36 results about "Bunte salt" patented technology

The present invention is directed to a pneumatic tire comprising at least one of an apex, flipper, and chipper, the at least one of an apex, flipper, and chipper comprising a rubber composition, the rubber composition comprising a diene based elastomer and from 5 to 40 parts by weight, per 100 parts by weight of elastomer, of a short aramid fiber having a length ranging from 0.5 to 20 mm and having a thickness ranging from 2 to 30 microns, said fiber having disposed on at least part of its surface a composition comprising an aliphatic fatty acid or synthetic microcrystalline wax; a Bunte salt; a polysulfide comprising the moiety —[S]n or —[S]o—Zn—[S]p, wherein each of o and p is 1-5, o+p=n, and n=2-6; and sulfur or a sulfur donor.

The invention discloses a synthesis method of aryl-aryl, aryl-alkyl and alkyl-alkyl asymmetric persulfides as shown in a formula (II) or a formula (IV). According to the synthesis method, with sulfinic acid sodium salt, and halogenated hydrocarbon and Na2S2O3 as reaction materials or Bunte salt as a reaction material instead of the halogenated hydrocarbon and Na2S2O3, the aryl-aryl, aryl-alkyl and alkyl-alkyl asymmetric persulfides are obtained by reaction in the absence of transition metal. The synthesis method has the advantages that the reaction is efficient; the yield is high; a vulcanizing reagent is cheap, easily available, stable, and free of pungent smell; no strong acid or alkali or extra oxidizing or reducing agent is added in reaction; the condition is relatively mild; and no transition metal is used as a catalyst in the reaction, and therefore the method is economical, practical and friendly to the environment; a reaction substrate is easy to prepare; the reaction efficiency is high after the reaction is amplified, and therefore, the synthesis method has a wide application prospect and practical value.

The present invention is directed to a pneumatic tire comprising at least one of an apex, flipper, and chipper, the at least one of an apex, flipper, and chipper comprising a rubber composition, the rubber composition comprising a diene based elastomer and from 1 to 50 parts by weight, per 100 parts by weight of elastomer, of aramid fiber having a length ranging from 0.5 to 20 mm and having a thickness ranging from 2 to 30 microns, said fiber having disposed on at least part of its surface a composition comprising an aliphatic fatty acid or synthetic microcrystalline wax; a Bunte salt; a polysulfide comprising the moiety -[S] n or - [S] o -Zn-[S] p , wherein each of o and p is 1-5, o + p = n, and n = 2-6; and sulfur or a sulfur donor.

According to the invention, Bunte salt is employed as a sulfur source to prepare 3-indole thioether. At a certain temperature, elementary iodine or hydroiodic acid and salts thereof is employed as a catalyst, dimethyl sulfoxide is employed as an oxidant, and the Bunte salt is employed as the sulfur source to react with an indole compound without or with other solvents to prepare the 3-indole thioether. Reagents in the method are low in cost and easy to obtain. The method is mild in reaction conditions and is wide in substrate application. The reagents are slight in smell. The method is low in environment pollution.

The invention discloses a method for synthesizing an aryl monofluoromethylthio compound from a Bunte salt. With a phenylboronic acid derivative and S-(monofluoromethyl) sodium thiosulfate in the Buntesalt as raw materials, copper iodide as a catalyst, 1,10-phenanthroline as a ligand, potassium carbonate as alkali and methanol as a solvent, a reaction is fully carried out at the reaction temperature of 80-90 DEG C. After the reaction is finished, a reaction solution is separated and purified to obtain the aryl monofluoromethylthio compound. The method is reasonable in process condition and easy and safe to operate; the use of thiophenol and other substrates with unpleasant smell is avoided, less waste gas, waste water and industrial residue are generated, and the method is environmentallyfriendly; the reagent is simple in synthesis route and is an odorless solid, treatment is convenient, and the method is a new approach to synthesizing the aryl monofluoromethylthio compound.

The invention relates to a styrene monomer containing alkyl sodium (potassium) thiosulfate and a preparation method thereof, belonging to the technical field of organic synthesis and high polymer. In the invention, styrene based compound containing halogenated methylene is used as raw materials, methanol or ethanol and water are used as mixed solvent, PEO400 is used as a phase transfer catalyst, the halogen on the halogenated methylene reacts with the Bunte Salts of excessive saturated sodium (potassium) thiosulfate and is stirred to react under the room temperature till the sodium (potassium) thiosulfate raw material is totally consumed, then the methanol or ethanol and part of water are removed from the mixture by pressure reduction, is cooled and crystallized and then carried out the pumping filtration and collection to obtain solid; and the solid is leached (eluted) sequentially by little cooling water and petroleum ether and dried under the temperature of 40 DEG C to obtain the monomer, the monomer releases active sulfhydryl-groups with the function of chain transfer under the action of strong polarity reagents or diluted acid such as DMSO, DMF, and the like to form an AB monomer containing polymerizable double bond as well as active sulfhydral-groups. The AB monomer has simple structure, is easily prepared and stored, and is expected to be applied to super branched polymer prepared by a sulfhydryl-group chain transfer super branched polymerization method.

