2622 results about "Thionyl chloride" patented technology

An improved process for chlorination of sugars produces chlorodeoxy derivatives, in particular the chlorination of sucrose-6-esters to produce sucralose (4,1′,6′-trichloro-4,1′,6′-trideoxy galactosucrose), with thionyl chloride and N,N-dimethyl formamide (DMF) at the ration of about 1 molar equivalent of thionyl chloride for every molar equivalent of free hydroxyl group.

The invention discloses a metal phthalocyanine/carbon nanometer pipe compound catalyst, a method for preparing the same and a lithium/thionyl chloride battery using the same, wherein the metal phthalocyanine/carbon nanometer pipe compound catalyst is prepared by evenly and closely loading metal phthalocyanine compounds on a carbon nanometer pipe; and the metal phthalocyanine/carbon nanometer pipe compound catalyst is mixed with carbon black and a binding agent, and the mixture subjected to forming and drying to prepare an anode carbon plate of the lithium/thionyl chloride battery using the catalyst. The metal phthalocyanine compounds are evenly and closely loaded on the carbon nanometer pipe. On one hand, the electrically discharged product of a LiCl film can be loosened by the catalysis of the metal phthalocyanine compounds; on the other hand, a network structure is built up in the carbon anode of the carbon nanometer pipe, which facilitates the electric communication of electrolytes and the improvement of electric conductivity of the electrodes. Due to the synergetic effect of the metal phthalocyanine compounds and the carbon nanometer pipe, the operating voltage of the lithium/thionyl chloride battery is improved. The method has advantages of simple process, simple operation, the suitability for industrialized production and obvious practical values and economic benefits.

The invention relates to a process for preparing 4,4'-dichlorodiphenylsulfone, in particular to a process for preparing 4,4'-dichlorodiphenylsulfone employing a sulfoxide oxidation method. The process comprises the following steps: carrying out friedel-crafts reaction with chlorobenzene and thionyl chloride under the action of a catalyst to obtain the 4,4'-dichlorodiphenylsulfone; dissolving the obtained 4,4'-dichlorodiphenylsulfone with a solvent; adding hydrogen peroxide and carrying out oxidation reaction to obtain a 4,4'-dichlorodiphenylsulfone crude product; carrying out secondary oxidation refining on the obtained 4,4'-dichlorodiphenylsulfone crude product; and finally preparing high-purity 4,4'-dichlorodiphenylsulfone. The purity of the 4,4'-dichlorodiphenylsulfone purified by the refining process is greater than 99.5%; the refining yield is greater than 98.5%; and the process completely meets the synthesis requirements of high-performance polymers.

The invention discloses a preparation method of improved 4,4-dichlorodiphenylsulfone. The method comprises steps that: (1) Al2Cl3 is adopted as a catalyst; chlorobenzene, thionyl chloride are adopted as reaction materials; the materials are subject to a Friedel-Crafts reaction; a mother liquor obtained after the reaction is hydrolyzed; the hydrolyzed mother liquor is refluxed for 45 to 60min under a temperature of 95 to 100 DEG C; after refluxing, the mother liquor is cooled to below 20 DEG C, such that the liquor is divided into an organic phase and a water phase; the organic phase is processed through reduced-pressure distillation and centrifugal washing until the organic phase turns neutral, and the organic phase is preserved as a product M for later use, wherein a main component in the product M is 4,4-dichlorodiphenylsulfone; (2) the product M and an oxidizing agent of hydrogen peroxide are adopted as raw materials, and 1,2-dichloropropane is adopted as an organic solvent; an oxidizing reaction is carried out upon the main component 4,4-dichlorodiphenylsulfone in the product M under the effect of a composite catalyst, such that a 4,4-dichlorodiphenylsulfone crude product is synthesized, wherein the composite catalyst is phosphotungstic acid or silicotungstic acid loaded on active carbon. Therefore, the method provided by the invention has advantages of high yield and good product quality. With the method, wastewater can be circulated and reused.

