481results about "Thiol preparation" patented technology

Provided herein is a pleuromutilin derivative containing a cycloalkyl group and preparation method and application thereof. Specifically, the pleuromutilin is reacted with p-toluenesulfonyl chloride to obtain an intermediate I, and the intermediate I is reacted with 1-amino-2-methylpropane-2-thiol hydrochloride to obtain an intermediate II, and then the intermediate II is reacted with cycloalkylcarbonyl chloride to obtain a target derivative. The synthesis process of these derivatives is simple, with a high yield and simple purification. These derivatives can effectively inhibit activities of Staphylococcus aureus and Streptococcus, and have superior activities to the marketed Tiamulin, and they also have good antibacterial activities against drug-resistant bacteria. In particular, the treatment effect of the derivative 2 of the target derivative is significantly superior to the clinical drugs Tiamulin and Valnemulin. They are suitable as new antibacterial drugs for prevention and treatment of infectious diseases caused by bacteria in humans or animals.

The invention discloses a method for preparing 12-mercaptan through solid organic acid catalysis, belongs to the technical field of 12-mercaptan preparation, and aims to solve the problems of low catalyst activity, harsh reaction conditions, serious pollution, high cost and dependence on import in the prior art. N-dodecanol and hydrogen sulfide are used as raw materials and are mixed according to the molar ratio of 1: 1.2-1: 1.3; the method comprises the following steps: gasifying n-dodecanol, mixing with purified hydrogen sulfide, preheating to 210-240 DEG C, introducing into a fixed bed reactor filled with a solid organic acid catalyst, and reacting at-0.08-3.0 MPa for 3.5-4 hours; and cooling and condensing the reaction product, carrying out gas-liquid separation, rectifying and purifying the liquid product to obtain 12-mercaptan with the purity of more than or equal to 99.5%, and recycling unreacted hydrogen sulfide. The solid organic acid can be a catalyst of p-toluenesulfonic acid and the like or mesoporous silica loaded nickel, cobalt and molybdenum metal oxides. The method has the advantages of high catalytic activity, mild reaction conditions, high product yield (the conversion rate of n-dodecanol is greater than or equal to 94.5%), environmental protection and low cost, can realize the domestic mass production of 12-mercaptan, and meets the market demand.

The invention relates to a carbon fiber sizing agent matched with (poly) dicyclopentadiene for use and application of the carbon fiber sizing agent, and belongs to the technical field of poly dicyclopentadiene. The two most important components, namely the coupling agent (component 1) and the film-forming agent (component 2), of the sizing agent are synthesized through a one-pot method, separation, solvent recovery and washing purification are not needed, and the sizing agent is efficient and environmentally friendly. Finally, the introduction strategy of the coupling catalyst (component 3) is optimized, and the reaction efficiency of the carbon fiber and the sizing agent layer is improved to the maximum extent. The method is simple to operate, energy-saving, environment-friendly, high in reaction efficiency and good in interface enhancement effect, can realize batch production of the sizing agent, and can realize batch production of special carbon fibers.

The invention relates to the technical field of optical fibers and adhesives, and particularly discloses a special ultraviolet curing adhesive for a reticular optical fiber ribbon and a preparation method of the special ultraviolet curing adhesive. The adhesive is prepared from a carboxyl-containing sulfydryl tertiary carbonate urethane acrylate prepolymer, a low-viscosity prepolymer, four-functional polyurethane modified organosilicone epoxy acrylate, a high-adhesion acrylate monomer, an acrylamide active monomer, ultraviolet-curable cellulose ester, a photoinitiator, a flatting agent, a photocuring defoaming agent and a polymerization inhibitor. The adhesive is small in viscosity and easy to dispense and spray, adopts UV / UV-LED light to initiate rapid curing and fixing, is good in adhesive force, can effectively improve the grid bonding strength, does not cause additional attenuation to optical fibers, is good in stripping performance, facilitates rapid separation of single optical fibers during construction, is free of VOC emission and low in odor, and meets the latest REACH regulations of European Union. The ultraviolet curing adhesive has the characteristics of small attenuation, good torsion and bending resistance, good stripping property and the like when being used for producing the net-shaped optical fiber ribbon.

