47 results about "Dithiosalicylic acid" patented technology

The present invention relates to a method for causing sodium sulfide or a mixture of sodium sulfide and sulfur to react with diazonium salt formed by diazotizing anthranilic acid, wherein the Na / S atomic ratio as calculated on the basis of the employed sodium sulfide and sulfur is adjusted to within the range of 1.33 to 2.0 during the reaction. Thus is made practicable the manufacture of thiosalicylic acid in a high yield without going through the individual route of isolating and reducing dithiosalicylic acid.

The invention provides a method for treating and recycling process waste water generated during the production of 1,2-Benzisothiazolin-3-One. The production of 1,2-Benzisothiazolin-3-One is as follows: dithio-salicylic acid is used as a raw material and is subjected to acylating chlorination, chloro-substitution, distillation, alkaline hydrolysis using ammonia, bleaching, acidification and refining. The method for treating and recycling the process waste water includes the following steps: adjusting the pH of the process waste water to be about 8, carrying out two-level serially connected preferential adsorption on 1,2-Benzisothiazolin-3-One using ultra-high cross-linked polystyrene-divinylbenzene polymeric adsorbent bed layer, the effluent after the second level of adsorption is subjected to triple effect evaporation, a part of the distillation effluent returns to the original production process for being used indiscriminately, and another part of the distillation effluent is subjected to aerobic biological treatment, and the treated effluent can reach national first-level discharge standards; the residual after distillation is subjected to cooling, crystallization and centrifugation, and then crude sodium chloride is recycled; the polymeric adsorbent used dilute sodium hydroxide solution is regenerated through desorption; all levels of resins can be used repeatedly; the desorption solution can be directly applied to the bleaching process of the original production process; recycling of organic matters is realized while the waste water is treated by using the method.

The invention discloses a preparation method of a nano-fluorescence probe for detecting ROS (reactive oxygen species) and the fluorescence probe, and mainly relates to the technical field of reactive oxygen species fluorescence detection. 2, 2'-dithio-salicylic acid serves as a ligand, 1, 10-phenanthroline serves as an auxiliary ligand, and polymerization reaction is performed by taking cadmium ions as central metal ions to obtain a nano-scale rodlike disulfide coordination polymer. The preparation method has the advantages that the preparation method is simple, toxic organic solvents are omitted in the preparation process, strict synthesis conditions are omitted, recognition of the ROS is based on response of disulfide bonds in the ligand to the ROS, good selectivity for the ROS is achieved, and other inorganic ions and organic molecules have no obvious effects on fluorescence signals of the nano-fluorescence probe.

The invention relates to a preparation method of 2,4-diethyl thioxanthone. The preparation method of the 2,4-diethyl thioxanthone is characterized by finally obtaining a product, i.e. the 2,4-diethyl thioxanthone, through the processes of condensation, extraction, washing, caustic washing, distillation, dissolution and crystallization, centrifugation, drying, and the like by taking o-diethylbenzene and dithio-salicylic acid as main raw materials and sulphuric acid, toluene, sodium carbonate, methanol, and the like as auxiliary raw materials. The preparation method of the 2,4-diethyl thioxanthone, which is disclosed by the invention, has the advantages of higher yield reaching 85 percent through experimental determination, little acid pollution, easy aftertreatment, moderate reaction condition and capability of reducing the energy consumption because the distillation is not needed by the aftertreatment of the product.

The invention discloses a tellurium semiconductor micro-nanometer crystalin a three-dimensional three dentrite shape, which is prepared by the following steps: dissolving tellurium salt in an organic solvent, reacting hermetically for 1-40h at 60-200 DEG C and 0.5-6MPa under effect of a reducing agent; and after reaction, centrifuging the reaction solution, taking precipitate, washing, and drying to obtain the tellurium semiconductor micro-nanometer crystal in a three-dimensional three dentrite shape. The reducing agent is selected from one or a mixture of any two of dithiosalicylic acid, ascorbic acid, citric acid, sodium borohydride or glucose at any proportion. The tellurium micro-nanometer crystal prepared by the invention has the advantages of uniform size distribution, low cost and stable quality of production as well as excellent pyroelectric, photoconductive, polarizing, piezoelectric properties and non-linear optic response and the like. The tellurium semiconductor micro-nanometer crystal in a three-dimensional three dentrite shape can be applied to optical device, micro-electronic and molecular sensitive components and the like.

