99results about "Hydropoly/poly sulfide preparation" patented technology

The invention discloses an unsaturated phenyl ether monomer, a holographic recording medium, a preparation method and a related device, the structural general formula of the monomer is as shown in G1 and G2, R1 represents any one of R2, A1 and A2 independently represent any one of hydrogen and phenyl, A3 represents hydrogen or methyl, A4 represents C1-C4 alkyl or phenyl, n is a positive integer and n = 1-5. The unsaturated phenyl ether monomer provided by the invention has high refractive index and is in a liquid state, and the holographic recording medium with high sensitivity, high diffraction efficiency and high refractive index modulation degree can be obtained by applying the unsaturated phenyl ether monomer to preparation of the photopolymer type holographic recording medium.

The present disclosure pertains to: an ester compound that is a transesterification reactant between a polyol and a dicarboxylic acid ester having a disulfide bond and that has, in a molecule chain, a disulfide bond and has, at a terminal, a hydroxy group; a method for synthesizing said ester compound; and a resin composition containing said ester compound and a photo-radical generator.

The invention discloses an asymmetric disulfide reagent (R1O-SS-SO2R2) as shown in a formula (3) and a synthesis method thereof, R1O-SS-OR1 as shown in a formula (1) and hyposulfonic acid as shown in a formula (2) are taken as reaction raw materials, no catalyst additive is needed, and the asymmetric disulfide reagent (R1O-SS-SO2R2) compound is obtained through reaction. The method has the advantages of mild reaction conditions, cheap and easily available raw materials, simple reaction operation, high yield, no need of any catalyst additive in the reaction, economy, practicability and environmental friendliness; reaction substrates are easy to prepare; the reaction efficiency is high after reaction amplification. The asymmetric disulfide reagent (R1O-SS-SO2R2) provided by the invention can be used for preparing an asymmetric polysulfide compound. The invention also discloses an asymmetric polysulfide compound synthesized by using the asymmetric disulfide reagent (R1O-SS-SO2R2) as shown in the formula (3) and a synthesis method of the asymmetric polysulfide compound. The method has wide application prospect and practical value.

The invention discloses an amphiphilic disulfide and a preparation method and application thereof, and belongs to the technical field of emulsion polymerization, the disulfide has the following structural general formula (I), in the formula (I), R1 is C1-C6 straight chain or branched chain alkyl; r2 is C2-C6 straight chain or branched chain alkyl; M1 is alkali metal ion or NH4 < + >; and M2 is alkali metal ion. A redox system formed by the disulfide and an oxidizing agent is used for post-treatment of a polymerized emulsion, residual monomers and free radicals in the emulsion can be efficiently cleared in a targeted mode, excellent emulsion stability is kept, and formaldehyde is not released.

The invention discloses a method for preparing a biomacromolecular drug delivery carrier based on a simple and efficient interface cross-linking system. An amphiphilic polymer monomer containing an epoxy group is prepared through RAFT polymerization so that the amphiphilic polymer monomer can exist on an oil-water interface, meanwhile, a three-arm cross-linking agent which has environmental sensitivity and is terminated by an amino group is prepared, and the amino group on the cross-linking agent and the epoxy group on the amphiphilic monomer are subjected to a cross-linking reaction on the oil-water interface; a drug delivery vehicle is formed. The carrier can entrap biomacromolecules and accurately target tumors through a high-permeability long-retention effect, and glutathione rich in a tumor microenvironment can break disulfide bonds in the carrier and release drugs entrapped in the carrier, so that the aim of treating the tumors is fulfilled. Therefore, the invention provides a drug delivery carrier which is simple, convenient, efficient in entrapment of biomacromolecules and high in stability, and the prepared carrier can be efficiently taken by tumor cells so as to regulate and control apoptosis of the tumor cells and is high in safety.