The invention discloses a preparation method and application of a CoxSy catalyst, and belongs to the technical field of catalyst preparation. According to the method, the morphology of CoxSy is regulated and controlled by using different solvents, so that four CoxSy catalysts with different morphology characteristics are synthesized. The catalyst is simple in preparation method and high in repeatability. The obtained CoxSy catalyst has a high specific surface area, more active sites can be exposed, reaction raw materials are in full contact with the active sites of the catalyst, and meanwhile, the catalyst has relatively high sulfur tolerance and rich sulfur vacancies, and is beneficial to adsorption and activation of H2S and CO2. Therefore, the obtained CoxSy catalyst shows high catalytic activity in a reaction for preparing methyl mercaptan through H2S and CO2 hydrogenation.

The invention relates to a CuKMoS2 / SiO2 catalyst for synergistically preparing methyl mercaptan from carbon dioxide and hydrogen sulfide. By introducing a small amount of copper (Cu) into a KMoS2 / SiO2 catalyst system, the selectivity of the catalyst to a reaction intermediate product methanol (CH3OH) is remarkably improved, so that the generation selectivity to a target product methyl mercaptan (CH3SH) is improved. The introduction of Cu promotes the electron transfer of active sites on the surface of the MoS2 catalyst, and optimizes the reaction path. The invention provides a preparation method of a catalyst with high efficiency, good selectivity and strong stability and a new process applied to methyl mercaptan production.

The invention discloses a preparation method of a cobalt-molybdenum catalyst and application of the cobalt-molybdenum catalyst in preparation of methyl mercaptan through CO2 / H2S hydrogenation. According to the method, a titanium source is used as a modification additive, ethanol is used as a structure-directing agent, a hydrotalcite-like precursor with a sheet-like characteristic is synthesized by a simple hydrothermal method, and an active component is further loaded on the basis, so that the cobalt-molybdenum catalyst with high dispersion and rich vacancies is finally obtained. The titanium source is added, so that the density of electron cloud around the active component is increased, transferred electrons promote the strength of Mo-S bonds and Co-S bonds to be reduced, the Mo-S bonds and the Co-S bonds are easier to break to form sulfur defects, and adsorption and activation of CO2 and H2S are promoted. Meanwhile, due to injection of extra charges, MoS2 is induced to generate phase change from a 2H phase to a 1T phase, and the catalytic hydrogenation capacity of MoS2 in the reaction process is improved. Finally, the cobalt-molybdenum catalyst shows considerable catalytic activity in a reaction system for preparing methyl mercaptan through CO2 / H2S hydrogenation.

The invention provides a preparation method and application of a catalyst for selective production of ethanethiol. The catalyst comprises an active component, an auxiliary agent and a molded alumina carrier, the active component comprises the following components in percentage by mass: 5-10% of VIII group transition metal oxide and 15-20% of VIB group metal oxide, and the auxiliaries comprise 0.5-4% of alkali metal, 1-3% of alkaline earth metal oxide, 0.6-2% of cerium oxide and 1-4% of phosphorus pentoxide. A bifunctional catalyst with moderate Lewis acid-base sites is constructed by compounding a multi-component aid and an active component, and the catalyst shows excellent catalytic activity that the ethylene conversion per pass is greater than or equal to 98%, the ethanethiol selectivity is about-95% and the ethanethiol yield is-90% under the reaction conditions that the hydrogen sulfide / ethylene feeding mass ratio is 3-5, the temperature is 180-210 DEG C, the pressure is 0.5-1.0 MPa and the volume space velocity is 200-300 h <-1 >. And the catalyst can stably run for 1250 hours or more.

