65 results about "Bromamine acid" patented technology

The invention provides a method for synthesizing anthraquinone type dye or chromophore by aromatic amination of bromamine acid. The method comprises the following steps: catalyzing a condensation reaction of bromamine and arylamine in a solvent by adopting a catalyst system containing cuprous complex. According to the method, the cuprous complex is used as the catalyst system, nearly 100% conversion of the bromaine acid can be realize, no bromamine acid hydrolyzed (purple byproduct) or debrominated byproduct is generated, generation of by products is remarkably reduced, the yield of condensation products is remarkably increased, emission of acid-containing wastewater with deep chromaticity is reduced; and copper powder is not used, the usage of catalyst can be reduced, the content of heavy metals in the condensation products can be reduced, the content of heavy metals in wastewater can be reduced, environmental pollution can be reduced, and production cost can be reduced.

The invention discloses a method for preparing active dye for blue wool. The preparation method comprises the following steps of: performing first condensation reaction on bromamine acid which serves as a raw material and phenylene diamine, and performing acid refining, sulfonation, second condensation reaction and aftertreatment to obtain the active dye. The method is advanced and low in cost and causes light pollution to the environment. The dye prepared by the method has bromo-acrylamide groups, and under a slightly acidic condition, by being used together with Sibagol B, the active dye has a high reactivity with wool and a high fixation rate and meets the 'machine washable' high fastness requirement of International Wool Secretariat, so the active dye is quite high in market competitiveness.

The invention relates to a method for recovering o-dichlorobenzene through a sulfonation process of bromamine acid produced by a solvent method, which comprises the following steps of: after 1-amino-anthraquinone is sulfonated by the chlorosulfonic acid in an o-dichlorobenzene solvent, adding 93-96 percent of sulfuric acid to extract 1-amino-anthraquinone-2-sulfonic acid from an o-dichlorobenzene layer; and carrying out distilling under reduced pressure on sulfuric acid solution to recover the o-dichlorobenzene. The sulfuric acid solution recovering the o-dichlorobenzene can be directly bromized. The method has the beneficial effects that the recovery rate of the o-dichlorobenzene reaches above 98 percent, the recovery rate of the solvent o-dichlorobenzene is greatly improved, the emission of an organic solvent is reduced, the environment is protected, and meanwhile, the energy consumption is low.

The invention discloses a preparation method of bromaminic acid sodium salt and an intermediate of the bromaminic acid sodium salt and a solvent recovery method. The preparation method of 1-aminoanthraquinone-2-sulfonic acid comprises the following steps that (1) in an inert solvent, a sulfonation reaction is conducted on 1-aminoanthraquinone and chlorosulfonic acid; (2) secondly, after the sulfonation reaction in the step (1) is ended, layered extraction is conducted with concentrated sulfuric acid, the upper layer is a solvent organic phase layer, and the lower layer is a material layer containing the 1-aminoanthraquinone-2-sulfonic acid and sulfuric acid. By the adoption of the preparation method of the 1-aminoanthraquinone-2-sulfonic acid, the extraction layering is complete, and the yield of the 1-aminoanthraquinone-2-sulfonic acid is high. Meanwhile, a method of recycling the solvent with water is adopted, the recycled solvent can be directly used for preparation of bromamine acid and sodium slat of the bromamine acid, and the bromamine acid is high in yield.

The invention provides an integrated method for catalyzing the condensation reaction of bromamine acid by using solid acid and degrading waste water produced by the condensation reaction. The method comprises the following steps of: preparing a solid acid catalyst SO42-/TiO2, forming a catalytic system of the condensation reaction of bromamine acid, forming an integrated system used for the catalysis of the condensation reaction of bromamine acid by using the solid acid catalyst SO42-/TiO2 and photocatalytic degradation of the waste water produced by the condensation reaction, and recycling the solid acid catalyst SO42-/TiO2. The integrated method has the advantages that: the method for preparing the solid acid catalyst SO42-/TiO2 is simple, the catalytic activity is high, the solid acid catalyst SO42-/TiO2 can be used for catalyzing the condensation reaction of bromamine acid for reducing a temperature needed for the reaction system, increasing a reaction yield, avoiding the use of solution H2SO4 and lowering difficulty in processing the production waste water in following steps, and the solid acid catalyst SO42-/TiO2 can be recycled after the reaction; and simultaneously, the production waste water used for the condensation reaction of bromamine acid is subjected to photocatalytic degradation, the decoloring rate of the production waste water is over 85 to 96.22 percent, the removal rate of TOC is 51 to 86 percent, the environmental pollution is lowered, and the integration of the solid acid catalysis reaction and the processing of the production waste water is realized.

