invention has an ultrahigh specific surface area.

The invention belongs to the technical field of medicine synthesis, and particularly provides a sevoflurane synthesis method which comprises the following steps: taking hexafluoroisopropyl chloromethyl ether as a raw material, and reacting under the action of sodium p-toluenesulfonate and tetrabutylammonium fluoride to obtain sevoflurane with high yield. No other solvent participates in the method, the problem that the yield is low due to the fact that the solvent participates in the reaction when an alcohol solvent such as polyethylene glycol or triethylene glycol is used in the prior art is solved, the post-treatment is simple, the operation is simple and mild, the reaction yield and purity are stable, and the method is suitable for industrial production.

The application relates to a preparation method of an NHC-PdCl2-3-chloropyridine complex, which comprises the following steps: reacting 2,6-diisopropylaniline, glyoxal and acetic acid in an ethanol solvent for 2-4 days to obtain glyoxal-bis-(2,6-diisopropylphenyl) imine; stirring and reacting a mixed solution of the glyoxal-bis-(2,6-diisopropylphenyl) imine, chloromethyl ether, tetrahydrofuran and water at 30-50 DEG C for 10-20 hours to obtain 1,3-bis(2,6-diisopropylphenyl) imidazolium chloride, and the molar ratio of the glyoxal-bis-(2,6-diisopropylphenyl) imine to water is 1:2%-10%; reacting 1,3-bis(2,6-diisopropylphenyl) imidazolium chloride, palladium chloride, cesium carbonate and 3-chloropyridine at 60-100 DEG C for 10-20 hours to obtain [1,3-bis(2,6-diisopropylphenyl) imidazol-2-ylidene](3-chloropyridyl) palladium (II) dichloride, the method has the advantages of easy raw material acquisition, simple operation, mild and easy-to-control reaction conditions and convenience in industrial large-scale production.

The application relates to a phosphoric acid derivative modified resin and a preparation method thereof, and comprises the following steps: S1, mixing styrene, divinylbenzene, benzoyl peroxide, isooctane, polyvinyl alcohol and water, stirring to form a ball, and reacting at high temperature to obtain resin white balls; S2, mixing and swelling the resin white balls with dichloroethane, adding chloromethyl ether and ZnCl2 to react to obtain resin chloro balls; S3, mixing and swelling the resin chloro balls with butyl phthalate, adding hexamethylenetetramine to react, and adjusting the pH to alkaline to obtain resin amine balls; S4, mixing and swelling the resin amine balls with disodium ethylenediaminetetraacetate, adding formaldehyde, monobutyl phosphoric acid and concentrated hydrochloric acid to react to obtain alpha interception resin, i.e. the phosphoric acid derivative modified resin. Compared with the prior art, the alpha interception resin prepared by the application has a plutonium adsorption capacity of greater than 0.20 mmol / g in 5-8 mol / L nitric acid waste liquid, a distribution coefficient of greater than 1000, and high-efficiency plutonium recovery.

The application belongs to the field of polymer synthesis and particularly relates to a preparation method of a chelating resin. The method comprises the following steps: 1) pretreating a carrier; 2) uniformly mixing the pretreated carrier, an amine compound and an amide compound in proportion to prepare an activated carrier; 3) uniformly mixing the activated carrier, a quaternary ammonium salt and an ionic liquid in proportion to prepare a precursor; and 4) uniformly mixing the precursor, a lipid heterocyclic compound and a cationic surfactant in proportion to prepare the chelating resin. The method is more green and efficient, all high-risk reagents such as toxic diazonium salt and carcinogenic chloromethyl ether commonly used in traditional processes are abandoned, the whole reaction process is carried out under mild temperature and pressure conditions, controllability is high, and the chelating treatment capacity for metal ions is high.

