24 results about "Haloacetic acids" patented technology

The invention discloses a method for electrocatalytic hydrogenation dehalogenation of haloacetic acid or halomethane in a water body, which is characterized in that a conductive material of which the surface is modified with ruthenium or platinum is used as a catalytic cathode, water is used as a hydrogen source, and the haloacetic acid or halomethane in the water body is subjected to electrochemical hydrogenation dehalogenation to form acetic acid or methane. The price of precious metal in the catalytic cathode is lower, and the unit price of ruthenium is far lower than that of palladium and rhodium; and compared with a palladium-modified catalytic cathode, the dechlorination selectivity is higher, and the selectivity of hydrodechlorination of trichloroacetic acid into acetic acid in a water body is improved by 11.7%.

The invention discloses a method for catalytically hydrogenating and dehalogenating haloacetic acid or halomethane in a water body, which comprises the following steps of: catalytically hydrogenating and dehalogenating haloacetic acid or halomethane in the water body into acetic acid or methane by taking a ruthenium or platinum-containing material as a catalyst and hydrogen as a reducing agent; the noble metal in the catalyst is cheaper, and the unit price of ruthenium is far lower than that of palladium and rhodium; according to the method, the dehalogenation selectivity is higher, and compared with a palladium catalyst, the selectivity of hydrodechlorinating trichloroacetic acid in a water body into acetic acid is improved by 10.3%-15.5%; and the selectivity of trichloromethane hydrodechlorination into methane is improved by 8.6%-10.0%.

The present invention provides an industrially advantageous method for producing sulfone derivatives useful as herbicides and intermediates thereof.

The present invention provides an industrially desirable production method for a sulfone derivative that is useful as a herbicide, and an intermediate thereof.

The invention relates to a method for determining haloacetic acid in different water qualities through liquid-liquid extraction derivative gas chromatography, and belongs to the technical field of water quality analysis and detection.According to the method, at least one gas chromatograph, a sampling bottle with a plug, an extraction bottle with a plug, a derivative bottle with a plug, a microsyringe, a vortex oscillator and a heating block are used for determination of the method, the method mainly comprises the test steps of water sample collection, water sample extraction, water sample derivation, water sample determination and optimization detection, wherein optimization items mainly comprise a strong electrolyte, a volume ratio of sulfuric acid to methanol, instrument working conditions and the like. The method realizes detection of haloacetic acid in different water qualities, is high in sensitivity, good in accuracy and high in precision, and is suitable for drinking water, seawater, lake water, industrial wastewater and the like.

The present invention relates to an ion exchange material for use as a stationary phase for separating anions, preferably haloacetic acids, in an analytical or preparative separation process. The material comprises: - a polymer support; - an acid group directly bonded to the surface of the polymer support, the acid group being selected from the group consisting of sulfonic acid groups, carboxylic acid groups or combinations thereof; - a polymer layer covalently bonded to the surface of the polymer support, the polymer layer containing an anion exchange group. The amount of the acid group ranges from 0.05 to 1.05 mmol / g, preferably from 0.1 to 0.9 mmol / g, particularly preferably from 0.16 to 0.85 mmol / g of the polymer support. The acid group and the anion exchange group are preferably spatially separated by at least 10 nm, preferably at least 50 nm, most preferably at least 100 nm via the polymer layer. The present invention also relates to a method for producing the ion exchange material, a chromatography column having the ion exchange material, a method for chromatographic separation of an analyte and the use of the ion exchange material.

The invention discloses an application of a CuxO (at) mC material in electrochemical dechlorination of chlorinated disinfection by-products. The application comprises the following steps: S1, obtaining a metal Cu organic framework material, and carbonizing to prepare the CuxO (at) mC material; and S2, the CuxO (at) mC material is added into an aqueous solution containing haloacetic acid, and electrolysis dehalogenation is conducted through an electrolytic tank device. The electrolytic tank device takes a CuxO (at) mC / metal electrode as a cathode and takes a graphite electrode as an anode. The CuxO (at) mC / metal electrode can be used for electrochemical dechlorination of chlorinated disinfection by-products. The method for dechlorinating the target object has the advantages of high targeting property, high dechlorinating efficiency, low cost, simple structure, safety and stability, the dissolution rate of metal copper ions in the using process is extremely low, secondary pollution is not caused, and safe control over chlorinated disinfection by-products in water is achieved.