The invention discloses bacteriostatic acid dye. The bacteriostatic acid dye is prepared from resorcinol, bromamine acid, sodium poly[(naphthaleneformaldehyde)sulfonate], sodium silicate, triphenylphosphine-3,3',3''-trisulfonic acid trisodium salt, pyrazolone, chitosan, nano-copper particles, nano-cuprous oxide particles, deionized water, a defoaming agent and an auxiliary. According to the bacteriostatic acid dye, the stability is high, and use is convenient; by optimizing the dye components and cooperatively using the home-made auxiliary, the coloring power of the dye is enhanced, the problem that the color fixing effect of traditional acid dye on a chinlon fabric dyed by the acid dye is not ideal is solved, and the effect of the wet treatment fastness is greatly improved; in the preparing process of the acid dye, the components are divided into two parts to be processed through mixing separately and then processed through total mixing, and by cooperating with the added auxiliary, the dye components can be greatly homogenized, and the coloring effect and the coloring quality of the dye are improved; the dye has the very good antibacterial property on escherichia coli, staphylococcus aureus and candida albicans.

The invention discloses a method for preparing blue reactive dyes. The method comprises the following steps: (1) primary condensation reaction, to be specific, taking copper sulfate pentahydrate, ferrous chloride or a mixture of copper sulfate pentahydrate and ferrous chloride as a catalyst, and enabling bromamine acid and M acid to be subjected to the condensation reaction; (2) refining, to be specific, refining all primary condensation compounds; (3) secondary condensation reaction, to be specific, enabling the refined compound and cyanuric chloride to react to obtain secondary condensation compounds; (4) ternary condensation reaction, to be specific, enabling the obtained secondary condensation compounds and aminobenzene sulfonic acid to react to obtain ternary condensation compounds, filtering, spray drying and packaging, so as to obtain the product. The method can synthesize a new blue reactive dye and has the advantages that the cycle of reaction is shortened, the reaction yield is increased, the reaction is more thorough, the reaction process is clean and environmentally-friendly, the sewage quantity is less, and the prepared product has bright colors.

The invention relates to a luleitadingmione oral calving tablet which can treat allergic rhinitis, etc. wherein, it has quick adsorption, high biological utilization, and simple intake method without water. It uses Loratadine and bromamine acid as materials, with some findings.

The invention relates to a preparation method of a water-soluble blue printing dye. The method includes the following steps of 1, dissolving M acid in water, adding bromamine acid, controlling pH to main within 8.0-8.5, raising the temperature to 70-80 DEG C for conducting a first condensation reaction, and adding a solid-supported catalyst in batches during the condensation reaction, wherein themolar ratio of M acid to bromamine acid is (1.8-2.2):1; 2, after the first condensation reaction is completed, adding water and diatomaceous earth and conducting stirring and filtering, adjusting thepH of the filtrate to 1.5-2.0, conducting filtering again, and adjusting the pH of the filtrate to neutrality to obtain a blue-based intermediate liquid; 3, after cyanuric chloride is subjected to icebath, beating and dispersion, adding the blue-based intermediate liquid, controlling the temperature to main within 3-8 DEG C and the pH to more than 6.0, and conducting a second condensation reaction; 4, after the second condensation reaction is completed, adding a mixture of m-aminobenzenesulfonic acid and p-aminobenzenesulfonic acid, raising the temperature to 40-45 DEG C, maintaining the pH within 6.0-7.0, and conducting a third condensation reaction to obtain raw pulp of the blue dye. The method can solve the problem that a large amount of high-COD high-salt colored wastewater is produced by traditional salting-out refining methods.

