56 results about "Sulfur tetrafluoride" patented technology

Continuous production of sulfur tetrafluoride is carried out by synthetic reacting, cooling to separate SF4 from halogen, returning and reutilizing halogen, gas-phase purifying, liquefying and filling. The halogen fluoride has synthetic reaction with pure industrial brim stone proportionally in a reactor, with reacting temperature of 110deg.C-500deg.C, reacting pressure 0.1-1.0MPs, the mole ratio of halogen fluoride to S = 4-5:5 and the excess of the halogen fluoride = 0-25%. It achieves low cost, simple process and higher efficiency.

Novel methods for preparing arylsulfur pentafluorides are disclosed. Arylsulfur halotetrafluoride is reacted with a fluoride source under hydrous conditions to form an arylsulfur pentafluoride. The purification method is also disclosed.

The invention discloses a method for synthesizing trifluoromethyl amine. The method comprises the following steps of: mixing amino acid, anhydrous hydrofluoric acid and sulfur tetrafluoride in a molar ratio of 1:(3-20):(1.8-3.2), and reacting at temperature of between 50 and 150 DEG C for 2 to 10 hours; and cooling, neutralizing, extracting and rectifying to obtain a trifluoromethyl amine product. According to the method, a process is short; and the product is easy to separate, high in yield and stable in quality, the highest yield is 88 percent, and the content of the product is over 97.5 percent.

The invention relates to a sulfur tetrafluoride production technique, belonging to the field of fluorochemicals. The sulfur tetrafluoride production technique comprises fluorine gas purification, iodine pentafluoride preparation, sulfur tetrafluoride reactive synthesis, sulfur tetrafluoride separation and trapping, sulfur tetrafluoride distillation and canning, secondary recycling of iodine pentafluoride as well as discharge of exhaust gas. By using a low-temeprature condensing device, the electrolytic fluorine is purified to remove a great amount of hydrogen fluoride, so the fluorine gas concentration is largely improved. A condensing and recycling device is employed to recycle iodine and iodine pentafluoride for re-use, thus the utilization ratio of iodine can reach above 70% and material losses can be reduced. Due to a constant distillation method, the purity of sulfur tetrafluoride products can reach above 99.9%, and the products can be charged into a steel cylinder more safely. In addition, the entire sulfur tetrafluoride production technique is controlled by a automatic DCS (distributed control system) device, which reduces artificial randomness and experience and improves the stability of product quality.

The invention relates to the field of medical chemistry and discloses a method for synthesizing a pyridine medical intermediate, namely 2-bromo-3-chloro-5-trifluoromethyl pyridine, for synthesizing anti-cancer auxiliary medicines. The method comprises the following steps of: (1) reacting 6-hydroxynicotinic acid, hydrofluoric acid and sulfur tetrafluoride at the temperature of between 100 and 120DEG C and under the pressure of 0.1-0.3MPa, and adding water to obtain 2-hydroxy-5-trifluoromethyl pyridine; (2) reacting with N-chlorosuccinimide, and performing water precipitation to obtain 3-chloro-5-trifluoromethyl-2-hydroxypyridine; and (3) adding excessive phosphorus oxybromide, reacting at the temperature of between 145 and 160DEG C for 5 to 8 hours, cooling, violently stirring at the temperature of between -5 and 0DEG C, extracting, combining organic phases, drying, filtering, performing spin drying, and purifying by using a silica gel column. According to the method, raw materials are readily available, the cost is low, the method is suitable for industrial production and the yield exceeds 38 percent.

Disclosed is a method for an energy-efficient improvement in the production of sulfur hexafluoride, and eliminates the generation of other byproducts. The process is an oxidative fluorination of sulfur tetrafluoride by CoF3 / F2, where CoF3 is solid stationary phase that can be regenerated.

Disclosed is a method for an energy-efficient improvement in the production of sulfur hexafluoride, and eliminates the generation of other byproducts. The process is an oxidative fluorination of sulfur tetrafluoride by CoF3 / F2, where CoF3 is solid stationary phase that can be regenerated.

