64 results about "Methylperidol" patented technology

The invention discloses a synthesizing technology of a hindered amine light stabilizer Tinuvin-770, which comprises the steps of: step 1, adding 2,2,6,6-tetramethyl-4-piperidinol, sebacic acid, catalyst and solvent into a four-neck flask to mix; step 2, starting a stirrer, heating, backflow distributing through a water segregator until no water drop is generated, and keeping back flowing for 1h; step 3, after finishing the back flowing, cooling the four-neck flask to 30-40 DEG C, washing with water for two times, and then steaming the solvent through reducing the pressure; and step 4, adding water to stir, after cooling and recrystallizing, carrying out the filtering centrifuging washing technology, and obtaining white crystalline powder, i.e. the sebacic acid bis(2,2,6,6-tetramethyl-4-piperidinol). The technology utilizes the sebacic acid for esterification reaction to substitute dimethyl sebacate for interesterification reaction and uses water for recrystallization to substitute organic solvent, so the cost of raw materials is reduced, the Tinuvin-770 which is synthesized by the technology has high yield and purity, good color and quality, and the technology is convenient to operate and is easy to carry out.

The invention belongs to the technical field of hindered amine light stabilizers, and discloses a method and a device for producing 2, 2, 6, 6-Tetramethyl-4-piperidinol through continuous catalytic hydrogenation. According to the technical scheme, the method includes steps as follows: tetramethyl piperidone and ethyl alcohol are mixed, so that a feed liquid is formed; then the feed liquid is placed in reaction kettles and taken as bottom materials, and a pumping mechanism is started and injects the feed liquid into a primary reaction kettle with a constant flow; the reaction temperatures of the reaction kettles are kept, a reaction fluid overflows from a previous reaction kettle to the next reaction kettle for reaction and then overflows to a rotary sedimentation separator; and the well reacted feed liquid is separated from a system through the separator. According the method and the device, relatively regular technological conditions can be realized, and the reaction can be always and continuously performed under conditions of high concentration, low temperature and lower pressure; hydrogen is not required to be evacuated and can be continuously and circularly used, the consumption of catalysts is reduced greatly, the operation condition is clear, stable and small in fluctuation, the operation safety is enhanced greatly, and the controllability is enhanced; and the reaction conversion rate of the process can reach 100%.

The invention discloses high-quality 4-methoxyl-2, 2, 6, 6-tetramethylpiperidinol (polymerization inhibitor 705 for short) and a preparation technology of the same. The high-quality polymerization inhibitor is prepared by the processes of: firstly, preparing tetramethylpiperidinol, and then, carrying out mixing, oxidizing, filtering, molecular distillation, packaging and on the like. The technology for preparing the polymerization inhibitor 705 comprises carrying out oxidization on tetramethylpiperidinol and acetaldehyde. According to the technology disclosed by the invention, the polymerization inhibitor 705 is obtained by molecular distillation and purification, thus, high-quality products can be provided for the clients and the company.

The invention relates to a reaction type hindered amine light stabilizer and a preparation method of the reaction type hindered amine light stabilizer. The light stabilizer is prepared by dissolving tetramethyl-4-piperidinol and a derivative of the tetramethyl-4-piperidinol into a solvent, adding a polymerization inhibitor and alpha-beta unsaturated carboxylic ester, implementing an esterificationreaction under the action of a catalyst, washing with water, and desolventizing. According to the disclosed reaction type hindered amine light stabilizer and the preparation method of the reaction type hindered amine light stabilizer, the process is simple, the condition is mild, the purity of a produced product is high, and the yield is more than 90%. The synthesis method is simple to operate, the color of the product is light, and the light transmittance of the product is good.

