25 results about "2,4,6-Tribromophenol" patented technology

The invention discloses an application of an electronic waste pollution human body exposure fingerprint spectrum in exposure risk prediction, and the human body exposure fingerprint spectrum is composed of more than three of exposure markers of 2, 4, 6-tribromophenol, 2, 4, 5-trichlorophenol, 4-bromophenol, 1-hydroxypyrene and bisphenol A. The invention further discloses an application of the electronic waste pollution human body exposure fingerprint spectrum in exposure risk prediction. According to the method, a systematic method of urine pollutant exposure omics is adopted for the first time, comprehensive screening and characterization of pollutant exposure markers related to specific components and by-products are achieved in electronic waste exposure worker groups, and the method is the most systematic organic pollutant exposure research known in the field at present.

The invention discloses a synthesis method of bromo-triazine, which belongs to the technical field of organic synthesis, and comprises the following steps: preparing an alumina-loaded N, N-dimethylaminopyridine catalyst, filling the alumina-loaded N, N-dimethylaminopyridine catalyst in a fixed bed reactor, introducing tribromophenol and metal oxide mixed slurry and cyanuric chloride slurry, carrying out a reaction for 2-4 hours, and carrying out a reaction for 2-4 hours to obtain the bromo-triazine. Raising the temperature for reaction to obtain a crude product solution; and performing post-treatment to obtain a bromo-triazine product. According to the invention, the aluminum oxide loaded N, N-dimethylaminopyridine catalyst is synthesized, and the N, N-dimethylaminopyridine enables the reaction speed to be higher and the yield to be higher; nano aluminum oxide is adopted for loading, so that on one hand, dealkalization synthesis of bromotriazine is realized, and on the other hand, the reaction efficiency is accelerated; the continuous process realizes non-aqueous medium and low-temperature short-time reaction, so that hydrolysis is further avoided; the aluminum oxide loaded N, N-dimethylaminopyridine catalyst is high in activity and stability, the synthesis method is simplified, and the aluminum oxide loaded N, N-dimethylaminopyridine catalyst is suitable for industrial large-scale production.

The invention relates to the technical field of fine chemical engineering and flame retardant preparation, and discloses a preparation method of bromo-triazine capable of improving thermal stability, and the preparation method comprises the following steps: mixing phenol, water and dichloromethane, controlling the temperature, and carrying out oxidative bromination reaction to prepare an organic phase containing tribromophenol; then, under the action of an organic amine catalyst, carrying out condensation reaction on the organic phase, liquid caustic soda and cyanuric chloride; after the reaction, washing with water to remove impurities; and in the presence of process water, firstly controlling the temperature at 38-42 DEG C for azeotropic desolvation, then raising the temperature to 85-95 DEG C for high-temperature crystallization and crystal growing, and finally cooling, filtering and drying to obtain the bromo-triazine product. By utilizing the high selectivity of the organic amine catalyst and a two-stage azeotropic crystallization process, the side reaction is effectively reduced, the solvent wrapped in the crystal is eliminated, the prepared product is high in main content and extremely low in volatile component, the temperature can reach 370 DEG C or above when the thermal weight loss is 2%, and the thermal stability is remarkably improved.

The invention belongs to the technical field of flame retardants, and particularly relates to a preparation method of bromotriazine, which comprises the following steps: adding phenol and deionized water into a reaction container, dropwise adding hydrogen peroxide and liquid bromine into a reaction system in a staggered manner, and adding a catalyst; after the reaction is finished, separating the catalyst, firstly carrying out quenching treatment on the filtrate, then carrying out extraction treatment, and carrying out reduced pressure distillation on the extracted organic phase to obtain tribromophenol; dissolving the prepared tribromophenol in dichloromethane, adding triethylamine and tetrabutylammonium bromide, stirring to form a homogeneous system, adding cyanuric chloride into the homogeneous system, and regulating and controlling the pH in stages; concentrating the organic phase which is washed to be neutral, adding n-hexane to initiate primary nucleation, dropwise adding ethyl acetate to adjust the polarity of the solvent, and promoting crystal growth; and filtering and drying in vacuum to obtain the bromo-triazine. Through staged pH / temperature regulation and control, the composite catalyst system realizes efficient synthesis of bromotriazine.

