223 results about "Oleum" patented technology

The invention relates to a preparation method of o-nitro-p-methysulfonyl benzoic acid. O-nitro-p-methylsulfonyl toluene is oxidized by persulphuric acid to obtain the o-nitro-p-methysulfonyl benzoic acid. The preparation method comprises the following processes: (a) oxyful and oleum are mixed at a low temperature to prepare persulphuric acid; (b) o-nitro-p-methylsulfonyl toluene is dissolved in sulphuric acid; and (c) the persulphuric acid obtained from the step (a) is dripped into the liquid obtained from the step (b) for purpose of reaction to obtain the o-nitro-p-methysulfonyl benzoic acid. In the method, the reaction of the oleum and the oxyful relatively improves the concentration and the oxidization capability of the oxyful and reduces the decomposition speed of the oxyful; as vanadic oxide is not used, waste acid treatment, recovery and the like are omitted; and the persulphuric acid in use is automatically transformed into sulphuric acid after the oxidization is finished and can finally be used indiscriminately with a mother liquid. Compared with the prior art, the amount of the oxyful in use is greatly reduced, and the production cost remarkably decreases. Compared with the nitric acid oxidization process, the preparation method is safer, environment-friendly and clean.

The invention is a potassium peroxy-monohydrosulfate compound salt preparing method, using oleum, perhydrol and potassium hydroxide as raw material. Firstly, adding stabilizing agent-containing perhydrol in the reactor, then dropping in the oleum to react, then dropping in potassium hydroxide solution and at the same time adding in crystal shape modifier, vacuum-condensing, cooling and crystallizing, and then drying to obtain its dried product; the perhydrol solution concentration is 45-80% and the oleum concentration 35-65%. It uses oleum to replace the vitriol oil and thick perhydrol solution to replace dilute perhydrol solution, and adds in potassium hydroxide to adjust the components. It has better stability.

A first portion of the converter feed gas comprising a SO 2 -enriched stripping gas is formed. Passing the converter feed through a plurality of catalyst beds in series to form a reformed gas comprising SO3 and residual SO2, the plurality comprising at least 2 and no more than 4 catalyst beds. The second portion of the SO2-enriched gas is introduced into at least one catalyst bed downstream of the most upstream catalyst bed of the plurality of catalyst beds to increase the SO2 concentration in the gas fed to the downstream bed. The invention also relates to a process for the production of sulfuric acid and/or oleum from a feed gas comprising SO2. The SO2-enriched stripping gas is passed through multiple series-connected catalyst beds to form a reformed gas comprising SO3 and residual SO2. mixing the reformed gas with water vapor to form a product acid gas comprising: (a) sulfuric acid from the gas phase reaction between SO3 from the oxidation product gas and water vapor, thereby generating gas phase heat of sulfuric acid formation; (b) SO3 ; and (c) SO2. Thermal energy is recovered from gas phase sulfuric acid generation heat by heat transfer from the product acid gas to steam or feed water in an indirect heat exchanger. The cooled product acid gas is then contacted with sulfuric acid liquid in the SO3 absorption zone to form additional sulfuric acid and/or oleum and SO3-depleted gas containing SO2.

The invention relates to a method for preparing lithium hexafluorophosphate. The method comprises the following steps: (1), enabling anhydrous hydrogen fluoride and phosphorus pentoxide to react underthe protection of inert gas to prepare hexafluorophosphoric acid; (2), adding oleum to the hexafluorophosphoric acid under cooling stirring to prepare phosphorus pentafluoride gas; (3), dissolving high-pure lithium fluoride in an anhydrous hydrogen fluoride solution to form an anhydrous hydrogen fluoride solution containing the lithium fluoride; (4), cooling the phosphorus pentafluoride gas at 40DEG C below zero, guiding the phosphorus pentafluoride gas to the anhydrous hydrogen fluoride solution containing the lithium fluoride, and reacting, crystallizing, separating and drying the phosphorus pentafluoride gas to obtain a pure lithium hexafluorophosphate product; and (5), continuously pumping the unreacted cooled phosphorus pentafluoride gas after a reaction to the other anhydrous hydrogen fluoride solution containing the lithium fluoride and continuously reacting to obtain a lithium hexafluorophosphate finished product. The invention has rich material resources and easily obtainable raw materials, low production cost, high reaction rate, high product quality and thorough reaction and can realize semi-continuous production by the series connection of double kettles.

