133 results about "Chloromethyl Ether" patented technology

The embodiment of the invention discloses a polymeric adsorbent and a preparation method thereof. The preparation method comprises the following steps of: preparing a bead-like resin from chloromethyl styrene serving as a polymerization monomer and divinyl benzene serving as a cross-linking agent by a suspension polymerization method; and adding a hydroxyl-containing monomer at the post-crosslinking stage to perform super cross-linking reaction so as to prepare the polymeric adsorbent. In the method, pores are formed in the polymeric adsorbent at the post-crosslinking stage of polychloromethyl styrene by using a chemical modification method, and polar groups are formed on the frame of the polymeric adsorbent by introducing the hydroxyl-containing monomer for modification, so the adsorption of an adsorbent substance by the polymeric adsorbent is increased. The preparation method provided by the invention is simple and the substances harmful to human body such as chloromethyl ether and the like and pore-forming agents are not used in the method. Experimental results show that the polymeric adsorbent prepared by the invention has the advantages of high specific surface area, small aperture, high adsorption selectivity and particularly high capacity of absorbing aromatic compounds.

The invention provides a preparation method of an ion exchange resin, which comprises the following steps: (1) mixing a dispersant solution and an organic phase, and gradually heating to carry out polymerization reaction; (2) adding chloromethyl ether into the obtained white ball, and adding a catalyst zinc chloride to carry out chloromethylation reaction; and (3) adding methanol into the obtained chlorine ball, dropwisely adding a trimethylamine water solution, adding a 10% sodium chloride solution, adding hydrochloric acid for neutralization, and washing with water to obtain the resin. The ion exchange resin provided by the invention has the advantages of favorable selectivity, high uranium adsorption capacity and high exchange speed.

A monolithic bipolar membrane and a preparation method thereof relate to functional polymer membrane materials. The monolithic bipolar membrane includes a cation exchange layer and an anion exchange layer. Preparation method 1: basement membrane pre-irradiation; simultaneous grafting on both sides; sulfonation; quaternization. Preparation method two: basement membrane pre-irradiation; double-sided step-by-step grafting; sulfonation; quaternization. The preparation of bipolar membranes by radiation grafting technology not only saves the film-forming process in the traditional bipolar membrane preparation process, but also does not need to add initiators and catalysts during the grafting process, and the prepared bipolar membranes are very uniform and pure. The steps are simple, and the thermal stability and chemical stability of the film are better. Even if it is used for a long time, there will be no problems such as bubbling and cracking in the middle interface layer that are easy to occur during the use of composite bipolar membranes. Good mechanical properties, thermal stability and chemical stability. Avoid the use of strong carcinogenic reagents such as chloromethyl ether, and reduce the harm to the human body and the environment.

The invention relates to an anion exchange membrane based on fluorinated polybenzimidazole and a preparation method of the anion exchange membrane. The general structure formula of the anion exchangemembrane based on the fluorinated polybenzimidazole comprises a repetitive unit as shown in formula (1), in formula as shown in specification, n is degree of polymerization; x is an integer of 2-12, yis an integer of 0-11; and R is H, methyl, ethyl, isopropyl or phenyl. The prepared membrane has excellent mechanical property, alkali resistance, heat resistance, low water absorption and high electrical conductivity; and moreover, the preparation process of the membrane is relatively simple and safe, and chloromethyl ether as a cancerogenic substance used in a preparation process of a traditional quaternary ammonium salt type anion membrane is avoided.

The invention discloses hyper cross-linking resin which is prepared by taking alpha methyl styrene and divinylbenzene as raw materials, changing the cross-linking degree or adding different pore-foaming agents, performing suspension polymerization so as to obtain aperture controllable gel type and porous precursor resin, enabling the precursor resin to react with a catalyst in a swelling state, performing Friedel-Crafts reaction, thereby obtaining the hyper cross-linking resin with a high specific surface area, a large pore volume and a controllable aperture. The invention further discloses a preparation method and application of the hyper cross-linking resin. Compared with the prior art, the preparation method is simple, carcinogenic substances such as chloromethyl ether is not adopted for chloromethylation, the cost is low, industrial production can be achieved, and the prepared hyper cross-linking resin is relatively good decoloring effect on organic acid.

