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

The invention discloses a Pseudomonas aeruginosa strain TBPY, which is screened from tribromophenol(TBP)-polluted sludge and purified. The purified strain is domesticated by a pressure type domesticating method with gradually increased TBP concentration in an organic salt culture medium, and the domesticated strain can be used for the biological control of waste water containing persistent organic pollutants such as phenol, pyrocatechol, resorcinol, benzoic acid, p-hydroxybenzoic acid, vanillin, 4-chlorophenol, 2,4-dichlorophenol, trichlorophenol and tribromophenol and has high research and application values.

The synthesis of fire retardant tri(bromophenoxy) cyanurate inside two-phase solution of water solution and organic solvent includes the following steps: reaction of bromized phenol and sodium hydroxide to produce bromized phenol sodium; and the reaction of bromized phenol sodium and cyanurichloride in the presence of catalyst and at proper temperature to produce tri(bromophenoxy) cyanurate. The catalyst is quaternary ammonium salt and quaternary phosphonium salt, and the proper temperature includes cyanurichloride dropping temperature of 20-35 deg.c and reaction temperature after finishing dropping of 40-55 deg.c. The bromized phenol may be bromophenol, dibromophenol or tribromophenol. The synthesis process of the present invention has high safety and low cost and is suitable for industrial production.

The invention relates to an optimized production method of Tri (tribromophenyl) cyanurate. Chlorobenzene is added into a reactor, phenol is added, hydrogen peroxide and bromine are dropwise added into the reactor in a staggering manner, extraction is performed by the aid of the chlorobenzene, a tribromophenol and chlorobenzene mixed liquid is obtained, cyanuric chloride is added into the mixed liquid, an initiating agent CTAB (cetyl trimethyl ammonium bromide), anhydrous sodium carbonate and methylbenzene are added for reaction, and a crude product is transferred to a heating kettle, the product is subjected to pressure reduction and suction filtration in a heating and dissolving state and is finally transferred to a distillation kettle and stirred and crystallized, edulcoration is realized before unit cell arrangement, and the product is obtained. According to the optimized production method of Tri (tribromophenyl) cyanurate, the produced by-products are reduced, the yield is improved, and the product quality is higher.

The invention discloses a method for continuously producing tri(tribromophenoxyl)triazine and production equipment used in the method. The method comprises the steps as follows: (1) an alkaline aqueous solution of tribromophenol and an organic solution of cyanuric chloride enter a raw material mixer to be mixed in the presence of a phase transfer catalyst, and then, the obtained mixture enters a tubular packed mixer to react through a circulating pipeline; (2) a primary product enters a reactor through the circulating pipe to react continuously; (3) the obtained material passes through a delivery pump and a cooler from the bottom of the reactor and enters the raw material mixer to be mixed and then subjected to a circular reaction; (4) a produced material flows out of an overflow port of the reactor and then is separated and purified, the product, namely, tri(tribromophenoxyl)triazine, is obtained. The method is simple to operate, the process is easy to control, the product has high yield and purity, continuous production can be realized, and the production efficiency can be effectively improved.

The invention relates to a synthesis method of a Beraprost sodium intermediate (III). Cyclopentene and N-bromo-succinimide (NBS) carry out free radical reaction to obtain dibromocyclopentene; and dibromocyclopentene reacts with 2,4,6-tribromophenol to directly generate 3,5-bis(2,4,6-tribromophenoxyl) cyclopentene (compound I) through a one-pot method. Then through Grignard reactions, a compound (I) and a compound (II) are obtained. N-bromo-succinimide and a commercial product namely cyclopentene are taken as the raw materials to synthesize dibromocyclopentene, 170 DEG C cracking and ultralow temperature reactions (-40 to -30 DEG C) are avoided, the using of bromine is also avoided, the reaction conditions are milder, and the synthesis method is more environmentally friendly and is convenient for industrial production.

The invention relates to a silicic acid-3-(3-bromophenyl)-chloropropyl ethyl ester compound used as a fire retardant and the preparation method thereof. The structural formula of the compound is shown in the specification. The preparation method comprises the following steps: filling ethylene oxide of which the mole is same as that of silicon tetrachloride in silicon tetrachloride organic solution at the temperature of below 20 DEG C, adding tribromophenol of which is three times the mole of silicon tetrachloride, carrying out the thermal reaction for 6-10 hours at the temperature of 100-120 DEG C, and reducing pressure and distilling to remove solvent and a small amount of low boiling point substances to obtain the silicic acid-3-(3-bromophenyl)-chloropropyl ethyl ester compound. The silicic acid-3-(3-bromophenyl)-chloropropyl ethyl ester compound is an excellent fire retardant plasticizer, has carbon-forming and anti-dripping functions and good compatibility with high polymer material, can be used as fire retardants made of polyvinyl chloride, unsaturated polyester, polyurethane, epoxy resin and the like, and is easy to access in raw material, low in production cost, small in equipment investment, simple in production technology, and easy for large-scale production.