The invention discloses a quinone-catalyzed trifluoromethylation photocatalytic synthesis method. According to the method, the using problem of highly-corrosive and highly-toxic fluorinating reagents such as hydrogen fluoride and sulfur tetrafluoride in an existing industrial trifluoromethylation reaction is solved, the heavy metal pollution problem of a catalyst in industry is avoided, and the good actual application prospect is achieved. The metal-free photocatalytic trifluoromethylation reaction is achieved by taking simplest and cheapest benzoquinone and derivatives thereof as a photocatalyst and taking a Langlois reagent-sodium trifluoromethanesulfinate (CF3SO2Na) as a trifluoromethyl source under the mild visible light condition, and a complete full-cycle reaction is achieved through a homemade fixed bed reactor. Trifluoromethyl modification can be further performed on organic molecules with the bioactivity and the pharmaceutical activity according to the actual needs. The method has the advantages that the synthesis condition is mild, the raw materials are cheap and easy to obtain, the environmental pollution is low, large-scale industrial production is facilitated, and the significant economic and social benefit is achieved.

The invention relates to a preparation method of carbonyl fluoride and belongs to the fluorine chemical field and the field of electronic industrial gas. The preparation method is used for preparing carbonyl fluoride through the reaction of carbon monoxide and fluorine-containing substance, wherein the fluorine-containing substance is at least one of carbon tetrafluoride, boron trifluoride, nitrogen trifluoride, sulfur tetrafluoride, sulfur hexafluoride, phosphorus trifluoride, phosphorus pentafluoride, sulfuryl fluoride or hexafluoroethane; the favourable conditions including temperature, pressure, a proportion of fluorine-containing substance to carbon monoxide and gas supply flow rate of the fluorine-containing substance are selected; dilution medium is further added in the method for diluting or carrying out catalytic reaction by virtue of catalyst. The preparation method of the carbonyl fluoride is free of fluorine gas, capable of lowering the corrosion to a reactor, reaction heat, reaction intensity, potential explosive risk and yield drop caused by side reaction, and capable of safely, economically and effectively preparing the carbonyl fluoride. The invention further provides dilution medium which is used in the preparation of the carbonyl fluoride through the reaction of carbon monoxide and fluorine gas.

The invention discloses a polyurethane elastomer based on sulfur tetrafluoride modification, and a preparation method thereof. The polyurethane elastomer is prepared from the following ingredients at a weight part ratio: 21-43 parts of polyurethane, 16-39 parts of acrylic ester, 12-26 parts of isocyanate, 12-25 parts of hexafluorobutyl acrylate, 7-18 parts of sulfur tetrafluoride, 4-11 parts of hexafluoride propyl alcohol, 7-18 parts of silicon carbide, 6-14 parts of magnesium oxide, 7-18 parts of montmorillonite and 5-12 parts of talcum powder. The polyurethane elastomer has the following advantages: (1) the fluorine content of the polyurethane elastomer based on the sulfur tetrafluoride modification is increased, a contact angle with water is increased, and surface tension is lowered; (2) the thermostability of the polyurethane elastomer disclosed by the invention is improved, and the polyurethane elastomer exhibits excellent water-resistance and solvent-resistance performance; and (3) the polyurethane elastomer keeps good hardness, breaking strength, elongation, storage modulus and surface performance.

The invention relates to automatic control of a sulfur tetrafluoride production process, comprising the automatic control of sulfur tetrafluoride synthesis reaction, the automatic control of sulfur tetrafluoride cooling, separating and capturing, the automatic control of iodine pentafluoride preparation, the automatic control of fluoride preparation and purification, the automatic control of rectification and purification and the automatic control of recycling. The invention ensures the stability of the quality of the sulfur tetrafluoride product by adopting measures of system process control analysis, product mass spectrum analysis and chemical analysis and also ensures the continuous and stable running of production; the production process for synthesizing sulfur tetrafluoride adopts DCS (Distributed Control System) automation device control in the whole course, reduces artificial randomness and experience, improves the stability of the product quality as well as the purity, the yield and the production efficiency of the product and reduces the raw material waste and the production cost.