The invention discloses an ortho-thiol modified triphenylene carboxylic acid ligand, an MS2O2 site-containing metal organic framework material as well as a preparation method and application of the ortho-thiol modified triphenylene carboxylic acid ligand and the MS2O2 site-containing metal organic framework material. The ligand has a triphenylene main body pi conjugated structure and ortho-position modified carboxyl and thiol groups, and is coordinated with metal ions through solvothermal reaction, and the bond length of an S-M bond formed by coordination is shorter than that of an O-M bond formed by coordination of the carboxyl and the metal ions, so that d-pi conjugation of the coordinated metal ions and the pi conjugated organic ligand is enhanced, and the metal ions and the pi conjugated organic ligand are combined to form the pi conjugated organic ligand. The electron conduction rate in the metal organic framework material is favorably improved, so that the reaction activity of the metal organic framework material is further improved. Especially, the photocatalytic hydrogen evolution rate (HER) can reach 4126.01 [mu] mol g <-1 > h <-1 > by taking Co as a coordination metal ion material, and the material has excellent photocatalytic hydrogen evolution activity. The metal organic framework material can be produced and prepared through solvothermal reaction, the preparation process is mature, the steps are simple, the yield is high, and large-scale preparation can be achieved.

The invention provides a novel preparation method of mercaptosuccinic acid betaine (1: 1), and the preparation method adopts betaine and mercaptosuccinic acid as main raw materials, adopts water as a solvent, and enables the mercaptosuccinic acid and the betaine to directly react under a heating condition, so that the mercaptosuccinic acid betaine (1: 1) represented by a formula (I) is obtained with high purity. # imgabs0 #

The invention provides a method for determining the content of penicillamine enantiomers by pre-column derivatization liquid chromatography, namely a method for detecting L-penicillamine in D-penicillamine or a method for detecting D-penicillamine in L-penicillamine, derivatization is carried out under conventional alkaline conditions, a termination reaction is carried out by conventional acid, the derivatization steps are simplified, the detection efficiency is improved, and the detection cost is reduced. According to the method, various interferences of other amino acids and corresponding isomers in the raw materials can be effectively avoided due to the gradient of the mobile phase, the damage to a chromatographic column is well reduced due to the fact that conventional reagents such as phosphoric acid and acetonitrile serve as the mobile phase, and the method is easy to operate, high in sample preparation speed and high in accuracy. The method has the advantages of strong anti-interference capability, good separation effect, high sensitivity, accurate result and good stability, realizes effective separation of penicillamine isomers, has a separation degree of greater than 2, can perform content determination on another main drug while performing impurity detection on one isomer, and has good practicability.

The present application provides a method for preparing a perovskite layer interface modifier and an interface modifier. The preparation method adopts a multi-metal synergistic coordination strategy, and introduces a multi-site coordination ability containing a thiol group (-SH) multifunctional ligand and two or more metal ions with complementary electronic structures to form a multi-metal thiol synergistic coordination solution as an interface modifier for the perovskite layer. After the interface modifier is spin-coated on the perovskite layer and annealed, the formed interface modification layer not only has self-repairing and dynamic regulation functions (the weak coordination bonds between the thiol group and the various metal ions can be broken and reorganized when stress or environmental changes occur), but also can regulate the acid-base environment of the perovskite surface under the synergistic action of multiple metals, reduce the migration of halide ions, inhibit interface degradation, and prevent moisture and oxygen from penetrating into the perovskite layer. The interface modifier provided in the present application has a dual repair effect of defect filling and interface reconstruction.

The invention provides a high-temperature-resistant bactericidal corrosion inhibitor as well as a preparation method and application thereof. The preparation method comprises the following steps: reacting a sulfydryl carboxylic acid compound and polyethyleneimine in an organic solvent at a first temperature for a first time to obtain a system containing a first compound; and adding halogenated hydrocarbon into the system containing the first compound, reacting at a second temperature for a second time to obtain a system containing a second compound, removing the organic solvent, and drying to obtain the high-temperature-resistant bactericidal corrosion inhibitor. The high-temperature-resistant bactericidal corrosion inhibitor disclosed by the invention is prepared by the preparation method. The invention also provides an application of the high-temperature-resistant bactericidal corrosion inhibitor in microbial corrosion protection and / or chemical corrosion protection of oil and gas fields. The high-temperature-resistant bactericidal corrosion inhibitor disclosed by the invention is simple in preparation method, good in high-temperature stability and excellent in bactericidal corrosion inhibition performance.