The invention relates to the technical field of dyes, in particular to a bromamine acid sodium salt bromination process which comprises the following steps: carrying out sulfonation reaction on 1-aminoanthraquinone and chlorosulfonic acid in an inert solvent to obtain 1-aminoanthraquinone-2-sulfonic acid; after the sulfonation reaction is finished, diluting the liquid with water, performing standing treatment for layering to remove an inert solvent layer, and recycling the solvent by a distillation kettle; pumping an aqueous solution of the sulfonation liquid into a bromination kettle to be subjected to bromination reaction with hydrobromic acid and an oxidizing agent; and alkalizing, filtering and refining the bromination reaction product to obtain the high-quality bromaminic acid sodiumsalt. The invention provides the bromination reaction process of bromamine acid sodium salt, wherein the hydrobromic acid and an oxidizing agent which are low in price and easy to obtain are selected;the reaction temperature is controlled at 30-35 DEG C, the brominated product is filtered and refined to obtain high-quality bromamine acid sodium salt, the generation of byproduct sodium chloramineis reduced, the purity is improved by 0.1-0.3% and reaches 99.6% or above compared with the prior art, and the generated wastewater is also easy to treat. The method is a new safe, green and environment-friendly production process.

The invention provides a method for preparing acid blue 260, which comprises the following steps: condensing bromamine acid and trimethylaniline, removing auxiliary lac dyes, refining for three times, activating, icing, neutralizing, refining again, drying, adjusting the color and the strength and packaging finished products. The method for preparing acid blue 260 consumes less raw material consumption, has high dye rate, generates less auxiliary lac dyes, improves the yield of the dyes and plays a promotion role in environmental protection.

The invention provides a method for preparing reactive brilliant blue 3G for wool. The method comprises the following steps of: (1) condensing bromamine acid and p-amine acetanilide under the action of a catalyst, and acidifying to obtain a condensation product; (2) sulfonating the condensation product by using fuming sulfuric acid, and performing basic hydrolysis to remove acetyl; and (3) condensing a hydrolysis product with 2,3-dibromo propionyl chloride, and performing debromination to prepare a reactive brilliant blue 3G dye. The preparation method provided by the invention is low in cost, energy consumption and pollution, and is suitable for industrial large-scale production. Various application performance indexes of the reactive brilliant blue 3G for wool, which is obtained by the preparation method provided by the invention, reach or exceed those of products of foreign companies.

The invention discloses a modified attapulgite used for immobilizing polycyclic aromatic hydrocarbon degrading bacteria. A preparation method of the modified attapulgite comprises the following steps: modifying attapulgite with a mixed solution prepared from sodium bicarbonate, cinnamaldehyde, 3-oxacyclobutanone, dibromobenzoquinone, methyl salicylate, anisole and laurene to prepare a substance B; modifying the substance B with a mixed solution prepared from isobutyl mercaptan, hexyl sulfide, o-chlorocinnamic acid and 3-methylthiophene to prepare a substance D; modifying the substance D with a mixed solution prepared from N-acetyl-DL-phenylalanine, 5-hydroxytryptophan and 3.3 g of D-homophenylalanine to prepare a substance F; and modifying the substance F with a mixed solution prepared from hydroxy propyl cellulose, galacturonic acid and bromamine acid to prepare a substance which is the modified attapulgite used for immobilizing polycyclic aromatic hydrocarbon degrading bacteria.

The invention discloses a treatment process of bromamine acid neutralizing wastewater. The treatment process mainly includes flocculation, electroreduction, low-temperature wet oxidation, electrodialysis and bipolar membrane dialysis. The treatment process using 'flocculation-electroreduction-LCWO-electrodialysis and bipolar membrane dialysis' as the main line has the advantages that the treatment process specially aims at the alkaline wastewater generated during the production of bromamine acid dye, the residual organic matter in the wastewater is gradually separated in a targeted manner, the COD and color in the wastewater are removed, acid and alkali of certain concentration are produced, and the treatment process is continuous and automatic in process flow, mild in reaction condition, simple to operate and evident in effect and has certain economic benefits.