The invention discloses a new preparation method of 4,4-dichlorodiphenyl sulfone. The method comprises the following steps: 1) through using AlCl3 as a catalyst, and chlorobenzene and thionyl chloride as reaction raw materials, performing a Friedel-Crafts reaction at 25-35 DEG C, then hydrolyzing the mother liquor obtained through the Friedel-Crafts reaction, refluxing at 95-100 DEG C for 45-60 minutes, cooling the obtained mother liquor to less than 20 DEG C after refluxing to obtain an organic phase and an aqueous phase; 2) performing reduced pressure distillation on the organic phase, centrifuging, washing the obtained product to be neutral and be used as a product A for later use, wherein the main component of the product A is 4,4-dichlorodiphenyl sulfoxide; and 3) through using the product A and the oxidant hydrogen peroxide as raw materials and acetic acid as satalytic solvent, carrying out an oxidation reaction on the main component 4,4-dichlorodiphenyl sulfoxide of the product A to obtain crude 4,4-dichlorodiphenyl sulfone. Therefore, the existing synthesis method of 4,4-dichlorodiphenyl sulfone is changed, the production cost of 4,4-dichlorodiphenyl sulfone is low, the product quality is good and the reaction time is short.

The invention discloses a method for preparing 4.4-dichlorodiphenyl sulfone by using sulfoxide oxidation. The method comprises the following steps of: (1) performing Frieldel-Crafts reaction at the temperature of 25-35 DEG C by taking AlCl3 as a catalyst and chlorobenzene and thionyl chloride as reaction raw materials; next, hydrolyzing mother liquor after the Frieldel-Crafts reaction is finished; refluxing at the temperature of 95-100 DEG C for 45-60 minutes after hydrolysis is finished; cooling to be below 20 DEG C to divide into an organic phase and a water phase after refluxing is finished; performing reduced pressure distillation and centrifugal washing on the organic phase to be neutral to serve as a product A for later use, wherein a main component in the product A is 4.4-dichlorodiphenyl sulfone; and (2) performing oxidation reaction on the 4.4-dichlorodiphenyl sulfone by taking the product A as the raw material, hydrogen peroxide as a catalyst and dichloromethane as a reaction solvent to synthesize a 4.4-dichlorodiphenyl sulfone rough product. Thus, the method has the advantages of mild reaction conditions, high product quality and low three wastes (waste water, waste gas and industrial residues).

A method for preparing multi-arm poly(ethylene glycol) (PEG) amines from multi-arm PEG polyols is described. The method comprises a two step process, wherein the multi-arm PEG polyol is first reacted with thionyl chloride to form a multi-arm PEG chloride, which is subsequently reacted with aqueous or anhydrous ammonia to yield the multi-arm PEG amine.

The invention discloses a synthetic process for efficiently and continuously producing 4,4-dichlorodiphenyl sulfone, which comprises the following steps: carrying out Friedel-Crafts acylation on thionyl chloride and excessive chlorobenzene under the action of a lewis acid catalyst, carrying out pyrohydrolysis and adding chlorobenzene to carry out layering after the reaction is finished, adding anoxidizing agent into a sulfoxide organic layer to carry out oxidization, adding activated carbon to carry out decoloration and filtering; cooling filtrate and carrying out rejection filtration to obtain 4,4-dichlorodiphenyl sulfone. The synthetic process has the advantage that chlorobenzene not only is a raw material, but also is a reaction solvent, so that cross use of various solvents is avoided. Particularly, use of a great amount of acetic acid used as an oxidation reaction solvent is avoided, and corrosion to equipment and environmental pollution are avoided. In the integral process flow,separation and extraction of an intermediate 4,4-dichlorodiphenyl sulfoxide are avoided, so that production time of the product is greatly shortened, and production cost is saved. By using hydrogen peroxide, acetic acid and concentrated sulfuric acid as mixed oxidizing agents, oxidization capacity of hydrogen peroxide is greatly improved, yield and purity of the product are greatly improved, yield of the product reaches 90% or more, and purity of the product is greater than 99.8%.