This invention discloses the application of human exposure fingerprinting of electronic waste pollution in exposure risk prediction. The human exposure fingerprinting consists of three or more of the following exposure markers: 2,4,6-tribromophenol, 2,4,5-trichlorophenol, 4-bromophenol, 1-hydroxypyrene, and bisphenol A. This invention is the first to employ the systematic method of urinary contaminant exposure profiling to achieve comprehensive screening and characterization of contaminant exposure markers related to specific components and byproducts in workers exposed to electronic waste. This is currently the most systematic organic contaminant exposure study known in this field.

The application discloses a synthesis method of bromotriazine, and belongs to the technical field of organic synthesis. The method comprises the following steps: preparing an alumina-supported N,N-dimethylaminopyridine catalyst, filling the catalyst into a fixed bed reactor, introducing a mixed slurry of tribromophenol and a metal oxide and a cyanuric chloride slurry, and performing reaction by increasing temperature to obtain a crude product solution; and performing post-treatment to obtain a bromotriazine product. The application synthesizes an alumina-supported N,N-dimethylaminopyridine catalyst. The N,N-dimethylaminopyridine makes the reaction speed faster and the yield higher. The nanometer alumina support realizes the dealkalization synthesis of bromotriazine and accelerates the reaction efficiency. The continuous process realizes non-aqueous medium and low-temperature short-time reaction, and further avoids the occurrence of hydrolysis. The alumina-supported N,N-dimethylaminopyridine catalyst has high activity and high stability, simplifies the synthesis method, and is suitable for industrial large-scale production.

The invention relates to the technical field of flame retardant preparation, in particular to a method for improving the quality of a bromo-triazine product based on a high-shear homogenization technology. According to the method, after a synthetic reaction of tribromophenol and a bromo-triazine product is completed, high-shear homogenization treatment is carried out on an organic solution of the tribromophenol and the bromo-triazine product, and the treatment can effectively crush coarse crystals and aggregates, so that wrapped impurities are exposed and further efficiently removed in the subsequent washing process. According to the method provided by the invention, the particle size of the product can be obviously optimized, the purity of the product is improved, and the dispersing performance of the product in a high polymer material is improved, so that a flame-retardant product with excellent performance is obtained. The method provided by the invention is simple and convenient in process, can fundamentally solve the problem of the quality pain point of the bromo-triazine product by introducing a simple and efficient high-shear homogenization treatment process, is convenient for industrial production, and has remarkable industrial application value and economic benefit.

The application provides a method for recovering tribromophenol, tetrabromobisphenol A and dibromophenol from bromine-containing solid waste by melting crystallization, and relates to the field of solid waste recovery. The method comprises the following steps: mixing bromine-containing solid waste, a solvent and a catalyst to perform a reaction, then performing liquid-liquid separation to obtain a bromine-containing organic phase and salt-containing wastewater; recovering the solvent in the bromine-containing organic phase to obtain a bromine-containing organic mixture; preheating the bromine-containing organic mixture, then performing melting, cooling, sweating and melting treatment to obtain crude tribromophenol and crude tetrabromobisphenol A; performing vacuum rectification on the crude tribromophenol to obtain dibromophenol and a column still product; performing recrystallization, solid-liquid separation, water washing and drying on the column still product to obtain tribromophenol; and performing recrystallization, solid-liquid separation, alkali washing and drying on the crude tetrabromobisphenol A to obtain tetrabromobisphenol A. The method provided in the application adopts reaction impurity removal and melting crystallization and is coupled with a recrystallization process, so that tribromophenol, tetrabromobisphenol A and dibromophenol products can be obtained at the same time, the process is simple, and the energy consumption is significantly reduced compared with the traditional method.

The application discloses a method for continuously preparing tris(tribromophenoxy) triazine, relates to the technical field of organic chemical synthesis, and is characterized in that 2,4,6-tribromophenol, cyanuric chloride and sodium hydroxide are used as raw materials, a complex organic solvent system is constructed, mixed solution A and mixed solution B are prepared respectively, and the two solutions and a sodium hydroxide solution are continuously fed into a multi-stage series reactor to react; the obtained crude product after the reaction is sequentially subjected to alkali washing, acid washing, water washing and a micro-washing system, and then subjected to a continuous solvent recovery and pressure filtration step, so that a high-purity tris(tribromophenoxy) triazine product is finally obtained. The method realizes full-liquid continuous feeding through the complex solvent, improves feeding stability and reaction control precision, strengthens reaction conversion efficiency and inhibits byproduct generation through the multi-stage liquid-liquid heterogeneous reaction system, improves washing efficiency and impurity control ability through the micro-washing system, and significantly improves product purity, yield and thermal stability, so that the method has a good industrial application prospect.