The present invention provides a method for producing amine series with an adamantane framework, including the following steps: step 1: reacting adamantane series in a mixed liquid containing oleum and organic nitrile compounds; step 2: performing hydrolyzing treatment to a reaction liquid obtained in the step 1 to form acidamide series with the adamantane framework; step 3: performing alkali treatment to the acidamide series obtained in the step 2 to form the amine series with the adamantane framework. A method for producing quaternary ammonium salts with the adamantane framework in sequence includes the following steps: step A: reacting the amine series with the adamantane framework dissolved in a dissolvant a with aminic acid and methylene oxide or paraformaldehyde, to form dimethylamine series with the adamantane framework; step B: dissolving the dimethylamine series with the adamantane framework obtained in the step A in a dissolvant b to react with halomethane so as to form quaternary ammonium salt halogenide with the adamantane framework; step C: performing ion exchange to the quaternary ammonium salt halogenide with the adamantane framework to form quaternary ammonium salt hydroxides with the adamantane framework.

The present invention discloses oximation and rearrangement process of preparing amide with aliphatic and/or cyclic aliphatic ketone as material. The preparation process includes catalytic reaction of ketone, hydrogen peroxide solution and ammonia inside inert solvent to produce ketoxime solution, Beckmann rearrangement of the oil phase product under the action of fuming sulfuric acid, and hydrolysis to neutralize and produce amide. The present invention has shortened technological process, lowered cyclohexyl ketoxime rearranging reaction temperature, lowered sulfuric acid consumption and reduced side product.

Process for the production of concentrated sulphuric acid and oleum from feed gases with up to 70% SO₂+SO₃ (SO_x) and a content of H₂O corresponding to H₂O/SO₃ molar ratios up to 1.6, particularly in the range of 0.5 to 1.6 upstream an intermediate sulphuric acid condenser comprising an air recycling loop with water addition. The process of the invention minimizes power consumption of the sulphuric acid plant by reducing the consumption of cooling water and obtaining maximum possible recovery of the heat liberated in the process for production of high pressure steam for power production. Up to 99.95% of the SO_x in the feed gas can be recovered as typically 98.5-99.5 wt % concentrated sulphuric acid and/or oleum with up to 25 wt % SO₃.

The present invention provides a process for the preparation of highly pure 2-acrylamido-2-methyl-1-propanesulfonic acid in high yield, with improved appearance, by the reaction of acrylonitrile with more than 98% sulfuric acid or oleum and liquefied isobutylene in presence of weak inorganic acids or organic sulfonic acids.

The invention discloses strong-acid cation exchange resin and a preparing method thereof. The strong-acid cation exchange resin relates to white spherical particles having a particle size of 0.42-1.4 mm prepared by suspension polymerization initiated by free radicals, wherein oil soluble unsaturated alkyl (aryl) sulfonate and styrene are adopted as monomers and raw materials, and a divinyl monomer is adopted as a crosslinking agent, the sulfonic acid group content of the cation exchange resin is 23.5-29.2%, and the ion-exchange capacity is 2.91-3.51 meq/g. The preparing method omits a sulfonation step in preparation processes of traditional cation exchange resin, and is free of use of concentrated sulfuric acid, fuming sulfuric acid and chlorosulfonic acid which have strong oxidizing properties as a sulfonation agent, thus solving an environment pollution problem caused by large-amount discharge of waste acid, and a production safety problem in traditional processes. The strong-acid cation exchange resin is used for removal of calcium ion and magnesium ion in water, and used for catalyzing heterogeneous organic synthesis reactions, such as condensation reactions of organic acids and alcohols, and alkylation reactions of phenols.