This invention discloses a method for synthesizing disulfide ether compounds using visible light-emitting two-dimensional olefin nanomaterials in synergistic catalysis. The method involves mixing a thiol-containing compound with a suitable solvent, and then, under mild light conditions in the presence of a catalytic amount of two-dimensional olefin nanomaterials, achieving efficient disulfide bond construction to obtain a series of disulfide ether compounds. This invention enables the efficient synthesis of disulfide ether compounds. The catalyst used is simple to synthesize, requires low dosage, and is inexpensive. It achieves efficient conversion under mild light conditions, reducing reaction costs and simplifying post-processing steps. The synthesis reaction in this invention can be carried out at room temperature and pressure without any additional additives, exhibiting mild conditions, rapid reaction, and high yield.

The invention discloses a method for synthesizing a dithio alkyl ketone compound by using diisopropylamine, which is characterized in that diisopropylamine is used as alkali, a cycloalkyl peroxy alcohol compound and a tetrasulfide compound are driven by illumination to generate a free radical coupling reaction, and the dithio alkyl ketone compound is successfully synthesized. The preparation method provided by the invention has the advantages of easily available raw materials and simple operation, has excellent functional group compatibility, can meet the synthesis requirements of target products with different structures, and has significant practical application value.

The present disclosure relates to a novel ionizable lipid containing a biodegradable disulfide bond. The ionizable lipid containing a disulfide bond, according to the present disclosure, stably delivers an anionic drug when prepared into lipid nanoparticles and exhibits an excellent effect, in particular, in delivering nucleic acids, and thus can be effectively used in related technical fields such as lipid nanoparticle-mediated gene therapy.

The present invention provides a method for producing a compound (1), the method comprising the following step 1a:　step 1a for reacting a compound (3) and a compound (4) in a two-phase system containing an organic base, an inorganic base, water, and a water-insoluble organic solvent, thereby obtaining the compound (1). The definitions of the symbols in the formula are as described in the description.

The invention relates to a method for the co-production of alkyl mercaptan and dialkyl disulfide, comprising the following successive steps:a) reacting a C1-C4 alcohol in the presence of hydrogen sulfide (H2S) to form a stream (M) comprising an alkyl mercaptan, water, and possibly unreacted hydrogen sulfide, b) purifying the stream (M) to obtain a stream (N) enriched in alkyl mercaptan, c) recovering a first portion of the stream (N) comprising alkyl mercaptan purified in step b), d) sulfur oxidation of the second portion of the stream (N) of alkyl mercaptan in order to form a stream (O) comprising a dialkyl disulfide, hydrogen sulfide, and possibly unreacted alkyl mercaptan, e) purifying the stream (O) to separate, on the one hand, the enriched dialkyl disulfide and on the other hand the hydrogen sulfide and the alkyl mercaptan possibly having not reacted in step d), f) recycling the hydrogen sulfide and possibly the alkyl mercaptan isolated in step e) to the stream (M) obtained in step a), g) recovering the dialkyl disulfide isolated in step e).

This invention relates to the field of sulfurizing agent preparation technology, and discloses an organic sulfurizing agent and its stepwise preparation method and application. The method includes: dissolving a first sulfur in a solvent to obtain a mixed sulfurized oil; contacting the mixed sulfurized oil with a second sulfur, olefin oil, and a solid catalyst under primary heating and reflux; then contacting the resulting mixture I with an optional additive under secondary heating and reflux, wherein the temperature of the primary heating and reflux is lower than the temperature of the secondary heating and reflux; distilling the resulting mixture II; and then separating the solid-liquid mixture to obtain the liquid phase as the organic sulfurizing agent; or, after separating the solid-liquid mixture II, distilling the resulting liquid mixture to obtain the heavy fraction as the organic sulfurizing agent. This method eliminates the need for hydrogen sulfide, and the resulting organic sulfurizing agent has a higher sulfur content, up to 65% by weight. Preferably, no hydrogen sulfide is released during the preparation process, making it more environmentally friendly.