The invention belongs to the technical field of synthetic methods of ion exchange resin and especially relates to a synthetic method of strong-basic anion exchange resin used in a compact bed. The synthetic method includes the steps of: 1) synthesizing a crosslinked polystyrene white sphere framework being 100-150 nm in particle size on the surface of inert crystal nucleus in a homogenous-phase wet chemical manner; adding chloromethyl ether as a chloromethylation reagent to carry out a Friedel-Crafts reaction to benzene rings in the styrene in the crosslinked polystyrene white spheres to obtain an intermediate product A; 2) performing an amination reaction to the intermediate product A with a tertiary amine containing a long carbon chain to generate the strong-basic anion exchange resin being 180-280 [mu]m in particle size. The framework synthetic method is novel and unique. The exchange resin is fine and uniform in particle size, has large specific surface area, is short in diffusion path and has high exchange speed during exchange, and is low in cost and has good application effects. The exchange resin can satisfy application demands in the compact bed.

The invention discloses a polymer anion exchange membrane based on imidazole onium salt and a preparation method thereof, and relates to an ion exchange membrane and a preparation method thereof. The preparation method comprises the following steps of: (1) synthesizing of an imidazole onium salt polymer through a radical copolymerizationic compound: adding a monomer A, a monomer B, a vehicle and an initiating agent in a reactor, carrying out sealing and a heating regurgitation reaction under the inert gas protection, and drying and washing a product to obtain the imidazole onium salt polymer; and (2) membrane formation: dissolving the obtained imidazole onium salt polymer in step (1) in an organic solvent to prepare a polymer solution, 5%-10% of mass percent concentration, casting to form a membrane through a phase inversion method, and drying to obtain the polymer anion exchange membrane based on the imidazole onium salt, wherein the imidazole onium salt polymer accounts for 5-10% of the organic solvent. The polymer anion exchange membrane provided by the invention has the advantages that the preparation method is simple, the cost is lower, the electric conductivity is higher, the anion exchange membrane has good heat stability and chemical stability, meanwhile, the use of chloromethyl ether in the traditional polymeric compound anion exchange membrane preparation process is avoided, and the polymer anion exchange membrane can reduce harms to human bodies and environment.

The invention relates to a synthetic method of strongly basic anion exchange resin, and particularly relates to a synthetic method of high temperature-resistant strongly basic anion exchange resin containing a long-carbon chain alkylamine group. A crosslinked polystyrene white ball is adopted as a skeleton, chloromethyl ether is adopted as an alkylating reagent to graft benzyl chloride on the white ball skeleton by Fourier reaction, and amination reaction is carried out on the long-carbon chain alkylamine, so as to obtain the strongly basic anion exchange resin. The synthetic method has the advantages that the strongly basic anion exchange resin with relatively high heat stability can be synthesized by adopting a simple production technology and cheap materials, so that the strongly basic anion exchange resin can be applied to unit operation in a high-temperature environment, such as preparation of super-pure water in a semiconductor industry, high-temperature condensate refined treatment of a power plant, removal of silicic acid of water in a high-pressure boiler, and use under a high-temperature condition as a catalyst.

The invention relates to a recycling system of chlorination mother solution and a recycling method thereof in an automatic anion exchange resin production system, white ball and chloromethyl ether are sent to a chloromethylation reaction kettle respectively by an airflow transmitting system and pump transmission, stirring is carried out at normal temperature; after inflating, ferric trichloride dissolvable in the chloromethyl ether is added for catalysis, and exothermic reaction is generated, the adding speed of the chloromethyl ether is regulated according to temperature, chlorine ball is prepared after the temperature is raised to 48 DEG C and temperature insulation is carried out for 10 hours, temperature reduction is carried out, the separated chlorine ball is washed sequentially by chloride methanol for two times, and by methanol for one time; then, solid-liquid separation is carried out, solid-phase chlorine ball enters amination reaction, liquid-phase chlorination mother solution and chlorine ball cleaning solution enter a chlorination liquid recycling reaction kettle, chloride methanol generated in the chlorination liquid recycling reaction kettle enters a chloromethyl ether reaction kettle; and then, solid methanol and chlorine hydride are added in the chloromethyl ether reaction kettle for reaction, chloromethyl ether volatilized in the reaction process enters a chloromethylation reaction kettle after condensation by a condenser, and noncondensable gas enters an alkali spray tower for absorption treatment.

