78 results about "Sulfur dichloride" patented technology

The invention relates to a continuous-pressure-changing rectification method and a device for preparing medicine-level sulfoxide chloride. With the adoption of the pressure-changing rectification method, an indirect sequence of carrying out heavy component removal and then carrying out light component removal is adopted as a rectification sequence, so that the decomposition of sulfoxide chloride at high temperature is reduced; sulfur is coarsely mixed with raw materials, sulfur is mixed with tower top gas of a heavy component removal tower, and a low-boiling-point substance, namely sulfur dichloride which is hard to remove, is fundamentally converted into a high-boiling-point substance, namely sulfur monochloride which is easy to remove, due to multistep sulfur adding; and a catalyst is added, so that the dissolution rate and reaction rate of the sulfur are accelerated. The heavy component removal tower is subjected to normal-pressure operation; and a light component removal tower is subjected to depressurized operation. The energy consumption of operation is reduced, and the decomposition reaction of the sulfoxide chloride hardly carries out under depressurized conditions, so that the probability that the color and luster of products are polluted by sulfur dichloride is greatly reduced, high-purity and colorless sulfoxide chloride products are produced from tower bottoms, and the content is over 99.9%.

The invention relates to a method for synthesizing thionyl chloride which takes a crude thionyl chloride product as an initial point. The method is a totally closed circulating process comprising the following steps: other materials in the synthesized crude thionyl chloride product is used to react with sulfur so as to mainly produce a sulfur monochloride product; the other materials comprises sulfur monochloride, sulfur dichloride, thionyl chloride, a small amount of chlorine and sulfur dioxide; and then the sulfur monochloride product is used to synthesize thionyl chloride together with chlorine, sulfur dichloride, and a gas product from the condenser after thionyl chloride synthesis and the crude product purification process.

The invention relates to a method for recovery and purification of sulfoxide chloride in acyl chloride production, which comprises the following steps of: implementing primary purification by a distilling way; converting sulfur dichloride which is difficult to separate into sulfur chloride which is easy to remove by sulfur powder; and adsorbing other colored components by active carbon; and obtaining pure sulfoxide chloride which reaches three-level color degree. The method disclosed by the invention can effectively recover the sulfoxide chloride, and is high in recovery rate, good in quality, safe in process and easy in control; the purified sulfoxide chloride can reach 98.5% in purity and three-level color degree in color.

The invention discloses a preparation method of thiodicarb. The preparation method comprises the following steps: (1) dividing a solvent into two portions, dissolving methomyl in one of the two portions to obtain a methomyl solution, and dissolving 4-dimethylaminopyridine in the other portion to obtain a solvent which contains a catalyst; and (2) dividing sulfur dichloride into two portions, dropwise adding one portion of the sulfur dichloride in the solvent which contains the catalyst under a closed condition, meanwhile, dropwise adding the other portion of sulfur dichloride and carrying outdropwise adding reaction on the other portion of sulfur dichloride and the methomyl solution obtained in step (1), and carrying out insulating reaction after dropwise adding is finished to obtain thethiodicarb. The preparation method of the thiodicarb has the advantages that the reaction selectivity is high, the purity of the obtained product is high, the content of thiodicarb isomer is smaller than 0.4%, the yield is high and the like.

The invention relates to a differential pressure thermal coupling rectification method and equipment for sulfoxide chloride. According to the equipment, a heavy component removing tower of a re-boiler is arranged at the bottom of a tower and a light component removing tower of a condenser is arranged at the top of the tower; a condensation re-boiler, an auxiliary condenser and a conversion reactor are arranged between the heavy component removing tower and the light component removing tower. An extract of a vapor-phase material at the top of the heavy component removing tower is divided into two parts, wherein one part is connected with a heating medium inlet of the condensation re-boiler, a heating medium outlet is connected with the auxiliary condenser and then returns back to the top of the heavy component removing tower, a liquid-phase material outlet at the bottom of the light component removing tower is connected with a heated medium inlet of the condensation re-boiler, and then a heated medium outlet returns back to the bottom of the light component removing tower; the other part is connected with the conversion reactor to carry out a reaction of converting sulfur dichloride to sulfur chloride, and a reacted material vapor phase enters the light component removing tower. The differential pressure thermal coupling is used for coupling heat at the top of the heavy component removing tower and heat at the bottom of the light component removing tower and the energy consumption is saved. The difficulty of blocking a pipeline by sulfur is overcome. A practical example shows that a differential pressure thermal coupling rectification process can save energy by more than 50% compared with a conventional process.

The invention belongs to the technical field of chemical production, and specifically relates to a method and a device for removing the impurity-sulfur dichloride in thionyl chloride. The method comprises the step of enabling thionyl chloride gas which is evaporated from the top part of a rectifying tower and contains 1 to 3 percent of sulfur dichloride to be subjected to temperature rising and to enter an over-vulcanization tank for reaction. The device comprises a crude product receiving tank, wherein the crude product receiving tank is sequentially connected with a sulfur preparing tank, the rectifying tower, a heater and the overvulcanization tank through pipelines; the top part of the sulfur preparing tank is provided with a hydraulic sulfur line. According to the method and the device, disclosed by the invention, 1 to 3 percent of sulfur dichloride which is contained in the thionyl chloride can be reduced to be below 0.004 percent; the requirement on color I of excellent products in industry standard is achieved; the problem that a pipeline arranged at the bottom part of the sulfur preparing tank is blocked can be solved, and continuous production is realized.

