60 results about "Sulfur monochloride" patented technology

This invention relates to a method for separating and purifying mixing exhaust gas of chlorine and hydrochloride, comprising: absorb the chlorine in the mixing exhaust gas using solvent A to separate from gas phase hydrochloride, the chlorine can be obtained after solvent A desorption, the hydrochloride can be obtained by removing solvent A in the gas phage hydrochloride using solvent B, wherein: solvent A is one of benzene, silicon tetrachloride, nonyl hydride, sulfur monochloride, carbon tetrachloride and chlorosulfonic acid, and solvent B is one of cyclopentadiene and hexachlorobutadiene. By washing with concentrated hydrochloric acid to remove trace amount of organic compounds, and chemical washing to remove heavy metal elements, the hydrochloride is absorbed by water to make hydrochloric acid. This invention is characterized of efficient separation of chlorine and hydrochloride, high efficiency of separation, low cost, high-usage of resources, high purity of chlorine up to 99%, recycling use, and the purity of hydrochloride meets the requirement of producing industrial hydrochloride and hydrochloride regent .

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 discloses a method for rectifying thionyl chloride. A two-stage continuous rectification process is adopted. The method comprises the following steps of: continuously feeding a crude product of the thionyl chloride into a first-stage rectification column, continuously extracting sulfur monochloride from a column bottom of the first-stage rectification column, and continuously extracting a semifinished product of the thionyl chloride from a lateral line; and continuously feeding the semifinished product of the thionyl chloride into a second-stage rectification column, continuously extracting a finished product of the thionyl chloride on a column top of the second-stage rectification column, and feeding a mixture on a column bottom into the first-stage rectification column. Overcuring devices are arranged between the first-stage rectification column and a condenser connected therewith and between the second-stage rectification column and a condenser connected therewith. The rectification method can realize continuous large-scale production, can maintain the relatively stable yield and quality of products and has high energy utilization rate, high degree of automation and easy control of operation. Compared with the conventional discontinuous rectification, the method for rectifying the thionyl chloride has the advantages of remarkable improvement of the production capability of a single device, large-scale production, guarantee of production safety, reduction of production cost, and good economic benefit.

The invention relates to a pressure-relief discharge, absorption, treatment and recycling method in production process of thionyl chloride. During the synthesis process of thionyl chloride, due to the specificity of reaction process, the unbalanced reaction of single-phase gas excessive sulfoxide is inevitably generated to cause the pressure increase situations of the system. The method comprises the following steps: (1) accelerating the gas flow by properly discharging condensed non-condensable gas to a sulfur monochloride tank; (2) absorbing chlorine gas in the gas discharged into the tank by use of sulfur monochloride, and then vulcanizing to leave sulfur dioxide gas and tiny inert gas; (3) quantitatively discharging inert gas in the sulfur monochloride tank into tail gas and carrying out absorption treatment so as to prevent excessive inert gas from causing the pressure increase of the system; (4) delivering the remaining sulfur dioxide gas to a buffer tank and metering so as to flow in the system for recycling, so that the synthesis reaction can return to a steady state. By virtue of the method, the purposes of improving the safety and high-efficiency production of a synthesis device can be achieved.

A process for preparing 3-alkylthiophenium includes such steps as addition reaction between 2-alkyl-1,3-butadiene and sulfur monochloride under action of catalyst, and high-temp condensation-ring forming reaction.

The invention provides a green synthesis technology of O,O-diethyl thiophosphoryl chloride and relates to the field of chemical synthesis. The green synthesis technology comprises the following steps:taking O,O-diethyl dithiophosphate to react with chlorine gas at low temperature, so as to obtain a crude product of the O,O-diethyl thiophosphoryl chloride; then transferring the crude product to react at high temperature; enabling the residual O,O-diethyl dithiophosphate to further completely react with the chlorine gas. Meanwhile, in a high-temperature reaction process, a polymeric compound isprevented from being generated when a compound catalyst is used and sulfur monochloride impurities are completely removed through reaction, so that a byproduct sulfur has a crystalline state and a product more easily separated and purified. Moreover, HCl and sulfur-containing odorous gas are pumped away through applying negative pressure and the tail gas is absorbed to prevent air pollution. In awhole reaction process, technological water does not need to be added, so that wastewater is not generated and the treatment cost of sulfur-containing and phosphorus-containing wastewater is reduced.The technology has the advantages of simplicity in operation, easiness for obtaining raw materials, moderate reaction conditions, small pollution and environment friendliness.

