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39 results about "Oleum" patented technology

Oleum (Latin oleum, meaning oil), or fuming sulfuric acid, is a term referring to solutions of various compositions of sulfur trioxide in sulfuric acid, or sometimes more specifically to disulfuric acid (also known as pyrosulfuric acid). Oleum is identified by the CAS number 8014-95-7 (EC/List number: 616-954-1 ; ECHA InfoCard: 100.116.872).

Method and system for efficiently utilizing phosphate fertilizer byproducts

The invention belongs to the field of inorganic chemical industry, and particularly relates to a method and a system for efficiently utilizing a phosphate fertilizer byproduct, the method comprises the following steps: carrying out acidolysis on fluosilicic acid with the concentration of more than or equal to 45% wt and concentrated sulfuric acid to generate a mixed solution of silicon tetrafluoride gas and fluorosulfonic acid; the mass ratio of the fluosilicic acid to the concentrated sulfuric acid is controlled to be 1: (4-15); pyrolyzing the obtained fluorosulfonic acid to generate dilute sulphuric acid, hydrogen fluoride and water vapor, forming 98% concentrated sulphuric acid from part of dilute sulphuric acid and fuming sulphuric acid, drying hydrogen fluoride to obtain crude hydrogen fluoride gas, and condensing and rectifying to obtain anhydrous hydrogen fluoride; the rest dilute sulphuric acid is partially compounded and then returned for acidolysis, and the rest dilute sulphuric acid is used for producing white carbon black and flows back to a wet-process phosphoric acid system; and circularly absorbing the obtained silicon tetrafluoride gas by using secondary concentrated fluosilicic acid to obtain fluosilicic acid with the mass concentration of more than or equal to 45%, recycling the fluosilicic acid for acidolysis reaction, and modifying the concentrated by-product silicon dioxide to obtain the high-activity white carbon black. The problems of energy consumption and cost are solved, and efficient circulation and poly-generation of fluorine and silicon resources are achieved in the whole process.
Owner:YUNNAN YUNTIANHUA

Method for producing SO3

PendingCN121247732ASulfur compoundsOleumCatalytic oxidation
The invention discloses a method for producing SO3, which comprises the following steps: carrying out combustion reaction on sulfur and first oxygen-containing gas, and outputting SO2-containing first mixed gas; the first mixed gas and second oxygen-containing gas are subjected to a catalytic oxidation reaction, and second mixed gas containing SO3 is obtained; carrying out first fuming sulfuric acid absorption treatment on the second mixed gas to obtain third mixed gas and second fuming sulfuric acid; circulating and returning the third mixed gas to be mixed with the sulfur and the first oxygen-containing gas; performing separation treatment on the second fuming sulfuric acid to obtain third fuming sulfuric acid and SO3 gas; and mixing the third fuming sulfuric acid with the first fuming sulfuric acid, and carrying out absorption treatment on the second mixed gas. The method can meet the practical requirements that the SO3 product is produced, but sulfuric acid is not produced or sulfuric acid is produced as little as possible.
Owner:CHINA NERIN ENGINEERING CO LTD

Integrated process for co-production of phosphorus pentafluoride (PF5) and fluorosulfonic acid (HSO3F)

PendingCN121666359APhosphorus halides/oxyhalidesFluorosulfonic acidOleumPhosphoric acid
An integrated process for co-production of phosphorus pentafluoride (PF5) and fluorosulfonic acid (HSO3F) in high yield and purity through a single reaction step is provided. The method comprises reacting a first reagent comprising an aqueous solution of hexafluorophosphoric acid (HPF6) and hydrofluoric acid (HF) with a second reagent comprising fuming sulfuric acid (H2SO4SO3), and recovering a product mixture comprising phosphorus pentafluoride (PF5) and fluorosulfonic acid (HSO3F).
Owner:SOZOTEX PERFORMANCE MATERIALS AMERICA INC

Multistage oleum absorption tower and process for absorbing sulfur trioxide with oleum