Process for the preparation of menthanecarbaldehyde, comprising the following steps: - Reaction of menthone with a haloacetic acid ester of the formula XCH2COOR, with X = chlorine or bromine and R = methyl or ethyl, to form the ester of menthaneglycitic acid, - Reaction of the ester of menthaneglycitic acid thus prepared to menthanecarbaldehyde, wherein, in order to react the prepared ester of menthaneglycitic acid to menthanecarbaldehyde, the ester is reacted with a strong base such that the ester is hydrolyzed, and the hydrolysis product, as menthaneglycitic acid or as a salt of menthaneglycitic acid, is decarboxylated after intermediate isolation or without intermediate isolation.

The invention relates to an ion exchange material for use as a stationary phase in the analysis or preparation of separation processes, in particular for the separation of anions, preferably haloacetic acid. The invention relates to a material comprising:-a polymeric support,-an acid group directly attached to the surface of the polymeric support, said acid group being selected from the group consisting of sulfonic acid groups, carboxylic acid groups or combinations thereof,-a polymeric layer covalently attached to the surface of the polymeric support, said polymeric layer comprising anion exchange groups. The amount of acid groups is in the range of from 0.05 to 1.05 mmol / g of polymer support, preferably from 0.1 to 0.9 mmol / g, particularly preferably from 0.16 to 0.85 mmol / g. The acid groups and anion exchange groups are spatially separated, preferably at least 10 nm, preferably at least 50 nm, most preferably at least 100 nm, by the polymer layer. The invention also relates to a method for manufacturing the ion exchange material, a chromatographic column with the ion exchange material, a method for chromatographic separation of an analyte and the use of the ion exchange material.

The invention discloses an antibacterial thermosetting coating / plastic system derived from phenoxy resin and capable of being degraded to original resin in a weak base mode, which is prepared by the following steps: dissolving phenoxy resin and haloacetic acid in a water-carrying agent, reacting at 80-130 DEG C for 1-12 hours, continuously separating generated water in the process, and after the reaction is finished, evaporating and precipitating to obtain the antibacterial thermosetting coating / plastic system. The halogenated acetic acid esterified phenoxy resin is obtained; mixing the obtained halogenated acetic acid esterified phenoxy resin with a poly-tertiary amine compound, and curing in a mold at 40-100 DEG C for 1-10 hours to obtain a thermosetting polymer; compared with the traditional phenoxy resin, the material prepared by the invention has the characteristics of organic solvent resistance, intrinsic antibiosis, degradability and the like, and the composite characteristic can enrich the application scene and the application range of the phenoxy resin.

The invention discloses a novel graphene oxide adsorption film and application thereof, and belongs to the technical field of film separation. Comprising the following steps: mixing a graphene oxide ethanol dispersion liquid with an RCC3 molecular cage aqueous solution, and carrying out ultrasonic dispersion and constant-temperature stirring reaction, so that a secondary amine group in a molecular cage and an epoxy group on the surface of graphene oxide are subjected to a nucleophilic ring-opening reaction, and covalent linkage is realized; and then coating the functionalized suspension on a porous membrane substrate to form an adsorption layer, carrying out protonation treatment through vacuum filtration of a hydrochloric acid solution, and finally drying and curing to obtain a finished product. The membrane can efficiently and selectively adsorb haloacetic acid disinfection byproducts (the rejection rate is greater than or equal to 90%) in drinking water, meanwhile, beneficial inorganic salt ions such as calcium, magnesium and sodium are allowed to permeate (the transmittance is greater than or equal to 80%), and high flux, high selectivity and anti-swelling stability are effectively considered. The preparation process is simple and controllable, is suitable for waterworks, underground water purification, industrial wastewater treatment and other scenes, and has significant industrialization potential.