The application discloses a hydrogenation catalyst vulcanizing agent and a preparation method and application thereof. The hydrogenation catalyst vulcanizing agent is an organic polysulfide, the organic polysulfide is calcined at 100 DEG C-280 DEG C under a hydrogen atmosphere, and the weight loss of the hydrogenation catalyst vulcanizing agent is as follows: 25-40% at 100 DEG C-180 DEG C, 20-35% at greater than 180 DEG C to less than 215 DEG C, and 20-30% at 215 DEG C-270 DEG C, with the total weight of the hydrogenation catalyst vulcanizing agent as the basis. The preparation method of the hydrogenation catalyst vulcanizing agent mainly comprises the following steps: reacting elemental sulfur and unsaturated hydrocarbons in the presence of alkaline substances and C8 or above aliphatic hydrocarbons, and obtaining the hydrogenation catalyst vulcanizing agent through separation after the reaction is completed. The hydrogenation catalyst vulcanizing agent not only has a simple preparation method and is easy to control, but also can slowly decompose and release hydrogen sulfide in a hydrogen atmosphere.

The present application pertains to a method of making carbon disulfide. The method comprises reacting methane and sulfur under conditions sufficient to produce carbon disulfide, hydrogen disulfide, and heat. At least a portion of the produced hydrogen disulfide is reacted with methane under conditions sufficient to produce a mixture comprising carbon disulfide and hydrogen. Advantageously, at least a portion of the heat from reacting methane and sulfur is employed in the reacting of at least a portion of the produced hydrogen disulfide with methane.

The application discloses a kind of ultrafast metal-free and solvent-free preparation method for preparing symmetric and asymmetric disulfide, which comprises the following steps: at room temperature, raw material R-SH, R'-SH and oxidant and base are added to reaction bottle, shake rapidly for 10-30 seconds, and R-S-S-R' is prepared after the reaction product is purified;Wherein R in R-SH is aliphatic or aromatic group, R' in R'-SH is aliphatic or aromatic group;R in R-SH and R' in R'-SH are same or different;The aromatic group has substituent or no substituent, and the aliphatic is straight chain or has branch;The oxidant is chloroform, and the base is N, N-diisopropylethylamine (DIPEA).The method is simple in operation, high in yield (60-99%), ultrafast in reaction kinetics, greatly improves production efficiency, wide in applicability, avoids the use of organic reaction solvent, raw material is cheap and easy to obtain, and does not contain residual metal and other sticky contaminants from reagent and ligand, provides a safer and more effective method for the synthesis and production of symmetric and asymmetric disulfide-containing compounds.

The invention discloses a method for catalytically synthesizing sulfurized isobutylene, which is used for preparing high-yield and high-purity sulfurized isobutylene in a mild synthesis mode under the combined action of ultrasound and a catalyst. The method comprises the following steps: mixing tert-butyl mercaptan and sulfur, and carrying out ultrasonic dispersion treatment to obtain a dispersion system; under the ultrasonic action, adding a catalyst into the dispersion system for reaction; the catalyst is aluminum oxide modified by ZnO and ZrO2; and after the reaction is finished, filtering the reaction system, separating out the catalyst, and carrying out reduced pressure distillation to obtain sulfurized isobutylene.

The invention belongs to the technical field of chemical synthesis, and discloses an asymmetric disulfide compound containing a sulfoxide group as well as a preparation method and application thereof, and the asymmetric disulfide compound containing the sulfoxide group has a structure as shown in a structural general formula (I). By improving the structure of the compound and the preparation method thereof, the obtained compound as shown in the structural general formula (I) is novel in structure and stable in property; the preparation method has the advantages of cheap and easily available raw materials, simple operation, high reaction yield, convenient separation and purification of intermediates and products, suitableness for industrial production, and high preparation efficiency. Moreover, the compound as shown in the structural general formula (I) can be particularly used as an activating reagent to be applied to glycosylation reaction, is simple and convenient to operate and high in reaction activity when being used for glycosylation reaction, and can be widely applied to activation of thioglycoside and selenoglycoside to construct various substrates such as oxygen glycoside, phenolic glycoside, ester glycoside, nucleoside and carbon glycoside.

A method for producing a polythiol composition including a reaction step of reacting a thiourethane resin and a nitrogen-containing compound that is at least one selected from the group consisting of a quaternary ammonium salt and an amine compound in the presence of water to generate a polythiol composition.