The invention relates to a preparation method of lithium hexafluorophosphate. The method comprises the following steps: (1), enabling anhydrous hydrogen fluoride and strong phosphoric acid to react under the protection of inert gas to prepare hexafluorophosphoric acid; (2), adding oleum to the hexafluorophosphoric acid prepared in the step (1) under cooling stirring to prepare phosphorus pentafluoride gas; (3), dissolving high-purity lithium fluoride in an anhydrous hydrogen fluoride solution to form an anhydrous hydrogen fluoride solution containing the lithium fluoride; (4), cooling and guiding the phosphorus pentafluoride gas into the anhydrous hydrogen fluoride solution containing the lithium fluoride, reacting, crystallizing, separating and drying to obtain a pure lithium hexafluorophosphate product; and (5), continuously guiding the unreacted and cooled phosphorus pentafluoride gas to the anhydrous hydrogen fluoride solution containing the lithium fluoride and continuously reacting to obtain a lithium hexafluorophosphate finished product. The phosphorus pentafluoride in the process is cooled to fully react so as to prevent incomplete reacted phosphorus pentafluoride powder from causing environmental-protection pressure.

A phthalocyanin-iron-cobalt-ammonium sulfonate as the dsulfurizing catalyst with high catalytic activity and desulfurizing efficiency (more than 99%) is prepared through preparing the sulfonated chemical from phthalic anhydride as raw material and smoking sulfuric acid as sulfonating agent, preparing phthalocyanin-iron-cobalt- ammonium sulfonate from said sulfonated chemical, ammonium molybdate as catalyst, urea, cobalt chloride and iron salt, drying, and pulverizing.

The invention relates to a chemical product preparation method, particularly a method for preparing sodium dimethyl isophthalate-5-sulfonate from high-concentration fuming sulfuric acid, which comprises the following steps: (1) mixing m-phthalic acid and 60-70% fuming sulfuric acid to carry out sulfonation reaction, thereby obtaining a sulfonated product; (2) adding methanol into the sulfonated product to carry out esterifying reaction, thereby obtaining the esterified product; (3) adding water into the esterified product, adding sodium carbonate at 20-55 DEG C to regulate the pH value to 5-7.5, thereby obtaining a neutralized material; and (4) separating and purifying the neutralized material, and drying to obtain the sodium dimethyl isophthalate-5-sulfonate finished product. The ternary-monomer generated in the invention has the advantage of high product quality, and the mother liquor process water can be utilized cyclically, thereby thoroughly implementing closed circulation of the process water and completely achieving zero discharge in the whole production process.

The invention provides a manufacturing method of anthypnotic wet tissue. During pulping, 2-5wt% wet strength agent and 1-2wt% softener are added, a large roll of toilet paper can be produced by the conventional paper-making process and, is subjected to back-rolled and is cut into small rolls. The paper is soaked in an anthypnotic liquid medicine so thatto enable that the water content is in a range of 40-100% and packaged tightly to form the product. The anthypnotic liquid medicine consists of components A and B. The component A is prepared by dissolving 6-12 parts of oleum menthae, 2-4 parts of wintergreen oil, 4-12 parts of menthol, 4-8 parts of camphor, 2-6 parts of borneol, 5-10 parts of ginger extract, 1-2 parts of clove oil and 1-3 parts of eucalypus oil in 100-400 parts of ethanol, and adding 5-20 parts of emulsifier. The component B is prepared by dissolving 20-100 parts of glycerol, 20-200 parts of propylene glycol, and 0.5-5 parts of acetic chlorhexidine in 500 parts of water. The product is flexible in texture and good in toughness, and can be used as anthypnotic and refreshing healthcare facial tissue.