The invention relates to a process for preparing isooctyl thioglycolate. The process provided by the invention is characterized in that chloroacetic acid is taken as a raw material, the chloroacetic acid and isooctanol are subjected to an esterification reaction in the presence of a catalyst to synthesize isooctyl chloroacetate; then the isooctyl chloroacetate and sodium thiosulfate are reacted to form a Bunte salt and the Bunte salt is subjected to acidolysis and reduction to obtain a rough product of the isooctyl thioglycolate; and the rough product is rectified to obtain the finished product of the isooctyl thioglycolate. The process for preparing the isooctyl thioglycolate has higher yield; the isopropanol is used as the solvent. the experiment shows that the yield can be about 65% and the yield is improved by about 5% compared with the yield obtained by taking methanol, ethanol and the like as the solvent; and the time for recycling the isopropanol is only about 2.5 hours and the time is shortened by about 2 hours compared with the time for recycling the methanol, ethanol and the like so that the relative energy consumption is greatly reduced.

The invention relates to a synthetic method of a 3-alkylmercapto-1-methyl-4-morpholinyl maleimide compound. The preparation method comprises: in an organic solvent, under the condition of oxygen, carrying out a cascade reaction catalyzed by transition metal copper by taking alkylmercapto Bunte salt, morpholine and N-methylmaleimide as reaction raw materials, so as to obtain the 3-alkylmercapto-1-methyl-4-morpholinyl maleimide compound. The method is simple in reaction condition and high in product yield and purity, opens up a synthetic route and method for preparation of the 3-alkylmercapto-1-methyl-4-morpholinyl maleimide compound, and has good application potential and research value.

The invention discloses a reuse method for Bunte salt in sodium hydrosulfite waste residue. The main processes include (1) acidolysis of Bunte salt, (2) oxidation of acidolysis product, (3) alkali neutralization, and (4) product precipitation. The method provided by the invention converts the waste Bunte salt in sodium hydrosulfite waste residue into high value-added sodium hydroxyethyl sulfonate, and turns waste into treasure, and the purity of the product can reach 95%. With the characteristics of mild reaction conditions and simple operation process, the method solves enterprise environmental pollution, and at the same time brings economic benefits and social benefits to enterprises.

The invention relates to a method for synthesizing asymmetric cyanoalkyl disulfide, which comprises the following step of: conducting reacting on thiourea and alkyl Bunte salt serving as sulfur sources, an alkyl halide serving as a raw material, sodium dodecyl benzene sulfonate serving as an auxiliary reagent and sodium carbonate serving as alkali in water to obtain an asymmetric cyanoalkyl disulfide compound. According to the method, mercaptan with pungent smell is prevented from being used as a sulfur source, the purpose of friendliness and environmental protection is achieved, meanwhile, the reaction operation is simple, the reaction conditions are mild, and the method is suitable for large-scale production.

The invention discloses a synthesis method of aryl-aryl, aryl-alkyl and alkyl-alkyl asymmetric persulfides as shown in a formula (II) or a formula (IV). According to the synthesis method, with sulfinic acid sodium salt, and halogenated hydrocarbon and Na2S2O3 as reaction materials or Bunte salt as a reaction material instead of the halogenated hydrocarbon and Na2S2O3, the aryl-aryl, aryl-alkyl and alkyl-alkyl asymmetric persulfides are obtained by reaction in the absence of transition metal. The synthesis method has the advantages that the reaction is efficient; the yield is high; a vulcanizing reagent is cheap, easily available, stable, and free of pungent smell; no strong acid or alkali or extra oxidizing or reducing agent is added in reaction; the condition is relatively mild; and no transition metal is used as a catalyst in the reaction, and therefore the method is economical, practical and friendly to the environment; a reaction substrate is easy to prepare; the reaction efficiency is high after the reaction is amplified, and therefore, the synthesis method has a wide application prospect and practical value.