The invention discloses a method for producing 4,4-difluoro cyclohexyl formic ether by using counter cyclohexanone formic ether through fluorination, which belongs to the technical field of chemical industry. The method comprises the steps of (1) respectively putting the counter cyclohexanone formic ether, sulfur tetrafluoride and hydrogen fluoride in a pressure kettle, starting blending, enabling the reaction temperature in the pressure kettle to be controlled at 0-80 DEG C, and enabling response time to be 0.5-24.0h; (2) opening an outlet valve of the pressure kettle, enabling surplus gas to be led in alkali liquid, and enabling the gas to be absorbed by the alkali liquid; (3) opening the pressure kettle, enabling reaction liquid to be poured in ice water, starting blending simultaneously, stewing and layering after completing pouring to separate an oil layer; and (4) adjusting the separated oil layer to be neutral by using the alkali liquid, stewing to remove a water layer, adding a desiccating agent to the oil layer, and filtering the desiccating agent to obtain the 4,4-difluoro cyclohexyl formic ether. The method synthesizes target products through a one-step reaction, and is simple in reaction, few in steps, few in secondary products, apt to obtain products with high purity through distillation, high in total recovery, good in safety and favorable for scale production.

The invention relates to a material recycling technique used during sulfur tetrafluoride production. Firstly, the coarse sulfur tetrafluoride gas is produced through reactive synthesis of iodine pentafluoride and sulfur in a sulfur tetrafluoride reactor and then raw materials are initially recycled through condensation, separation and trapping. The impure gases obtained by gas pahse purification during condensation, separation and trapping of sulfur tetrafluoride are evacuated and recovered again through a secondary condensation recovery device. The condensation recovery devices in the initial and secondary stages are utilized to recycle iodine and iodine pentafluoride, which can increase the utilization rate of iodine by more than 70%. The technique can not only reduce material losses and lower production cost but also cut down the volumes to be purified.

Fluorinated pentacene derivatives, for example, the novel compounds tetradecafluoropentacene, 5,6,7,12,13,14-hexafluoropentacene, 5,7,12,14-tetrafluoropentacene, and 6,13-difluoropentacene, and intermediates therefor are provided. And a method of producing fluorinated pentacene derivatives and intermediates therefor is also provided. Pentacene derivatives fluorinated at desired positions of the pentacene skeleton are obtained by introducing the oxo group, hydroxyl group, or alkoxyl group into the pentacene skeleton followed by fluorination with sulfur tetrafluoride and partial defluorination using a reducing agent.

The invention discloses a purification and rectification process of sulfur tetrafluoride. The preparation process of sulfur hexafluoride is controlled through inductance elements. The process is carried out by using the following devices: a weighing device, a containing box, a quantitative valve, a sulfur tetrafluoride reactor, a stirrer, temperature sensors, a pressure sensor, an air pump, a cooler, a condensation catcher and a rectification tower. The process comprises the following operation steps: proportioning raw materials, preparing sulfur tetrafluoride, cooling crude gas, purifying thecrude gas and rectifying sulfur tetrafluoride. According to the invention, the condensation temperatures of the temperature control cooler and the condensation catcher are measured by the temperaturesensors, so that preparation of the sulfur tetrafluoride product is facilitated; and pressure in the sulfur tetrafluoride reactor is measured through the pressure sensor, so that scientific export ofthe crude gas is facilitated. The electric appliance elements used in the process do not need manual operation, the effect of full-automatic operation is achieved, the error of preparing the sulfur tetrafluoride product is reduced, purification precision is improved, and the purification precision is improved by 37% compared with purification precision of manual operation.