The invention relates to a preparation method of calcium sulfonate salt with low alkali value. The preparation method comprises the following steps that: synthesis alkylbenzene with the molecular weight between 300 and 450 is sulfonated by oleum, a certain amount of water is added after sulfonation for 2-5 hours, then nitrogen gas is used for purging, an inert solvent and base oil are used for dilution, then standing and stratification are carried out to obtain coarse sulfonic acid of an upper layer, an alkali filter aid is used for filtration to obtain synthesis alkyl benzene sulphonate diluted by a purifying solvent, the total acid value of the synthesis alkyl benzene sulphonate is 60 to 120mgKOH/g, and the concentration of free acid is controlled below 0.2%; and then, a sodium hydroxide water solution is used for carrying out a neutralization reaction, then solid calcium chloride is added to carry out a double-decomposition reaction, and finally, stratification, water washing and distillation are carried out to obtain low-alkali-value synthesis alkyl benzene calcium sulfonate salt which does not contain or contains trace sulfate radicals and chlorine radicals and has good antirust performance and superior cleaning performance.

The invention discloses a method for preparing an emulsified medicinal composition containing oleum fructus bruceae, which comprises the following steps: (1) mixing a proper amount of water and 1 to 10ml of glycerin; (2) adding at least one of yolk lecithin and poloxamer into liquid prepared in step (1), and performing shear mixing uniformly, wherein the yolk lecithin is between 0.5 and 10g, and the poloxamer is between 0.1 and 5g; and (3) slowly adding 5 to 30ml of oleum fructus bruceae into liquid prepared in step (2), adding water to make the total content be 100ml, adjusting the pressure of a high pressure homogenizer, adopting two-step emulsification method, and continuously circulating 3 to 6 times to prepare the emulsified medicinal composition containing the oleum fructus bruceae.The oleum fructus bruceae emulsion injection prepared by the method has good stability, no hemolysis in a period of validity, and safety, and is favorable for clinical promotion and application.

The invention provides a method for preparing high-purity beta elemene from natural plants containing the beta elemene such as curcuma zedoary (earthnuts or tubers of the curcuma zedoary), cedronella (fresh leaves of the cedronella), yellowtop (roots, stems, leaves, flowers and seeds of the yellowtop) and so on, which can improve the production efficiency from starting materials to the high-purity beta elemene and reduce the production cost. Compared with the prior art, the method is mainly different in that the roots, stems, leaves, flowers and seeds of the natural plants are taken as raw materials; oleum volatile of specific parts of the natural plants is obtained by methods for extracting different oleum volatiles, and is rectified by the rectification method to obtain the beta elemene with high content; impurity compositions are removed by the macroporous adsorption resin separation method or macroporous adsorption resin combined with the ethanol extraction method, and the silver nitrate complex extraction method in turn; and finally the beta elemene with the content between 95.0 and 99.9 percent is obtained through reduced pressure distillation or rectification. The bulk pharmaceutical chemicals not only can be prepared into oral dosing preparation such as emulsion oral liquid, self-emulsifying/ self-microemulsifying capsules, soft capsules and so on, but also can be prepared into non-alimentary dosing preparation such as emulsion injection, liquid drugs injection, transdermal absorbent, lung sprays, suppository and so on. The method has the advantages of novel design, simple apparatus, concise operating steps, obvious shortened operating time, improvement of the production efficiency and high yield coefficient, and is suitable for industrialized production.

The invention discloses a preparation method for hyperpure sulphuric acid, and fuming sulphuric acid is taken as raw materials. The preparation method comprises the following steps of 1 distilling; 2 purifying and filtering; 3 sulfur trioxide liquid separating; 4 evaporating; 5 multi-stage absorbing; 6 gas stripping tower impurity removing; 7 finished product obtaining. In the hyperpure sulphuric acid, the concentration of particles with the particle size larger than or equal to 0.5 micrometer is smaller than 5 p/ml, the concentration of particles with the particle size larger than or equal to 0.2 micrometer is smaller than 100 p/ml, the content of single metal ions is smaller than 0.1 ppb, and the content of sulfur dioxide is smaller than 3 ppm. According to the preparation method for hyperpure sulphuric acid, the technology is simple, the energy consumption is low, purified sulfur trioxide gas is firstly obtained through a reasonable purifying and impurity removing technology, then ppt-grade hyperpure sulphuric acid is obtained through multi-stage absorbing and gas stripping, the content of trace sulfur dioxide impurities in hyperpure sulphuric acid is effectively controlled, and a foundation is laid for production of a new generation of hyperpure sulphuric acid.