The invention discloses a synthesis technology of tetramethylpiperidine, comprising the steps of: first, adding triacetonamin, a catalyst, flake caustic soda and water into a high-pressure reaction kettle; second, introducing N2 to the kettle, then introducing H2 to replace N2; third, controlling the pressure within the kettle to be maintained at 0.8MPa, when the pressure in the kettle decreases, supplementing H2 timely to a pressure of 0.8MPa, conducting stirring simultaneously to raise the temperature which is controlled between 70 to 100DEG C, then repeating the above operations till the pressure in the kettle is constant at 0.8MPa; fourth, introducing N2 into the kettle to replace H2, and simultaneously delivering cooling water into a coiled pipe inside the kettle so as to lower the temperature in the kettle below 50DEG C, the stopping stirring, filtering out the catalyst, and distilling out part of the water; fifth, stirring and cooling the left oversaturated mother solution in ice water bath for crystallization, then carrying out filtering and washing, thus obtaining tetramethylpiperidine. The tetramethylpiperidine synthesized by the technology of the invention has the advantages of high yield and purity, good color and quality, and no environmental pollution, so that the technology provided in the invention is good for promotion and application.

The invention discloses a yellowing inhibitor based on naphthalimide fluorescent whitening agent, and a preparation method and application thereof. The preparation method comprises the following steps: taking cyanuric chloride as a crosslinking monomer, introducing free group trapping agent 2,2,6,6-tetramethyl piperylhydrazine or 2,2,6,6-tetramethyl piperidinol and naphthalimide fluorescent whitening agent into the same molecule, and further introducing an amino water-soluble compound, thus synthesizing a new pulp yellowing inhibitor having high yield. According to the invention, multiple functional groups are grafted in the same molecular structure, the yellowing of paper pulp is inhibited through multiple mechanisms and approaches, and the novel concept of multifunctional molecule design is embodied; and the yellowing inhibitor has a favorable effect of inhibiting the yellowing of paper pulp.

The invention relates to a water-soluble paper light stabilizer and a preparation method thereof. The preparation method of the water-soluble paper light stabilizer comprises the step of enabling 3-chloro-2-hydroxypropylsulfonate to react with 7-hydroxyl-4-methylumbelliferone fluorescent brightener, hindered amine light stabilizer amino-1,2,2,6,6-pentametylniperidine, hindered amine light stabilizer 1,2,2,6,6-pentamethyl-piperidinol respectively, so as to obtain a series of paper light stabilizers with better water solubility; the applications are as follows: matching the synthesized water-soluble coumarin fluorescent brightener with any water-soluble hindered light stabilizer for use, dissolving with gelatinized oxidized starch solution to obtain paper light stabilizer surface sizing material with better water solubility, and coating the sizing material on a high-yield size handsheet for inhibiting the yellowing of paper. The water-soluble paper light stabilizer has the advantages of being simple in the synthesis method, desirable in fluorescent brightening effect, good in thermal stability and the like, and the light-induction yellowing degree of the paper can be effectively reduced by fully utilizing the synergistic effect of the coumarin fluorescent brightener and the hindered amine light stabilizer.

The invention provides an epoxy resin composition good in transparency. The epoxy resin composition is prepared from the following components in parts by weight: 30 to 70 parts of bisphenol A epoxy resin, 10 to 35 parts of organic clay modified epoxy resin, 0.1 to 2 parts of light stabilizer, 0.1 to 2 parts of antioxidant, 10 to 25 parts of curing agent, 0.1 to 15 parts of diluting agent, 20 to 40 parts of filling matrial, 0.5 to 1.5 parts of coupling agent and 0.5 to 3 parts of thixotropic agent, wherein organic clay in the organic clay modified epoxy resin is a compound composition of sodium dodecyl sulfate grafted 2,4,6-trihydroxybenzoic acid and acrylic attapulgite clay; the curing agent comprises a polymercaptan curing agent and a modified amine curing agent; the light stabilizer is a compound macromolecular light stabilizer; the compound macromolecular light stabilizer is a copolymer of 2-phenylbenzimidazole-5-sulfonic acid and 2,2'-dihydroxy-4,4'-dimethoxybenzophenone grafted polyvinyl chloride and fumaric acid 2,2,6,6-tetramethylpipradrol polyethylene glycol monomethyl ether diester.