Disclosed is a process for the preparation of 11-(4-[2-(2-hydroxyethoxy)ethyl]-1-piperazinyl)-dibenzo[b,f][1,4]thiazepine. In the process, low-priced 2,2′-dithiosalicylic acid as starting material is subjected to bond formation reaction with 1-chloro-2-nitrobenzene in a basic aqueous solution, a nitro group reduction reaction is conducted, cyclization and chlorination reactions are simultaneously carried out in the presence of a equivalent amount of halogenating agent, a reaction with piperazine is continuously conducted without separation, and a reaction with 2-haloethoxyethanol is conducted, thereby it is possible to economically producing Quetiapine, that is, 11-(4-[2-(2-hydroxyethoxy)ethyl]-1-piperazinyl)-dibenzo[b,f][1,4]thiazepine, in an environmentally friendly manner. Particularly, the process is advantageous in that economic efficiency is assured because of use of the low-priced starting material, use of an organic solvent is minimized because a reaction is conducted in an aqueous solution, and it is possible to achieve the environmentally friendly and economical process having high commercial usefulness because the number of reaction steps of the process is reduced and because generation of acidic waste is minimized.

The invention discloses a polyester environment-friendly mirror surface material, which is prepared from the following raw materials in parts by weight: 0.7 to 1 part of butyltin trioctane, 1 to 2 parts of 2,2-methyl dithiophenyl glycolate, 3 to 5 parts of aluminum dihydrogen phosphate, 4 to 6 parts of polytetrahydrofuran ether glycol, 4 to 5 parts of maleated rosin, 0.8 to 1 part of dithio-salicylic acid, 110 to 130 parts of polycarbonate and 17 to 20 parts of amination polyester solution. The dithio-salicylic acid is used for treating maleated rosin; then, blending reaction is performed withamination polymers; an aluminum dihydrogen phosphate water solution is used as a reaction solvent; the effective compatibility of the rosin and the polymer is realized; the heat resistant stability of a finished product material is improved. The mirror surface material has good environment-friendly performance and excellent comprehensive performance.

The invention discloses a novel synthesis method of an N-substituted benzisothiazoline-3-ketone derivative. The preparation method comprises the following steps: by taking a dithiosalicylic acid derivative and sulfur as raw materials, introducing chlorine or bromine to obtain a halogenated thiobenzoyl halide derivative, then preferably dropwise adding a mixed solution of primary amine and tertiaryamine, and carrying out reaction and ring closing to obtain the N-substituted benzisothiazole-3-ketone. The method disclosed by the invention is simple in process, safe and controllable, and easy forindustrial large-scale production.

The invention discloses a one-pot synthesis technology of a photo initiator 2,4-diethylthioxanthone. The invention belongs to the field of fine chemical engineering, and specifically relates to a one-pot synthesis technology of a photo initiator 2,4-diethylthioxanthone. According to the technology, thiosalicylic acid (or dithiosalicylic acid) and 1,3-diethylbenzene are taken as the raw materials,concentrated sulfuric acid is taken as a catalyst and a solvent, and under the action of a co-catalyst, condensation reactions are carried out for 4 to 8 hours at a temperature of 0-70 DEG C. Post treatment technologies (condensation, extraction, concentration, and recrystallization) are carried out in one reaction unit; the obtained product is filtered and dried to obtain high purity 2,4-diethylthioxanthone. The technology has the advantages of good selectivity, low reaction temperature, short reaction time, high yield, simple and convenient operation, and high efficiency of single kettle, the equipment investment, the energy consumption, the operation strength, and the production cost are reduced, and the technology is suitable for industrial production.

A rubber composition containing (A) 100 parts by mass of a rubber component containing 30 parts by mass or more of a diene-based rubber, (B) 0.1 to 1.0 parts by mass of dithiosalicylic acid and (C) 0.05 to 0.5 part by mass, in terms of a metal content of an organic metal salt and a pneumatic tire using the same, whereby an alternative to DCBS exhibiting adhesion characteristics of rubber with steel cord equivalent to that of DCBS and capable of being applied to rubber for a belt cord and / or an edge cushion of a tire can be developed.