The invention relates to a method for preparing high-concentration isooctyl thioglycolate with short reaction time, high conversion rate, low cost and little pollution, comprising esterification, salt formation, hydrolysis and reduction, and the specific steps are (1) in a weight ratio of (1.3 ~ 1.5): 1 isooctyl alcohol and chloroacetic acid solution, add 2% ~ 5% rare earth solid superacid catalyst by weight of chloroacetic acid, react at 70°C ~ 90°C for 0.5h ~ 0.7h, generate chloroacetic acid (2) Under the condition of normal pressure and 120°C to 160°C, add sodium thiosulfate to the above-mentioned isooctyl chloroacetate, and reflux the mercaptolation reaction in isopropanol solvent for 0.5h to 0.8h, Prepare bunte salt; by weight, the consumption ratio of isooctyl chloroacetate, sodium thiosulfate and isopropanol is 1: (1.33~1.61): 0.98; (3) add dilute sulfuric acid to the prepared bunte salt Hydrolyze and reduce for 0.8h to 1.1h, then wash with water and rectify to obtain high-concentration isooctyl thioglycolate.

The invention relates to the chemical field and in particular relates to a siloxy alkyl sulfur ether compound and a preparation method thereof. One the one hand, the compound can be involved into the sulfuration reaction process of a sizing material after being added into the sizing material and soft alkyl chain is connected to sizing material macromolecule to improve the crosslinking density of the sizing material and improve the anti-sulfuration reversion characteristics of the sizing material, and on the other hand, alkoxy / hydroxyl of end group of the compound can be used for improving consistency of an inorganic filler and rubber macromolecule to improve the processing property and the mechanical property of the sizing material. The invention also provides the preparation method of the compound. Under alkaline conditions, a matter with double bunte salt structure is used as a raw material to be reacted with sulfydryl silane to obtain the siloxy alkyl sulfur ether compound. The method is simple in process, low in energy consumption, low in aftertreatment pollution, high in modified efficiency and good in repeatability, and has great industrial application prospect.

The invention discloses a method for synthesizing a beta-thiocarbonyl compound by taking Bunte salt as a sulfur source. According to the method, the Bunte salt serves as the sulfur source, a chalcone derivative or maleimide derivative serves as an electrophilic reagent, and the Bunte salt and the chalcone derivative or maleimide derivative are reacted for 6 hours under acid conditions to obtain a target product. Compared with the prior art, the method has the remarkable advantages that the Bunte salt serves as the sulfur source, is free of odor as compared with sulfur alcohol in a traditional method and can be made of low-cost sodium thiosulfate and halogenated hydrocarbon, high in yield, economical and environmentally friendly, the shape of most Bunte salt is solid powder which is easily operated, the reaction does not need transition metal serving as a catalyst, and environmental pollution caused by the reaction is reduced.

The invention relates to a preparation method of an N-substituted-3-methylmercapto-4-morpholinyl maleimide compound, which comprises the following steps: in an organic solvent and under the oxygen condition, taking methylmercapto-Bunte salt, morpholine and N-substituted maleimide as reaction raw materials and obtaining the N-substituted-3-methylmercapto-4-morpholinyl maleimide compoundthrough a cascade reaction catalyzed by transition metal copper. The method is simple in reaction condition and high in product yield and purity, opens up a synthetic route and method for preparation of the N-substituted-3-methylmercapto-4-morpholinyl maleimide compound, and has good application potential and research value.

The invention discloses a preparation method of tiamulin and tiamulin fumarate based on Bunte salt, which comprises the following steps: mixing the Bunte salt and pleuromutilin p-toluenesulfonate, reacting at 45-65 DEG C for 3-5 hours to synthesize tiamulin, preparing the Bunte salt through a reaction formula 1, and preparing the pleuromutilin p-toluenesulfonate through a reaction formula 2, the molar ratio of the 2-diethylaminoethanol to the sodium thiosulfate to the chlorination reagent in the reaction formula 1 is 1: (1-1.3): (1-1.5), and the molar ratio of the pleuromutilin to the paratoluensulfonyl chloride to the pyridine in the reaction formula 2 is 1: (1-1.2): (1-1.2); the prepared tiamulin and fumaric acid are used as raw materials for a salt forming reaction, the reaction temperature ranges from 55 DEG C to 65 DEG C, the reaction time ranges from 40 min to 80 min, and after the reaction is finished, the tiamulin fumarate is prepared through cooling, crystallization, centrifugation and drying; the tiamulin fumarate disclosed by the invention is high in content, low in total amount of impurities, few in variety and stable in quality under high-temperature and high-humidity conditions, and the preparation method is simple and easy to operate and good in product quality.