The invention relates to a PVC stabilizer with good heat and light stability, and a preparation method thereof, and belongs to the technical field of PVC plastic assistants. The chemical structural formula of the PVC stabilizer is shown in the description; and in the formula, R is a carboxylic group, R1 is an organic acid radical, x is the valence of the R1, m is 0, 1, 2, 3, 4..., mx is less than n, M is a metal, and n is the valence of the metal. The preparation method comprises the following steps: carrying out an esterifying reaction on a phenyl diacid compound and 2,2,6,6-tetramethyl-4-piperidinol to generate a phenyl diacid ester of mono(tetramethylpiperidine), reacting the phenyl diacid ester of mono(tetramethylpiperidine) with the R1 acid and sodium hydroxide to generate a sodium salt, adding metal salt, and carrying out a metathesis reaction to obtain the target stabilizer, or directly reacting the phenyl diacid ester of mono(tetramethylpiperidine) with metal hydroxide or metal oxide at a high temperature to obtain the target stabilizer. The PVC stabilizer has good heat stability and good light stability, and the preparation method has the advantages of simplicity, easiness in condition control, good reappearance, and good development potential and application prospect.

The invention discloses a technology for removing ammonia in ammoniacal smell ethanol in tetramethylpiperidinol. The technology comprises an adsorption stage and an elution stage. The technology is characterized in that in the adsorption stage, an ammoniacal smell ethanol mixed solution enters into a highly acidic ion exchange resin fixed bed at a flow rate of 1 to 1.5L/min and liquid ammonia is adsorbed by a highly acidic ion exchange resin and eluate is a qualified ethanol solution; and in the elution stage, after adsorbed ammonia is saturated, the adsorbed ammonia is eluted from the highly acidic ion exchange resin fixed bed by a hydrochloric acid solution at a flow rate of 0.3L/min and liquid ammonia is recovered. The technology provided by the invention utilizes the highly acidic ion exchange resin fixed bed to treat ammonia in ethanol, replaces the existing neutralization ammonia-removal method, has simple processes, is convenient for operation and reduces energy consumption.

The invention belongs to the technical field of lignin materials and discloses hindered amine modified lignin as well as a preparation method and an application thereof. According to the preparation method, 2,2,6,6-tetramethyl-4-piperidinol and epichlorohydrin are subjected to a reaction under the catalysis of a catalyst, and a chloro-tetramethylpiperidine intermediate is obtained; the chloro-tetramethylpiperidine intermediate and lignin react in an alkaline solution, and tetramethylpiperidine grafted lignin is obtained. The hindered amine modified lignin is prepared from components in parts by mass as follows: 100 parts of lignin, 10-20 parts of epichlorohydrin, 1-3 parts of a catalyst and 30-60 parts of 2,2,6,6-tetramethyl-4-piperidinol. The hindered amine modified lignin prepared with the method is novel modified lignin containing hindered amine groups, has photo-stabilization groups of hindered amine and aromatic ring structures of lignin, can serve as a polymeric photostabilizer to be used in various photodecomposition resisting fields such as pesticide preparations, coatings, ink, sun cream, high polymer materials and the like.

The invention provides a preparation method of a hindered amine light stabilizer 770. According to the method, sebacic acid and tetramethylpiperidinol as reactants and an oxide and / or organic compound of the fourth main group element tin as a catalyst are subjected to a heating refluxing reaction in a solvent to obtain the hindered amine light stabilizer 770. The invention uses sebacic acid as raw material instead of dimethyl sebacate, and the sebacic acid under the effect of an appropriate catalyst performs a direct esterification dehydration reaction with tetramethylpiperidinol; and appropriate technology conditions such as an appropriate proportion of raw materials, reaction temperature adjustment and suitable solvent are employed to solve the technical problems of low esterification rate and poor light transmittance of a final product in a common direct esterification reaction, and to prepare the light stabilizer 770 product in line with the requirements of market quality standards. Compared with the ester exchange method in the prior art, the method has the advanategs of cheap raw materials, higher yield, low requirements for equipment, simple process and easiness for scale production.