The invention discloses a high-performance and high-chemical-stability composite anion exchange membrane containing a rigid structure, a preparation method and application, and belongs to the technical field of high polymer chemistry and alkaline anion exchange membranes. The composite anion exchange membrane is prepared by taking a synthetic polymer as a base material, performing ionization treatment and adding 4-tert-butyl calix [6] arene as a functional additive. 4-tert-butylcalix [6] arene has a macrocyclic steric hindrance phenol type structure to endow the polymer with the characteristic of oxidative degradation resistance, the polymer has an excellent scavenging effect on active free radicals, especially hydroxyl free radicals, in a fuel cell environment, and meanwhile, the rigid cavity structure can increase the free volume in a polymer membrane and is beneficial to improving the ionic conductivity. The preparation method disclosed by the invention is simple, mild in condition and low in cost, avoids the steps of high-toxicity chloromethyl etherification, noble metal catalyst use, complex polymerization and the like related to a common method, and has a good industrial application prospect.

The present application relates to the technical field of impurity removal, and particularly relates to a high-efficiency removal process of residual hydrogen chloride in chloromethyl ether crude product, comprising the following steps: first, taking magnesium-aluminum hydrotalcite as raw material, preparing guanidine salt intercalated hydrotalcite through amino guanidine bicarbonate ion exchange, and then preparing a core-shell structure composite deacidification agent through in-situ coating of low-formaldehyde urea-formaldehyde resin; after the chloromethyl ether crude product is pretreated through low-temperature sodium bicarbonate neutralization and salt water washing, the composite deacidification agent is added and stirred at room temperature to deeply remove acid, and finally, the finished product is obtained through reduced pressure distillation. The process can efficiently remove trace hydrogen chloride in the crude product, and the residual amount of the finished product is less than 80 ppm, while effectively inhibiting the hydrolysis side reaction of the material, and the product yield can reach more than 93%, and the process is stable and suitable for industrial production.

The invention relates to the technical field of chlorfenapyr processing technologies, and discloses a chlorfenapyr processing technology with inorganic salt Na2CO3 as an acid-binding agent, the processing technology comprises the following steps: pumping 540 kg of 4-bromo-2-(p-chlorphenyl)-5-(trifluoromethyl)-pyrrole-3-nitrile into a reaction kettle, then pumping 2100 L of toluene into the reaction kettle, uniformly stirring, carrying out heat preservation for 2-3 h, and carrying out filtration, washing and drying to obtain the chlorfenapyr. Cooling to about 25 DEG C; slowly dropwise adding 510kg of chloromethyl ethyl ether, and controlling the temperature to be 25-35 DEG C in the dropwise adding process; slowly adding 252kg of Na2CO3, and controlling the temperature to be 45-55 DEG C in the dropwise adding process; after adding, keeping the temperature at 50-60 DEG C and refluxing for 1 hour; according to the invention, the inorganic salt Na2CO3 is used as the acid-binding agent for the chlorfenapyr process, the inorganic acid-binding agent Na2CO3 is utilized and has the advantages of greenness, low toxicity, environmental protection, low price and the like, and the content of a product synthesized by the new acid-binding agent Na2CO3 can be increased by 0.5% and reaches 99%, so that the comprehensive cost of the product is reduced.

The application discloses a production method of high-purity chloromethyl ether, and belongs to the technical field of chloromethyl ether, wherein a composite special catalyst is added in the production process, so that the reaction path is accurately controlled, the generation of by-products such as polychlorinated compounds and oligomers is greatly reduced, and the product purity is improved; the composite special catalyst adopts iron-calcium double active sites to synergistically catalyze the chloromethylation reaction, and the existence of the double sites makes the catalytic efficiency high; the composite special catalyst takes a carbon fiber skeleton as a carrier, the carbon fiber skeleton has a high specific surface area and a porous structure, and after being modified on a calcium base, the pore distribution is uniform, so that the uniform loading of active components can be realized, the diffusion and contact of reactants can be accelerated, the reaction can be promoted, and the impurity content is reduced; and the carbon fiber skeleton has good mechanical stability, can be quickly separated through filtration after the reaction, and can be reused after regeneration treatment, so that the catalyst cost is reduced, solid waste emission is reduced, and the green chemical industry concept is met.