A disclosed antiwear rubber sole is prepared from the following raw materials in parts by weight: 10-20 parts of natural rubber, 6-12 parts of styrene-butadiene rubber, 5-10 parts of sulfur monochloride, 2-8 parts of trichlorofluoromethane, 8-16 parts of white carbon black, 6-13 parts of white oil, 8-12 parts of zinc carbonate, 6-12 parts of diantimony trioxide, 5-10 parts of salicylic acid, 5-10 parts of stearic acid, 3-7 parts of sulphur, 4-8 parts of an anti-ageing agent, 7-11 parts of high styrene, 4-8 parts of magnesium oxide, 7-14 parts of ethylene-vinylacetate copolymer, 8-14 parts of magnesium oxide, 4-8 parts of nanometer zinc oxide, and 3-6 parts of solid cumarone. The provided antiwear rubber sole is excellent in wet slippery resistance, fracture resistance and cold resistance, extremely good in oil resistance, relatively good in heat resistance and strong in adhesive force.

Provided is a preparation method of dialkoxyl xanthate polysulfide. The preparation method comprises the steps that fatty alcohol, carbon disulfide and powdered sodium hydroxide synthesize sodium dimethyldithiocarbamate in an organic solvent, sulfur chloride (sulfur monochloride or sulfur dichloride) is dropwise added, and the dialkoxyl xanthate polysulfide is obtained through a reaction; after the reaction is completed, pumping filtration is conducted to separate out inorganic salt sodium chloride, inorganic salt sodium chloride is subjected to simple treatment to serve as a by-product for sale, liquid is subjected to rotary distillation separation to obtain the product, and the distilled organic solvent can be recycled. The preparation method is short in process, the product yield and quality are stable, and the production efficiency is high. The recovery technology of inorganic salt sodium chloride is simple, no other inorganic salt impurity is contained, the purity is high, and recycling is promoted.

The invention discloses a synthetic method of 1,1'-dicaprolactam disulfide. Caprolactam is used as an initiator, and sulfur monochloride and caprolactam inorganic salt are used as raw materials. Sulfur monochloride firstly reacts with caprolactam to form 1,1'-dicaprolactam disulfide and acid; caprolactam inorganic salt is continuously converted to caprolactam under the action of the acid formed bythe reaction; and caprolactam continuously reacts with sulfur monochloride to form 1,1'-dicaprolactam disulfide. According to the method, there is no need to add other types of acid-binding agents, and the raw material caprolactam can be synthesized by itself in the reaction process. The production technology is simple, has strong operationality and simple post-treatment, and has industrial application value. The product is white solid powder in the appearance, and the yield is 88% and above, the purity is 99% and above. The product meets the use requirements.

The present invention provides a reclaimed rubber activator sulfo synthetic method, and relates to reclaimed rubber additive production technical field, the reclaimed rubber activator sulfo synthetic method comprises the following steps: antioxidant mother liquor is melted, the melted antioxidant mother liquor is pumped into a reactor, each reactor is fed with 2.8 tons of the material; the antioxidant mother liquor is heated to 120 DEG C, and stirred and dewatered for 40 minutes, and the temperature is dropped to 80 DEG C; under stirring conditions, a certain quantity of sulfur monochloride is dropwise added, the temperature gradually rises to 140 to 145 DEG C for high temperature synthesis; after the material is fed, the material is stirred for 30 minutes, the reactor is heated to 120 DEG C, after 2 hours of thermal insulation, the reactor is heated to 140 DEG C, after 2 hours of thermal insulation, the material in the reactor is transferred into a finished product packaging kettle, and stirred and cooled to 85 DEG C, and the material is packed to obtain a finished product. The reclaimed rubber activator sulfo synthetic method has the advantages of simple process and easy control of the process conditions, and the synthesized reclaimed rubber activator has the characteristics of no smell, less dosage and good effect, and compared with the activator synthesized by a conventional method, the dosage can be reduced by more than 50%.