The invention discloses a functional graphene oxide for adjusting and controlling the dispersibility of a solvent by using an organic chain segment as well as a preparation method thereof. The structural formula of the functional graphene oxide is shown in specification, wherein R is equal to R1, R2 and R3. The preparation method comprises the following steps: 1, dispersing graphite oxide prepared by a Hummers method in N, N-dimethylformamide to form uniform dispersion liquid; 2, adding a thionyl chloride agent into the product obtained in step 1 to perform reflux reaction to synthesize an intermediate product of graphite oxide activated by acyl chloride; 3, distilling the mixed liquor obtained in step 2 under reduced pressure to remove excessive thionyl chloride; 4, adding pyridine and graft organic molecules into the product obtained in step 3, and heating and stirring the mixture; and 5, filtering, washing and then drying the mixed liquor obtained in step 4. The functional grapheneoxide can disperse well in different solvents, particularly solvents with low polarity and low boiling point, can be preferably compatible with multiple polymer molecules, leads the preparation of nano particles/ polymer nano composite materials to be possible, and has good application prospects and economic benefits.

The invention discloses a synthetic method of thiophene-3-ethanol. The method comprises the following steps of: adding a halogenated hydrocarbon solvent and ethylene glycol into a reaction kettle, dropwise adding thionyl chloride and preserving heat for reacting; separating liquid and extracting to obtain an organic phase containing a substance shown in the specifications; adding a ruthenium trichloride aqueous solution and a sodium bicarbonate aqueous solution in the presence of the halogenated hydrocarbon solvent and dropwise adding a sodium hypochlorite aqueous solution; after detecting that a system does not have oxidizing property, performing liquid separation, concentration, devitrification and drying to obtain a substance shown in the specifications, adding an ester solvent and butyl lithium into a reaction kettle, adding a prepared ester solution of tribromothiofuran and a prepared ester solution of the substance, separating the liquid and extracting to obtain a system containing a substance shown in the specifications; and adding a dilute sulfuric acid into the system containing the substance shown in the specifications, concentrating, neutralizing, extracting and concentrating to obtain an end product. The method has the advantages of high reaction purity and yield, stable process condition, easiness for operation and mass production capability; and the thiophene-3-ethanol is prepared from tribromothiofuran by performing low-temperature lithiation, so that the use of epoxy ethane serving as an explosive hazard is avoided, and mass production becomes possible.

The invention discloses a preparation method of vinyl sulfate. The preparation method comprises the following steps: (1) substitution reaction: carrying out substitution reaction on thionyl chloride and ethanediol used as raw materials, washing the reaction solution with deionized water to a neutral state, standing, stratifying, and separating to obtain vinyl sulfite; (2) oxidation reaction: adding dichloromethane and a ferric sulfate solution into the vinyl sulfite, cooling to 0-5 DEG C, dropwisely adding a sodium percarbonate solution to obtain a water-phase/organic-phase-coexistent reaction solution, standing the reaction solution, stratifying, separating out the water phase, and carrying out reduced pressure distillation on the organic phase, thereby obtaining the vinyl sulfate crude product; and refinement: recrystallizing the vinyl sulfate crude product by using dichloromethane to obtain the high-purity vinyl sulfate. The preparation method has the characteristics of high mole yield, high product purity, low moisture content, low acid value and low preparation cost. The mole yield can reach 85% or above, the purity can reach 99% or above, the moisture content is less than or equal to 60 ppm, and the acid value is less than or equal to 60 ppm.

The invention opens a high orientation carbon nano-pipe complex fiber, which is composed of carbon nano pipe and polymer (1: 2-1000). The process is: the pipe is dispersed by ultrasonic in the strong acid for 0.5-10h; the pipe reacts with the thionyl chloride or the diisocyanate for 4-24hrs in 60-75 Deg C.; The micro/macro molecule reacts with the COCI and the NCO for 4-24hrs in 50-250 Deg C.; Last to get the complex fiber by high voltage electrostatic spinning with the space length of the pole is 1mm-100mm.