The application discloses a recycling method of by-product cyclohexene distillation still residue, and belongs to the technical field of recycling of by-product cyclohexene distillation still residue. The still residue is analyzed by liquid chromatography-mass spectrometry, and the chlorocyclohexane in the still residue is reacted with sodium disulfide under the condition of a catalyst. After static separation, the oil phase is refined to obtain dicyclohexyl disulfide and cyclohexene, and the water phase can be recycled. The catalyst is composed of sulfonated castor oil and a phase transfer catalyst, can improve the conversion rate of chlorocyclohexane and the selectivity of dicyclohexyl disulfide, and greatly shortens the reaction time. The application can realize recycling and utilization of the still residue, avoids waste of resources and pollution to the environment, saves the chemical production cost, and meets the environmental protection concept of green chemical industry.

The invention provides a preparation method of a 2-amino-3-methyl-5-chloro-benzoic acid compound, which comprises the following synthesis route: wherein the definitions of R1 and R2 are the same as those in the specification.

The invention discloses a synthesis process of high-yield sodium benzenesulfinate, and belongs to the technical field of synthesis of sodium benzenesulfinate. The synthesis process of the high-yield sodium benzenesulfinate comprises the following preparation steps: S1, mixing a first catalyst, sodium hydroxide and a first solvent, then adding powdered sulfur, reacting for a first reaction time under microwave radiation, then adding chlorobenzene, continuously reacting for a second reaction time under microwave radiation, then filtering, carrying out reduced pressure distillation to remove the solvent, and recrystallizing, so as to obtain the high-yield sodium benzenesulfinate. The diphenyl disulfide is obtained; s2, mixing the diphenyl disulfide prepared in the step S1, alcohol, an oxidizing agent and a second solvent, stirring in the air at room temperature for a third reaction time, diluting with ultrapure water, extracting with ethyl acetate for multiple times, combining organic layers, drying, concentrating and purifying to obtain benzene sulfinate, and keeping in a dark place and in an oxygen-isolated manner; s3, under the dark and nitrogen conditions, benzene sulfinate prepared in the step S2 is hydrolyzed and refined under the alkaline condition, and sodium benzene sulfinate is obtained.

The invention belongs to the technical field of chemical synthesis, and particularly relates to a dimethyl polysulfide composition and a preparation method and application of dimethyl disulfide. According to the dimethyl polysulfide composition provided by the invention, the content of each component in the composition is specially regulated and controlled, the composition is used as a raw material to react with methyl mercaptan to prepare dimethyl disulfide, the purity is greater than 99.8%, the appearance is colorless transparent liquid, the chromaticity is less than 25 Hazen, and the dimethyl disulfide is free of foul smell and is an environment-friendly superior product; the product can be sold as a food flavor fumigant, and has great market competitiveness. According to the preparation method of dimethyl disulfide provided by the invention, the reaction process is carried out in a protective atmosphere, the technological process is simple, no toxic reagent is used, the operation is safe and non-toxic, and potential safety hazards are avoided.

The invention relates to cationic cyclic oligomeric disulfide as well as a synthesis method and antimicrobial application thereof, and belongs to the technical field of chemical synthesis. The synthesis method provided by the invention comprises the following steps: carrying out primary reaction on a monomer M and an acid solution in a solvent to obtain an intermediate M '; pKa of acid in the acid solution is less than 3, and the monomer M conforms to a specific general formula (I); and S2, adjusting the system to enable the concentration of the acid to be greater than or equal to 0.25 mol / L, carrying out secondary reaction at 25-65 DEG C to obtain a reaction solution, and then carrying out drop precipitation and separation to obtain the cationic cyclic oligomeric disulfide. According to the synthesis method provided by the invention, the cationic cyclic oligomeric disulfide can be selectively obtained, and the product does not contain high-molecular-weight linear high-molecular-weight polydisulfide, so that the yield is high, the oligomer conversion rate is high, and the method is suitable for industrial production. Diversified modification of cation types is beneficial to further research, development and preparation of broad-spectrum antimicrobial agents capable of resisting fungi and mixed bacterial infection.