The invention discloses a process and a device for continuously synthesizing tribromophenol by using microreactors, belonging to the technical field of tribromophenol synthesis. The process comprises the following steps that a phenol dichloroethane solution and deionized water enter a microreactor I through a metering pump and are fully mixed, and then enter a microreactor II for a reaction with a metered bromine dichloroethane solution; after a full reaction in a microreaction pipeline I, a formed mixture enters a microreactor III to continue to react with a hydrogen peroxide solution; after a full reaction in a microreaction pipeline II, the mixture is pumped into a curing kettle; and after curing, a tribromophenol product is obtained through post-treatment. The invention also discloses a device for continuously synthesizing tribromophenol. The device comprises the microreactors and the microreaction pipelines. According to the method, a reaction rate is increased, the problems of long tribromophenol production time, incapability of continuous production, low safety performance and the like of the existing intermittent reactor are solved, and the method has an important application prospects.

The invention discloses a synthesis method of 2, 4, 6-tribromophenol, which comprises the following steps: dissolving phenol and metal bromide in water to obtain a mixed solution of phenol and metal bromide, and recording the mixed solution as a first mixed solution; dropwise adding a bromate solution and hydrochloric acid into the first mixed solution for reaction; and after the reaction is finished, adding sodium sulfite into the reaction liquid until the light brown color in the reaction liquid completely disappears, filtering, washing and drying to obtain the 2, 4, 6-tribromophenol. According to the synthesis method disclosed by the invention, the bromide salt is used as a bromine source, so that available resources are fully utilized, and the use of an organic solvent is avoided; after the reaction is finished, a crude product is separated out in a water phase, and a product with enough purity is obtained after simple filtering treatment; according to the process method, the production cost is greatly reduced, meanwhile, potential safety hazards in transportation and production are reduced, and the working environment is improved.

The invention relates to a flame-retardant epoxy resin composition comprising, based on the total weight of the composition, A) 25-65% by weight of an epoxy resin, B) 16-30% by weight of a brominated epoxy resin having end-capping groups selected from epoxy groups and tribromophenol groups, and C) 10-25% by weight of an organophosphorus flame retardant. In addition, the invention also relates to a method for preparing a composite material by using vacuum infusion of the flame-retardant epoxy resin composition and to an article obtained by the method.

The invention relates to the technical field of chemical analysis, in particular to a conjugated microporous polymer and a preparation method and application thereof. A repeating unit of the conjugated microporous polymer is shown in the specification, and the conjugated microporous polymer is formed by polymerizing two monomers, namely 1, 3, 5-tri (4-acetylene phenyl) benzene and tribromophenol. The OH-CMP material is of a spherical structure, has an average diameter of 30-50 nm, has high hydrophobicity, has a specific surface area up to 534 m < 2 >. G <-1 >, and has high thermal stability and chemical stability. The OH-CMP has relatively high specific surface area, excellent adsorption capacity and satisfactory repeatability. A novel method for analyzing triazine herbicide pollutants in the environment and food samples by solid-phase extraction-liquid chromatography-tandem mass spectrometry established on the basis of the material is wide in linear range and low in detection limit, and results can meet detection requirements. The polymer has a good application potential in rapid analysis of triazine herbicide pollutants in environment and food.

The invention discloses a production process of high-whiteness and high-thermal-stability bromotriazine, and relates to the technical field of flame retardants, phenol and an organic solvent are added into a reaction kettle, and then bromine and hydrogen peroxide are added to prepare an intermediate product tribromophenol; according to the method, tribromophenol and cyanuric chloride are catalyzed to react under an alkaline condition by using a compound catalyst to prepare bromo-triazine. The bromo-triazine prepared by the method has high whiteness, high thermal stability, high purity and good product quality.

A flame retardant composition for flammable plastic materials and a method for producing the same are disclosed. The flame retardant composition comprises 2,4,6-tris(2,4,6-tribromophenoxy)-1,3,5-triazine that contains 1 to 1000 ppm of a metal species of a water-insoluble polyvalent metal compound selected from the group consisting of oxide, hydroxide, carbonate, phosphate, sulfate and silicate present in the particles of 2,4,6-tris(2,4,6-tribromophenoxy)-1,3,5-triazine. The flame retardant composition is produced by reacting an alkali metal salt of 2,4,6-tribromophenol and cyanuric chloride in the presence of said water-insoluble polyvalent metal compound.