PendingCN122355243AOleumFlue gas
The application discloses a multi-stage fuming sulfuric acid absorption tower and a process method for absorbing sulfur trioxide by using the fuming sulfuric acid absorption tower. The multi-stage fuming sulfuric acid absorption tower comprises a primary absorption assembly and a secondary absorption assembly. The primary absorption assembly is provided with a first containing cavity. A first acid distributor is arranged in the first containing cavity and is arranged close to the upper wall surface of the first containing cavity and used for spraying acid liquid into the first containing cavity. The primary absorption assembly is provided with a flue gas inlet communicated with the first containing cavity. The secondary absorption assembly is arranged above the primary absorption assembly. The secondary absorption assembly is provided with a second containing cavity. The second containing cavity is communicated with the first containing cavity and used for receiving flue gas from the first containing cavity. A second acid distributor is arranged close to the upper wall surface of the second containing cavity and used for spraying acid liquid into the second containing cavity. The upper end of the secondary absorption assembly is provided with a flue gas outlet communicated with the second containing cavity. In this way, the sulfur trioxide absorption rate can be improved, and the product purity can be ensured.
Owner:THE SIXTH CONSTR CO LTD OF CHINA NAT CHEM ENG

Ethylene bistetrabromophthalimide, process for its preparation and use

PendingCN122277460AChemical synthesisOleum
This invention relates to the field of flame retardant chemical synthesis technology, and discloses ethylene bis(tetrabromophthalimide) and its preparation method and applications. The method includes reacting phthalic anhydride and ethylenediamine in an aqueous medium at a controlled mass ratio of 3.0-5.5:1 to obtain an intermediate; reacting the intermediate with bromine in a fuming sulfuric acid medium, controlling the dropping temperature at 45-60℃ and the holding temperature at 130-150℃; and washing the reaction product followed by high-temperature heat treatment at 150-220℃ to constant weight. This invention effectively inhibits residual active amino groups and organic carbonization by strictly controlling the intermediate synthesis ratio and the temperature range of the bromination reaction. By utilizing high-temperature heat treatment, it thoroughly removes deep-seated acidic volatiles that cannot be removed by conventional drying, solving the problems of yellowing appearance, poor heat resistance, and easy corrosion of processing equipment in existing products. It is applicable to the field of flame-retardant engineering plastics.
Owner:SHOUGUANG LONGHAO CHEM CO LTD

Cyclohexanone-oxime transposition process flow and device with sulfuric acid concentration supply in different regions

The invention provides a cyclohexanone-oxime transposition process flow and a cyclohexanone-oxime transposition device for partitioned sulfuric acid concentration supply, which are used for partitioned supply and accurate control of sulfuric acid concentration in different stages of transposition reaction, in the transposition process flow, fuming sulfuric acid is proportionally distributed to a high-concentration acid channel and a low-concentration acid channel through an intelligent metering and acid adding module, and the high-concentration acid channel and the low-concentration acid channel are communicated with the high-concentration acid channel and the low-concentration acid channel; the high-concentration acid channel is used for a one-step transposition reactor of a one-step reaction zone of the two-step transposition process, the low-concentration acid channel is used for a two-step transposition reactor of a two-step reaction zone of the two-step transposition process, and in the transposition process flow, a multi-mode fuzzy self-adaptive prediction PID control algorithm is adopted, control modes are switched according to reaction stages, and the multi-mode fuzzy self-adaptive prediction PID control algorithm is adopted. The first-step reaction zone adopts high-precision temperature-acid concentration cascade control, and the second-step reaction zone adopts by-product prediction feedforward control; according to the invention, partitioned supply and accurate control of sulfuric acid concentration in the first-step reaction zone and the second-step reaction zone can be realized, the reaction efficiency and selectivity are improved, and acid consumption and by-product generation are reduced.
Owner:NANJING COLLEGE OF CHEM TECH

A method for the continuous flow reaction production of boron trifluoride and complexes thereof

PendingCN122444769AHydrogen fluorideOleum
The present application belongs to the field of boron trifluoride production, and relates to a method for preparing boron trifluoride and its complex by continuous flow reaction. The method comprises the following steps: uniformly mixing boric acid with concentrated sulfuric acid, then adding oleum or continuously introducing sulfur trioxide gas to obtain an oleum solution of boric acid; introducing the obtained solution and anhydrous hydrogen fluoride gas into a continuous flow reactor at a uniform speed to obtain boron trifluoride gas; purifying and removing impurities from the boron trifluoride gas generated in the reaction; continuously introducing the purified boron trifluoride gas into a complexing solvent for a complexing reaction to obtain a boron trifluoride complex. The method uses a continuous flow reactor to react anhydrous hydrogen fluoride with the oleum solution of boric acid, so that the raw materials can be continuously and uniformly mixed, the reaction is rapid and complete, the process conditions are simplified, the sulfuric acid waste liquid can be recycled after treatment, and the method has economic advantages and process innovation, and is suitable for industrial production.
Owner:YUNNAN YUNTIANHUA