The invention discloses a preparation process for improving the whiteness of kaolin, and relates to the field of removing iron from ore. The preparation process for improving the whiteness of kaolin is characterized by comprising the following steps that 1, mining and impurity removing are conducted, wherein kaolin ore is excavated, clay and impurities are initially separated out, and a base material is obtained; 2, pulping and sand removing are conducted, wherein the base material is subjected to pulping and sand removing, and an ore pulp initial material is obtained; 3, hydrochloric acid isintroduced into the ore pulp initial material, and dissolved iron ore pulp is obtained; 4, hydrogen peroxide is introduced into the dissolved iron ore pulp, and iron ion ore pulp is obtained; 5, anhydrous hydrofluoric acid is introduced into the iron ion ore pulp, and iron fluoride ore pulp is obtained; 6, a sulfur tetrafluoride solution is introduced into the iron fluoride ore pulp, and iron hexafluoride ion ore pulp is obtained; 7, a sodium chloride solution is introduced into the iron hexafluoride ion ore pulp, and after uniform mixing, the mixture is introduced into a filter press for pressure filtration. The preparation process has the advantages of improving the whiteness of the kaolin and expanding the application field of the kaolin.

The invention discloses a perfluoroalkyl styrene monomer and application thereof. The perfluoroalkyl styrene monomer is prepared by the following steps of using monohalogenated thiophenol and perfluoro-iodoalkane as the raw materials, so as to obtain an intermediate, namely perfluoroalkyl thiohalobenzene; further fluorinating, so as to obtain perfluoroalkyl tetrafluorothio methylene halobenzene; finally, reacting with vinyl magnesium bromide, so as to obtain perfluoroalkyl tetrafluorothio methylene styrene. The prepared tetrafluorothio methylene-containing perfluoroalkyl styrene has the advantages that the reaction property is realized, and the tetrafluorothio methylene-containing perfluoroalkyl styrene can be used for preparing fluorine-containing surface treatment materials and liquid-repelling surfaces; because the perfluoroalkyl is bonded with rigid benzene rings, the whole structure of the fluorine-compound has larger crystallizing property, and the excellent liquid-repelling property is obtained; the tetrafluorothio methylene is used as a bridge group, and is directly bonded with the benzene ring, and the good heat-resistant stability is provided by the electron stable reaction of large phi bond of the benzene ring corresponding to the sulfur tetrafluoride; the tetrafluorothio methylene-containing perfluoroalkyl styrene is easy to degrade under the radiation by ultraviolet light, and the obtained fluorine-containing material is environment-friendly.

The invention relates to the technical field of analyzers, in particular to a sulfur tetrafluoride analyzer comprising a gas chromatograph, a feed tube, a micro sample injection needle, a positioningmechanism, a lifting mechanism and a push block. The feed tube is fixedly communicated with the top of the gas chromatograph. The micro sample injection needle arranged above the feed tube is fixedlyconnected with the push block and is connected to the positioning mechanism; and the positioning mechanism is fixedly connected to the lifting mechanism fixedly connected to the top of the gas chromatograph. According to the invention, the positioning mechanism clamps and locates the push block at the micro sample injection needle rapidly and the lifting mechanism lifts the micro sample injectionneedle stably, so that the micro sample injection needle can be inserted into the feed tube conveniently. The lifting is stable; and the collision damage, caused by shaking, of the micro sample injection needle is avoided. The long-time manual holding is avoided; and the sulfur tetrafluoride product is detected conveniently.

The invention provides a method for synthesizing 2-chloro-5-(trifluoromethyl)pyrazine by using 5-chloro-pyrazine-2-carboxylic acid, anhydrous hydrogen fluoride and sulfur tetrafluoride. The method forsynthesizing 2-chloro-5-(trifluoromethyl)pyrazine has the advantages of simple technology, easily available raw materials, and high yield.

Provided is an inexpensive and industrially advantageous method for preparing (3R,4S)-3-(N-substituted aminomethyl)-4-fluoropyrrolidine or an enantiomer thereof which can be an intermediate for producing pharmaceuticals. It relates to a method for preparing (3R,4S)-3-(N-substituted cyclopropylaminomethyl)-4-fluoropyrrolidine derivative or ait's enantiomer, or their salts, comprising a step of fluorinating a 4-hydroxy-3-(N-substituted aminomethyl)pyrrolidine derivative represented by the general formula (1) or an enantiomer thereof using a sulfur tetrafluoride derivative. [In the formula (1), PG represents a protective group for the amino group, and R1 represents a C1 to C6 alkyl group which may be substituted, or a C3 to C8 cycloalkyl group which may be substituted].