The invention relates to a diethylamine anion exchange resin and a preparation method thereof, belonging to the technical field of anion exchange resins. The resin is prepared from the following raw materials in parts by weight: 10-20 parts of macroporous styrene-divinylbenzene copolymer microsphere, 100-120 parts of dichloromethane, 15-25 parts of anhydrous aluminum trichloride, 10-20 parts of chloracetyl chloride, 5-9 parts of chloracetylated resin, 50-60 parts of diethylamine, 50-60 parts of tetrahydrofuran and 3-12 parts of NaHCO3. Chloracetylation reaction is performed on crosslinked polystyrene microspheres by Friedel-Crafts reaction to introduce chloracetyl group, and amination is performed to obtain the weakly alkaline tertiary-amine anion exchange resin. The method avoids using chloromethyl ether and other carcinogenic substances, and avoids secondary crosslinking, polysubstitution and other side reactions.

The invention relates to an alkaline polymer electrolyte membrane and a preparation method thereof, in particular to a method for preparing an alkaline polymer electrolyte membrane by preparing a quaternary random copolymer from styrene, 4-chloromethyl styrene, an alkyl acrylate monomer and an acrylic ester monomer as raw materials, and carrying out quaternization or quaternary phosphonium reaction and membrane forming. In the invention, the 4-chloromethyl styrene is directly adopted and chloromethyl ether is not used, thereby solving the problems of the additional crosslinking of methylenem, the pollution of a metal catalyst and the like. The prepared alkaline polymer electrolyte membrane has stable structural performance and good electrochemical stability, and the conductivity of the alkaline polymer electrolyte membrane reaches 10-3S/cm.

The invention discloses a preparation method of chloromethyl styrene resin. The preparation method is as follows: first reacting a long chain diol with trioxymethylene in the presence of dry hydrogen chloride, thionyl chloride or benzene sulfonyl chloride for preparing long chain chloromethyl ether; performing chloromethylation reaction of the obtained long chain chloromethyl ether and styrene resin in conditions of aluminum chloride, stannous chloride, concentrated sulfuric acid or titanium tetrachloride catalysis, filtering an obtained reaction liquid to obtain resin balls, and washing with a mixed solution to remove a surface catalyst to obtain the chloromethyl polystyrene resin. The preparation method of the chloromethyl styrene resin has the advantages of environmental protection and no pollution, at the same time, the used long chain diol also can be recycled, so that the preparation method has the characteristic of low production cost.

The invention discloses a production method of polyphenylene sulfide-based adsorption separation resin. The production method comprises the following steps: adding a solvent to polyphenylene sulfide resin to swell the polyphenylene sulfide resin adding anhydrous tin tetrachloride and chloromethyl ether, heating and reacting above materials, and post-processing the obtained reaction product to obtain CH2Cl-containing CMPPS resin; and adding a solvent to the obtained CMPPS resin to swell the CMPPS resin, adding a catalyst and a functionalized monomer, heating and reacting above materials, and post-processing the obtained reaction product to obtain the final product polyphenylene sulfide-based adsorption separation resin. Functional groups comprising a thienyl group, a 3-aminopyridyl group and a mercapto group, introduced to the invention, have good coordination adsorption ability to heavy metal ions, and the functional groups contain N and S hetero atoms, have small relative molecular mass, and can easily coordinate with the heavy metal ions, so an excellent adsorption purpose can be reached.

The invention discloses a block copolymer anion-exchange membrane for a fuel battery and a preparation method of the block copolymer anion-exchange membrane, and relates to an alkaline fuel battery. The molecular structure of the block copolymer anion-exchange membrane comprises a hydrophilic segment containing a phenolphthalein side group and a hydrophobic segment containing a benzonitrile structure. The preparation method comprises the following steps: (1) synthesizing the hydrophilic segment; (2) synthesizing the hydrophobic segment; (3) synthesizing a block copolymer; (4) synthesizing a bromomethylated block copolymer; and (5) preparing the block copolymer anion-exchange membrane. In the preparation process, a chloromethyl ether reagent is not used, and a phenolphthalein side group structure is introduced into the hydrophilic segment of the membrane and a strong-polarity nitrile group structure is introduced into the hydrophobic segment of the membrane by virtue of molecular design to ensure that the membrane has the characteristics of developed ion transport passage, high water content and low swelling capacity, and shows relatively high ionic conductivity and relatively good fuel battery performance.