This invention discloses a method for the electrocatalytic hydrogenation dehalogenation of haloacetic acids or halomethanes in water. A conductive material surface-modified with ruthenium or platinum is used as the catalytic cathode, and water is used as the hydrogen source to electrochemically hydrogenate and dehalogenate haloacetic acids or halomethanes in water into acetic acid or methane. The precious metals in the catalytic cathode of this invention are cheaper; the unit price of ruthenium is much lower than that of palladium and rhodium. Compared with palladium-modified catalytic cathodes, the dechlorination selectivity is higher, with an 11.7% increase in the selectivity for the hydrogenation and dechlorination of trichloroacetic acid in water to acetic acid.

The application relates to the technical field of organic synthesis and pharmaceutical intermediates, in particular to a (2S, 4R)-1-Fmoc-4-(O-allyloxycarbonylmethyl)-proline and a synthesis method thereof. The method comprises the following steps: performing silicon-based protection on (2S, 4R)-4-hydroxypyrrolidine-2-carboxylic acid; refluxing and dehydrating the alkyl aldehyde to construct a tetrahydropyrrolooxazolone bicyclic intermediate; after the silicon-based group is removed, etherification is performed with 2-haloacetic acid allyl ester under strong alkali to introduce a side chain; and finally, acid ring-opening hydrolysis and Fmoc protection are performed to obtain the target product. The amino group and the carboxyl group are protected in situ by constructing a bicyclic structure, the sensitive allyloxycarbonylmethyl side chain is introduced in a non-water system, and the hydrolysis of the side chain ester bond is effectively avoided. The product prepared by the application has high purity and good stereoselectivity, and an efficient and low-cost industrialization approach is provided for the synthesis of high-performance polypeptide blocks.

The invention discloses a method for monitoring the concentration of a water body disinfection by-product DBPs based on electron donating ability, and belongs to the technical field of environmental engineering.The method comprises the steps that S1, a water body sample is collected, first pretreatment is conducted, and the EDC value is measured through an ABTS + free radical reduction decolorization method; s2, carrying out second pretreatment on the water body sample subjected to the first pretreatment, and measuring the concentrations of trihalomethane and haloacetic acid in the water body sample by utilizing a gas chromatographic method; s3, by taking the EDC value as an independent variable and the trihalomethane concentration and the haloacetic acid concentration as dependent variables, establishing a first prediction model for predicting the trihalomethane concentration based on the EDC value and a second prediction model for predicting the haloacetic acid concentration based on the EDC value; and S4, predicting the concentration of trihalomethane and the concentration of haloacetic acid by using the first prediction model and the second prediction model based on the EDC value of the target to-be-detected water body sample. The method solves the problems that a traditional DBPs detection method is long in time consumption and complex in operation.

The invention discloses a method for rapidly determining haloacetic acid and oxyhalide, and belongs to the technical field of water quality analysis and detection. The method for rapidly determining haloacetic acid and oxyhalide comprises the following steps: S1, detecting a water sample to be detected by adopting liquid chromatography-mass spectrometry; wherein acetonitrile is added into the water sample to be detected, and the volume fraction of the acetonitrile is 15-50%; the chromatographic column is an AG18 chromatographic column; the phase A of the mobile phase is an ammonia water solution with the concentration of 0.3-3 mol / L; the phase B of the mobile phase is acetonitrile or methanol; the volume fraction of the phase A in the mobile phase is 5-50%; and S2, substituting the detected peak area of the substance into the standard working curve to calculate the concentration of the target substance.