The invention discloses a method for converting benzene into benzotrifluoride through heterogeneous catalysis. Benzene is catalyzed to generate benzotrifluoride at lower temperature and normal pressure with manganese sulfate monohydrate as a catalyst, sodium trifluoromethanesulfinate as a trifluoromethyl source and acetonitrile as solvent. The raw materials are low in price and easy to obtain, conditions are mild, environment pollution is low, products are easy to separate, hydrogen fluoride, sulfur tetrafluoride and other highly-corrosive and highly-toxic fluorinated reagents used in current industrial trifluoromethylation reactions are avoided, large-scale industrial production is facilitated, and the method can be further used for trifluoromethyl modification of organic compounds with biological activity and medicine activity and has good application prospects and economic benefits.

The invention discloses sulfur-containing long-heterochain perfluoroalkyl acrylate and a preparation method thereof. Nonafluorobutyl halogenated sulfur tetrafluoride serves as an end-capping reagent, and after tetrafluoroethylene is subjected to telomerization, 1H,1H,2H,2H-7-perfluoroundecanoic sulfide-1-halogen is prepared from obtained 5-perfluor nonyl sulfide-1-halogen and ethylene gas through single-electron addition reaction; the product and silver olefine acid have esterification reaction to obtain 1H,1H,2H,2H-perfluoroundecanoic acrylate sulfide. The prepared sulfur-containing long-heterochain perfluoroalkyl acrylate contains carbon-carbon double bonds for easy free radical polymerization, and can be used for preparing fluorine-containing polymer and copolymer. Long-heterochain perfluoroalkyl has crystallinity, so that when the prepared fluorine-containing polymer makes contact with liquid, no surface reconstruction phenomenon exists, and excellent liquid repellency. Meanwhile, perfluoroalkyl long heterochain has carbon-sulfur heterodesmic structures, is easy to degrade, does not have accumulative toxicity and does not belong to the sulfur-containing chemical inhibition range.

The invention discloses a raw material recovery technology in sulfur tetrafluoride production, and relates to the technical field of production of fluorine chemical products. The raw material recoverytechnology in the sulfur tetrafluoride production comprises following steps: protective measures before preparation of sulfur tetrafluoride, preparation work of sulfur tetrafluoride, pre-preparationof sulfur tetrafluoride, preparation of sulfur tetrafluoride, standby work after product preparation, primary fractional distillation of sulfur tetrafluoride, secondary fractional distillation of sulfur tetrafluoride, capturing of sulfur tetrafluoride, tail gas treatment of product preparation, recovery of product raw materials and detection of product raw materials. According to the technology, sulfur tetrafluoride is subjected to fractional distillation two times firstly, crude sulfur tetrafluoride can be effectively changed into primary sulfur tetrafluoride, needless impurities are removedby one step, then impurities in tail gas can be effectively removed, a processing instrument is effectively cleaned, so that degree of purification of sulfur tetrafluoride by the instrument is increased, and the raw material recovery rate of sulfur tetrafluoride is further increased.

The invention provides a sulfur tetrafluoride synthesis method and a reaction system, and relates to the technical field of chemical engineering. The sulfur tetrafluoride synthesis method comprises the following steps: fluorine gas and liquid sulfur are subjected to a gas-liquid reaction to generate sulfur tetrafluoride, the reaction pressure is 90-120KPa, and the distance between an outlet of the fluorine gas and the liquid level of the liquid sulfur during the reaction is 3-10mm. The method has the advantages that by controlling the reaction temperature, the reaction pressure and the gas-liquid distance, high-quality, stable and high-yield sulfur tetrafluoride can be realized, and the benefit maximization is realized.