The invention discloses a preparation method of p-(methylthio)benzaldehyde, which comprises the following steps: generating a bunte salt by adopting sodium thiosulfate in place of sodium methyl mercaptide; and carrying out acid hydrolysis and methylation reactions to synthesize the p-(methylthio)benzaldehyde. According to the method, the defect that sodium methyl mercaptide is used as a substituting agent in an existing production process line is overcome, the smell problem in the using process of the sodium methyl mercaptide is effectively solved, the raw materials are cheap and easy to obtain, clean and free of pollution, the operation procedure is simple, the total yield is high, and good industrial prospects are achieved.

The invention discloses a reuse method for Bunte salt in sodium hydrosulfite waste residue. The main processes include (1) acidolysis of Bunte salt, (2) oxidation of acidolysis product, (3) alkali neutralization, and (4) product precipitation. The method provided by the invention converts the waste Bunte salt in sodium hydrosulfite waste residue into high value-added sodium hydroxyethyl sulfonate, and turns waste into treasure, and the purity of the product can reach 95%. With the characteristics of mild reaction conditions and simple operation process, the method solves enterprise environmental pollution, and at the same time brings economic benefits and social benefits to enterprises.

The invention discloses a method for synthesizing a S-substituted thiobenzoate derivative by Bunte salt. The method takes Bunte salt and benzaldehyde or its derivative as raw materials, under existence of a radical initiator di-tert-butyl peroxide, benzaldehyde, ethyl acetate or acetonitrile are taken as solvents, nitrogen protection is carried out, the materials are fully reacted at the temperature of 100-150 DEG C, after the reaction is completed, a reaction solution is separated and purified to obtain the S-substituted thiobenzoate derivative. The process condition of the method is reasonable, operation is easy and safe, usage of substrates such as thiophenol having bad smell is avoided, three wastes are little, the method is environmentally friendly, a free radical principle is used for synthesizing the product, metal catalysis is not required, and the method is a novel application of a carbon hydrogen activation reaction.

The invention relates to a novel synthetic method of bis-(sodium sulfopropyl)-disulfide; the traditional hydrogen sulfide alkalization sulfonation process is abandoned, Bunte salt is generated by the reaction of sodium thiosulfate with 1,3-propanesultone, and the Bunte salt is then subjected to hydrolysis and oxidation two-step process under acid condition to prepare the high-purity bis-(sodium sulfopropyl)-disulfide. The reaction conditions of the method are simple and controllable, no toxic gas is involved in the method, no high-pressure equipment is used, the method is simple to perform, the product yield and purity are high, the method has good repeatability, the reaction process is a common reaction operation with no special reaction equipment involved, little wastewater and solid waste are produced, and the alcohol solvent is recyclable after the reaction.

This invention provides a preparation process for tiamulin fumarate, belonging to the field of compound synthesis technology, comprising the following steps: truncated pleuromedullary is reacted with a bifunctional solid organic base and 2,4,6-trimethylbenzenesulfonyl chloride in a mixed solvent A to obtain a concentrated intermediate of truncated pleuromedullary trimethylbenzenesulfonate; 2-diethylaminochloroethane hydrochloride is deacidified in a fixed bed packed with a bifunctional solid organic base, reacted with sodium thiosulfate, and exchanged with tetrabutylammonium bromide to obtain 2-diethylaminoethyl Bunte salt tetrabutylammonium salt; after the reaction, the two react with fumaric acid to form a salt crystallization, yielding tiamulin fumarate. This invention can improve the reaction efficiency and selectivity of the truncated pleuromedullary sulfonation reaction, and further improve the yield and content of tiamulin fumarate.

According to the invention, Bunte salt is employed as a sulfur source to prepare 3-indole thioether. At a certain temperature, elementary iodine or hydroiodic acid and salts thereof is employed as a catalyst, dimethyl sulfoxide is employed as an oxidant, and the Bunte salt is employed as the sulfur source to react with an indole compound without or with other solvents to prepare the 3-indole thioether. Reagents in the method are low in cost and easy to obtain. The method is mild in reaction conditions and is wide in substrate application. The reagents are slight in smell. The method is low in environment pollution.

The invention discloses a preparation method of p-methylthiobenzaldehyde. Sodium thiosulfate is used to replace sodium methylthiolate to generate bunte salt, and then p-methylthiobenzaldehyde is synthesized through acid hydrolysis and methylation reaction. The invention avoids the disadvantages of using sodium methyl mercaptide as a substitute in the existing production process line, effectively solves the odor problem in the use process of sodium methyl mercaptide, and the raw materials are cheap and easy to obtain, clean and pollution-free, and the operation process is simple. The yield is high and has good industrialization prospects.

