33 results about "Nitroxide radical" patented technology

A method for continuously producing oxetane methyl methacrylate by transesterification, which utilizes dibutyl tin oxide, methyl methacrylate and 4-hydroxy-2,2,6,6-tetramethylpiperidine-1-oxyl radical to prepare a catalyst; methyl methacrylate is subjected to transesterification with 3-ethyl-3-oxetanemethanol, a polymerization inhibitor tetramethylpiperidine nitroxide phosphite triester and the catalyst to obtain a transesterification reaction liquid; the transesterification reaction liquid is subjected to vacuum rectification in a transesterification reactor, after recovering methyl methacrylate and 3-ethyl-3-oxetanemethanol, vacuum rectification is continued to obtain oxetane methyl methacrylate. The advantage is that the process is simple and reasonable, not only high in conversion rate and selectivity, but also high in purity, low in color and acid value of the obtained product, friendly to the environment and fully capable of meeting the application requirements in high-end fields.

Provided is a polarizing plate in which the decrease in transmittance in a high-temperature environment is suppressed. A polarizing plate has a polarizing element in which a dichroic dye is adsorbed and oriented in a polyvinyl alcohol-based resin layer, a first transparent protective film laminated on one face of the polarizing element, and a second transparent protective film laminated on the other face of the polarizing element, the polarizing element and the transparent protective films being bonded with a first adhesive layer formed from a first adhesive containing a first compound, the polarizing element and the second transparent protective film being bonded with a second adhesive layer formed from a second adhesive containing a second compound, the first compound being at least one selected from the group consisting of urea, a urea derivative, thiourea, and a thiourea derivative, and the second compound being a compound having a nitroxyl radical or a nitroxide radical.

This invention relates to a high-efficiency outdoor flame retardant additive, its preparation method, and its application, belonging to the field of polymer material additives technology. This high-efficiency flame retardant additive has N,N'-di(3-aminopropyl)-1,2-ethylenediamine as its main chain, linked with dialkoxy-monochlorotriazine, containing six N-cyclohexyloxy hindered amine groups, with a purity ≥99.5% and a total yield ≥80%. It is prepared from 2,2,6,6-tetramethylpiperidone nitroxide radical, cyclohexane, etc., via N-cyclohexyloxylation, reductive amination, N-acylation, and nucleophilic substitution reactions. Adding 0.5~3.0 wt% of this stabilizer to polypropylene materials can impart UL-94 VTM-0 flame retardancy and excellent photothermal stability. Furthermore, the preparation process is low-cost and environmentally friendly, solving the technical problems of easy deactivation of hindered amines, functional separation of additives, and low yield in traditional synthesis processes. It is suitable for polypropylene fibers, films, nonwoven fabrics, and other polyolefin products.

The invention discloses a preparation method of sulfoalkyl (methyl) acrylate, which is characterized in that (methyl) acrylic acid and hydroxyalkyl sulfonic acid are used as raw materials, an acidic resin catalyst is adopted, and the sulfoalkyl (methyl) acrylate is prepared by reaction in the presence of a solvent and a compound polymerization inhibitor, the compound polymerization inhibitor is a combination of a phenolic compound and at least one of the following compounds (A)-(D): (A) a quinone compound; (B) a nitroxide radical compound; (C) an inorganic salt compound; and (D) copper N, N-di-n-butyl dithiocarbamate. By using the method, the polymerization side reaction in the reaction process can be effectively inhibited, and the method has the advantages of short reaction time, simple post-treatment and low content of the hydroxyalkyl sulfonic acid dimer in the product.

This invention discloses a fluoropiperidine nitroxide radical derivative, a positive electrode electrolyte containing the same, and its applications. The fluoropiperidine nitroxide radical derivative is a compound represented by Formula I. The piperidine nitroxide radical derivative of this invention exhibits high stability and high solubility as a positive electrode active material in organic flow batteries, showing promising application prospects.