The invention discloses a preparation method of a light stabilizer. Pent-amethyl and dimethyl sebacate conduct heating reaction under the function of a catalyst; the reaction product is cooled and added with measured petroleum ether; the mixture is washed by tap water into neutral for refining treatment, vacuum distillation is then conducted and qualified distillate is collected, thus obtaining the light stabilizer. The method adopts solvent-free transesterification reaction, conducts the reactions under the protection of inert gas while limitedly improving transesterification reaction temperature, ensuring fast reaction with less side reaction products; the post treatment purification adopts a combined rectification device, improving distillate producing rate and quality; the method eliminates chromogenic factors that can be produced, and can produce low-colority high-quality liquid light stabilizer GW508 products.

The invention provides a sPS (syndiotactic polystyrene) film and a preparation method thereof. The film is prepared from the following raw materials in parts by weight: 100 to 120 parts of modified sPS, 60 to 80 parts of adhesive resin, 10 to 15 parts of Degussa Dyhard 100, 5 to 10 parts of polyether modified polysiloxane, 5 to 10 parts of bis(3,5-tert-butyl-4-hydroxyphenyl) thioether, 1 to 4 parts of decabromodiphenyl ethane, 1 to 3 parts of bis(2,2,6,6-tetramethyl-4-piperidyl)sebacate and 1 to 3 parts of aminopropyltriethoxysilane. The modified syndiotactic polystyrene is added into the film; through the modification by oxidized graphene and aluminium oxide, the prepared modified syndiotactic polystyrene has good mechanical performance and high polarity; the conductivity and the flame-resistant performance are obviously improved; the wide application prospects are realized.

The invention discloses a scratch-resistant waterborne UV curing coating which is prepared from, by weight, 40-45 parts of aliphatic waterborne polyurethane acrylate, 2-2.5 parts of vinyltriethoxysilane, 38-40 parts of alumina sol, 2-3 parts of 2-hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone, 2-2.5 parts of bis(1,2,2,6,6-pentamethyl-4-piperidyl) sebacate and 10-15 parts of water. The water-soluble aliphatic polyurethane acrylate is used as the main material, the vinyltriethoxysilane is used as a modifying additive, and the water-soluble aliphatic polyurethane acrylate and the vinyltriethoxysilane are mixed with the alumina sol to prepare the organic-inorganic hybrid coating. The surface of paper or leather is coated with the coating, after UV curing, Si-O-Si and Si-O-Al bonds are formed in a coating film and formed between the coating film and a base material, and therefore the adhesive force of the coating film for the base material and the scratch resistance of the surface of the film are improved.

The invention discloses a method for synthesizing bis(1-alkoxy-2,2,6,6-tetramethyl piperidine-4-yl) sebate. The bis(1-alkoxy-2,2,6,6-tetramethyl piperidine-4-yl) sebate is synthesized through transesterification by using dimethyl sebate and 1-alkoxy-2,2,6,6-tetramethylpipradrol as raw materials. According to the method, lithium hydroxide is adopted as a catalyst, a quaternary ammonium salt is adopted as a phase transfer catalyst, n-heptane is adopted as a methanol-carrying solvent, and methanol is separated continuously from the reaction system through a water knockout vessel. The process comprises the steps: adding dimethyl sebate, 1-alkoxy-2,2,6,6-tetramethylpipradrol, lithium hydroxide, the phase transfer catalyst and n-heptane to a reaction kettle with the water knockout vessel, performing heating to a reflux state so as to separate methanol continuously, stopping the reaction (about 5 hours later) until no separation of methanol, performing cooling to room temperature, performingwashing with deionized water, performing reduced pressure distillation on the oil phase so as to isolate the solvent and unreacted 1-alkoxy-2,2,6,6-tetramethylpipradrol and obtain a crude product, washing the crude product three times with a mixed solvent of methanol and water, and then performing distillation so as to isolate the solvent and obtain the final product. The method has the advantagesthat the process and the devices are simple, the catalyst has safe use, the product has easy separation, the product has high yield and high purity, and emission of three wastes is little.