The present invention relates to a method for large-scale production of a benzo [d] thiazole intermediate for preparing torametinib, and a method for large-scale preparation of torametinib using the intermediate, the method avoiding a column chromatography operation which is expensive and complicated to operate while significantly improving the yield of the benzo [d] thiazole intermediate, and the method for large-scale production of torametinib using the intermediate. And thus, the yield of the final product torametinib is improved. Therefore, according to the method, the cost is greatly reduced, the yield is improved, and the method is suitable for large-scale production.

The present invention relates to a method for preparing tert-dodecyl mercaptan using a modified Y molecular sieve catalyst, wherein the modified Y molecular sieve catalyst is used for the reaction of triisobutylene and hydrogen sulfide to prepare tert-dodecyl mercaptan. The method of the present invention has high product selectivity, long catalyst life, low reaction energy consumption, obvious economic advantages, and is particularly suitable for large-scale production.

A method of producing pentaerythritol mercaptocarboxylate including subjecting a mercaptocarboxylic acid and pentaerythritol to a dehydration reaction under solvent-free conditions, a polymerizable composition containing the pentaerythritol mercaptocarboxylate, a resin which is a cured product of the polymerizable composition, an optical material containing the resin, and a spectacle lens containing the resin.

The invention belongs to the field of organic matter synthesis, and particularly discloses a preparation method of tert-dodecyl mercaptan, which is characterized in that hydrogen sulfide and dodecene are used as raw materials, and an addition reaction is performed under the catalytic action of a solid acid catalyst by adopting a liquid-solid heterogeneous process and a fixed bed reactor to obtain the tert-dodecyl mercaptan. The continuous liquid-solid reaction is realized, the diffusion time of hydrogen sulfide to a liquid phase main body is shortened, the heat capacity and the heat transfer coefficient of a reaction system are improved, the catalytic efficiency of the catalyst and the temperature controllability of the reaction process are improved, and the reactor design is simplified. Under proper operation conditions, the conversion per pass of dodecene is greater than or equal to 85%, the selectivity is close to 100%, the technological process is simple, few three wastes are generated, treatment is easy, and the method is suitable for industrial production.

The invention relates to the technical field of chemical synthesis, in particular to a preparation method of 2-sulfydryl-6-chlorobenzoic acid, which comprises the following steps: dissolving chlorobenzoic acid in dimethyl sulfoxide, adding sodium hydrogen sulfite, and stirring at room temperature; the preparation method comprises the following steps: dissolving mercaptobenzoate in dimethyl sulfoxide, adding sodium carbonate and dimethylamino, and reacting at high temperature; cooling to room temperature, and adjusting the pH value to be neutral by using dilute acid; adding into diethyl ether, uniformly mixing, adding into dilute acid, and standing for layering to obtain 2-sulfydryl-6-chlorobenzoic acid; the preparation method of the chlorobenzoic acid comprises the following steps: mixing parachlorotoluene with water, adding a supported catalyst, stirring and heating; after the temperature rises to 80 DEG C, adding potassium permanganate in batches for reaction; and filtering, adjusting the pH value to be acidic by using dilute acid, and then carrying out suction filtration and drying to obtain the chlorobenzoic acid. According to the preparation method disclosed by the invention, chlorobenzoic acid and mercaptobenzoate are subjected to a reaction to obtain 2-mercapto-6-chlorobenzoic acid with high yield; the method has the characteristics of simplified operation, energy consumption reduction, shortened production period and low production cost.

The invention relates to a method for catalytically synthesizing 3-mercaptopropionic acid by an MgO-loaded molecular sieve, and belongs to the technical field of organic synthesis. In order to solve the problems that an existing solid-phase catalyst is not easy to regenerate and the selectivity of 3-mercaptopropionic acid is low, the preparation method comprises the following steps: firstly, mixing a roasted molecular sieve, magnesium acetate tetrahydrate powder and distilled water to obtain an impregnated solid mixture, and carrying out temperature programming roasting on the solid mixture to obtain an MgO-loaded molecular sieve catalyst with the MgO loading capacity of 0.5-20%; and mixing the MgO-loaded molecular sieve catalyst, acrylic acid and an organic solvent, introducing hydrogen sulfide, and carrying out a heating reaction to obtain 3-mercaptopropionic acid. The MgO-loaded molecular sieve is used for catalyzing the addition reaction of hydrogen sulfide and acrylic acid to synthesize 3-mercaptopropionic acid, and the selectivity and selectivity of 3-mercaptopropionic acid are both higher than 90%. The MgO-loaded molecular sieve catalyst prepared by the invention has the characteristics of high catalytic activity, simple synthesis and mild catalytic synthesis conditions.