Preparation method of environment-friendly and efficient sulfamic acid

PendingCN122126806AAmidosulfonic acidOther chemical processesOleumExhaust fumes
This invention proposes an environmentally friendly and efficient method for preparing aminosulfonic acid, belonging to the field of chemical technology. It includes: (1) sulfonation reaction; (2) crude product filtration; (3) dissolution and crystallization; and (4) drying and packaging. The reaction process of this invention features mild reaction conditions, short reaction time, and a yield exceeding 97%. The process, using fuming sulfuric acid and urea at a lower temperature, significantly reduces polluting components in the waste gas. It has many advantages, including simple operation, low cost, high yield, and greater environmental friendliness.
Owner:SHANDONG JINJIA ENVIRONMENTAL PROTECTION CO LTD

Sulfur trioxide production device

The utility model relates to the technical field of sulfur trioxide separation and evaporation, and discloses a sulfur trioxide production device, which aims to solve the problem in sulfur trioxide evaporation in the prior art, and comprises a fuming sulfuric acid storage tank, the fuming sulfuric acid storage tank is connected with a film evaporator, and the film evaporator is connected with a saturated steam or heat-conducting oil pipeline and a fuming acid pipeline. The top of the film evaporator is connected with a gaseous sulfur trioxide pipeline, the gaseous sulfur trioxide pipeline is connected with a condenser, the condenser is connected with a liquid sulfur trioxide tank, a swirler is arranged in the film evaporator and comprises a first-stage swirling vane arranged at the lower part in the film evaporator, and a second-stage swirling vane is arranged at the upper part in the film evaporator; the film evaporator is utilized to separate gas-phase sulfur trioxide from low-concentration fuming acid, so that the sulfur trioxide is evaporated quickly, the swirlers are arranged in the film evaporator, materials are prevented from being carried by gas, and the swirlers are arranged in an upper stage and a lower stage, so that the evaporation rate of the sulfur trioxide can be effectively improved.
Owner:TIANHUA INSTITUTE OF CHEMICAL MACHINERY AND AUTOMATION CO LTD

A process suitable for the production of chromatographic grade cyclohexane

This invention discloses a method for producing chromatographic grade cyclohexane, comprising the following steps: A) Taking cyclohexane as raw material, adding fuming sulfuric acid to the cyclohexane raw material, stirring and allowing it to stand, and then separating the cyclohexane; B) Adding pure water to the cyclohexane obtained in step A, stirring and allowing it to stand, and then separating the cyclohexane; C) Adding activated alumina and 10X molecular sieve to the cyclohexane obtained in step B, stirring and allowing it to stand, and then filtering; D) Distilling the cyclohexane obtained in step C to obtain chromatographic grade cyclohexane. This invention uses fuming sulfuric acid to remove impurities from the cyclohexane raw material, then washes it directly with pure water, followed by adsorption filtration using molecular sieves and alumina, and finally distillation to obtain chromatographic grade cyclohexane with optical properties meeting market customer requirements. The preparation process of this invention is not complex, the consumption of auxiliary agents is low, and the cost is within a controllable range, achieving the goal of industrial production of chromatographic grade cyclohexane with high optical properties.
Owner:CHENGDU KELONG CHEM CO LTD

Process and plant for the production of ε-Caprolactam and ammonium sulfate on industrial scale

ActiveUS12486225B2Lactams preparationBeckmann rearrangementOleum
The invention provides a process and a plant for the production of ε-caprolactam and crystalline ammonium sulfate in an industrial-scale plant, wherein the plant comprises a Beckmann rearrangement reaction section, an ammonium sulfate crystallization section, and one or more heat exchangers configured to transfer heat from the Beckmann rearrangement reaction section to the ammonium sulfate crystallization section and wherein the process comprises the steps of:a) feeding(i) cyclohexanone oxime and(ii) oleum and / or sulfuric acidto the Beckmann rearrangement reaction sectionb) reacting components (i) and (ii) in the Beckmann rearrangement reaction section to form a reaction mixture comprising ε-caprolactam, whereby heat of reaction is generated;c) discharging the reaction mixture comprising ε-caprolactam from the Beckmann rearrangement reaction section;d) removing partially or fully the heat of reaction generated in the Beckmann rearrangement reaction section by one or more heat exchangers configured to transfer heat from the Beckmann rearrangement reaction section;e) feeding an aqueous liquid comprising ammonium sulfate to the ammonium sulfate crystallization section;f) introducing heat into the ammonium sulfate crystallization section comprising the aqueous ammonium-sulfate-comprising liquid by one or more heat exchangers configured to transfer heat into the ammonium sulfate crystallization section;g) forming ammonium sulfate crystals by evaporative crystallization in the ammonium sulfate crystallization section;characterized in thath) the heat of reaction removed from the Beckmann rearrangement reaction section in step d) is at least partially or fully transferred to the ammonium sulfate crystallization section in step f).
Owner:CAP III