The present invention is directed to a pneumatic tire comprising at least one of an apex, flipper, and chipper, the at least one of an apex, flipper, and chipper comprising a rubber composition, the rubber composition comprising a diene based elastomer and from 1 to 50 parts by weight, per 100 parts by weight of elastomer, of aramid fiber having a length ranging from 0.5 to 20 mm and having a thickness ranging from 2 to 30 microns, said fiber having disposed on at least part of its surface a composition comprising an aliphatic fatty acid or synthetic microcrystalline wax; a Bunte salt; a polysulfide comprising the moiety -[S] n or - [S] o -Zn-[S] p , wherein each of o and p is 1-5, o + p = n, and n = 2-6; and sulfur or a sulfur donor.

The invention discloses a method for synthesizing N-thiobenzyl imine or its derivatives from Bunte salt. The method uses benzylamine or benzylamine derivatives and Bunte salt as raw materials, uses cuprous bromide as a catalyst, and uses N,N-dimethylformamide as a solvent to fully react at 70 to 90°C. , the reaction solution is separated and purified to obtain N-thiobenzyl imine or its derivatives. The method of the invention is simple and safe, does not require the presence of oxidants and additives, adds cuprous bromide as a catalyst, reduces the reaction temperature, improves the reaction yield, avoids the use of raw materials such as mercaptan with bad smell, has less three wastes, and is environmentally friendly.

A hair treatment agent is provided herein. The hair treatment agent includes in a cosmetic carrier (a) at least one compound of the general formula (I). R1 denotes a hydrogen atom or a structural element of formula (II). x denotes an integer from 1 to 100. The radical R2 in each of the structural elements of formula (II) can be selected independently of the preceding structural element of formula (II). M1 denotes the grouping —OM2 or a structural element of formula (III). y denotes an integer from 1 to 100. M2 denotes a hydrogen atom, an equivalent of one or more cations or an ammonia ion (NH4)+.

The invention discloses a synthetic process for bis-(3-sulfopropyl)disulfide, belonging to the technical field of synthesis of the bis-(3-sulfopropyl)disulfide. The synthetic process provided by the invention comprises the following steps: with 1,3-propanesultone as a raw material, carrying out a reaction with sodium thiosulfate in a mixed solution of an alcohol substance and water so as to prepare bunte salt, then subjecting the prepared bunte salt to alkalization and oxidation, and carrying out purification and concentration so as to prepare the bis-(3-sulfopropyl)disulfide. The bis-(3-sulfopropyl)disulfide prepared by using the method provided by the invention has high yield and purity, wherein the yield can reach 98.1%, and the purity can reach 99.5%; meanwhile, the synthetic process provided by the invention has the advantages of easily available raw materials, less synthetic steps and applicability to industrial production.

The invention provides a synthetic method of 1-(3-mercapto-2-D-methyl propionyl)-L-proline which comprises the following process steps: a. allowing 1-(3-bromo-2-D-methyl propionyl)pyrrolidine-2-carboxylic acid to react with a sodium bicarbonate solution to obtain 1-(3-bromo-2-D-methyl propionyl)pyrrolidine-2-sodium carboxylate; b. allowing 1-(3-bromo-2-D-methyl propionyl)pyrrolidine-2-sodium carboxylate to react with sodium hyposulfite to synthesize Bunte salt; c. allowing the Bunte salt to react with a sodium sulfide solution, performing acidification and filtration to directly obtain a disulphide solid of 1-(3-mercapto-2-D-methyl propionyl)-L-proline; d. reducing the disulphide solid with zinc powder in a sulfuric acid solution, performing extraction and recrystallization to obtain the disulphide 1-(3-mercapto-2-D-methyl propionyl)-L-proline product. The invention overcomes the disadvantage of low yield of original process, and is suitable for industrial production.

The invention relates to a method for synthesizing asymmetric cyanoalkyl disulfide, which comprises the following step of: conducting reacting on thiourea and alkyl Bunte salt serving as sulfur sources, an alkyl halide serving as a raw material, sodium dodecyl benzene sulfonate serving as an auxiliary reagent and sodium carbonate serving as alkali in water to obtain an asymmetric cyanoalkyl disulfide compound. According to the method, mercaptan with pungent smell is prevented from being used as a sulfur source, the purpose of friendliness and environmental protection is achieved, meanwhile, the reaction operation is simple, the reaction conditions are mild, and the method is suitable for large-scale production.