The invention relates to a preparation method of chlorfenapyr, wherein, 4-bromine-2-(4-chlorphenyl)-5-trifluoromethyl pyrrole-3-nitrile and chloromethyl ethers are taken as raw material, alkali carbonate or organic amine is taken as acid-binding agents, and esters are taken as reaction solvent so as to prepare chlorfenapyr. The preparation method adopts ester solvent, reduces the treatment difficulty of waste water in the later period, lowers the manufacturing cost greatly, and reduces the environmental protection treatment pressure; the manufacturing cost is 20 percent lower than the diethoxymethane technology and is 10 percent lower than the ketones solvent technology; the wastewater quantity is only about 10 percent of the diethoxymethane technology and is about 25 percent of the ketones solvent technology; and unforeseen benefits can be achieved by compared with the traditional ketones solvent.

The invention relates to a synthetic method for chelate adsorbing resin suitable for heavy oil wastewater. The method comprises the following steps: adding an initiator in an oil phase, stirring the initiator to fully dissolve, adding the oil phase to a water phase in a stirring state, heating the temperature to 60-75 DEG C and insulating for 8-10 hours, heating to the temperature of 80-90 DEG C and insulating for 14-16 hours, cooling to obtain polystyrene series white ball, mixing the polystyrene series white ball and chloromethyl ether for chloromethylation reaction to obtain polystyrene series chlorine ball, mixing the polystyrene series chlorine ball and acetate phthalimide for esteryl reaction to obtain polystyrene series ester ball, mixing the polystyrene series ester ball and liquid alkali for hydrolysis reaction to obtain polystyrene series amine ball, mixing the polystyrene series amine ball, liquid alkali and chloroacetic acid for chelating reaction to obtain the chelate adsorbing resin suitable for the heavy oil wastewater. The chelate adsorbing resin suitable for heavy oil wastewater has good organic matter pollution resistance performance, and can be taken as secondary softening to prevent ions leakage in the heavy oil wastewater water quality.

The invention discloses a preparation method of a photocurable phosphorylcholine polymer, comprising the following steps: Step 1, carrying out free radical polymerization on a styrene monomer and a vinyl monomer containing a phosphorylcholine group under the action of an initiator so as to obtain a phosphorylcholine polymer containing phenyl ring; Step 2, mixing zinc chloride, chloromethyl ether and the phosphorylcholine polymer containing phenyl ring to carry out chloromethylation so as to obtain a chloromethylated phosphorylcholine polymer; and Step 3, carrying out nucleophilic substitution on the chloromethylated phosphorylcholine polymer by the use of sodium azide under the alkaline condition so as to obtain the photocurable phosphorylcholine polymer. The preparation method is simple and the conditions are mild. The invention provides a new approach to obtaining of the photocurable phosphorylcholine polymer. The invention is of great academical significance for modification of biocompatibility of biological materials. The prepared photocurable phosphorylcholine polymer will have a wide application prospect in fields of material implantation in vivo, tissue engineering, drug sustained release and biosensor, etc.

The invention discloses a modification method of a polystyrene resin for adsorbing flavones, which comprises the following steps: adding the polystyrene resin and chloromethyl ether into a three-neck flask which is provided with a stirrer, a thermometer and a reflux condenser, carrying out chloromethylation reaction under the action of a catalyst zinc chloride, carrying out vacuum filtration on the chloromethylation resin obtained by reaction, separating from the reaction solution, cleaning with ethanol, and swelling; and adding a chloromethylated resin and an amino reagent methylamine into the three-neck flask which is provided with the stirrer, thermometer and reflux condenser, and heating in a water bath to 45 DEG C to react for 12 hours, thereby obtaining the amino modified resin. When the modified resin is used for extracting total flavones in the ethanol extract, the adsorption capacity of every gram of modified resin reaches 58.776mg. The modification method has the advantages of mild reaction conditions, high practicality and the like, and is widely applicable to the polystyrene resin.