The invention relates to a method for synthesizing 6-methyl-dibenzothienophridine, comprising the following steps of: in mixed solvent of ethanol and water, taking 2,2-dithiosalicylic acid as shown in the formula (II) and pyridine derivative as shown in the formula (III) as raw materials; reacting for 24-60 hours at 80-200 DEG C and in 2-3 atmospheric pressures in the presence of sodium azide; and processing the reaction liquid after the reaction is finished to obtain the 6-methyl-dibenzothienophridine as shown in the formula (I), wherein the molar ratio of the 2,2-dithiosalicylic acid to the pyridine derivative is 1-10:1; the molar ration of pyridine derivative to the sodium azide is 1:1-5; and the volume ratio of ethanol to water in the mixed solvent is 1-5:2. The method has simple operation and little environmental pollution and reduces the production cost. The product synthesized by the method can be used for preparing nano devices.

The invention discloses a storage-stable inflaming retarding optical cable material which is prepared from the following raw materials in parts by weight: 2-3 parts of polyisoprene, 6-7 parts of guanidine sulfamate, 20-23 parts of carbon nanotubes, 0.3-0.4 part of N,N'-dicyclohexyl carbimide, 4-5 parts of hexachlorocyclotriphosphazene, 0.2-0.4 part of sodium hydroxide, 1-2 parts of sulfocarbamide, 0.7-1 part of calcium naphthenate, 0.1-0.3 part of N-phenyl-2-naphthylamine, 0.1-0.2 part of dithio-salicylic acid, 4-6 parts of dibutyl maleate, 0.3-1 part of sp80, 2-3 parts of aluminum dihydrogen phosphate, 3-4 parts of polyether diol, 0.2-1 part of hexamethyl cyclotrisiloxane, 17-20 parts of nylon and 120-130 parts of polyvinyl chloride. The graft-modified nylon and polyvinyl chloride which are added into the optical cable material provided by the invention have quite good compatibility, and effectively improve the storage stability of a finished product.

The invention discloses a solid acid based catalytic synthesis method for photoinitiator DETX (2,4-diethyl thioxanthone). According to the method, solid acid is taken as a catalyst, dithiosalicylic acid and m-diethylbenzene are added to a reaction kettle containing an organic solvent for a reaction, and the required product, namely, the photoinitiator DETX is obtained through extraction, recrystallization, filtering and drying. Compared with the prior art, the yield is increased, side reactions are reduced greatly, and the method is suitable for industrialization and environmentally friendly.

The invention discloses an environment-friendly flame-retardant PE material and a preparation method thereof. High density polyethylene, hydroxyethyl acrylate, triphenyl phosphite and polyvinylidene fluoride are used as main ingredients, dicumyl peroxide, maleic anhydride, sucrose acetoisobutyrate, isophorone diisocyanate, attapulgite, expanded perlite, hydrated zinc borate, vanadium diboride, aluminum titanate, bamboo charcoal powder, dithio-salicylic acid, an auxiliary agent and a silane coupler are added, processes of ball-milling, ultrasonic treatment, calcining, hot blending, foaming, curing, extruding and the like are carried out, so that the prepared environment-friendly flame-retardant PE material has excellent flame retardance, is environment-friendly, and meanwhile is high in strength, and application level of the material is increased.

The invention relates to a preparation method and application of a metal organic nanometer compound. The metal organic nanometer compound with a chemical formula of {[Zr(BPDC-S-S)]}infinity is named as UIO-67-S-S and is formed by precipitation of zirconium tetrachloride, used as a metal salt, and 4,4-dithiosalicylic acid, used as organic ligand, in DMF mixed liquor through coordination. The UIO-67-S-S nanometer compound can be used as a drug release carrier for response to dual pH and redox stimulation.