The invention discloses a novel strongly and weakly alkaline anion exchange resin with adsorption and ion exchange functions and a preparation method thereof, and relates to the field of anion exchange resin and a preparation process thereof. The novel anion exchange resin with the adsorption and ion exchange functions comprises a strong alkali group and a weak alkali group, the exchange capacityof strong alkali is 2.9 to 5.7meq for each gram of dry agent, and the exchange capacity of weak alkali is 2.8 to 3.2meq for each gram of dry agent. The preparation method of the resin comprises the following steps of: performing nucleophilic substitution reaction on macroporous chloromethylated polystyrene resin serving as a raw material and an alcohol amine compound, and reacting with thionyl chloride for further quaternization to obtain the strongly and weakly alkaline anion exchange resin.

The invention provides carbon nano tubes modified by polymers with maleic anhydride chain segments and a preparation method of the carbon nano tubes. The carbon nano tubes are processed in one-step acidification treatment with concentrated sulfuric acid and concentrated nitric acid, and then have reaction with thionyl chloride after being processed in two-step acidification treatment with concentrated sulfuric acid and hydrogen peroxide. The product obtained from the above process has reaction with dihydric alcohol to obtain the modified carbon nano tubes with hydroxyl. Then the carbon nano tubes modified by polymers with maleic anhydride chain segments are obtained by means of the polymerization reaction between the hydroxyl and the polymers with maleic anhydride chain segments. Thereby, the carbon nano tubes can disperse into the composite materials well, the compatibility of the carbon nano tubes with the other materials are improved, so that the carbon nano tubes can take the advantages maximally and realize the functional design and application.

The invention relates to a processing method of thionyl chloride acyl-chlorinated tail gas. Mixed tail gas produced by a acyl chlorinating process contains hydrogen chloride and sulfur dioxide; the sulfur dioxide is liquefied under a certain temperature condition; the incondensable hydrogen chloride and a little sulfur dioxide are absorbed in two stages by water; the absorbed tail gas in a first stage is pure hydrogen chloride gas; after being absorbed in a second stage, the qualified chlorhydric acid is obtained; first-stage falling film absorption liquid is resolved by heating; then the tail gas is sent to a liquefying process again; the liquid sulfur dioxide can be canned as a product; or after being vaporized, the liquid sulfur dioxide is absorbed by 30 percent of sodium hydroxide solution to obtain sodium sulfite aqueous solution which is further dried after low temperature crystallization or distillation to obtain 97 percent of sodium sulfite solid. With the method, the hydrogen chloride, the sulfur dioxide and a little thionyl chloride produced by an acyl chlorination synthetic process can be separated out to obtain the chlorhydric acid and the pure sodium sulfite solid. The processing method of the thionyl chloride acyl-chlorinated tail gas of the invention is capable of effectively recovering the thionyl chloride acyl-chlorinated tail gas, which has the advantages of safety process and easy control.

The invention belongs to the technical field of crossing of chemical engineering, materials engineering and environmental engineering, particularly relates to an improvement technology of cellulose membrane materials and a chemical grafting and fixing technology for treating anthraquinones compound carriers of wastewater containing nitrogen, and particularly relates to a method for preparing an anthraquinone functional cellulose membrane by fixing an anthraquinone compound on microcrystalline cellulose by chemical grafting. According to the method, the microcrystalline cellulose is used as a raw material; firstly, ionic liquid is used as a solvent for dissolving the microcrystalline cellulose; thionyl chloride modified cellulose is used for preparing cellulose chloride and then the cellulose chloride is reacted with amino anthraquinone in dimethylformamide to prepare an anthraquinone functional cellulose membrane material; the substitution degree of the prepared cellulose chloride can reach 1.89 and the anthraquinone grafting rate of the anthraquinone functional cellulose membrane reaches 82%; the anthraquinone functional cellulose is prepared by the two-step reaction; the content of anthraquinonyl is high and the grafting rate is high; the fixing effect is stable; finally, the anthraquinone functional cellulose is changed into the membrane by a phase transferring method; the membrane material can be used for accelerating and strengthening the biological degradation process in the treatment of the wastewater containing the nitrogen.