Sulfonic acid monomer preparation device and method

The invention discloses a preparation device and method of a sulfonic acid monomer, and relates to the technical field of chemical engineering. The preparation method comprises the following steps: S1, pumping acrylonitrile and fuming sulphuric acid into a premixer for mixing; s2, the mixed liquid enters a heat exchanger to be heated, and the temperature is controlled to range from 15 DEG C to 20 DEG C; s3, the heated mixed liquid enters a first-stage dynamic tubular reactor, gasified isobutene is introduced from lower, middle and upper layers of gas inlet branch pipes at the same time, and the reaction temperature is 40-45 DEG C; s4, after the materials react in the first-stage dynamic tubular reactor for 3-7 min, the materials enter a second-stage dynamic tubular reactor, and the reaction temperature ranges from 45 DEG C to 50 DEG C; and S5, cooling, carrying out solid-liquid separation, and drying to obtain the product. By adopting the method disclosed by the invention, the continuous and stable preparation of the sulfonic acid monomer 2-acrylamido-2-methylpropanesulfonic acid can be realized, and compared with the traditional process, the reaction time is greatly shortened, and the product purity (without refining and washing) can reach 99% or above.
Owner:WEIFANG JINSHI NEW MATERIALS CO LTD

Processes for the oxidation of methane and ethane using iodine-based catalysts

The invention relates to the production of methanol via the partial oxidation of methane using iodine(III) catalysts, which allow the reaction to be performed at low temperatures and pressures. Similar chemistry can be used to make methyl bisulfate from methane in the presence of oleum, and to make ethylene glycol via the partial oxidation of ethane.
Owner:IMPERIAL COLLEGE INNVOATIONS LTD

Preparation method of 4, 5-diaminobenzene-1, 3 disulfonic acid

The invention relates to a preparation method of 4, 5-diaminobenzene-1, 3 disulfonic acid, which comprises the following steps: a, adding concentrated sulfuric acid into a container provided with a thermometer and a stirring device, controlling the temperature and slowly adding o-phenylenediamine to obtain a sulfuric acid solution of o-phenylenediamine; b, slowly dropwise adding fuming sulfuric acid into the sulfuric acid solution of o-phenylenediamine in the step a, carrying out heat preservation reaction, and cooling; c, pouring the product in the step b into an ice-water mixture, adding activated carbon, stirring, and filtering to remove the activated carbon to obtain a diluent; d, carrying out reduced pressure distillation, concentration and cooling on the diluent; e, cooling, stirring, filtering and taking a solid to obtain a 4, 5-diaminobenzene-1, 3 disulfonic acid crude product; and f, adding the crude product into an organic solvent, pulping, washing acid, stirring, filtering to obtain a solid, and drying to obtain the 4, 5-diaminobenzene-1, 3-disulfonic acid. The method has the advantages of mild reaction conditions, normal pressure reaction, high yield, easily available raw materials and simple process, can be directly obtained by one-step sulfonation, and is suitable for industrial production.
Owner:HEBEI JIANXIN CHEM IND CO LTD

Filtrate reducer, oil-based drilling fluid, and preparation method and application of filtrate reducer and oil-based drilling fluid

PendingCN121991282ANot much viscosityGood filter loss reduction effectDrilling compositionOleumFiltration
The invention provides a filtrate reducer and an oil-based drilling fluid as well as a preparation method and application of the filtrate reducer and the oil-based drilling fluid. The preparation method of the filtrate reducer comprises the following steps: mixing acrylonitrile, isobutene and acetone, heating and stirring for a first reaction, and dropwise adding fuming sulfuric acid in the heating and stirring process to obtain a first mixture; mixing N-alkyl acrylamide with the first mixture, and heating for second reaction to obtain a second mixture; dimethylaminoethyl methacrylate and the second mixture are mixed and heated for a third reaction, and a third mixture is obtained; ethyl benzene, carbon tetrachloride and the third mixture are mixed and heated for a fourth reaction, and a fourth mixture is obtained; and extracting and washing the fourth mixture with absolute ethyl alcohol to obtain a white floccule, namely the filtrate reducer. The oil-based drilling fluid comprises an oil phase, bentonite, the filtrate reducer provided by the invention, a flow pattern regulator, a weighting agent and sodium hydroxide. The oil-based drilling fluid provided by the invention has good high-temperature drop filtration performance and is suitable for drilling of deep wells and ultra-deep wells.
Owner:PETROCHINA CO LTD