The invention relates to a method for synthesizing 3-mercaptopropionic acid by catalyzing acrylic acid and hydrogen sulfide through an acidic molecular sieve, and belongs to the technical field of organic synthesis. In order to solve the problems of low selectivity and difficulty in regeneration of 3-mercaptopropionic acid prepared from an existing basic catalyst, the method comprises the following steps: firstly, pretreating a molecular sieve catalyst to obtain a required acidic molecular sieve catalyst; and mixing the acidic molecular sieve catalyst, acrylic acid and an organic solvent according to a certain mass volume ratio, introducing hydrogen sulfide to a certain pressure, heating to a reaction temperature, and reacting for a certain time to obtain 3-mercaptopropionic acid. The acidic molecular sieve used in the invention has the characteristics of high catalytic activity, high selectivity, high mechanical strength and reproducibility, and can catalyze the addition of acrylic acid and hydrogen sulfide to synthesize 3-mercaptopropionic acid in one step, the conversion rate of 3-mercaptopropionic acid is higher than 90%, the selectivity is higher than 85%, and the method has the characteristics of simple catalytic synthesis method, mild conditions and the like.

The invention relates to the technical field of copper-molybdenum separation inhibitors, and discloses a preparation method of a polythiocarboxylic acid amine copper-molybdenum separation inhibitor, which comprises the following steps of: separating and purifying tail liquid generated by preparing thionocarbamate to obtain sodium thioglycolate, and reacting with carbon disulfide by taking potassium hydroxide as a catalyst to obtain the polythiocarboxylic acid amine copper-molybdenum separation inhibitor. The novel polythiocarboxylic acid amine copper-molybdenum separation inhibitor is obtained. The resource utilization of the thionocarbamate tail liquid is realized, the raw materials are cheap and easy to obtain, and the process is green and environment-friendly. The polythiocarboxylic acid amine copper-molybdenum separation inhibitor has the advantages of being good in adaptability, safe, environmentally friendly, good in inhibition effect, simple in process, wide in production raw material source and the like.

The invention is applied to the technical field of compound preparation, and discloses a synthesis method of o-aminothiophenol, which comprises the following steps: uniformly mixing 2-chloronitrobenzene, water and strongly basic anion exchange resin, heating, dropwise adding a hydrosulfide aqueous solution, carrying out heat preservation reaction, cooling and filtering after the reaction is finished, and drying to obtain the o-aminothiophenol. Eluting the filter cake with liquid alkali, acidifying and layering to obtain an o-aminothiophenol crude product, and distilling to obtain the product. The thiophenol and the basic group of the resin are salified, the main reaction for generating 2-nitrothiophenol is promoted in the early stage, and the generation of a nitroreduction byproduct 2-aminochlorobenzene is greatly reduced, so that the product yield is greatly improved; the product stability is improved by salifying, so that disulfides are prevented from being formed by bimolecular oxidation of thiophenol, reduction is not needed, the product can be obtained by acidification after alkali elution, the process is shortened, and the cost is reduced; the production process is simple to operate, pressure reaction is avoided, the requirement on equipment is low, and the yield is high and can reach 95% or above; the purity of the obtained product can reach 99% or above.

A method for producing a polythiol composition, the method including a reaction step of reacting a thiocarbamate resin with a quaternary ammonium salt comprising a quaternary ammonium cation and a counter anion to produce a polythiol composition.