The present invention relates to a novel process for the preparation of 1-alkyl or 1-cycloalkyl derivatives of 3-hydroxy-4-oxo-1,4-dihydropyridine-2-carboxamide of formula I. The process includes reacting an amine R²NH₂ with a compound of formula II in a solution of metal hydroxide in water to give a compound of formula III. Subsequent reaction of the compound of formula III with an acid chloride formation reagent in an inert solvent gives compounds of formula I. The acid chloride formation reagent is selected from oxalyl chloride and dimethylformamide, dimethylchloromethylene-ammonium chloride and thionyl chloride and dimethylformamide. If desired, a compound of formula I where R⁵ is hydrogen may be formed when an intermediate substituent is used wherein R⁵ is an alcohol protective group removable by catalytic hydrogenation.

The invention relates to a functionalized carbon nanotube which can be used as epoxy resin curing agent and the preparation method, which belongs to the technical field of the nano-material. After a purified carbon nanotube is treated with strong oxidative acid, a carboxylated carbon nanotube is obtained; the carboxylated carbon nanotube is chlorided by thionyl chloride, and the obtained product is reacted with polyhydric alcohol or polybasic amine to obtain a modified carbon nanotube with hydroxyl or amidogen; then the hydroxyl is utilized to react with aromatic polybasic acid anhydride compound to obtain the functionalized carbon nanotube with anhydride group and carboxyl group, which can be further used as curing agent to ensure carbon nanotube well dispersed in epoxy resin, thus to improve the compatibility between the carbon nanotube and the epoxy resin, both the mechanical property and the thermal stability of the epoxy resin can be improved, thereby the advantage of the carbon nanotube can be exerted to the maximum, and the functional design and the application of the carbon nanotube can be achieved.

The invention relates to a method for preparing the designed herbicide pretilachlor intermediate chloride ether. Under the action of organic amine catalyst, the chloride ether can be obtained by ethylene glycol monopropyl ether and bis (trichloromethyl) hydroxyphenyl in the organic solvent through the following chemical equation: HOC2H4OC3H7+Cl3COCOOCCl3 arrow ClC2H4OC3H7+CO2+HCl. The method replaces the traditional chlorination reagent with the bis (trichloromethyl) hydroxyphenyl, such as, thionly chloride, phosphorus oxychloride and hydrogen chloride, etc., and the potential safety hazard can be eliminated from the process source by using the novel chlorination reagent. Simultaneously, the emissions of pollutants are greatly reduced, and the method is a cleaning process with mild reaction conditions, safe and reliable operating process and high product yield, and has good industrialization implementation value and social economic benefits.

The invention provides a cationic fluorosurfactant (I) and a preparation method thereof. The method comprises adopting perfluorobutenyloxy benzoic acid and thionyl chloride as raw materials to perform a chloroacylation reaction at -30 DEC C to 70 DEC C in polar solvent, adding N,N-dimethyl propylene diamine and base catalyst, performing an amidation reaction at -20 DEC C to 120 DEC C, separating the reactant liquor to obtain N-[3-(p-perfluorobutenyloxybenzamido)propyl]-N, N-dimethyl amine, dissolving into non-proton polar solvent, adding iodomethane, performing a quaternization reaction at 0 DEC C to 100 DEC C, and filtering the reactant liquor to obtain N-[3-(p-butenyloxybenzamido)propyl]-N,N,N-trimethyl ammonium iodide. The method has simple synthetic method and high reaction yield. Aqueous solution prepared from the N-[3-(p-butenyloxybenzamido)propyl]-N,N,N-trimethyl ammonium iodide has low surface tension.