Preparation process of ethylene bis-tetrabromophthalimide with high thermal stability

PendingCN122325375AImidePtru catalyst
The application relates to the field of flame-retardant materials, and particularly discloses a preparation process of ethylene bis-tetrabromophthalimide with high thermal stability; the preparation process of ethylene bis-tetrabromophthalimide with high thermal stability comprises the following specific steps: phenolic anhydride and ethylenediamine are mixed in water, heated to react, centrifuged, dried to obtain an intermediate; the intermediate is mixed with bromine, fuming sulfuric acid and a catalyst to obtain a reaction solution, heated to react, deacidified, washed with water and dried to prepare ethylene bis-tetrabromophthalimide; the catalyst is a composite of ferric chloride and iodine; the ethylene bis-tetrabromophthalimide intermediate is synthesized by phenolic anhydride and ethylenediamine, and then bromination reaction is carried out, so that the instantaneous intense heat release caused by excessively high local bromine concentration is reduced, the escape of HBr and the loss of bromine are reduced, and the purity of the product is improved.
Owner:SHOUGUANG LONGHAO CHEM CO LTD

System for flexibly preparing nitrate

The invention discloses a system for flexibly preparing nitrate ester. The system comprises a Meilan acid storage tank, a fuming sulfuric acid storage tank, a first acid mixing ejector, a second acid mixing ejector, a first acid cooler, a second acid cooler, a polyhydric alcohol storage tank, a spraying nitrator, a coil pipe cooler, a kettle type continuous overflow nitrator, a centrifugal separator, a first dynamic washing separator and a second dynamic washing separator. The device comprises a first dynamic washing separator, a second dynamic washing separator, a third dynamic washing separator, a jet conveyor, a jet conveying water tank, a nitrate finished product temporary storage tank, a wastewater curved channel device, a nitrate-containing waste acid temporary storage tank, a flow meter, a gear pump, a three-way valve A, a three-way valve B, a three-way valve C and a three-way valve D, according to the system for preparing the nitrate ester, the nitrate ester can be prepared by selecting a spraying nitration process or a kettle type continuous overflow nitration process according to the characteristics of the nitrate ester.
Owner:SHANXI BEIFANG XINGAN CHEM IND

Production process of deuterated sulphuric acid-d2

The invention discloses a production process of deuterated sulphuric acid-d2, and belongs to the technical field of fine chemical engineering. In the production process of the deuterated sulphuric acid-d2 provided by the invention, the deuterated sulphuric acid-d2 is obtained by utilizing the reaction of the sulfur trioxide gas and the heavy water, meanwhile, the sulfur trioxide gas is firstly mixed with the argon before the reaction, and the argon is used as an inert carrier, so that the concentration of the sulfur trioxide gas can be effectively diluted, and violent reaction caused by local excessive heat release when the sulfur trioxide gas is in contact with the heavy water is avoided; and the introduction rate of the sulfur trioxide gas can be accurately controlled by adjusting the argon flow. In addition, the addition amount of the sulfur trioxide gas is not deliberately controlled to be excessive during the reaction, the deuterated fuming sulphuric acid is conveniently obtained firstly, then the deuterated sulphuric acid-d2 with the target concentration is obtained through dilution treatment in cooperation with nuclear magnetic resonance hydrogen spectrum detection, the technological process can be greatly simplified, and the deuterated sulphuric acid-d2 product with the accurate concentration can be obtained.
Owner:骏承(徐州)新材料科技有限公司

5-fluoro-2, 4-dinitro-3-(trifluoromethyl) aniline compound as well as preparation method and application thereof