The invention discloses efficient scaling powder. The scaling powder comprises, by weight, 30-35 parts of modified maleated rosin, 0.2-0.3 part of epoxy octyl stearate, 0.6-1 part of succinic acid, 0.2-0.3 part of dimethylimidazole, 0.2-1 part of 2-bromine-4-methylphenol, 0.1-0.2 part of dehydrate gypsum powder, 0.7-1 part of 2-methylpropanoate, 1-2 parts of dist coconut fatty acid polyoxyethylene ether, and 70-80 parts of organic solvents. The scaling powder contains no halogen and needs no cleaning after welding, and therefore efficiency is high and cost is low. The modified maleated rosin is added into the scaling powder, viscosity is adjusted by sa-son seed gum, the surface tension of fusing scolder can be improved by lanolin dissolved by ethyl alcohol, the wetting effect can be enhanced, the generation of mycete can be avoided through dithio-salicylic acid, and oxides on the surface of the fusing scolder can further be removed through the dithio-salicylic acid. The scaling powder has the advantages of being high in welding activity, capable of easily removing scolder residues, incapable of generating toxic gas, and good in environment protection property.

The invention provides a water-based washing-free antibacterial mildew-proof soldering flux and a preparation method of the water-based washing-free antibacterial mildew-proof soldering flux. The water-based washing-free antibacterial mildew-proof soldering flux is prepared from the following raw materials of by weight, 10-16 parts of dithiosalicylic acid, 7-13 parts of itaconic acid, 6-14 parts of o-aminobenzoic acid, 4-8 parts of isoamyl acetate, 5-10 parts of n-decanol, 2-5 parts of methyl tert-butyl ether, 3-6 parts of alkylphenol polyoxyethylene ether, 1-3 parts of N-dodecyl-N-methyl glucosamine, 2-5 parts of coconut oleic acid diethanolamide, 2-4 parts of dipropylene glycol butyl ether, 1-5 parts of propylene glycol phenyl ether, 3-8 parts of modified nano silver, 2-6 parts of an antioxidant, 3-7 parts of a corrosion inhibitor and 10-18 parts of a water solution. The prepared soldering flux has good antibacterial effect, high shear strength and strong wettability and corrosion resistance, so the soldering flux has wide application prospect as the water-based washing-free antibacterial mildew-proof soldering flux.

The invention provides a dithiosalicylic acid refining device which comprises a dissolution reaction kettle, wherein a liquid caustic soda inlet and a softened water inlet are formed in the top of thedissolution reaction kettle; a stirring device is mounted inside the dissolution reaction kettle; a jacket is mounted on the outer wall of the dissolution reaction kettle; a filter is connected withthe bottom of the dissolution reaction kettle through a conveying pipeline; a filtering cylinder is mounted inside the filter; a filtering net is arranged at the top of the filtering cylinder; the lower part of the filter is connected with the top of an acidification reaction kettle through a conveying pipeline; a hydrochloric acid inlet is formed in the top of the acidification reaction kettle; ajacket is mounted on the outer wall of the acidification reaction kettle; the bottom of the acidification reaction kettle is connected with a centrifuge through a conveying pipeline. The dithiosalicylic acid refining device has the advantages that in processes of alkali dissolution, decontamination and acidification, high-quality products are prepared to the maximum extent, and the product puritycan be improved; in addition, the jackets are mounted on outer walls of the dissolution reaction kettle and the acidification reaction kettle, and heat inside the reaction kettles can be carried awaythrough heat exchange of circulated water and the reaction kettles, so that product damage caused by too high temperatures can be avoided; in addition, an alkali solution or an acid solution does notneed to be continuously dropped, so that the labor can be saved, and the working efficiency can be improved.

The invention relates to stable isotopic labeled 2-isopropylthioxanthone and a synthetic method thereof. The stable isotopic labeled 2-isopropylthioxanthone is 2-isopropylthioxanthone labeled by D or 13C. The synthetic method comprises the following steps of using benzene and acetone which are labeled by stable isotopic D or 13C as raw materials; reacting the benzene and the acetone with magnesium to obtain Grignard reagent after benzene bromination; performing reduction and hydroxide radical bromination on the acetone to obtain 2-bromic propane; performing Grignard reaction to obtain isopropyl benzene; reacting the isopropyl benzene with dithio-salicylic acid; and synthesizing to obtain the 2-isopropylthioxanthone labeled by the stable isotopic D or 13C. Compared with the prior art, the stable isotopic labeled 2-isopropylthioxanthone has the advantages that a process route is simple, the 2-isopropylthioxanthone is easy to synthesize, products are easy to separate and purify, the chemical purity of the products is above 99.0%, isotope abundance is above 98.0% atom, requirements of trace detection in the field of food safety can be met fully, and economical efficiency and using value are excellent.