The invention discloses a synthesis method of thiodicarb, which comprises the following steps: (1) dividing a solvent into two parts, dissolving methomyl in one of the two parts to obtain a methomyl solution, and dissolving 18-crown ether-6 in the other part of the mixture to obtain a solution of the 18-crown-6; and (2) under a closed condition, dropwise adding a part of sulfur dichloride into the 18-crown-6 solution, after dropwise adding is completed, dropwise adding the residual sulfur dichloride to react with the methomyl solution, and after dropwise adding is completed, continuing to carry out heat preservation reaction to obtain the thiodicarb. The method is high in reaction selectivity, by-products are reduced, the obtained product is high in purity and yield, and meanwhile, the problem that a pipeline is easily blocked in the production process can be effectively solved. The method is simple in process operation and suitable for large-scale industrial production.

The invention discloses a preparation method for synthetizing sulfur dichloride through gas phase catalysis. Granular activated carbon supported by ferric chloride (FeCl3/C) is taken as a catalyst, disulfur dichloride and chorine are taken as a reaction raw material and a carrier gas, a vaporized gas mixture of the disulfur dichloride and the chorine enters a fixed bed catalysis tubular reactor, the sulfur dichloride is prepared with a continuous gas phase catalysis method, the sulfur dichloride produced through the reaction is cooled by a condenser to be collected, and the excess chlorine is recycled. The sulfur dichloride product obtained with the method is free of catalyst residues, distillation is not required, and the content of sulfur dichloride in the product is higher than 90%. The excess chlorine is recycled. The preparation method is simple to operate, continuous, stable, high in conversion rate and free of waste gas and waste liquor emissions, so that the environmental pollution is reduced.

The invention discloses a synthesis method of 4,4'-thiobisbenzenethiol. The method comprises the following steps of: 1) esterfying, namely adding acetic anhydride into phenthiol serving as an initiative raw material dropwise for reacting, and laminating; 2) etherifying, namely adding a solvent, iodine and sulfur dichloride into an organic layer I obtained in the step 1) for reacting, laminating, decompressing an organic layer II and removing the solvent to obtain a yellow solid; 3) hydrolyzing, namely adding sodium hydroxide and the yellow solid into water for a warming reflux reaction, adding hydrochloric acid solution dropwise, and filtering to obtain a white solid; and 4) recrystallizing, namely recrystallizing the white solid with a recrystallizing solvent to obtain white crystalline 4,4'-thiobisbenzenethiol. The 4,4'-thiobisbenzenethiol synthesized by the method has the characteristics of simple process and high yield.

The present invention belongs to the field of lubricating oils, and relates to antioxidants, particularly to a high-temperature antioxidant and a preparation method thereof, and applications of the high-temperature antioxidant in gear oil. The high-temperature antioxidant comprises p-tert-octylphenol, n-hexane, sulfur dichloride, alkenyl succinic acid phenol, benzene, thio bis-p-tert-octyl phenol benzene, and hydrated copper acetate. Compared with the high-temperature antioxidant, the preparation method and the applications thereof in the prior art, the high-temperature antioxidant, the preparation method and the applications thereof of the present invention have the following advantages and positive effects that the high-temperature antioxidant is provided and is added to the gear oil so as to improve excellent anti-oxidation capacity of the gear oil, effectively reduce the carbon deposition on the vehicle gear surface, reduce the oil seal wear, prolong the oil change period, and improve the economic benefits.

The invention discloses a synthetic method of perchloromethyl mercaptan. According to the synthetic method, trichloromethane and sulfur dichloride are used as reaction raw materials, and organic alkali is used as a catalyst and an acid-binding agent to prepare the perchloromethyl mercaptan. The method has the advantages of simple operation, strong operability, avoidance of the use of carbon disulfide and chlorine, effective solving of potential safety hazards caused by the use of carbon disulfide and chlorine and high safety; and the obtained perchloromethyl mercaptan appears to be yellow oilyliquid, has yield of 85% or above and density of 1.69 or above, meets use requirements, and presents industrial application value.

The invention relates to a thiodicarb synthesis method with high methomyl conversion rate. The method comprises the following steps: adopting xylene and toluene as solvents; reaction: when the temperature in the synthesis kettle is reduced to be lower than 0 DEG C, starting to dropwise add SCl2, after the SCl2 is dropwise added, adding methomyl into the synthesis kettle, introducing nitrogen into the kettle, heating, and reacting; after the reaction is finished, centrifuging to obtain centrifugate and a centrifugal filter cake; primary water washing and filter pressing; carrying out secondary washing and centrifugation; washing with methanol, and centrifuging; and carrying out vacuum drying on a filter cake obtained by centrifuging the methanol washing material to obtain a thiodicarb finished product. According to the synthesis method provided by the invention, when the intermediate thiobipyridine hydrochloride is synthesized, a toluene and xylene double-component solvent is adopted, pyridine is used as a raw material and a solvent, and the reasonable material ratio avoids the influence on the reaction process of pyridine and sulfur dichloride due to overhigh solid material concentration in a reaction system; the yield of the thiobipyridine hydrochloride and the conversion rate of methomyl in the subsequent reaction between the thiobipyridine hydrochloride and methomyl are improved.