The invention discloses application of haloacetic acid in enrichment of small molecule nucleic acid in a biological sample, and belongs to the technical field of molecular biology. According to the application, the haloacetic acid is utilized to enrich the micromolecular nucleic acid in the liquid biological sample, so that not only can the influence of interferents be eliminated, but also the enriched micromolecular nucleic acid sample can be stably stored at room temperature, and the micromolecular nucleic acid sample can be directly subjected to amplification detection without being extracted, so that the application value is very important.

The invention provides a method for simultaneously detecting eight haloacetic acid disinfection byproducts in human urine. The method comprises the following specific steps: S1, preparing a mixed standard solution; s2, preparing an internal standard solution; s3, drawing a standard working curve; s4, sample pretreatment: putting urine into a 15mL centrifugal tube, sequentially adding concentrated sulfuric acid and anhydrous sodium sulfate, uniformly mixing, adding an extracting agent MTBE containing an internal standard, vigorously oscillating, centrifuging, putting an upper organic phase into the 15mL centrifugal tube, adding acidified methanol, uniformly mixing by vortex, and carrying out esterification reaction in a water bath at 50 DEG C for 2 hours; after derivation is finished, taking out the centrifugal tube, placing the centrifugal tube in a refrigerator for cooling, adding an anhydrous sodium sulfate solution with the concentration of 150g / L, uniformly shaking to terminate esterification reaction, standing for layering, taking an upper-layer organic phase, adding an isometric saturated sodium bicarbonate solution, uniformly mixing, standing, transferring the upper-layer organic phase into a small sample injection bottle, and standing for on-machine detection. The method has the advantages of being high in sensitivity, small in sample usage amount and high in practicability, and can be used for conventional biological monitoring of HAAs of people.

The invention discloses a method for removing haloacetic acid in water by using a Fe-C nano material. The method comprises the following steps: S1, obtaining a metal Fe organic framework material; s2, carbonizing the metal Fe organic framework material in a tubular furnace at the high temperature of 800 DEG C to obtain a Fe-C nano material; and S3, adding the Fe-coated C nano material into the water to be treated in the electrolytic tank device, and carrying out electrolytic dehalogenation on the haloacetic acid. The electrolytic tank device takes a steel electrode as a cathode and a graphite electrode as an anode or takes a Fe-coated C / magnetic electrode as the cathode and takes the graphite electrode as the anode. The Fe-coated C nano material and the Fe-coated C / modified magnetic electrode can be used for acid dechlorination of halogenated organic matters in electrochemical water treatment, and have the characteristics of targeted dehalogenation, high dehalogenation efficiency, low cost, simple preparation method, safety and stability, and the Fe-coated C / modified magnetic electrode abandons an adhesive in a nano material modified electrode method.

The invention discloses a preparation method of a halide perovskite thin film, which comprises the following steps of: dissolving monovalent cation acetate such as cesium / rubidium / formamidine acetate, divalent metal acetate such as lead / tin acetate and water-soluble acetate such as haloacetic acid by adopting water as a solvent, coating the solution on a substrate by adopting a spin coating, blade coating or spray coating manner, and drying to obtain the halide perovskite thin film. And heating and annealing to form the halide perovskite thin film. The prepared perovskite thin film can be applied to the fields of perovskite solar cells, photoelectric detectors and the like. Compared with a previously reported method for preparing the perovskite thin film through an aqueous solution, the method has the advantages that the step of synthesizing raw materials such as lead iodide, cesium iodide and iodoformamidine is omitted, and haloid acids such as hydriodic acid and hydrobromic acid are prevented from being used as halogen sources. Acetate is used as a raw material, water is used as a solvent, the preparation process is remarkably simplified, and the economic effect is huge.

The invention discloses a method for determining haloacetic acid and oxyhalide, and belongs to the technical field of water quality analysis and detection. The method for determining haloacetic acid and oxyhalide comprises the following steps: S1, detecting a water sample to be detected by adopting liquid chromatography-mass spectrometry; wherein the chromatographic column is an AG18 chromatographic column; the phase A of the mobile phase is an ammonia water solution with the concentration of 0.3-3 mol / L; the phase B of the mobile phase is acetonitrile or methanol; the volume fraction of the phase A in the mobile phase is 5-50%; and S2, substituting the detected peak area of the substance into the standard working curve to calculate the concentration of the target substance.