The invention discloses an aerogel lubrication plastic material. The aerogel lubrication plastic material is prepared from, by weight, 3-4 parts of linoleic acid, 0.1-0.2 part of copper naphthenate, 0.7-1 part of 2-bromo-4-methylphenol, 1-2 parts of diisopropyl ethanol amine, 4-6 parts of hydroxyethyl cellulose, 0.8-2 parts of 3-aminopropyl trimethoxy silane, 1-2 parts of sucrose acetate isobutyrate, 13-20 parts of silicon dioxide aerogel, 1-2 parts of dithiosalicylic acid and 110-130 parts of high-density polypropylene. By adding of cellulose ester solution, oxidation resistance of finished products of the plastic material can be improved to further improve storage stability, and toughness and dynamic strength of the finished products can be improved. By adding of the silicon dioxide aerogel, high compatibility to a polypropylene base material is achieved after organic treatment, and high dynamic stability and excellent comprehensive performances of the finished products are realized.

The invention discloses a preparation method of 2,2'-dithio-salicylic acid shown as the formula I, and the method comprises the following steps: taking o-aminobenzoic acid as raw material, using sodium nitrite and hydrochloric acid for carrying out diazotization at the temperature of 0-10 DEG C, obtaining diazotized solution, leading the diazotized solution to be reacted with liquid sulfur dioxide for 0.5-3 hours at the temperature of minus 20-minus 10 DEG C in the presence of a catalyst and a co-catalyst, then keeping the temperature at 80-100 DEG C for 0.5-2 hours, cooling, filtering and obtaining the 2,2'-dithio-salicylic acid. The preparation method has the advantages of high reaction yield, good product purity, simple separation, a small amount of produced waste water, low productioncost and the like.

The invention discloses a synthesis method of photoinitiator isopropylthioxanthone. According to the method, an isopropylthioxanthone crude product is prepared from raw materials including dithiosalicylic acid and isopropylbenzene with a chlorination-friedel-crafts reaction synthesis route, and a product is obtained through high-vacuum distillation purification. The raw and auxiliary materials are easy to obtain, reaction conditions are mild, the operation is safe, simple and convenient, the conversion rate of the raw materials is high, and the product quality is stable.

The invention discloses an environment-friendly polyvinyl chloride plastic pipe which consists of the following raw materials in parts by weight: 1-2 parts of sucrose acetate isobutyrate, 0.8-1 part of benzotriazole, 2-3 parts of phosphorous acid bisphenol A ester, 3-4 parts of carbon nanotubes, 40-60 parts of 90-93% sulfuric acid, 60-70 parts of 95-97% nitric acid, 1-2 parts of acryloyl chloride, 0.01-0.02 part of 1,4-dioxane, 0.2-0.3 part of azodiisobutyronitrile, 6-10 parts of hydroxyethyl acrylate, 7-8 parts of triethylamine, 10-14 parts of a liquid ethylene-propylene-diene monomer, 1-1.2 parts of dicumyl peroxide, 100-120 parts of polyvinyl chloride, 0.7-1 part of lauryl dimethyl amine oxide, 2-3 parts of beewax, 0.1-0.3 part of dithiosalicylic acid, 1-2 parts of zinc ricinate and 10-16 parts of bentonite. The environment-friendly polyvinyl chloride plastic pipe disclosed by the invention is free of toxic or harmful substance volatilization, good in environmental friendliness and excellent in comprehensive property.