The invention discloses a 5-fluoro-2, 4-dinitro-3-(trifluoromethyl) aniline compound, which is prepared by the following method: reacting 3, 5-difluorotrifluoromethyl benzene at the high temperature of 160 DEG C by using fuming sulphuric acid and sodium nitrate as nitrating agents for 6 hours, cooling, separating out by using ice water after the temperature is reduced to room temperature, filtering, washing and drying to obtain 1, 5-difluoro-2, 4-dinitro-3-(trifluoromethyl) aniline, and separating out 1, 5-difluoro-2, 4-dinitro-3-(trifluoromethyl) aniline from the 1, 5-difluoro-2, 4-dinitro-3-(trifluoromethyl) aniline to obtain 1, 5-difluoro-2, 4-dinitro-3-(trifluoromethyl) aniline. The catalyst is 2, 4-dinitro-3-(trifluoromethyl) benzene. The preparation method comprises the following steps: dissolving 1, 5-difluoro-2, 4-dinitro-3-(trifluoromethyl) benzene in tetrahydrofuran, slowly dropwise adding an ammonia water solution, and naturally volatilizing to obtain the 5-fluoro-2, 4-dinitro-3-(trifluoromethyl) aniline (PFDNTN). The 5-fluoro-2, 4-dinitro-3-(trifluoromethyl) aniline prepared by the invention has a proper melting point (100 DEG C), and is relatively high in decomposition rate (322 DEG C), and the impact sensitivity is not lower than 40J; and the friction sensitivity is not lower than 360 N. The detonation velocity is 7066 m s <-1 >, and the detonation pressure is 24.65 Gpa, which is superior to that of TNT. And the explosive is expected to become a casting carrier explosive for replacing TNT.
Owner:SOUTHWEAT UNIV OF SCI & TECH

Single-tower production system of fuming sulfuric acid

The utility model discloses a single-tower production system for fuming sulfuric acid, and belongs to the technical field of sulfuric acid production equipment. The device comprises a first-stage fuming sulfuric acid tower, and a bottom discharge port of the first-stage fuming sulfuric acid tower is sequentially connected with a first-stage fuming sulfuric acid circulating tank and a first-stage fuming sulfuric acid cooler through pipelines to form closed-loop circulation; a sulfur trioxide gas inlet is formed in the side part of the first-stage tower, and the tower is filled with ceramic filler so as to improve the gas-liquid contact efficiency. In addition, a redundant second-stage fuming sulfuric acid tower is additionally arranged and connected with a tail gas outlet of the first-stage cooler through a pipeline, the height of a filler layer in the tower is reduced, and an acid mist trapping mechanism is additionally arranged and used for emergency starting and acid mist backflow under the abnormal working condition. Through main operation of the single tower, standby of the redundant secondary tower, pipeline interconnection optimization and filler structure adjustment, the purposes of energy conservation and consumption reduction are achieved, meanwhile, the system resistance is reduced, the operation process is simplified, and the production safety is improved.
Owner:HUBEI SANNING CHEM

Tank arrangement for the metering of fuming sulfuric acid

ActiveCN224676954UOleumLiquid level measurement
The utility model relates to liquid level measurement technical field, concretely relates to the storage tank device for the fuming sulfuric acid measurement, including the first storage tank for loading fuming sulfuric acid, the top of first storage tank is connected with tail gas absorber, first storage tank and tail gas absorber are communicated through first connecting pipeline, install first suction pump on first connecting pipeline, the tail gas absorber includes the casing, the inside of casing forms the tail gas absorption chamber for purifying flue gas, the bottom of casing is provided with the gas inlet hole, the gas inlet hole is communicated with first connecting pipeline, the top of casing is provided with the exhaust hole that supplies the flue gas after purifying and exports, the top of first storage tank is installed and is used for detecting the radar liquid level meter group of fuming sulfuric acid liquid level.
Owner:CHONGQING SHUANGXIANG ELECTRONIC MATERIALS CO LTD

Preparation method of high-purity phosphorus pentafluoride

The invention relates to the field of production of chemical products, in particular to a preparation method of high-purity phosphorus pentafluoride. The preparation method of the high-purity phosphorus pentafluoride provided by the invention comprises the following steps: mixing apatite and hydrofluoric acid, and carrying out first reaction to generate phosphoric acid; adding fuming sulfuric acid, carrying out second reaction to generate crude phosphorus pentafluoride gas, and purifying to obtain the phosphorus pentafluoride, the purified reagent comprises an ether solvent and sterically hindered amine. The phosphorite is directly used as the raw material to prepare the phosphorus pentafluoride, so that the process route from phosphorite to the phosphorus pentafluoride is remarkably shortened, and the utilization rate of phosphorus is increased. Meanwhile, a mixed reagent of an ether solvent and sterically hindered amine is adopted during purification, and the Lewis acidity of phosphorus pentafluoride is far higher than that of silicon tetrafluoride, so that the complexing ability of phosphorus pentafluoride and the ether solvent is higher, and phosphorus pentafluoride and silicon tetrafluoride are efficiently separated by utilizing the difference of solubility; and the sterically hindered amine selectively forms a precipitate with silicon tetrafluoride, so that the separation degree of phosphorus pentafluoride and silicon tetrafluoride is further improved, and a high-purity phosphorus pentafluoride product is obtained.
Owner:HUNAN NONFERROUS METALS INVESTMENT CO LTD