A method of repairing damaged low-k dielectric materials is disclosed. Plasma-based processes, which are commonly used in semiconductor device manufacturing, frequently damage carbon-containing, low-k dielectric materials. Upon exposure to moisture, the damaged dielectric material may form silanol groups. In preferred embodiments, a two-step approach converts the silanol to a suitable organic group. The first step includes using a halogenating reagent to convert the silanol to a silicon halide. The second step includes using a derivatization reagent, preferably an organometallic compound, to replace the halide with the suitable organic group. In a preferred embodiment, the halogenating agent includes thionyl chloride and the organometallic compound includes an alkyllithium, preferably methyllithium. In another preferred embodiment, the organometallic compound comprises a Grignard reagent. Embodiments disclosed herein advantageously enable the manufacturer to engineer the density, polarization, and ionization properties of the low-k dielectric material by selective incorporation of the organic group.

The invention provides a preparation method of mesotrione. The preparation method comprises is capable of preparing the target product from raw materials such as ortho-nitrotoluene, chlorosulfonic acid, sulfoxide chloride, sodium sulfite, chloroactic acid, 1,3-cyclohexanedione in the presence of a catalyst and acid-base. The preparation method is based on common chemical raw materials, the reaction flow of each step is implemented under conventional operation conditions, the amount of three wastes is low, the total yield is above 61%, the purity of the product is high, the purity of the coarse product of the mesotrione is greater than 98%, and the coarse product of the mesotrione can be further purified; as a result, the preparation method of mesotrione is applicable to large-scale industrial production.

The invention relates to the field of graphene materials, in particular to a novel method for preparing a graphene material by reducing graphene oxide (GO). The method is suitable for reducing various graphene-oxide-based powder and thin-film materials. In the method, a graphene oxide product is soaked for 10 seconds-24 hours in a halogenating reagent, such as hydroiodic acid, hydrobromic acid, sulfoxide chloride and the like, in a temperature range from minus 5 DEG C to 140 DEG C, and is taken out and dried, thereby the reduction of the graphene oxide material is completed; and the graphene material obtained after reduction has an excellent electric conduction performance and can maintain the flexibility of thin-film products. The method is simple and is easy to control, can realize the reduction on lots of graphene materials at low temperature with high efficiency and low cost and is beneficial to solving of the problems of environment pollution, high cost and the like in the prior art.

The invention relates to a preparation method of a multicomponent-modified carbon-fiber-reinforced epoxy resin composite material, which comprises the following steps: oxidizing carbon nanotubes (CNTs) with strong acid; carrying out acyl-chlorination and amination on the oxidized CNTs sequentially with thionyl chloride and diamine to introduce amino functional group; oxidizing carbon fiber with strong oxidizing acid, and carrying out acyl-chlorination treatment with thionyl chloride to introduce acyl chloro group; mixing the prepared modifying CNTs and modifying carbon fiber to perform graft reaction, thereby obtaining the CNTs-grafted carbon fiber; mixing the CNTs-grafted carbon fiber with polyhedral oligomeric silsesquioxane (POSS) to perform graft reaction, thereby obtaining the binary POSS-grafted carbon fiber; and sufficiently infiltrating the binary POSS-grafted carbon fiber in the base resin, and carrying out hot pressing to perform curing formation. The CNTs and POSS cografted on the carbon fiber surface can improve the surface topography of the carbon fiber, increase the contact area with the resin base and penetrate into the resin base under the anchoring action, so that the interfacial mechanical mesh action is higher.

The invention provides a Monochamus alternatus adult attractant. The Monochamus alternatus adult attractant comprises an artificially-synthesized compound, and the compound is prepared through adding reagents comprising undecyl alcohol, thionyl chloride, glycol, metallic sodium and the like. The Monochamus alternatus adult attractant comprises the artificially-synthesized compound, so the effective application amount is less; the Monochamus alternatus adult attractant has a high trapping effect on Monochamus alternatus, and can be used as an effective means for monitoring and controlling the Monochamus alternatus to inhibit and delay the propagation of the pine wilt disease; and the Monochamus alternatus adult attractant generally has the advantages of simple components, low production cost, safety, environmental protection, high insect trapping efficiency, and advantage obviousness.