The invention relates to a method of mineralization of aerobiont of bromamine acid, belonging to the technical field of water treatment of environmental engineering. The method is characterized in that high-efficiency absorbing material is added into an aerobiont reactor, and not only can be used as carrier fixed microorganism but also can be used as decolorizing products so as to lead the decolorizing products in liquid phase to keep lower concentration; and in the regeneration process of in-situ or of the absorbing material, the degradation rate of the decolorizing products is larger than the autooxidation rate thereof, thus effectively avoiding the autooxidation of the decolorizing products and leading the bromamine acid to be mineralized completely. The method of mineralization of aerobiont of bromamine acid has the effects and benefits that the used high-efficiency absorbing material has wide source and simple and convenient technological operation, effectively solves the problem that the complete biodegradation is blocked by autooxidation products hard to degrade formed in the decolorization of the aerobiont of the bromamine acid, provides an aerobic mineralization of the bromamine acid technology being economic and high efficiency and has wide application prospect in the treatment of the waste water of anthraquinone dye and intermediates thereof.

The invention provides a method for synthesizing 1-amino-anthraquinone-2-sulfonic acid from 1-amino-anthraquinone. The method comprises the following steps: generating a sulfate solid of 1-amino-anthraquinone through reaction of the 1-amino-anthraquinone and sulfuric acid, and then performing transposition on the sulfate solid of the 1-amino-anthraquinone to generate the 1-amino-anthraquinone-2-sulfonic acid. A process of synthesizing the 1-amino-anthraquinone-2-sulfonic acid by a sulfuric acid method is fundamentally improved; the sulfate of the 1-amino-anthraquinone is efficiently subjectedto transposition reaction under a solid-phase condition without a solvent after generated water is removed, so that the reaction yield is high, and no side effects are caused; furthermore, no 1-amino-4-chloroant-2-sulfonic acid is generated, and no wastewater, waste gas and waste residues are generated; an obtained product is further synthesized into bromamine acid, and the purity of the obtainedbromamine acid is close to 100 percent; the quality and the yield of the bromamine acid are both higher than the quality and the yield of bromamine acid synthesized by a chlorosulfonic acid method, afuming sulfuric acid method and a conventional sulfuric acid method.

The invention provides a preparation method of a reactive brilliant blue K-GR intermediate. The preparation method comprises following steps: carrying out a condensation reaction between bromamine acid and 2,4-diaminobenzene sulfonic acid or sodium 2,4-diaminobenzene sulfonate with a catalyst system containing a cuprous complex for catalyzing the reaction to obtain the reactive brilliant blue K-GR intermediate (sodium 1-amino-4-((4-amino-3-sulfonylphenyl)amino)-anthraquinone-2-sulfonate). By means of the preparation method of the reactive brilliant blue K-GR intermediate, usage amounts of cuprous chloride and copper powder can be effectively reduced, thereby reducing the content of heavy metals in a dye product, reducing the content of heavy metals in waste water and reducing environmental pollution and production cost. In addition, the preparation method can avoid generation of a hydrolyzed by-product (a purple by-product) of the bromamine acid, can greatly reduce the generation of a debromination by-product, can significantly reduce the generation of a double-condensation substance, can increase yields of the condensation reaction and the dye product and can reduce discharge amount of waste water containing acids and being high in chroma.

The invention discloses a preparation method for bromamine acid. The preparation method comprises the following steps: 1) taking 1-amino anthraquinone as a raw material and reacting with fuming sulfuric acid and sodium sulfate in a solvent, thereby acquiring a reaction liquor containing sulfonating products, wherein temperature of sulfonating reaction is at 100-150 DEG C and reaction time is 3-10h; 2) cooling the reaction liquor to 60-80 DEG C, adding iodine and anti-foaming agent, slowly dropwise adding bromine for 5-8h, and keeping temperature for 2-3h after the ending of dropwise adding; 3)ending bromination reaction, removing excessive bromine through reduced pressure distillation, adding a certain amount of water, cooling to 50-60 DEG C and filtering, thereby acquiring bromamine acidsulfate; 4) placing bromamine acid sulfate into a large amount of water, heating to 70-90 DEG C, adding sodium hydroxide for regulating pH to 8-9, cooling to 20-30 DEG C and performing suction filtration, thereby acquiring the product bromamine acid. The yield of product is 91% and the purity detected through liquid chromatogram is 99%.