The invention discloses a preparation method for sulfur-containing carbofuran derivative with less than 0.1% of harmful impurity carbofuran. The preparation method comprises the following steps of: using di-n-butylamine or N-isopropyl-beta-alanine ethyl ester derivative and sulfur monochloride as raw materials to prepare into disulphide in the presence of an acid-binding agent triethylamine and an organic solvent 1, 2-dichloroethane; and then reacting with a chlorinating agent sulfuryl chloride to obtain nitrogen sulfur chlorine; and finally reacting with carbofuran under the effect of a cosolvent N-methyl-2-pyrrolidone or dimethylformamide so as to obtain the sulfur-containing carbofuran derivative with not less than 96% of quality percentage composition and less than 0.1% of main harmful impurity carbofuran. By adopting the preparation method, the problem that the carbofuran cannot be completely reacted during being reacted can be solved, the defects due to low content and low yield of sulfur-containing carbofuran derivatives such as benfuracarb and carbosulfan caused by a solid-liquid two-phase reaction can be avoided, the technical problem due to relatively high content of main harmful impurity carbofuran can be solved, and the content of the sulfur-containing carbofuran derivatives such as benfuracarb and carbosulfan can reach a value not less than 96%, and the yield is 97 to 98%, and the main harmful carbofuran in the product is less than or equal to 0.1%, so that the preparation method has a wide popularization and application prospect.

The present invention relates to a preparation method of chloropolyaniline, and is characterized by that the polyailine and sulfur monochloride are heated and returned under the action of lewis acid catalysis in the polar aprotic solvent so as to obtain the invented chloropolyaniline. Every 6 carbon atoms of the chloropolyaniline contain 2-3 chlorine atoms, and its yield rate is up to 93-97%, it can be used as precursor raw material of positive material of lithium secondary cell.

The invention discloses a method for synthesizing 4,4'-dithiodimorpholine. Sulfur monochloride and morpholine are used as raw materials, anhydrous trisodium phosphate is used as an acid binding agent,the sulfur monochloride and morpholine are reacted to produce 4,4'-dithiodimorpholine and hydrochloric acid, and the anhydrous trisodium phosphate can react with the hydrochloric acid generated in the reaction to avoid the hydrochloric acid with from reacting morpholine and the morpholine from losing the reactivity. The acid binding agent anhydrous trisodium phosphate is added in the method of the invention, so the dosage of the raw material morpholine is reduced, and the production cost is saved; and the product and impurities can be separated by washing with water after the reaction is finished, so the method has the advantages of simple production, high operability, simplicity in post-treatment and industrial application values. The appearance of the obtained product is a white needlecrystal, the yield is 90% or above, the purity is 98% or above, and use requirements are met.

The invention discloses a synthesis method of bis(di-n-butylamine) disulfide. The synthesis method comprises the following steps: (1) respectively introducing an organic solution of di-n-butylamine and an organic solution of sulfur monochloride into a first reactor containing a reaction channel, mixing to initiate a reaction, and carrying out a partial reaction in the reaction channel of the firstreactor to obtain a reaction mixed solution; and (2) continuously introducing the reaction mixed solution into a second reactor containing a reaction channel, introducing a sodium hydroxide solutioninto the second reactor, and fully reacting to obtain bis(di-n-butylamine) disulfide. The continuous synthesis method improves the yield of bis(di-n-butylamine) disulfide, reduces the generation of byproducts, reduces the feeding amount of sulfur monochloride and sodium hydroxide, can greatly slow down the reaction heat release speed, and has the advantages of simple process flow, high productionefficiency, low cost, high safety and the like.