The invention provides a method for recovering tribromophenol, tetrabromobisphenol A and dibromophenol in bromine-containing solid waste through melt crystallization, and relates to the field of solid waste recovery. The method comprises the following steps: mixing the bromine-containing solid waste, a solvent and a catalyst for reaction, and then carrying out liquid-liquid separation to obtain a bromine-containing organic phase and salt-containing wastewater; recovering the bromine-containing organic phase solvent to obtain a bromine-containing organic mixture; preheating the bromine-containing organic mixture, melting, cooling, sweating and melting to obtain a tribromophenol crude product and a tetrabromobisphenol A crude product; carrying out reduced pressure rectification on the tribromophenol crude product to obtain a dibromophenol product and a tower kettle product, and carrying out recrystallization, solid-liquid separation, washing and drying on the tower kettle product to obtain a tribromophenol product; and carrying out recrystallization, solid-liquid separation, alkali washing and drying on the crude tetrabromobisphenol A product to obtain the tetrabromobisphenol A product. According to the method, reaction impurity removal, melt crystallization and recrystallization are coupled, tribromophenol, tetrabromobisphenol A and dibromophenol products are obtained at the same time, the process is simple, and energy consumption is remarkably reduced compared with traditional methods.

Provided is an electrical insulation resin composition capable of achieving both flame retardancy and tracking resistance. The electrical insulation resin composition according to an embodiment comprises a polyalkylene terephthalate and a condensate of tetrabromobisphenol, cyanuric chloride, and tribromophenol. The amount of the condensate with respect to 100 parts by mass of polyalkylene terephthalate is 9-19 parts by mass.

The invention relates to the field of flame-retardant products, and particularly discloses a preparation method of bromotriazine capable of improving reaction selectivity. Comprising the following specific steps: adding phenol, water and dichloromethane into a reaction container, dropwise adding hydrogen peroxide into a reaction system for reaction, dropwise adding bromine into the reaction system for mixed reaction to obtain a reaction solution, treating the reaction solution with sodium sulfite, washing with water, and separating to obtain an organic phase containing tribromophenol, the method comprises the following steps: mixing an organic phase containing tribromophenol with magnesium oxide, a catalyst and cyanuric chloride for reaction to obtain a crude product solution, washing the crude product solution, mixing the washed crude product solution with process water, heating for azeotropic desolvation, and finally crystallizing and drying to obtain bromotriazine; the catalyst is a multi-walled carbon nanotube loaded amine compound; according to the present invention, the amine compound is loaded by using the tubular structure of the multi-walled carbon nanotube, such that the reaction rate of the main reaction can be improved through the multiple effects, the side reaction can be inhibited, and the yield and the purity of the bromo-triazine product can be improved.

The application relates to the field of chemical substance preparation and purification, and particularly discloses a highly purified brominated triazine and a preparation method thereof. The preparation method of the highly purified brominated triazine comprises the following steps: (1) a bromination reaction: phenol, bromine and hydrogen peroxide are reacted in a mixed solvent of water and dichloromethane at 5-40 DEG C to obtain a bromination reaction liquid; (2) washing treatment: after the bromination reaction liquid is reacted with a sodium sulfite solution, washing is performed to obtain tribromophenol; (3) a condensation reaction: tribromophenol, liquid alkali, a recyclable catalyst and cyanuric chloride are subjected to a condensation reaction in a synthesis kettle; (4) crystallization and post-treatment: process water is added into the condensation reaction liquid in an amount equal to that of the condensation reaction liquid, crystallization is performed, and the final product is obtained through filtration and drying; in addition, the preparation method has the advantages of improving the product purity of a brominated triazine synthesis process.