This application provides a semiconductive shielding material, its preparation method and application, and cables, belonging to the field of cable material technology. The semiconductive shielding material comprises the following components in parts by weight: 50-65 parts matrix resin, 25-35 parts conductive carbon black, 5-10 parts acrylate-terminated polyalphaolefin, 1-3 parts antioxidant, 1-2 parts dispersant, 0.1-1 parts thermally triggered free radical stabilizer, and 0.5-2 parts crosslinking agent; wherein the thermally triggered free radical stabilizer includes nitroxide free radical compounds. The combined use of these components significantly improves the scorching resistance, crosslinking density, and mechanical properties of the semiconductive shielding material, exhibits excellent processability, and significantly enhances the safety and service life of cables. The introduction of acrylate-terminated polyalphaolefin and the thermally triggered free radical stabilizer is beneficial for improving melt flowability and inhibiting early crosslinking during processing, and for forming a highly dense three-dimensional network structure during the crosslinking stage.

The invention discloses a dimerization nitroxide free radical type flow battery positive electrode material as well as a preparation method and application thereof. The preparation method comprises the following steps: firstly, carrying out Favorskii rearrangement reaction and extraction on 4-oxo TEMPO, an iodine solution and potassium hydroxide dissolved in ammonia water to obtain pyrrole amide, preparing pyrrole carboxylic acid by utilizing the pyrrole amide, preparing pyrrole dimethyl amide by utilizing the pyrrole carboxylic acid, and then preparing the pyrrole dimethyl amide by utilizing the pyrrole dimethyl amide. Dissolving pyrrole dimethyl amide, adding a lithium aluminum hydride solution, carrying out a reduction reaction to prepare pyrrole methylene dimethyl tertiary amine, and finally carrying out a substitution reaction on the pyrrole methylene dimethyl tertiary amine and the dimer bridging intermediate to prepare the positive electrode material disclosed by the invention. The preparation method is simple in synthesis process and relatively high in reaction yield, and the problem of capacity fading caused by transmembrane permeation of the positive electrode material of the flow battery can be effectively inhibited.

The invention discloses a UV (ultraviolet) curing hot-melt pressure-sensitive adhesive with high cohesive strength. The UV curing hot-melt pressure-sensitive adhesive comprises butyl acrylate, 2-ethylhexyl acrylate, acrylic acid, a benzophenone derivative containing carbon-carbon double bonds, a solvent, an initiator BPO (benzoyl peroxide) and a nitroxide free radical TEMPO. Butyl acrylate and 2-ethylhexyl acrylate are used as main monomers, acrylic acid is used as a functional monomer, the inherent viscosity characteristic of an acrylic pressure-sensitive adhesive is reserved, the initial binding force with a base material is ensured, and a benzophenone derivative containing carbon-carbon double bonds has the dual functions of photo-initiation activity and cross-linking reaction point positions and can be copolymerized with the monomers to realize UV cross-linking; the nitroxide free radical TEMPO captures free radicals at low temperature and releases free radicals at high temperature, so that the molecular weight distribution is uniform, the initiator BPO and the solvent synergistically guarantee stable polymerization, the product is low in melt viscosity at 130-150 DEG C, small molecular chain segments are few, the molecular weight is large under the combined action of the three, and the hot-melt coating is realized while the cohesion strength is high.

The invention discloses a method for photocatalytic synthesis of a free radical initiator alkoxy amine, which comprises the following steps: mixing a compound containing nitroxide free radicals, an organic photocatalyst, peroxide and an organic solvent, and reacting at normal temperature under ultraviolet irradiation; removing the organic solvent, and purifying to obtain alkoxy amine; wherein the organic solvent is selected from at least one of aromatic hydrocarbon compounds, aromatic heterocyclic compounds and ether compounds. According to the method, the low-cost and high-efficiency synthesis of the alkoxy amine is realized under the reaction conditions of normal temperature and ultraviolet light by using a synthesis strategy that an organic photocatalyst and peroxide are used as oxidants. The synthesis conditions are mixed, low temperature is not needed, the method is insensitive to water and oxygen, the light source is more friendly, the operation is simple, and the experiment and industrial amplification difficulty is greatly reduced; a metal photocatalyst is not needed, the bottleneck of yield and cost is broken through, the technical problem of low yield of an existing photocatalysis strategy theory is solved, and the yield can reach 56-91%.