The invention discloses a preparation method for a beraprost intermediate. The preparation method comprises the following steps: (1) preparation of cyclopentadiene: a step of weighing dicyclopentadiene, adding BHT, carrying out heating to 180-200 DEG C for distilling, collecting fractions at 40-50 DEG C, and after collection is finished, carrying out secondary distillation so as to obtain the cyclopentadiene; and (2) preparation of the beraprost intermediate: a step of adding the cyclopentadiene into a solvent A, carrying out cooling in a cold trap to minus 72 DEG C, diluting a bromine reagentwith the solvent A, slowly dropwise adding a solvent A solution of the bromine reagent, controlling a temperature at minus 70 DEG C, and carrying out a reaction so as to obtain 3,5-dibromocyclopentene, then dissolving 2,4,6-tribromophenol into an anhydrous solvent B, carrying out a reaction, and carrying out post-treatment operation B so as to prepare the beraprost intermediate. By adoption of the preparation method disclosed by the invention, impurities generated in the process production process are effectively reduced; the yield is improved; meanwhile, the process is green and environmentally-friendly; and the cost of environmentally-friendly treatment is reduced.

The invention relates to a synthesis method of 2,4,6-tribromophenyl allyl ether, which solves the problem of complex synthesis process, slow process of etherification reaction, serious hydrolysis of allyl chloride, low product yield and dark product color in the prior art , Low purity affects the technical problem of flame retardant performance. The present invention provides a kind of synthetic method of 2,4,6-tribromophenyl allyl ether, it comprises the following steps successively: 1) the synthesis of the ethanol solution of tribromophenol sodium salt: add catalyst in the organic solvent of phenol 1. Add brominating agent at 15-20°C, then raise the temperature to 25-30°C and keep warm to react to obtain tribromophenol; then add tribromophenol to the ethanol solution of sodium ethoxide to obtain the ethanol solution of tribromophenol sodium salt; 2) Synthesis of 2,4,6-tribromophenyl allyl ether: add dispersant and catalyst II to the ethanol solution of tribromophenol sodium salt prepared in step 1), and drop the ethanol solution of allyl chloride , keep warm until the end of the reaction to get 2,4,6-tribromophenyl allyl ether. The invention is widely used in the field of flame retardant synthesis.

The invention relates to a fire retardant silicic acid di(tribromophenyl)dichloroethyl ester compound and its preparation method. The structure of the compound is shown in the specification. The preparation method comprises the following steps: controlling the temperature to below 20 DEG C, letting equimolar oxirane be blown below the liquid level of a silicon tetrachloride organic solution, adding tribromophenol which accounts for two times larger than equimolar oxirane, keeping the temperature at 65-90 DEG C and reacting for 3-6h, letting a certain mol ration of oxirane be blown below the liquid level, keeping the temperature at 40-60 DEG C and reacting for 2-4h, and carrying out underpressure distillation to remove a solvent so as to obtain a product silicic acid di(tribromophenyl)dichloroethyl ester. The silicic acid di(tribromophenyl)dichloroethyl ester provided by the invention is an excellent flame retardation plasticizer, has charcoal-forming and antidrip effects, has good compatibility with a high-molecular material, and can be used as a fire retardant of materials such as polyvinyl chloride, nonsaturated polyester, polyurethane and epoxy resin, etc. Raw materials of the fire retardant provided by the invention are cheap and easily available. Production costs are low. Equipment investment is little. The production technology is simple. The preparation method is easy for large-scale production.

The invention relates to a fire retardant dibromopropyl tri(tribromophenoxy)silane compound and its preparation method. The structure of the compound is as shown in the formula in the specification, wherein R2=CH2Br when R1=H; and R2=H when R1=CH2Br. The preparation method comprises the following steps: dropwisely adding equimolar dibromopropyl alcohol into a silicon tetrachloride organic solution at 8 DEG C, keeping the temperature at 35 DEG C to react for 1h, adding three molar rations of tribromophenol, reacting at 90-120 DEG C for 8-11h, neutralizing free acid by the use of oxirane, and carrying out underpressure distillation to remove a solvent so as to obtain a product dibromopropyl tri(tribromophenoxy)silane. The product is an excellent flame retardation plasticizer, has charcoal-forming and antidrip effects, and can be used as a fire retardant of materials such as polyvinyl chloride, nonsaturated polyester, polyurethane and epoxy resin, etc. Raw materials of the product are cheap and easily available. Production cost is low. Equipment investment is little. The production technology is simple. The preparation method is easy for large-scale production.