The invention relates to the field of organic matter degradation, and discloses a humin-mediated 2, 4, 6-tribromophenol biodegradation preparation and application thereof. The biodegradation preparation takes an anaerobic mineral salt culture medium as a matrix, and the matrix contains 25-35 g / L of humin, 1-2 mL / L of an organic acid salt electron donor, 1-2 mL / L of a vitamin solution and 1.5-2.5 mg / L of anaerobic microorganisms. The biodegradation preparation disclosed by the invention contains humin, so that the degradation efficiency of anaerobic microorganisms on 2, 4, 6-tribromophenol can be greatly improved. Humin has the advantages of being environmentally friendly, free of toxicity, wide in source and good in stability in a degradation system.

The invention relates to the technical field of epoxy resin, and particularly discloses brominated epoxy resin, and an environment-friendly brominated epoxy resin formula and a preparation method thereof. The formula of the environment-friendly brominated epoxy resin comprises 100 parts of brominated epoxy resin, 5-10 parts of nano toughened epoxy resin, 5-10 parts of o-cresol formaldehyde epoxy resin, 10-30 parts of a curing agent, 0.1-1 part of a curing agent accelerant, 15-20 parts of dimethyl sulfoxide, 5-10 parts of silica powder and 30-50 parts of filler. The preparation method of the brominated epoxy resin comprises the following steps: heating and uniformly mixing a brominated epoxy resin oligomer, tetrabromobisphenol A and tribromophenol at 140-160 DEG C, adding a composite catalyst, and prepolymerizing under a microwave condition to obtain a brominated epoxy resin prepolymer; and mixing the brominated epoxy resin prepolymer with a single catalyst, and polymerizing under a microwave condition to obtain the brominated epoxy resin. The epoxy resin formula provided by the invention has excellent mechanical strength, electrical insulation performance and heat resistance after being cured.

The invention discloses an analysis method for detecting bromophenol flavor substances in seafood condiments, and belongs to the technical field of food detection. A metal organic framework material (MIL-101-Cr) is prepared through a hydrothermal synthesis method, and the metal organic framework material (MIL-101-Cr) is used as an adsorbent to manufacture a solid phase extraction (SPE) column and is used for separating and enriching bromophenol flavor substances (BPs). Under optimized SPE (Solid Phase Extraction) conditions, a gas chromatography-mass spectrometry technology is combined, and an analysis method for detecting four BPs (4-bromophenol, 2, 4-dibromophenol, 2, 6-dibromophenol and 2, 4, 6-tribromophenol) is established. The method has good linearity (R2 is greater than or equal to 0.996), low detection limit (1.3-5.7 ng.L <-1 >) and high precision (1.5-8.3%, n = 6). The method is applied to detection of seafood condiments such as oyster sauce, seafood soy sauce and the like, and the detected contents of 4-bromophenol in the seafood soy sauce and oyster sauce are 57 ng.kg <-1 > and 63 ng.kg <-1 > respectively. Through low, medium and high standard addition recovery experiments, the recovery rate is measured to be 81.2-103.4%.

To provide an electric insulating resin composition that allows simultaneous realization of flame retardancy and tracking resistance.SOLUTION: An electric insulating resin composition according to an embodiment comprises a polyalkylene terephthalate and a condensate of tetrabromobisphenol, cyanuric chloride, and tribromophenol. The amount of the condensate is 9-19 pts.mass relative to 100 pts.mass of the polyalkylene terephthalate.SELECTED DRAWING: None

The invention discloses a method for continuously preparing tris (tribromophenoxy) triazine, and relates to the technical field of organic chemical synthesis processes, the scheme is as follows: 2, 4, 6-tribromophenol, cyanuric chloride and sodium hydroxide are used as raw materials to construct a compound organic solvent system, a mixed solution A and a mixed solution B are respectively prepared, and the mixed solution A and the mixed solution B are mixed to prepare a mixed solution B; introducing the mixed solution and a sodium hydroxide solution into a multi-stage series reactor in a continuous feeding manner for reaction; a crude product obtained after the reaction is sequentially subjected to alkali washing, acid washing, water washing and micro-washing systems and continuous solvent recovery and filter pressing steps, and finally a high-purity tri (tribromophenoxy) triazine finished product is obtained. All-liquid-state continuous feeding is realized through a compound solvent, and the feeding stability and the reaction control precision are improved; the multi-stage liquid-liquid heterogeneous reaction system enhances the reaction conversion efficiency and inhibits the generation of by-products; the micro-washing system improves the washing efficiency and the impurity control capability, obviously improves the purity, the yield and the thermal stability of the product, and has a good industrial application prospect.