The invention relates to the technical field of organic synthesis and medical intermediates, in particular to (2S, 4R)-1-Fmoc-4-(O-allyloxycarbonyl methyl)-proline and a synthesis method thereof. The method comprises the following steps: carrying out silicon group protection on (2S, 4R)-4-hydroxypyrrolidine-2-carboxylic acid; carrying out reflux dehydration on the tetrahydropyrrolo-oxazolone and alkyl aldehyde to construct a tetrahydropyrrolo-oxazolone bicyclic intermediate; after removing a silicon base, etherifying with 2-halogenated allyl acetate under strong base to introduce a side chain; and finally, carrying out acidic ring-opening hydrolysis and Fmoc protection to obtain a target product. According to the preparation method, amino and carboxyl are subjected to in-situ protection by constructing a bicyclic structure, and a sensitive allyloxycarbonyl methyl side chain is introduced by utilizing an anhydrous non-aqueous phase system, so that hydrolysis of ester bonds of the side chain is effectively avoided. The prepared product is high in purity and good in stereoselectivity, and an efficient and low-cost industrial approach is provided for synthesis of high-performance polypeptide building blocks.

The application discloses a method for electrocatalytic hydrogenation dehalogenation of haloacetic acid in water by using a ruthenium / nickel hydroxide catalyst, wherein a conductive material with a surface modified ruthenium / nickel hydroxide is used as a catalytic cathode, the cathode potential is-0.3~‑1.0 V vs. silver / silver chloride reference electrode, and water is used as a hydrogen source, so that the haloacetic acid in water is electrochemically hydrogenated and dehalogenated into acetic acid. Under the condition of the same Ru loading, the catalytic activity of Ru / Ni(OH)2 is higher, the conversion rate of trichloroacetic acid is 9% higher, the acetic acid yield is 14% higher, and the acetic acid selectivity is 5% higher.

The invention discloses a water-resistant quaternary ammonium salt / epoxy thermosetting material and a preparation method thereof, comprising the following steps: adding epoxy resin and halogenated acetic acid into a reactor, stirring and reacting at 100°C to 150°C for 1 to 30 hours; extracting, drying, decompressing and distilling to obtain a halogenated acetic acid ester epoxy resin after the reaction is completed; mixing a polyacrylate compound with a methyl-free dialkylamine for reaction; after the reaction is completed, decompressing and distilling to obtain a tri(dialkylamine) compound curing agent; uniformly mixing the halogenated acetic acid ester epoxy resin obtained in step (1) and the tri(dialkylamine) compound curing agent obtained in step (2), putting the mixture into a mold for curing, and obtaining the water-resistant quaternary ammonium salt / epoxy thermosetting material. The synthesis of the water-resistant quaternary ammonium salt / epoxy thermosetting system has the characteristics of simple process, high conversion rate, high yield, etc., and is resistant to water swelling and has a bactericidal effect.

The present invention relates to a gas chromatography-mass spectrometry analysis method for haloacetic acids in drinking water, belonging to the technical field of analytical chemistry. Compared with the prior art, the present invention uses GC-MS to establish a quantitative method for haloacetic acids in drinking water, overcomes the drawbacks of the standard method provided by the US Environmental Protection Agency (USEPA, 552.3), the supporting method of the "Drinking Water Quality Standard" in China (GB / T 5749-2006), and the diazomethane derivatization method, realizes one-step liquid-liquid extraction, can be directly analyzed quantitatively after simple derivatization, and obtains high sensitivity, high spiked recovery rate, low method detection limit, and low quantification limit. The method of the present invention can efficiently, rapidly and accurately determine haloacetic acids in drinking water.