The invention relates to a synthesizing method for fipronil intermediates. The synthesizing method for the fipronil intermediates effectively solves problems of low production yield in preparation of the fipronil intermediates, complicated operation, low purity and difficulty in industrialized production. The method includes steps of adding 5-amino-3-cyano-1-(2, 6-dichloro-4-trifluoromethyl phenyl) pyrazole into a polar solvent at first and blending the 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethyl phenyl) pyrazole evenly, heating the 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethyl phenyl) pyrazole to 30-70 DEG C under 0.3-0.6 atmosphere, distilling one sixth of the polar solvent, and then cooling the 5-amino-3-cyano-1-(2, 6-dichloro-4-trifluoromethyl phenyl) pyrazole to 20 DEG C, quickly adding sulfur monochloride to react for half an hour under the conditions of 35-40 DEG C and negative pressure of -0.095--0.01MPa, obtaining a mixture which is standing for half an hour under the conditions of 35-50 DEG C and one atmosphere so as to remove hydrogen chloride, adding an amine regulator to regulate a PH value as 7, cooling the mixture to </=5 DEG C, filtering to obtain a filtered object which is washed by water, and drying to obtain 5-amino-1-(2,6-dichloro-4-trifluoromethyl phenyl)-3-cyano pyrazole-4-base double sulfur. The synthesizing method for the fipronil intermediates is prepared by simple process and operated under mild reaction conditions, high in production yield and purity, low in production cost, easy to produce in an industrialized manner and capable of serving as the intermediate to effectively prepare fipronil.

The invention discloses an insulating resin having a good electromagnetic shielding effect. The insulating resin consists of the following components in parts by weight: 8 parts of polysiloxane, 0.5 part of sulfur monochloride, 4 parts of chlorosulfonic acid, 7 parts of diphenol propane, 3 parts of aluminium trichloride, 6 parts of chlorobenzene, 2 parts of polyamide-imide, 1 part of tributyl citrate, 1 part of glass fibers, 43 parts of an anhydride curing agent and 1 part of a latent accelerator. The insulating resin provided by the invention has low costs, has a good electromagnetic shielding effect and good properties.

The invention provides a synthetic process for a sulfurized calcium alkyl phenolate clearing agent. The synthetic process comprises the following steps: adding dodecylphenol into a three-neck bottle with a stirring function, mounting a condenser tube and an absorption bottle and adding sulfur monochloride into the three-neck bottle for sulfuration so as to obtain sulfurized alkyl phenate; pouring sulfurized alkyl phenate into a neutralization kettle, adding base oil and an aqueous solution of calcium chloride and adding calcium oxide for a neutralization reaction; after completion of neutralization, adding the solvent glycol, stearic acid and calcium oxide, introducing CO2 and carrying out carbonation once; after completion of carbonation, adding calcium oxide into the neutralization kettle, introducing CO2 and continuing carbonation twice to three times; and carrying out pressure-reduced distillation and filtering so as to obtain the product sulfurized calcium alkyl phenolate. The synthetic process has the advantages that the process is simple and rational, can prevent the unsafe factor of spontaneous combustion of sulfur dust at high temperature and the accident of hydrogen sulfide poisoning caused by leakage of hydrogen sulfide, overcomes the problem of emission of exhaust gas and waste water in the process of sulfuration of alkylphenol, and enables by-products to be recycled.

The invention provides sulfurized erucic acid as well as a preparation method and application thereof. Sulfurized erucic acid has a chemical structure formula as shown in the specification and is prepared by performing low-temperature sulfurization reaction on sulfur monochloride and erucic acid in the presence of protection gas. Sulfurized erucic acid provided by the invention is light in color and excellent in anti-wear and anti-friction performances, and has excellent oil solubility in whether protection synthetic oil of base oil I or protection synthetic oil of base oil II or above.

The invention relates to a method for optimizing a production process of thionyl chloride and belongs to the technical field of chemical engineering. Liquid sulfur in a liquid sulfur tank is metered by a metering pump and then pumped into an atomizing device in a distillation column; a crude thionyl chloride product is mixed with the liquid sulfur at the top of the distillation column; sulfur dichloride in the crude thionyl chloride product and the liquid sulfur are subjected to a reaction, a heavy component, namely, sulfur monochloride, is produced and withdrawn from the bottom of the distillation column, remaining crude thionyl chloride product is condensed by a condenser and enters a return tank, a part of liquid phase in the return tank is pumped into the distillation column by a reflux pump to be recycled, and the remaining liquid-phase material is recovered from the return tank. By means of the method, automatic sulfur addition is realized, time and labor cost are saved, and thedecoloration effect is better.