The invention discloses a sulfonated polysulfoneamide proton exchange membrane and a preparation method thereof. By selecting the new materials of the polysulfoneamide as raw materials, the invention prepares the sulfonated membrane materials. The amide and the sulfonyl group in the PSA molecule are connected with each other on the para phenyl and form a linear macromolecule with the para phenyl; as the strong electro-withdrawing phenyl group exists on the macromolecular chain, the molecular structure is driven to have more excellent heat resistance, thermal stability and thermal oxidation resistance than the traditional acromatic polyamide through the double-bond conjugation of the benzene ring. The mixed acids comprising the concentrated sulfuric acids and oleums are selected as the sulfonating agents, thus lowering material viscosity and helping heat transfer and being beneficial to uniform and complete implementation of the sulfonation and reducing occurrence of the side reaction. The high activity of the oleums is helpful for enhancing the sulfonation degree of the sulfonated bodies. The introduction of the sulfonic group (-SO3H) in the main-chain structure of the polymer can remarkably enhance the proton conductivity and water content of the polymers. The invention has the advantages that the invention provides a proton exchange membrane which endures high temperature, has stable chemical performance, high proton conductivity, excellenet antioxidation property and thermal stability, etc., and has low cost and is suitale for fuel cells, and also can be used as various ultrafiltration membranes, nanofiltration membranes or reverse osmosis membranes and has wide application prospect.

The invention discloses a preparation method of high-pure phosphorus pentafluoride gas, which comprises: phosphorus pentoxide is put into a reaction container lined with PTFE and is introduced with anhydrous hydrogen fluoride, and the temperature is preserved to be minus 20 to 0 DEG C; according to the chemical reaction counting, the anhydrous hydrogen fluoride is overdosed by 50 to 60 percent; the reaction is carried out for 3 to 5 hours. After the reaction is completed, 60 percent of oleum is added in an intermittent way with stirring and the dosage of the oleum is 35 to 40 percent more than a theoretic value. The intermediate outcome of the reaction is heated for decomposing under the temperature of 120 to 150 DEG C so as to generate the phosphorus pentafluoride; the product is guided into a condenser for cooling the impurity and then the high-pure phosphorus pentafluoride is obtained. The content of PF<5> obtained by the method is greater than 99.9 percent, the content of impurity is low, the water content is less than 10ppm, HF content is less than 50ppm; moreover, the process equipment is comparatively simple, thus being beneficial to the industrial manufacturing.

The invention relates to a method for preparing gemini long-chain alkyl benzene disulfonate oil displacement agents. The method comprises: adding 100 mL of distilled water and N,N-dimethylformamide mixed solvent in a volume ratio of 1:1, 0.05 mol of iron powder and 0.005 mol of copper powder and aging the materials for 10 minutes at 30 DEG C; adding 0.004 mol of cuprous chloride; raising the temperature to 70 DEG C and adding 0.1 mol of long-chain alkyl benzyl chloride dropwise; performing reaction for 20 hours at 90 DEG C; diluting filtrate with petroleum ether and rotationally steaming organic layers to remove the petroleum ether; diluting 0.04 mol of the obtained product with 40 mL of carbon tetrachloride, controlling the temperature below 5 DEG C and adding 10 mL of 50 percent oleum dropwise; and diluting reactant with 200 mL of water and 50 mL of carbon tetrachloride, removing aqueous solution in an upper layer and performing neutralization by use of sodium hydroxide solution or ammonia. The oil displacement agents with the concentration of 20 mg/kg can reduce interfacial tension to 5.8*10<-3>mN/m.