A cementitious material and a concrete and use thereof

ActiveCN121517131BPtru catalystOleum
The application provides a cementing material and a concrete and application thereof, and belongs to the technical field of concrete. The cementing material provided by the application comprises the following components in percentage by mass: modified burned gypsum 55-85%, silicate 5-10%, magnesium type activated zeolite 5-10%, fuming sulfuric acid 3-4%, attapulgite 1.5-3.5% and active alumina 0.5-2%; the modified burned gypsum is obtained by mixing gypsum, potassium sulfate and anhydrous sodium sulfate after electromagnetic radiation and calcination in sequence. The application adopts the modified burned gypsum, the silicate, the magnesium type activated zeolite and the attapulgite as the base material, and the active alumina as the catalyst, and adopts the fuming sulfuric acid chemical excitation and the electromagnetic radiation physical excitation, so that the pH value of the concrete prepared from the cementing material is stabilized at 6.5-8.5.
Owner:JIANGSU ZHUODIAN DRILLING & TUNNELING TECH CO LTD

Sulfonating method of alkylaniline compound

The invention discloses a sulfonation method of an alkylaniline compound, and belongs to the technical field of organic synthesis. According to the method, sulfur trioxide is used as a sulfonating agent, 1, 2-dichloroethane, dichloromethane or trichloromethane is selected as a solvent, and efficient sulfonation of the alkylaniline compound is realized by controlling key parameters such as reaction temperature, sulfur trioxide introduction speed, heat preservation time and the like. The technical problem that a large amount of dilute sulphuric acid wastewater and sodium sulfate solid waste are generated in a traditional fuming sulphuric acid sulfonation process is solved, the solvent can be recycled infinitely, the HPLC purity of the product is larger than or equal to 99.4%, the yield is larger than or equal to 94%, and the method has the remarkable advantages of being environmentally friendly, efficient and low in cost and is suitable for industrial large-scale production.
Owner:SHANSHAN HONGFENG NEW MATERIALS CO LTD

Synthetic method of environment-friendly sulfonated para-ester

According to the environment-friendly synthetic method of the sulfonated para-ester, para-ester powder is directly dissolved in 60-70% fuming sulfuric acid, the solubility of the para-ester in the fuming sulfuric acid can be increased, side reactions generated when the dissolution rate is low are reduced, then heating sulfonation is conducted, the product sulfonated para-ester is prepared, the yield and purity are high, the purity ranges from 90% to 92%, and the yield of the sulfonated para-ester is high. The yield is about 95%, salting-out refining is not needed, the raw material consumption is low, no wastewater or waste acid is generated, the whole synthesis method is simple and low in cost, the problems of long reaction time, low yield, much waste acid water, difficulty in treatment and the like in the production process can be solved, and the method is suitable for industrial production.
Owner:TAIXING JINYUN DYESTUFF

High-capacity amphiphilic adsorption resin and preparation method thereof

A preparation method of the adsorbent resin comprises the following steps: S1, adding styrene, divinylbenzene, a pore-foaming agent and an initiator into a water phase, and heating and stirring for reaction; s2, slowly adding the porous microsphere matrix into a mixed solution of concentrated sulfuric acid and fuming sulfuric acid in an ice-water bath, carrying out heating reaction, dropwise adding into ice water after the reaction is finished, filtering, and washing with water until the solution is neutral; s3, adding the sulfonated microspheres into toluene for swelling, then adding glycidyl methacrylate, divinylbenzene and an initiator, and carrying out heating reaction under the protection of nitrogen; and S4, adding the epoxy microspheres into ethidene diamine, heating for reaction, washing and drying. The adsorption resin provided by the invention is large in capacity and has stable amphiphilic adsorption performance.
Owner:JIANGSU JINSHAN NEW MATERIAL CO LTD