The invention discloses a cellulose woodenware coating, which is made from the following raw materials, by weight part, 2-3 of a dammar resin, 6-10 of cellulose proprionate, 2-3 of sodium pyrophosphate, 0.1-0.13 of potassium periodate, 1-2 of sodium acetate, 7-10 of chitosan, 24-30 of polyvinyl alcohol, 0.1-0.2 of nanometer alpha-Fe2O3, 1.3-2 of polyglyceryl fatty acid ester, 2-3 of sericin, 5-7 of beeswax, 70-100 of natural latex, 1-2 of linoleic acid, 2-3 of maleopimaric acid anhydride, 560-600 of an acrylic acid emulsion, 140-160 of titanium dioxide, 1-2 of ammonium paratungstate, 2-3 of dithiosalicylic acid, 1-2 of polylactic acid, 3-4 of polytetramethylene ether glycol and 2-3 of hydroxyethyl cellulose. Through addition of cellulose proprionate and hydroxyethyl cellulose, dispersion of particles in the emulsion is improved, and the stability of a coating film is improved.

The invention discloses a shock absorber oil seal with good rebound resilience, which comprises the following raw materials in parts by weight: 100 to 104 parts of fluorous rubber F26, 3 to 5 parts of wannianhui, 2 to 3 parts of polyethylene glycol 1000, 1 to 2 parts of dithiosalicylic acid, 3 to 4 parts of propolis, 10 to 14 parts of fumed silica, 2 to 3 parts of 1-stearoyl-rac-glycerol, 6 to 8 parts of SG-3 type PVC (polyvinyl chloride) resin, 1 to 2 parts of absolute ethyl alcohol, 6 to 8 parts of cresyl diphenyl phosphate, 1 to 2 parts of imethylaminopropylamine, 1 to 2 parts of magnesium chloride, 1 to 2 parts of di-tert-butyl peroxide, 0.3 to 0.5 parts of sulphur, 1 to 2 parts of an accelerant CZ, 1 to 2 parts of an antiager 4010, and 18 to 26 parts of composite fillers. The shock absorber oil seal has the advantages that the original shape of the oil seal is kept, the tracking performance is excellent, the sealing effect is good, the mechanical property is good, the weather resistance is good, and the service life is long.

Disclosed is a process for the preparation of 11-(4-[2-(2-hydroxyethoxy)ethyl]-1-piperazinyl)-dibenzo[b,f][1,4]thiazepine. In the process, low-priced 2,2′-dithiosalicylic acid as starting material is subjected to bond formation reaction with 1-chloro-2-nitrobenzene in a basic aqueous solution, a nitro group reduction reaction is conducted, cyclization and chlorination reactions are simultaneously carried out in the presence of a equivalent amount of halogenating agent, a reaction with piperazine is continuously conducted without separation, and a reaction with 2-haloethoxyethanol is conducted, thereby it is possible to economically producing Quetiapine, that is, 11-(4-[2-(2-hydroxyethoxy)ethyl]-1-piperazinyl)-dibenzo[b,f][1,4]thiazepine, in an environmentally friendly manner. Particularly, the process is advantageous in that economic efficiency is assured because of use of the low-priced starting material, use of an organic solvent is minimized because a reaction is conducted in an aqueous solution, and it is possible to achieve the environmentally friendly and economical process having high commercial usefulness because the number of reaction steps of the process is reduced and because generation of acidic waste is minimized.

The invention discloses a preparation method of a nano-fluorescence probe for detecting ROS (reactive oxygen species) and the fluorescence probe, and mainly relates to the technical field of reactive oxygen species fluorescence detection. 2, 2'-dithio-salicylic acid serves as a ligand, 1, 10-phenanthroline serves as an auxiliary ligand, and polymerization reaction is performed by taking cadmium ions as central metal ions to obtain a nano-scale rodlike disulfide coordination polymer. The preparation method has the advantages that the preparation method is simple, toxic organic solvents are omitted in the preparation process, strict synthesis conditions are omitted, recognition of the ROS is based on response of disulfide bonds in the ligand to the ROS, good selectivity for the ROS is achieved, and other inorganic ions and organic molecules have no obvious effects on fluorescence signals of the nano-fluorescence probe.

The present invention relates to a method for causing sodium sulfide or a mixture of sodium sulfide and sulfur to react with diazonium salt formed by diazotizing anthranilic acid, wherein the Na / S atomic ratio as calculated on the basis of the employed sodium sulfide and sulfur is adjusted to within the range of 1.33 to 2.0 during the reaction. Thus is made practicable the manufacture of thiosalicylic acid in a high yield without going through the individual route of isolating and reducing dithiosalicylic acid.