The invention relates to a fire retardant tribromophenoxy tri(dichloro propanolato)silane compound and its preparation method. The structure of the compound is as shown in the formula in the specification, wherein R2=CH2Cl when R1=H; and R2=H when R1=CH2Cl. The preparation method comprises the following steps: dropwisely adding equimolar dichlorohydrin into a silicon tetrachloride organic solution to react at 35 DEG C for 1h, adding equimolar tribromophenol to react at 50-80 DEG C for 2-5h, dropwisely adding double mole times of dichlorohydrin to react at 50-70 DEG C for 3-6h, and carrying out underpressure distillation to remove a solvent so as to obtain a product tribromophenoxy tri(dichloro propanolato)silane. The product is an excellent flame retardation plasticizer, has charcoal-forming and antidrip effects, and can be used as a fire retardant of materials such as polyvinyl chloride, nonsaturated polyester, polyurethane and epoxy resin, etc. Raw materials of the product are cheap and easily available. Production costs are low. Equipment investment is little. The production technology is simple. The preparation method is easy for large-scale production.

The invention discloses an efficient constant-temperature process for preparing tribromophenol by a sodium bromide method, wherein the process comprises the following steps: a) pre-reaction: adding raw materials and a solvent into a constant-temperature reaction kettle to obtain a solid-liquid mixture A, wherein the raw materials comprise phenol, sodium bromide, water and hydrochloric acid, and the solvent is dimethyl sulfoxide; b) dropwise adding a reaction reagent: dropwise adding a hydrogen peroxide solution into the constant-temperature reaction kettle in the step a); c) reacting and stirring: reacting to obtain a solution B; d) constant-temperature reaction: performing constant-temperature water bath on the solution B to obtain a solid-liquid mixture C; e) concentration: transferring the solid-liquid mixture C into a constant-temperature evaporation concentrator, and adding water for constant-temperature evaporation to obtain a solid D; f) washing: washing the solid D with water and carrying out vacuum filtration; and g) drying: placing the solid D in a drying oven and drying to obtain the tribromophenol. The invention relates to the technical field of chemical production, and in particular, relates to the efficient constant-temperature process for preparing the tribromophenol by the sodium bromide method, wherein the process can reduce the production cost and improve the utilization rate of the raw materials.

The invention discloses a process for recovering and reusing tribromophenol in bromotriazine production wastewater, and relates to the technical field of chemical wastewater treatment. The method comprises the following steps: adjusting the pH value of alkaline wastewater containing tribromophenol to 1-2 by using hydrochloric acid, and separating out white precipitate tribromophenol; adding dichloromethane for extraction, standing for 20-60 minutes, filtering, filtering an organic phase for later use, and discharging acidic wastewater into a wastewater collection tank; transferring the recovered organic phase into a reaction kettle, adding a sodium sulfite solution, heating, stirring for 30 minutes, and recovering; the method comprises the following steps: adding deionized water and alkali liquor into a recycled tribromophenol organic phase and a newly prepared tribromophenol organic phase, adjusting the pH value, and adding a catalyst and cyanuric chloride to prepare bromotriazine. According to the method, the recovered tribromophenol is used for preparing the bromo-triazine, so that the treatment cost and the peculiar smell of a workshop are reduced, the solid waste in the workshop is reduced, and the solid waste recovery rate is increased.

The invention relates to a flame retardant tri(dibromopropyl)tribromophenyl silicate esterification compound and a preparation method thereof. The structure of the compound is shown in the specification, wherein R2=CH2Br if R1=H; and R2=H if R1=CH2Br. The preparation method comprises the following steps of: dropwise adding equimolar dibromopropyl alcohol into an organic solvent of silicon tetrachloride at a temperature below 8 DEG C, and reacting for 1 hour at 35 DEG C; adding equimolar tribromophenol, and reacting for 2-4 hours at 50-80 DEG C; dropwise adding dibromopropyl alcohol of twice molar weight, and reacting for 3-5 hours at 50-70 DEG C; and performing reduced-pressure distillation to remove the solvent to obtain the product tri(dibromopropyl)tribromophenyl silicate. The product is an excellent flame-retardant plasticizer with a charring anti-drop effect and can be used as a flame retardant for the materials such as polyvinyl chloride, unsaturated polyester, polyurethane, epoxy resin and the like; and moreover, the flame retardant has the advantages of cheap and easily-available raw materials, low production cost, low equipment investment and simple production technology, and is easy to produce in a large scale.