The present application relates to the chemical technology field, specifically to a kind of preparation method of high-purity o-vanillin.The method uses o-methoxyphenylamine as starting material, with chloral hydrate and hydroxylamine hydrochloride is condensed, hydroxylamine oximation reaction, and cyclization reaction is carried out under strong acid condition, and compound 2 is generated;Compound 2 is oxidized under strong base condition, and compound 3 is generated;Compound 3 is esterified with primary alcohol to generate corresponding ester, and then reduction hydrogenation reaction is carried out under the action of strong reducing agent, and compound 4 is generated;Compound 4 is reacted with oxidizing agent in the presence of nitroxyl radical catalyst, and compound 5 is generated;Compound 5 carries out diazotization hydrolysis reaction, and o-vanillin is generated.The method avoids the problem of regioselectivity of traditional formylation reaction through specific reaction sequence, eliminates the generation of isomer impurities from the source, realizes the efficient, environmentally friendly, economic synthesis of high-purity o-vanillin, and provides high-quality raw material guarantee for downstream pharmaceutical.

The invention discloses a pyrrolidine nitroxide free radical connected with a hydrophilic group through a carbon chain, a preparation method of the pyrrolidine nitroxide free radical and application of the pyrrolidine nitroxide free radical in a flow battery. The positive electrode of the aqueous organic flow battery comprises a positive electrode electroactive material and an aqueous solution supporting electrolyte; the positive electrode electrolyte active substance is pyrrolidine nitroxide free radical connected with a hydrophilic group through a carbon chain; and the supporting electrolyte is a single-component or multi-component chloride ion inorganic salt. The hydrophilic group and the pyrrolidine nitroxide free radical are connected through the carbon chain, so that the problems of low water solubility and low stability of the existing pyrrolidine nitroxide free radical serving as a positive electrode electroactive material of the aqueous organic flow battery can be solved at the same time.

The application discloses a halogen-free phosphonate hindered piperidine ammonium salt ionic liquid flame retardant and a preparation method and application thereof, a flame-retardant polypropylene material and a preparation method, and belongs to the technical field of chemical synthesis. The preparation method of the halogen-free phosphonate hindered piperidine ammonium salt ionic liquid flame retardant comprises the following steps: performing a solvothermal reaction on di-ester phosphate and 4-amino hindered piperidine amine as raw materials, and then performing vacuum distillation to obtain the halogen-free phosphonate hindered piperidine ammonium salt ionic liquid flame retardant. That is, the halogen-free phosphonate hindered piperidine ammonium salt ionic liquid flame retardant is synthesized by a one-step method. The nitrogen and phosphorus synergistic effect is utilized to release organic phosphorus and nitrogen free radicals to capture gas phase free radicals during combustion, and the hindered piperidine amine is decomposed to generate non-combustible gas, thereby playing a role of heat absorption and combustible gas dilution. In daily use, the hindered piperidine amine can be converted into stable nitrogen-oxygen free radicals to play a catalytic anti-ultraviolet aging function, and the halogen-free phosphonate hindered piperidine ammonium salt ionic liquid flame retardant has the dual performance of high-efficiency flame retardation and anti-aging.

The application belongs to the field of organic synthesis and particularly relates to a preparation method of ortho-carboxybenzaldehyde. The method comprises the following steps: (a) ring-opening hydrolysis of a compound of formula (3) with a strong alkali solution to prepare a compound of formula (2) or a salt thereof; and (b) oxidation of the compound of formula (2) or the salt thereof with an oxidant in a solvent under the catalysis of a nitrogen-oxygen free radical to prepare a compound of formula (1) or a salt thereof. The ortho-carboxybenzaldehyde prepared by the method is an important intermediate for synthesis of antipyretic analgesics. The method solves the problems of environmental pollution and personnel injury and high energy consumption and cost in the prior art which generally uses bromine, chlorine and a large amount of toxic solvents and high-temperature reflux reaction, and initiatively provides a method for directly ring-opening hydrolysis under the action of a strong alkali and then oxidation in a homogeneous system to prepare ortho-carboxybenzaldehyde, which is simple and convenient to operate, safe and controllable, and suitable for large-scale industrial production.