The invention discloses a caprolactam preparation method. The method is characterized in that caprolactam is prepared from cyclohexanone through oximation and rearrangement, and the method comprises the following steps: carrying out a catalytic reaction on cyclohexanone, hydrogen peroxide and ammonia to generate cyclohexanone oxime, extracting and separating by using a solvent A, adding a solvent B to the above obtained oil phase, carrying out a Beckmann rearrangement reaction under the action of oleum, carrying out slaking flash evaporation separation on the obtained product, hydrolyzing, extracting by using water, and carrying out original process refining to prepare finished caprolactam. The method shortens the caprolactam production process flow, reduces the consumption of raw materials and energy, generates less ammonium sulfate than original technologies, and improves the quality of the caprolactam product.

A novel class of proton exchange membrane materials, sulfonated poly(phthalazinones), were prepared by modification of poly(phthalazinone). Sulfonation reactions were conducted at room temperature using mixtures of 95-98% concentrated sulfuric acid and 27-33% fuming sulfuric acid with different acid ratios in order to get SPPEK with degree of sulfonation (DS) in the range of 0.6 to 1.0. The presence of sulfonic acid groups was confirmed by FT-IR analysis, and the DS and structures were characterized by NMR. The introduction of sulfonic groups into the polymer chains led to an increase in the glass transition temperature and a decrease in the decomposition temperature. Membrane films were cast from solution in N,N-dimethylformamide or N,N-dimethylacetamide. Water uptakes and swelling ratios of the membrane films increased with DS and sulfonated polymers with DS>1.2 were water soluble at 80° C. Proton conductivity increased with DS and temperature up to 95° C., reaching 10⁻²S/Cm.

The invention relates to a new clean resorcinol production method, in particular to a process of the new clean resorcinol production method. The process comprises the following steps: respectively adding gaseous SO3 and liquid SO3 as sulfonating agents and benzene to a circular injection reactor for a secondary sulfonating reaction; and recycling a byproduct NaCl generated in a sulfonating working procedure in a sodium fluosilicate workshop. The method consumes acid in one third amount of oleum, generates a sulfoacid product containing little waste acid, reduces alkali consumption for neutralization, greatly decreases the raw material cost, provides self-sufficiency industrial salt and has wide industrialized production prospects.

The invention provides a kind of healthy harmonized oil containing linoleic acid and linolenic acid at a ratio of 4:1 for pregnant women. The harmonized oil is composed of perillartine, oleum lini, sunflower oil, oleum camelliae and bean oil at an uncertain ratio. There is 50wt.% essential fatty acid, 40wt.% linoleic acid, 10wt.% linolenic acid in the harmonized oil. Linolenic acid (C18:3, Omega-3) which can grow to eicosapentaenoic acid (EPA, C20:5, Omega-3) under the affect of enzyme of human liver is added into the edible vegetable oil. EPA is considered to be the main substance capable of cleaning blood dirties in blood vessels and is called as street sweeper of blood vessels by medical experts. EPA can also grow to docosahexaenoic acid (DHA, C22:6, Omega- 3) which is the core substance for forming brain and amphiblestroid membrane occupying one quarter of the whole brain and is called as brain gold by nutritionist. Thus, the prescription has influential contribution in promoting infant intelligence, protecting eyesight, promoting brain formation and reinforcing remembrance.

The present invention discloses one kind of normal temperature efficient hydrogen sulfide eliminating agent prepared with sodium 1-nitroanthraquinone disulfonate. Sodium 1-nitroanthraquinone disulfonate is prepared through reaction of 1-amino anthraquinone and oleum to obtain 1-nitroanthraquinone disulfonic acid solution, dropping 1-nitroanthraquinone disulfonic acid solution into water via stirring and adding oxidant to react for obtaining 1-nitroanthraquinone disulfonic acid solution, adding alkali to neutralize and to obtain sodium 1-nitroanthraquinone disulfonate solution, heating and filtering, vacuum dewatering the filtrate, cooling to normal temperature, filtering and drying to obtain sodium 1-nitroanthraquinone disulfonate product. The present invention has simple preparation process, and the hydrogen sulfide eliminating agent has low desulfurizing temperature, desulfurizing efficiency up to 99.99 %.