The present invention discloses a manufacturing process of a light stabilizer 298. The process provides a crude product which is synthesized through the reaction of methyl oleate and light stabilizer intermediate 2, 2, 6, 6-tetramethyl piperidinol in quantitative petroleum ether under the condition with a load catalyst tetrabutyl phthalicate, the methyl oleate is extracted with waste oil and has no toxicity or methyl oleate groups of large component, and the methyl oleate is added into the light stabilizer to prepare a novel highly efficient and non-toxic light stabilizer. On one hand, the light stability is maintained in the structure of the product; on the other hand, the adoption of double bond activity groups can lead the processing of the product into an auxiliary agent of larger molecular weight. The present invention can be used in the plastic packing, in particular in the food packing, and has excellent prospects for application.

The invention relates to a polymerization inhibitor used for inhibiting polymerization of a petroleum cracked C5 fraction. The polymerization inhibitor consists of a component 1, a component 2, a component 3 and a solvent, wherein the component 1 is di methyl ketoxime; the component 2 is 2,2,6,6-tetramethyl-4-piperidinol; the component 3 is ortho-aminophenol; the solvent is acetonitrile or dimethylformamide; a weight ratio of the component 1 to the component 2 to the component 3 is 1:(0.1-2):(0.2-2.5); the component 1, the component 2 and the component 3 are 2 to 10 percent based on the weight of the solvent; and the using amount of the polymerization inhibitor in the petroleum cracked C5 fraction is 20 to 800ppm according to weight. The polymerization inhibitor provided by the invention has better polymerization inhibiting effect, can effectively inhibit auto polymerization or polymerization of diolefins in the petroleum cracked C5 fraction in a separating column, and avoids blockageof a reboiler; the using amount of the polymerization inhibitor is small and the production cost can be reduced; and the difference between boiling points of various components and the solvent of thepolymerization inhibitor and the boiling point of the petroleum cracked C5 fraction is great, so the petroleum cracked C5 fraction is easy to separate.

The invention discloses a method for preparing a rubber or resin multifunctional anti-aging agent. The synthesis of the anti-aging agent comprises the following two steps of: synthesizing a highly symmetrical intermediate with a dendritic structure from phenylenediamine and methyl acrylate through a Michael addition reaction; and carrying out an ester exchange reaction on the intermediate and 1,2,2,6,6-pentamethyl-piperidinol to synthesize the anti-aging agent under the condition of taking tetraisopropyl titanate as a catalyst. The anti-aging agent contains heat-resistant oxygen groups and light-stabilizing groups, and when the anti-aging agent is added into rubber or resin, the period of heat oxygen resistance and light aging resistance is delayed.

The invention relates to a preparation method of UV770. The preparation method comprises the following steps: (S1) adding (a) 2,2,6,6-tetramethylpiperidine alcohol with the formula shown in the specification and (b) sebacic acid with the formula shown in the specification into a reaction tank, and carrying out fusion mixing; (S2) introducing nitrogen to protect the reaction; (S3) adding titanium catalysts into the reactor, and carrying out thermal response reaction; (S4) cooling reactants to 100-110 DEG C after the reaction is finished, and immediately filtering; and (S5) cooling filtrate, separating out crystals, washing, and further refining rough products to obtain the purified product UV770, or evaporating water to directly obtain the product. The preparation method has the characteristics of high reaction efficiency and convenience in refining.