The application belongs to the technical field of pharmaceutical chemistry, and particularly relates to a gentiopicroside nitroxide radical derivative as well as a preparation method and application thereof. A series of gentiopicroside nitroxide radical derivatives with specific structures are prepared and synthesized through a chemical process. The derivatives exhibit good in-vitro COX-2 enzyme inhibition activity and in-vitro ROS scavenging activity. In-vivo and in-vitro experimental results show that each derivative can effectively inhibit the release of inflammatory mediators and oxidative stress during inflammation, thereby more effectively inhibiting the progress of inflammation and protecting tissues, and the derivatives have a wide application prospect in the preparation of drugs with the efficacy of preventing, relieving or treating inflammation.

Provided are: a method for producing a nitroxide having excellent safety without using a peroxide such as hydrogen peroxide; and a curable composition having excellent curing temperature, curing speed and wettability.　A nitroxide is generated without using a peroxide by simultaneously irradiating a reactive compound with atmospheric-pressure, low-temperature plasma and ultrasonic waves, and a curable composition having excellent curing temperature, curing rate, and wettability can be obtained by constituting the curable composition using the reactive compound containing the nitroxide.

The application discloses a piperidine nitroxide radical derivative containing an ether chain and application thereof to a positive electrode material. The application provides a compound as shown in a formula I. The piperidine nitroxide radical derivative of the application exhibits a low cross-diffusion phenomenon as a positive electrode active material in an organic liquid flow battery, and excellent chemical and electrochemical stability, which jointly promotes the improvement of the cycle life of the organic liquid flow battery. The achievement enhances the practical application value of the organic active material, and promotes the development of a commercialization process.

To provide a highly safe method for producing nitroxides that does not use peroxides such as hydrogen peroxide, and to provide a curable composition with excellent curing temperature, curing speed, and wettability. [Solution] By simultaneously irradiating a reactive compound with atmospheric pressure low-temperature plasma and ultrasound, nitroxides are generated without using peroxides. By constructing a curable composition using the reactive compound containing these nitroxides, a curable composition with excellent curing temperature, curing speed, and wettability can be obtained.

The application belongs to the technical field of medicine and spice synthesis, and particularly relates to a synthesis method of trans-2-octenal. The synthesis method comprises the following steps: 1-octene-3-ol is subjected to isomerization reaction under the catalysis of 3,4-dinitrobenzoic acid to obtain a trans-2-octene-1-ol intermediate; and the trans-2-octene-1-ol is subjected to oxidation by interchloroiodobenzene, 4-hydroxy-TEMPO (4-hydroxy-2,2,6,6-tetramethylpiperidinooxy) and peroxoacetic acid to obtain the trans-2-octenal. The preparation method has mild reaction conditions, simple operation and does not need to use expensive reagents or catalysts.

A method for producing acetone glyceryl methacrylate via transesterification involves adding methyl methacrylate and glyceryl acetone, a polymerization inhibitor tetramethylpiperidine nitroxide radical triphosphite, and a catalyst calcium acetylacetonate or zinc acetylacetonate, to an esterification reactor. The reactor is stirred and heated to 103℃-107℃ for 3-6 hours. Heating is then stopped. By controlling the reflux ratio of the reflux device at the top of the esterification reactor, the temperature inside the reactor is maintained at 121-131.5℃, and the temperature at the top of the distillation column is maintained at 92-96℃. After esterification, vacuum distillation is performed to obtain acetone glyceryl methacrylate. The advantages are: continuous reaction, simple operation, use of an organotin catalyst that does not contain heavy metal tin, and a final product yield of 94.5%-96% with a purity of over 97%, an acid value of 0.001 mg / g KOH, and a platinum-cobalt color of 5-20.