The application belongs to the technical field of organic chemical synthesis, and specifically provides a preparation method of tri(trisbromophenoxy) triazine, which comprises the following steps: S1, a bromination reaction is performed to obtain 2,4,6-trisbromophenol, and a phase transfer catalyst is prepared in situ after purification of a by-product aqueous phase containing sodium bromide generated in the reaction; S2, mixed preparation solutions A and B are prepared; S3, the mixed solution is reacted with a sodium hydroxide solution to obtain a crude product solution; S4, the crude product solution is subjected to alkaline washing, acid washing and water washing, and an organic phase of a washing product is obtained after phase separation; S5, waste water after water washing and a back-extraction solvent are back-extracted to obtain an organic phase; S6, waste liquid after alkaline washing and acid washing is collected, and is regenerated into inorganic alkali aqueous solution and inorganic acid aqueous solution for reuse in alkaline washing and acid washing; and S7, the organic phase of the washing product in step S4 and the organic phase back-extracted in step S5 are combined, and tri(trisbromophenoxy) triazine is obtained through continuous solvent recovery and continuous pressure filtration.

The present application relates to the field of epoxy resins and specifically discloses a brominated epoxy resin, an environmentally friendly brominated epoxy resin formula, and a preparation method thereof. The brominated epoxy resin formula comprises: 100 parts of brominated epoxy resin, 5-10 parts of nano-toughened epoxy resin, 5-10 parts of o-cresol epoxy resin, 10-30 parts of curing agent, 0.1-1 parts of curing agent accelerator, 15-20 parts of dimethyl sulfoxide, 5-10 parts of silicon micropowder, and 30-50 parts of filler; wherein the preparation method of the brominated epoxy resin comprises: heating and mixing brominated epoxy resin oligomer, tetrabromobisphenol A, and tribromophenol at 140-160°C, adding a composite catalyst, and prepolymerizing under microwave conditions to obtain a brominated epoxy resin prepolymer; and mixing the brominated epoxy resin prepolymer with a single catalyst and polymerizing under microwave conditions to obtain the brominated epoxy resin. The epoxy resin formula provided in the present application has excellent mechanical strength and electrical insulation after curing.

The invention relates to the technical field of wastewater treatment, in particular to a tribromophenol recovery process in bromotriazine production, which comprises the following steps: adjusting the pH value of wastewater to 8.0 + / -0.2; dichloromethane is added for extraction according to the volume ratio of dichloromethane to wastewater being 2.5: 50-3.5: 50, and standing layering is performed after extraction is completed; transferring the wastewater phase to a neutralizing tank, and adjusting to be neutral; dehydrating the organic phase through an anhydrous magnesium sulfate column to obtain enriched liquid; transferring the enriched liquid into a glass-lined distillation kettle for desolventizing under reduced pressure; carrying out pre-concentration on the distillation residual liquid, then cooling to 4-6 DEG C, and adding normal hexane for crystallization; then carrying out centrifugal separation to obtain white needle-like crystals, and leaching the crystals twice with cold n-hexane at the temperature of-1 to 1 DEG C; and performing vacuum drying to obtain the tribromophenol. Through a precise pH regulation-extraction-desolvation-crystallization process chain, efficient recovery of tribromophenol in wastewater is realized, meanwhile, the COD (Chemical Oxygen Demand) of the wastewater is reduced to 1500mg / L or below, and the risk of environmental pollution is remarkably reduced.