The invention relates to a process for purifying and rectifying sulfur tetrafluoride, which comprises the following steps of: reacting iodine pentafluoride and sulfur in a sulfur tetrafluoride reactor to synthesize crude sulfur tetrafluoride gas, obtaining a liquid primary sulfur tetrafluoride product with purity of more than or equal to 95 percent through a cooler, a condensation separator and acondensation trap, obtaining a liquid sulfur tetrafluoride product with purity of more than or equal to 99.9 percent by a rectifying process, and continuously charging the product into a steel bottle. The liquid sulfur tetrafluoride product is directly trapped and produced and continuously liquefied and bottled, so damage of low-temperature bottling to the steel bottle is avoided, and the safety is higher. The purity of the sulfur tetrafluoride product is greatly improved by the cooling, separation, trapping and continuous rectification technology adopted in the process.

The invention discloses a technology of producing sulfur hexafluoride by adopting a sulfur tetrafluoride oxidation method. The technology comprises the following steps of: firstly, reacting cupric fluoride, silver fluoride or mercuric fluoride or mixture of the cupric fluoride, the silver fluoride or the mercuric fluoride with molten sulfur to obtain sulfur tetrafluoride and converting metal fluoride into sulphide; secondly, oxidizing the sulfur tetrafluoride with oxygen or air at about 500DEG C to obtain the sulfur hexafluoride and a byproduct of sulfur dioxide; and finally, reacting the metal fluoride fluorine hydride in the presence of oxygen and converting the mixture into fluoride for recycling; and absorbing the byproduct of sulfur dioxide by using a sodium hydroxide solution and converting the mixed solution into sodium sulfite for recycling. The process is reasonable, simple in production and is a most simple and convenient ideal technology for preparing the sulfur hexafluoride.

Provided is an inexpensive and industrially advantageous method for preparing (3R,4S)-3-(N-substituted aminomethyl)-4-fluoropyrrolidine or an enantiomer thereof which can be an intermediate for producing pharmaceuticals. It relates to a method for preparing (3R,4S)-3-(N-substituted cyclopropylaminomethyl)-4-fluoropyrrolidine derivative or ait's enantiomer, or their salts, comprising a step of fluorinating a 4-hydroxy-3-(N-substituted aminomethyl)pyrrolidine derivative represented by the general formula (1) or an enantiomer thereof using a sulfur tetrafluoride derivative.[In the formula (1), PG represents a protective group for the amino group, and R1 represents a C1 to C6 alkyl group which may be substituted, or a C3 to C8 cycloalkyl group which may be substituted.]

The invention provides a method for synthesizing 2-chloro-5-(trifluoromethyl)pyrazine by using 5-chloro-pyrazine-2-carboxylic acid, anhydrous hydrogen fluoride and sulfur tetrafluoride. The method forsynthesizing 2-chloro-5-(trifluoromethyl)pyrazine has the advantages of simple technology, easily available raw materials, and high yield.

The invention relates to a sulfur tetrafluoride production technique, belonging to the field of fluorochemicals. The sulfur tetrafluoride production technique comprises fluorine gas purification, iodine pentafluoride preparation, sulfur tetrafluoride reactive synthesis, sulfur tetrafluoride separation and trapping, sulfur tetrafluoride distillation and canning, secondary recycling of iodine pentafluoride as well as discharge of exhaust gas. By using a low-temeprature condensing device, the electrolytic fluorine is purified to remove a great amount of hydrogen fluoride, so the fluorine gas concentration is largely improved. A condensing and recycling device is employed to recycle iodine and iodine pentafluoride for re-use, thus the utilization ratio of iodine can reach above 70% and material losses can be reduced. Due to a constant distillation method, the purity of sulfur tetrafluoride products can reach above 99.9%, and the products can be charged into a steel cylinder more safely. In addition, the entire sulfur tetrafluoride production technique is controlled by a automatic DCS (distributed control system) device, which reduces artificial randomness and experience and improves the stability of product quality.