The application discloses an anti-aging recycled PP composite material and a preparation method thereof. The composite material comprises the following raw materials in parts by weight: recycled PP material 80-100 parts, high-density polyethylene 10-15 parts, modified additive 2-3 parts, and dicumyl peroxide 0.5-1 part. In the raw material melting and blending process, the modified additive is grafted with the molecules of the recycled PP material and the high-density polyethylene under the action of the dicumyl peroxide. The modified additive contains a hindered amine structure and a nickel complex structure in the molecules. The hindered amine structure is oxidized into a nitrogen-oxygen free radical under the conditions of light or thermal oxidation. The free radical can efficiently capture alkyl free radicals and alkoxy free radicals generated in the process of PP light aging, and block the free radical chain reaction. The nickel complex structure can capture excited state molecules generated in the process of PP light aging. After capturing energy, the nickel complex converts the energy into heat energy through non-radiative transition and releases the heat energy, thereby preventing the excited state molecules from causing PP chain rupture or oxidation reaction.

The application relates to a cross-linked polyethylene composition for manufacturing a medium and high voltage cable insulator, a cross-linked polyethylene material, a preparation method thereof and a medium and high voltage cable. The cross-linked polyethylene composition comprises the following components in parts by weight: 90-98 parts of polyethylene, 1-3 parts of a peroxide cross-linking agent, 0.05-1 part of a hindered phenolic antioxidant and 0.05-1 part of a piperidine nitroxyl radical polymerization inhibitor. The cross-linked polyethylene composition can improve the scorch resistance and long-term thermal stability of the existing medium and high voltage cable insulator.

This invention relates to the field of chemical engineering, specifically to a method for the highly selective synthesis of high-quality ortho-vanillin. Using 3-methoxysalicylic acid as a starting material, a hydroxyl group protection reaction is performed under weakly alkaline conditions to generate compound 2. Compound 2 undergoes esterification, followed by reductive hydrogenation under a strong reducing agent to generate compound 3. In the presence of a nitrile radical catalyst, compound 3 reacts with an oxidizing agent to generate compound 4. In the presence of an acidic catalyst, compound 4 undergoes aldehyde group protection to generate compound 5. In the presence of a transition metal catalyst, the hydroxyl protecting group of compound 5 is removed to generate compound 6. Under strong acid conditions, compound 6 undergoes acetal hydrolysis to generate ortho-vanillin. This method achieves high regioselectivity and a simple process flow from the source through directional functional group transformation and protecting group strategies, avoiding the use of toxic and harmful reagents; it meets the requirements of industrial production for selectivity, environmental friendliness, and economy.

The application provides a method for capturing, identifying and evaluating environmental persistent organic free radicals. The method for identifying provided by the application adopts a CATT capturing agent, and the structure is shown as formula (1). The CATT capturing agent has good free radical dissociation groups, can capture environmental persistent organic free radicals (EPFRs) in a to-be-detected substance, can release a stable TEMPO nitrogen-oxygen free radical in a 1:1 ratio while capturing the EPFRs, the TEMPO nitrogen-oxygen free radical can be clearly captured by electron paramagnetic resonance (EPR), there is no side reaction, and the free radical capturing adduct generated can be clearly identified by mass spectrometry (MS), that is, EPR and MS information are obtained simultaneously through the CATT capturing agent. Subsequently, ferulic acid with high solubility and few side reactions is screened as an inhibitor, the transfer of free radicals can be realized to inhibit the reaction, and then the contribution evaluation of the target EPFRs is completed.

This invention belongs to the field of plant growth regulator preparation, and relates to a method for preparing brassinolide intermediates, particularly a method for preparing propionyl brassinolide, 28-homobrassinolide, and 24-epibrassinolide intermediates. The invention provides a novel preparation method comprising the following steps: In a solvent, compound 2 is oxidized with an oxidant under the action of a nitrogen-oxygen free radical catalyst to obtain compound 1. The synthetic route is shown in Figure I below: where R represents a "carbon-carbon single bond" or "carbon-carbon double bond"; R represents: (C1-C4)alkyl, (C1-C4)haloalkyl, (C3-C8)cycloalkyl, (C1-C4)alkoxy, (C1-C4)haloalkoxy, (C2-C6)alkenyl, (C2-C6)alkynyl; preferably methyl or ethyl. This invention is simple to operate, has optimized conditions, is environmentally friendly, has high conversion rate, low cost, and high yield, making it suitable for industrial production.