Device for improving yield of sulfur trioxide

A device for improving the yield of sulfur trioxide comprises an absorption tower, a sulfur trioxide evaporator, a heat exchanger, a steam heater, a plurality of self-control instrument interlocks and the like. SO3-containing flue gas enters the absorption tower, SO3 in the flue gas is circularly absorbed by fuming sulphuric acid, the concentration of the fuming sulphuric acid is increased, the fuming sulphuric acid is pressurized and sequentially fed into the heat exchanger, the steam heater and the sulfur trioxide evaporator, the fuming sulphuric acid is heated to the boiling point, SO3 is evaporated and escaped from the fuming sulphuric acid to prepare high-purity SO3, and low-concentration fuming sulphuric acid flows back to the absorption tower and circularly absorbs SO3 in the flue gas. When the device is in 50% load production operation, the heat of high-temperature flue gas of a heating medium of the sulfur trioxide evaporator is correspondingly low, the temperature rise of fuming sulfuric acid in the sulfur trioxide evaporator is reduced, the SO3 evaporation efficiency is reduced, the temperature of the fuming sulfuric acid entering the sulfur trioxide evaporator is increased through steam heating by using a steam heater, and the SO3 evaporation efficiency is improved; and through interlocking control of a self-control electric instrument, the device operates automatically, and the safety and stability are high.
Owner:HUBEI SINOPHORUS ELECTRONIC MATERIALS CO LTD

Sulfur dioxide gas removal device in sulfur trioxide preparation process

The utility model provides a sulfur dioxide gas removal device in a sulfur trioxide preparation process, which relates to the field of sulfur trioxide preparation devices and comprises a hydrogen peroxide storage tank, a metering pump, a liquid delivery pipe and a plurality of branch pipes, hydrogen peroxide is arranged in the hydrogen peroxide storage tank, and a liquid inlet of the metering pump is communicated with the hydrogen peroxide storage tank through a pipeline. A liquid outlet of the metering pump is connected with a 7-shaped liquid feeding pipe, the top ends of the branch pipes are communicated with the liquid feeding pipe, the bottom ends of the branch pipes are inserted into a gas conveying pipe and then connected with a spraying head, sulfur trioxide gas prepared from fuming sulfuric acid is arranged in the gas conveying pipe, and the sulfur trioxide gas contains a small amount of sulfur dioxide gas. The multiple spraying heads are arranged at intervals in an up-down staggered mode, the distance between the multiple spraying heads and the inner wall of the gas conveying pipe is larger than or equal to 3 mm, and the multiple branch pipes are each provided with an electromagnetic valve. The method has the beneficial effects that under the condition that sulfur trioxide is gaseous, sulfur dioxide gas is removed through hydrogen peroxide, and the quality of a sulfur trioxide finished product is improved.
Owner:TIANJIN BODA SULFURIC ACID IND

Method for producing fuming sulfuric acid from waste sulfuric acid and preparation system

The invention provides a method for producing fuming sulfuric acid from waste sulfuric acid and a preparation system. The method comprises the following steps: (S1) collecting a waste sulfuric acid solution containing H2O2; step (S2), SO2 is provided in the reaction tank, H2O2 and SO2 are subjected to a reaction, and a first sulfuric acid solution is obtained; s3, the first sulfuric acid solution is guided into a first heating tank to be heated to 100-220 DEG C, and a second sulfuric acid solution is obtained; a step (S4) of heating the second sulfuric acid solution to decompose the sulfuric acid to obtain a mixture containing SO3 and water; and (S5) separating SO3 from water in the mixture, and carrying out an absorption procedure on SO3 to obtain high-concentration fuming sulfuric acid. The preparation system sequentially comprises a waste sulfuric acid solution storage unit, a reaction unit comprising a sulfur dioxide supply group and a reaction tank, a heating assembly comprising a first heating tank and a second heating tank, a water separation module and a sulfur trioxide absorption unit.
Owner:张进兴 +2

Sulfur trioxide gas impurity removal device

ActiveCN223906546USulfur compoundsProduction lineOleum
The utility model relates to the field of electronic-grade sulfuric acid production equipment, in particular to a sulfur trioxide gas impurity removal device which is arranged at the rear end of a fuming sulfuric acid evaporator and comprises a cooling device and a defoaming device, and a gas inlet pipeline of the cooling device is connected with an outlet of the fuming sulfuric acid evaporator through an external pipeline. A gas outlet pipeline of the cooling device is connected with a feeding port of the defoaming device through a pipeline, a discharging port of the defoaming device is connected with follow-up equipment of a production line, gas sulfur trioxide firstly passes through the cooling device, the temperature of the gas sulfur trioxide is reduced to about 80 DEG C, then the gas sulfur trioxide is conveyed into the defoaming device, and the gas sulfur trioxide is discharged out of the production line. Acid mist in sulfur trioxide gas is removed in the defoaming device, so that the purity and the quality of sulfur trioxide are improved, meanwhile, damage to equipment caused by a high-temperature acid environment is avoided, and the service life of the device is effectively prolonged.
Owner:TIANJIN BODA SULFURIC ACID IND