The invention provides a method for separating and recovering tribromophenol and tetrabromobisphenol A from bromine-containing solid waste, and relates to the field of solid waste recovery and disposal. The method comprises the following steps: stirring and mixing the bromine-containing solid waste and an extracting agent, extracting and desalting, and then carrying out solid-liquid separation to obtain waste salt solid and desalted liquid; mixing the desalted liquid with a stripping agent, performing stripping to obtain an extraction phase and a raffinate phase, rectifying the extraction phase to obtain a recycled stripping agent and a rectifying kettle bottom material, and recycling the raffinate phase and the recycled stripping agent as an extraction agent; mixing the rectifying still bottom material with an anti-decomposition solvent to obtain a mixed solution, and rectifying the mixed solution to obtain a tribromophenol crude product and a tetrabromobisphenol A crude product; performing recrystallization, solid-liquid separation and drying on the tribromophenol crude product to obtain a tribromophenol product; and carrying out solvent recovery, recrystallization, solid-liquid separation and drying on the crude tetrabromobisphenol A product to obtain the tetrabromobisphenol A product. According to the method, the tribromophenol and the tetrabromobisphenol A can be effectively recovered from the bromine-containing solid waste, and the purity is high.

The application provides a method for separating and recovering tribromophenol and tetrabromobisphenol A from bromine-containing solid waste, and relates to the field of solid waste recycling and disposal. The method comprises the following steps: mixing and stirring bromine-containing solid waste and an extractant to perform extraction desalination, and then performing solid-liquid separation to obtain waste salt solid and desalted liquid; mixing the desalted liquid with a stripping agent to perform stripping, to obtain an extraction phase and a raffinate phase, the extraction phase is subjected to rectification to obtain recovered stripping agent and rectification kettle bottom material, and the raffinate phase and the recovered stripping agent are used as the extractant for recycling; mixing the rectification kettle bottom material with an anti-decomposition solvent to obtain a mixed solution, and subjecting the mixed solution to rectification to obtain tribromophenol crude product and tetrabromobisphenol A crude product; subjecting the tribromophenol crude product to recrystallization, solid-liquid separation and drying to obtain tribromophenol product; and subjecting the tetrabromobisphenol A crude product to solvent recovery, recrystallization, solid-liquid separation and drying to obtain tetrabromobisphenol A product. The method can effectively recover tribromophenol and tetrabromobisphenol A from bromine-containing solid waste, and the purity is high.

The present invention relates to a production process of a biodegradable courier bag, and belongs to the technical field of polymer materials. The present invention adopts dimethyl sulfoxide as a solvent, polyvinyl alcohol and itaconic acid as raw materials, performs an esterification reaction under the action of concentrated sulfuric acid as a catalyst to synthesize an alcohol ester compound, and then uses octadecylamine and thioglycolic acid to synthesize an intermediate, and the thiol group in the intermediate and the carbon-carbon double bond of the alcohol ester compound undergo an addition reaction to synthesize modified polyvinyl alcohol. The present invention also combines a compound synthesized by tribromophenol and 1-(chloro-methylphosphoryl)ethylene as raw materials with DOPO to form a modified flame retardant. Finally, the modified polyvinyl alcohol, the modified flame retardant, starch, a plasticizer, cellulose, a leveling agent and a defoamer are mixed to form a stock solution, and the stock solution is dried and cut to obtain a biodegradable courier bag. The biodegradable courier bag stock solution of the present invention has a low viscosity, is easy to process, has a better flame retardant effect after being prepared into a bag, and has good tensile resistance.

The invention discloses a preparation method of an environment-friendly anti-freezing corrosion-resistant fire-fighting liquid, which specifically comprises the following steps: S1, ingredient treatment: respectively weighing required parts by weight of an anti-freezing compound, tris (2, 2, 6-trimethyl-1, 3-pentanediolmono)-2, 3, 6-trimethyl-1, 3-pentanediolmono ( The flame-retardant coating is prepared from the following raw materials: 1, 3-dibromopropyl) isocyanurate, melamine cyanurate, tribromophenol, a flame-retardant composition, inositol hexaphosphate, carbamide, acetic acid, phytic acid, a permeable compound and water; s2, first-time mixing treatment and S3, second-time mixing treatment. The invention relates to the technical field of fire-fighting liquid preparation. According to the preparation method of the environment-friendly anti-freezing corrosion-resistant fire-fighting liquid, tris (2, 3-dibromopropyl) isocyanurate, melamine cyanurate and tribromophenol are added into the fire-fighting liquid, so that the flame-retardant effect of the fire-fighting liquid is greatly improved, and the fire-fighting liquid is well improved by adding inositol hexaphosphate, acetic acid and phytic acid into the fire-fighting liquid. Therefore, the flame-retardant effect and the corrosion resistance of the anti-freezing fire-fighting liquid are greatly enhanced.