This invention discloses a polyEDOT with nitrogen and oxygen radicals in its side chain, having the structure shown in Formula I, and also discloses its preparation method and its application as an electrochemical oxidation catalyst. The PDOT-TEMPO prepared by this invention exhibits catalytic activity similar to TEMPO, and its use in the electrocatalytic oxidation of alcohols to aldehydes demonstrates excellent catalytic oxidation performance. Furthermore, PDOT-TEMPO adheres to the electrode, is easily separated after the catalytic reaction, and the electrode can be directly removed; it can be reused multiple times after rinsing.

This invention relates to the field of quantum dot diffuser technology, and more particularly to a high-temperature resistant quantum dot diffuser and its preparation method. By weight, it comprises the following components: 90-99.9 parts of diffuser particles; 0.1-10 parts of quantum dots; and 0.1-5 parts of stabilizer. The stabilizer includes at least one of nitrile radical light stabilizers, hindered amine light stabilizers, and hydroquinone light stabilizers. The multi-level scattering structure not only provides a high transmittance of over 90%, but also achieves an ultra-low haze of less than 1.5%. This significant improvement in optical performance stems from the precise control of the refractive index gradient and stress field distribution. The modified interface layer exhibits excellent stress buffering capacity, maintaining over 98% integrity during thermal cycling from -40°C to 120°C. In particular, the gradient structure of the interface layer effectively suppresses thermal stress concentration, significantly improving the reliability of the product.

This invention belongs to the field of scale inhibitor preparation technology, and more specifically, relates to a multi-component scale inhibitor and a method for preventing scale formation in petrochemical production. The multi-component scale inhibitor includes a first component, a second component, and a third component; the first component includes diene succinimide and di-sec-butyl-p-phenylenediamine; the second component includes a dodecylbenzenesulfonic acid organic amine salt; and the third component includes a 2,2,6,6-tetramethylpiperidinol nitroxide radical. The product obtained by this invention has excellent scale inhibition performance.

The application relates to a preparation method of terephthalate-glycolate monomers and a preparation method of degradable polyesters, wherein the preparation method of the terephthalate-glycolate monomers comprises the following steps: mixing esterification, a nitroxyl radical type catalyst, water and an organic solvent in a reaction device, then filling NO / NO2 mixed gas and oxygen-containing gas into the reaction device to perform an oxidation reaction, and after the reaction is completed, the terephthalate-glycolate monomer shown in formula (2) is obtained through cooling and separation. Through the synergistic catalysis of the nitroxyl radical type catalyst and the NO / NO2 mixed gas, the structural unit of glycolic acid can be effectively introduced into the polyester monomer, the method has high conversion rate, selectivity and stability, the process is safe and reliable; meanwhile, after the reaction is completed, the terephthalate-glycolate monomer is precipitated from the reaction solution in the cooling process, and is easy to purify and separate.

The present application belongs to the technical field of pharmaceutical chemistry, and particularly relates to a sulfonamid compound and application thereof in inflammation treatment. The present application performs structure splicing of a sulfonamid skeleton and a gentiopicroside nitroxide radical derivative, realizes advantage complementation of two types of active skeletons, and is worth a series of sulfonamid compounds with good anti-inflammatory activity. The present application has the following beneficial effects: on the one hand, the sulfonamid skeleton can improve water solubility and metabolic stability of the gentiopicroside nitroxide radical derivative, and improve its drug property; on the other hand, the anti-inflammatory activity of the gentiopicroside nitroxide radical can further enhance the free radical scavenging capacity and inflammation pathway regulation effect of the sulfonamid compound, form a double anti-inflammatory mechanism, inhibit excessive activation of an inflammation signal pathway through the sulfonamid skeleton, remove excessive ROS, NO and other inflammation mediators through the gentiopicroside nitroxide radical, and synergistically improve the anti-inflammatory activity.