The invention discloses a preparation method of alcohol-soluble quaternary amine type or tertiary amine type anion exchange resin. The preparation method of the alcohol-soluble quaternary amine type or tertiary amine type anion exchange resin comprises the following steps: taking a linear poly(styrene-ethylene) alternating copolymer as a raw material, completely dissolving the linear poly(styrene-ethylene) alternating copolymer into halogenated hydrocarbon, then adding an industrial chloromethyl ether solution dissolved with a catalyst, and carrying out homogeneous-phase chloromethylation reaction; then enabling a reaction product to pass through a stainless steel high-pressure nozzle; extruding the reaction product into water which contains a dispersing agent and sodium hydroxide; rapidlydispersing into a suspension system by using a stirring paddle with a cutting function; carrying out reduced pressure distillation to recycle the halogenated hydrocarbon; after filtering and drying the suspension particles, washing the suspension particles with water thoroughly, and adding an organic amines aqueous solution to react; filtering and drying residual reaction liquid, adding diluted hydrochloric acid to neutralize, filtering and drying, and then washing for multiple times by using deionized water; and finally filtering and drying, and blowing and drying the solid particles to obtain an alcohol-soluble quaternary amine type or tertiary amine type anion exchange resin product. Quaternary amine or tertiary amine groups in the product prepared by the method are distributed uniformly, and can be completely dissolved in low-toxicity organic alcohol.

The invention provides a preparation method of an ion exchange membrane used in a vanadium battery. The preparation method comprises the steps of dissolving sulfonated polycondensate and a sulfonated addition polymer in a first solvent; pouring at 60-80 DEG C for membrane formation so as to obtain the ion exchange membrane used in the vanadium battery. Compared with the prior art, the ion exchange membrane prepared by the method abovementioned has the characteristics of a polymer imidazole salt ionic liquid membrane and a polycondensate membrane; the polymer imidazole salt ionic liquid membrane and the polycondensate membrane are cross-linked through an ionic bond to further improve the chemical stability and mechanical property thereof; and the ionic bond is good for formation of an ionic channel, so that the ionic conductivity thereof is also ensured while good mechanical property and good chemical stability are ensured. According to the preparation method of the ion exchange membrane used in the vanadium battery, use of chloromethyl ether and concentrated sulfuric acid is avoided, and damage to a human body and the environment is reduced. The prepared ion exchange membrane used in the vanadium battery has relatively low vanadium ion permeability, relatively high ionic conductance and chemical stability and relatively good mechanical property. In addition, the preparation method of the membrane is simple in preparation and low in price, and has low requirements on equipment.

The invention discloses a secondary crosslinking post-modification method of a polymeric adsorbent. The secondary crosslinking post-modification method comprises the following steps: epoxying and activating a residual double bond on a poly styrene-co-divinyl benzene resin, forming a polyhydroxy surface through hydrolysis, and enabling a hydroxide radical and an epoxy group to perform secondary crosslinking. The hydrophobic polymeric adsorbent forms the polyhydroxy surface through activation and hydrolysis, the hydrophily is improved, the modified functional group is also provided, and the polymeric adsorbent does not need to be modified on a benzene ring. The epoxy chloropropane is used for secondary crosslinking to obtain a poly styrene-co-divinyl benzene resin microsphere with higher strength and more stable space structure. The chloromethyl ether with strong cancerogen or the expensive vinylbenzyl chloride is not used, and the cost is relatively low. The invention further discloses the polymeric adsorbent prepared through the secondary crosslinking post-modification method and a blood perfusion device using the polymeric adsorbent.

The invention discloses an industrial preparation method of sevoflurane. The method comprises the following steps: adding chloromethyl ether and alkali metal fluoride to a solvent, uniformly stirring and heating for a reflux reaction; after the reaction, cooling a reaction liquid to be less than 20 DEG C and filtering, combining a filtrate with reaction residual liquor and distilling under normal pressure; collecting fraction less than 80 DEG C so as to obtain crude sevoflurane, and rectifying so as to obtain a finished sevoflurane product. By optimizing the crude sevoflurane preparing step, namely adding a filtering and impurity removing step after fluoridation reaction, the industrial preparation method disclosed by the invention can be used for relieving a side reaction during distilling and avoiding the generation of some impurities, and especially impurities similar to the sevoflurane in retention time, so that rectifying difficulty is reduced, rectifying time is reduced and product quality is guaranteed; the content of the finished sevoflurane product can reach 99.999%, so that manpower and material resources can be saved and product yield can be improved to 92.4%; and meanwhile, generated cauldron bottom residue can be recycled, so that the industrial preparation method can be used for further improving yield and reducing cost, and the preparation method is more conducive to industrial production.