The invention discloses a method of preparing 1,4-diaminoanthraquinone-2-sulfonic acid. According to the method, bromamine acid is taken as a raw material and ammoniated in an ammonia water medium to directly obtain 1,4-diaminoanthraquinone-2-sulfonic acid. The method specifically comprises the following steps: uniformly mixing diluted ammonia water, bromamine acid and sodium carbonate in a pressure container in a mass ratio of (4 to 10):1:(0.1 to 0.3), heating while stirring, heating to 70-110 DEG C within 1-2 hours, insulating for 2-4 hours, cooling to 50-60 DEG C after the reaction is concluded, heating to distill off ammonia water occupying 30-40% of the volume of the mother liquor, then cooling to 50-70 DEG C, adjusting the pH value to 1-1.5 by hydrochloric acid or sulphuric acid, and filtering to obtain a 1,4-diaminoanthraquinone-2-sulfonic acid filter cake. According to the method disclosed by the invention, because the purity of the bromamine acid raw material is high, the contents of industrial products are generally greater than 99%, and moreover, obvious by-products are not generated during the reaction process, and high-purity 1,4-diaminoanthraquinone-2-sulfonic acid can be obtained during production.

The invention relates to a method for manufacturing a pigment red 3BL condensation intermediate, which is characterized by comprising the following steps of: adding 25 parts by weight of bromamine acid and 280 to 450 parts by weight of catalysts consisting of an organic solvent, a surface active agent and copper powder into to a 500-mL four-neck bottle provided with a thermometer, a stirrer and a reflux condensing tube; stirring the mixture for reacting for 150 min at 68-72 DEG C, filtering when the mixture is hot , moving the filtrate to a distilling bottle for distilling and recycling the organic solvent; after the organic solvent is distilled, adding 300 to 350 parts by weight of hot water, heating to boiling, adding 50 parts by weight of sodium chloride at 70 to 80 DEG C, salting out and filtering; washing a filter cake washed by 10% sodium chloride solution, and then, drying the washed filter cake in a drying box to obtain the pigment red 3BL condensation intermediate. The invention has the advantages of having high activity and good chemical stability, improving the reaction speed and productivity, having no corrosion to equipment and low cost, and realizing zero discharge of acid containing waste water.

The invention relates to the technical field of chemistry and chemical engineering, and discloses a method for synthesizing 2,4-dinitro-6-bromoaniline by using bromamine acid product wastewater. The method comprises the steps of 1, adding sodium cyanide for reaction, synthesizing a disperse dye from byproducts in mother liquor and separated trace main products, filtering, and washing a filter cake with hot water to obtain the disperse dye; 2, adding an oxidizing agent into the filtrate and the washing liquid to oxidize and remove sodium cyanide, then reacting with 2,4-dinitroaniline, pulping in a sulfuric acid medium, dropwise adding sodium chlorate, reacting at the temperature of 35-75 DEG C, filtering the reaction liquid after bromination, washing a filter cake until the pH value is 6-7, and drying to obtain the product 2,4-dinitro-6-bromoaniline; and 3, decolorizing the mother liquor with activated carbon, performing membrane treatment, concentration and separation, recycling low-concentration salt water, and spraying high-concentration salt to be dry to serve as industrial salt (or serving as an active or acid dye assistant for internal digestion of a company). The problems of high COD and high-salt mother liquor wastewater of bromamine acid dye products in the prior art are solved.

The invention relates to a method for preparing an improved reactive dye brilliant blue KN-R. The preparation method improves color radicle esterification rate, quality, color fixing rate and hoisting rate. Specifically, the invention provides a method for preparing a reactive dye brilliant blue KN-R used for fur, the method comprises condensation, refining, esterification and dilution of bromamine acid and metaposition oil and is characterized in that in esterification, 100% sulphuric acid is adopted, so that chromophore esterification is more complete.