The invention relates to a formaldehyde removal and odor removal spraying solution, which comprises the following raw materials by weight: 15-19 parts of 1-chloro-2,2,6,6-tetramethylpiperidinol, 10-14parts of N,N-dichloro-4-methylbenzenesulfonamide, 5-10 parts of carboxymethyl cellulose, 4-6 parts of essential oil, 6-8 parts of a dispersant, and 40-50 parts of a solvent. According to the presentinvention, the formaldehyde removal and odor removal spraying solution has characteristics of non-toxic and harmless raw materials, low cost and good formaldehyde removal and deodorization effect.

The invention discloses a light stabilizer for a weather-resistant PVC material, and a preparation method and application thereof. The preparation method for the light stabilizer comprises the following steps: sequentially adding cyanuric chloride, 2,2,6,6-tetramethyl pipradrol compound and potassium carbonate into a tetrahydrofuran solution in a nitrogen atmosphere, and performing stirring under reflux; and cooling reaction liquid to room temperature, performing suction filtration to obtain a crude product, washing the crude product with hot water a plurality of times, and performing drying so as to obtain the light stabilizer for the weather-resistant polyvinyl chloride material. According to the light stabilizer of the invention, a triazine structure and a piperidine structure are combined together, so the light stabilizer absorbs ultraviolet light while capturing free radicals generated during the photodegradation process of PVC, thereby greatly improving the weather resistance of the PVC material; a heat stabilizer system of the invention has the stability mechanisms of three different heat stabilizers; the preparation method is simple; and after the heat stabilizer is added into the PVC material, the thermal stability of the PVC material is greatly improved.

The invention relates to a novel hindered amine light stabilizer preparation method, which specifically comprises: (1) dissolving vanillin in a solvent, adding sodium chlorite, and performing an oxidation reaction to form a carboxyl group-containing compound; (2) adding methanol to the carboxyl group-containing compound, and performing an esterification reaction to obtain an ester compound; and (3) mixing the generated ester compound and tetramethylpiperidinol, adding a catalyst, and performing a reaction to obtain the hindered amine light stabilizer. According to the present invention, the synthetic raw material vanillin of the hindered amine light stabilizer is easy to obtain and non-toxic, the product synthesis steps are less, and the reaction conditions are mild; and the light stabilizer has good compatibility with polymers, especially engineering plastics, and further has excellent processing performance and excellent anti-aging effect.

The invention discloses a preparation method of a compound type macromolecular light stabilizer based on Diels-Alder click chemistry. The preparation method comprises the following steps: performing a Diels-Alder reaction by using 3-(N,N-2-maleimido ethyl propionate-aminomethyl)-2,4-dihydroxy benzophenone and sebacic acid difurfuryl ester as raw material monomers; and then adding 2,2,6,6-tetramethyl-piperidine maleimide propionate as an end-capping reagent to prepare the compound type macromolecular light stabilizer, wherein the added amount of the end-capping reagent is 0.1-2% of the total weight of the raw material monomers. The invention discloses the compound type macromolecular light stabilizer based on the Diels-Alder click chemistry. The compound type macromolecular light stabilizer prepared by the preparation method disclosed by the invention has an excellent broad-spectrum ultraviolet absorption function, has a dual-light stabilizer effect of ultraviolet absorption and free radical capturing function, and has good compatibility with most high polymer materials.

The invention provides a preparation method of a light stabilizer intermediate 2,2,6,6-tetramethyl-4-piperidine ester compound (1) obtained by chemical reaction of both 2,2,6,6-tetramethyl-piperidine and unsaturated organic dibasic acid shown in the formula (II). The invention further provides a 2,2,6,6-tetramethyl-4-piperidine ester light stabilizer conforming to the formula (I), and the light stabilizer is mainly applied to plastic films, coatings, paper-making, engineering plastics and other high polymer materials, and can directly participate in chemical reaction and remarkably improve the product light aging resistance and prolong the product service life. As a (SO4)2-/TiO2-ZnO mixed crystal solid-acid support coordination catalyst is adopted, the advantages of easy separation from a reaction system, no equipment corrosion and good environmental protection performance are achieved.