The invention discloses a vulcanizing agent and a preparation method and application thereof, a rubber vulcanizing method, a rubber composition, rubber and a product, and the preparation method of the vulcanizing agent comprises the following steps: preparing a maleic acid solution; adding sulfur into the maleic acid solution to obtain a sulfur-containing turbid solution; the sulfur-containing turbid liquid is heated to 151-250 DEG C and then subjected to a constant-temperature reaction for 1 min to 24 h, after the reaction is completed, the sulfur-containing turbid liquid is rapidly decompressed and cooled to obtain a cooled product, solid in the cooled product is obtained through separation, and the primary vulcanizing agent is obtained.

This invention relates to the field of chemical technology, specifically to a method for refining isobutylene sulfide, comprising: adding sulfur to a high-pressure reaction vessel; adding triethylamine to the high-pressure reaction vessel under nitrogen atmosphere; heating to 120-150°C; adding isobutylene and hydrogen sulfide under a high-pressure reaction vessel pressure of 2-6 MPa; maintaining the temperature for 1-3 hours; cooling to obtain crude isobutylene sulfide; distilling the crude isobutylene sulfide under reduced pressure; adding 0.1%-5% cobalt-molybdenum catalyst; heating to 100°C-180°C; reacting for 0.5-6 hours; then cooling to room temperature; filtering to remove the cobalt-molybdenum catalyst; obtaining isobutylene sulfide; distilling the isobutylene sulfide under reduced pressure; and adding 10-1000 ppm surfactant to the isobutylene sulfide. Through this method, the content of highly corrosive components is significantly reduced, the copper corrosion level decreases, the irritating odor is reduced, the catalyst can be recovered, and no wastewater is generated throughout the process.

One exemplary embodiment can be a process for oxidizing one or more thiol compounds from an alkaline stream. The process may include passing a mixed stream having the alkaline stream to a vessel having an oxidation section, a separation section and a vent gas section. Often, the oxidation section includes a body containing one or more packing elements. The process can further include passing an oxidized alkaline stream to the separation section containing a first chamber and a second chamber. Usually, the first chamber contains a coated mesh and packing. The two sections further form a neck contains a packing, a distributor, and a mesh.

The application discloses a vulcanizing agent and a preparation method and application thereof. The preparation method of the vulcanizing agent comprises the following steps: reacting low-carbon olefins and a sulfur source under the action of an organic base and / or an inorganic base, monitoring the gas phase pressure of a reaction system during the reaction, stopping the reaction when the gas phase pressure increases by 0.05-0.6 Mpa / min, preferably 0.1-0.4 Mpa / min, and separating after cooling to obtain the vulcanizing agent. The vulcanizing agent not only has a simple preparation method and is easy to control, but also has high sulfur mass content, contains cyclic organic polysulfides with long sulfur chains, and has high mass content of the cyclic polysulfides.

The invention provides a novel lubricating oil detergent, a preparation method thereof and a lubricating oil composition. The preparation method comprises the following steps: mixing alkylphenol, base oil, a vulcanizing agent and a first part of calcium source, adding a first part of accelerant, and carrying out vulcanization reaction; then adding cyclic anhydride to carry out esterification reaction; and adding a second part of accelerant and a second part of calcium source, then carrying out carbonation reaction, and purifying the product after the reaction is finished to obtain the novel lubricating oil detergent. Wherein the cyclic anhydride is selected from one or a combination of more than two of maleic anhydride, succinic anhydride, adipic anhydride and phthalic anhydride; the addition amount of the cyclic anhydride is 0.01-0.25 part by weight based on 1 part by weight of alkylphenol. The cyclic anhydride participates in the reaction, so that the content of free phenol in the product can be reduced, and the wear resistance of the product can be improved. The novel lubricating oil detergent provided by the invention has no free phenol residue, and has more excellent detergency, oxidation resistance, wear resistance and the like.

The invention belongs to the technical field of medicinal chemistry, and relates to a lafaramycin intermediate as well as a preparation method and application thereof.

A method of producing a polyamine compound, the method including: a first step of generating a polyurea compound by reacting a thiourethane resin and an amine compound A with each other; and a second step of generating a polyamine compound by reacting the polyurea compound and an amine compound B with each other.

A method of producing a thiourethane resin raw material, the method including comprising the step of generating the thiourethane resin raw material by reacting a thiourethane resin and an active hydrogen compound with each other.