The invention discloses a bimetallic asymmetric reduction Schiff base catalyst for synthesizing ethylene carbonate and a preparation method of the bimetallic asymmetric reduction Schiff base catalyst. According to the catalyst, a diamine compound is subjected to selective single-side protection, the imine reduction position is controlled, and a bimetallic active center is introduced; the controllable synthesis of a product for reducing the outer side imine and a product for reducing the inner side imine is realized; the obtained product is recrystallized to obtain a monoimine-monoamine type ligand with a clear asymmetric structure, the monoimine-monoamine type ligand and metal salt form a bimetallic catalyst, and the catalyst generates a synergistic effect through double active sites and shows high catalytic activity and excellent product selectivity.

The present invention relates to a method for producing methyl mercaptan, comprising the following steps: A) methanol is reacted with hydrogen sulfide to form a stream (M), preferably in the gas state, comprising methyl mercaptan, unreacted H2S and possibly sulfur-bearing by-products; B) optionally, said stream (M) is condensed; C) at least one step of purifying said stream (M) is carried out in order to obtain a methyl mercaptan-enriched stream; D) the gaseous effluents resulting from said at least one purification step are recovered, said gaseous effluents comprising at least one sulfur-bearing compound, preferably H2S; E) a gas-liquid extraction of said at least one sulfur-bearing compound, preferably H2S, is carried out using liquid methanol so as to obtain a liquid methanol enriched in sulfur-bearing compound(s), preferably in H2S; and F) optionally, said enriched methanol is used as a reactant for the reaction of step A).

The invention relates to a preparation device and method for isooctyl thioglycolate, and particularly to the technical field of chemical intermediate preparation. A synthesis tank and a stirring mechanism are provided, the stirring mechanism is placed in a synthesis space of the synthesis tank, raw materials for isooctyl thioglycolate to be synthesized are placed into the synthesis space of the synthesis tank according to a set molar ratio, a first driving member arranged outside the synthesis tank is connected to a portion of a first stirring member extending out of the synthesis space, and a free end of the first stirring member is connected to a second stirring member via a cross universal joint, a sliding member is slidably sleeved on the outer periphery of the first stirring member, and the sliding member is slidable along the first stirring member until it engages with the cross universal joint. The first driving member drives the first stirring member to rotate, thereby stirring different areas in the synthesis space and uniformly dispersing thioglycolic acid and isooctyl alcohol, thereby improving the manufacturing efficiency of isooctyl thioglycolate.

The invention provides a preparation method of a magnetic recoverable catalyst and a method for synthesizing 3-mercaptopropionic acid, and mainly solves the problem that a large amount of acid and alkali solutions are needed in the existing acrylonitrile-sodium hydrosulfide and acrylic acid-thiourea process routes. The thiohydracrylic acid synthesis catalyst is prepared. The use conditions of the catalyst are as follows: the temperature is 30-80 DEG C, the reaction pressure is 0.5-3 MPa, the mass ratio of the acrylic acid to the solvent is 0.1-5, and the mass ratio of the acrylic acid to the catalyst is 0.2-20. Compared with the prior art, the catalyst disclosed by the invention is used as a synthetic catalyst for preparing thiohydracrylic acid through reaction of acrylic acid and hydrogen sulfide, a solid catalyst and a liquid reaction system can be completely separated by adopting simple methods such as filtration, centrifugation or magnetic separation, and a complicated pickling step is not needed; and the problem that a homogeneous catalyst is difficult to rectify after salification in the use process is avoided.

The invention belongs to the technical field of chemistry, and particularly relates to a preparation method of ethyl thioglycolate. Comprising the following steps: successively dropwise adding thioacetic acid and potassium carbonate into # imgabs0 # 4-bromobenzenesulfonic acid acetonitrile and acetonitrile at room temperature, fully reacting, purifying, and concentrating under reduced pressure until the mixture is dry to obtain acetyl mercaptoacetonitrile; hydrochloric acid and ethanol are added into acetyl mercaptoacetonitrile, water and dichloromethane are added after heating reaction, an organic phase is obtained through phase splitting, and the organic phase is dried and concentrated under reduced pressure to be dry to obtain ethyl mercaptoacetate. The method is simple in post-treatment, suitable for industrial production and high in reaction yield.

The present invention provides a polythiol obtained by thiolating a hydroxyl group of a plant-derived polyol.