The method of obtaining elemental sulfur
(57) Abstract:The method of obtaining elemental sulfur by restoring phosphogypsum (gypsum, calcium sulphate) gaseous mixture at an elevated temperature. The new method is the use of gaseous mixtures containing natural gas-methane and water vapour in the following ratio of components, about. % : methane 0,5 - 2,1, water vapor and 97.8 - 99,5, and the restoration is carried out at 950 - S within 30 - 60 minutes the Degree of extraction of sulfur is 57.3 - sampled at 74.25% . table 1. The invention relates to methods for sulfur.The known method  sulfur from gypsum by restoring its solid or gaseous reducing agent at 800-1000aboutFor 20-120 min with intermediate receiving calcium sulfide and carbon dioxide. The resulting sulfide is treated with water and hydrogen sulphide, and the product of this processing is mixed with soda ash, resulting in a gain precipitate of calcium carbonate and a solution of sodium hydrosulfide NaHS. This solution is then blown with carbon dioxide from the stage of recovery of gypsum, while receiving the precipitate of sodium bicarbonate NaHCO3and hydrogen sulfide (H2S, which is then transferred to sulfur using the Claus process ilocandia after recovery of sulfate calcium sulfide is treated with hydrogen chloride HCl at 650-690aboutWith, and released when the hydrogen sulfide is then converted to sulfur.The disadvantages of the above methods are the multi-stage: a) restoring the source of calcium sulfate to sulfide; b) obtaining sulphide of calcium sulfide; b) the processing of hydrogen sulfide (H2'sv sulfur; and bulkiness and complexity of the process (crushing, dissolving, filtering, large energy consumption, the presence in the exhaust gases of significant quantities of harmful HCl, SO2and H2S, which requires additional cleaning, use of hazardous to human health and causes corrosion of the equipment of the hydrogen chloride with the formation of ballast - chloride of calcium, which significantly increases the cost of production of sulfur.The aim of the invention is to simplify the technology by conducting the process in a single stage direct receipt of sulfur, and deeper disposal of phosphogypsum, reduced consumption of reagents.This goal is achieved by the fact that in the proposed method of obtaining sulfur by restoring phosphogypsum (gypsum, calcium sulphate) gaseous mixture at elevated temperature, according to the invention, use of a gaseous mixture containing natural gas-methane and water PA at 950-1050aboutC for 30-60 minComparative analysis of the proposed solutions with the prototype shows that the inventive method differs from the known fact that the composition of the gas recovery mixture includes water vapor.Using the proposed method allows to obtain sulfur in one stage, without intermediate obtain hydrogen sulfide, and the solid residue is simultaneously formed lime (calcium oxide), which can be immediately used in the building materials industry.The process of recovery of phosphogypsum (gypsum, calcium sulphate) indicated a mixture of features to make an educated result of the recovery process, the sulphide of calcium is immediately converted to steam. The temperature interval is chosen so as to achieve the desired degree of conversion of sulfate sulfur. The increase in temperature is undesirable due to excessive conversion of reducing methane steam and pyrolysis of CH4and the decrease in temperature will lead to incomplete recovery of calcium sulfate CaSO4. For these same reasons, it is recommended to use the mentioned interval, the duration of the process. Excess water p is p, as follows.For sulfur used phosphogypsum of Rozdolskaja FOR "Sulfur" (Lviv region) having the following composition, wt. % (calculated on dry substance): R2ABOUT51,0-1,25; F 0,25-0,35; SiO22,5-3,5; Al2O3the 0.05-0.1; Fe2O30,05-0,1; Na2O 0,15-0,2; organic matter < 0,01, CaSO494-96; p. p. p. 14,13.As the reductant phosphogypsum used natural gas containing about 97. % CH4.The experiment was as follows.A portion of phosphogypsum ( 2 g) was loaded into the boat and put her in a quartz reactor placed in an electric furnace COOL-0,25.1/12-M1. Included heat at a given temperature started feeding natural gas and water vapor. The consumption of natural gas for the recovery of phosphogypsum was calculated, assuming that the process described by the reaction equation:
CaSO4+ CH4= CaS + CO2+ 2H2O (1)
The flow of water vapor is 1.3-1.4 l/min At the end of the experience cut off supplies of gas mixture and cooled reactor. Then the solid residue after recovery of phosphogypsum were analyzed for the presence of sulfate sulfur in the chemical way (according to GOST 125-79). Exhaust gases caught in the process and analyzed iodometrically on the soda is sulfide, sulfite and sulfate sulfur after recovery of phosphogypsum.In this series of experiments was implemented a full factorial experiment with plan type 23. Varied temperature and duration of the recovery phosphogypsum and reductant consumption of natural gas is methane, respectively, in the range 950-1050aboutC, 30-60 min and 175-290% of the consumption of CH4from the stoichiometric required standards for the equation (1). The flow rate of water vapor was not changed. The results of the experiments presented in the table.The solid residue after recovery of phosphogypsum in addition to the chemical were subjected to x-ray phase analysis in the rays of copper Cukon the diffractometer DRON-3,0. The analysis showed that the residue contained along with the calcium sulfide (CaS line d/n - 2,85, 2,01, 1.64 and others ) also calcium hydroxide CA(Oh)2(line d/n - 2,62, 4,90, and others ) and calcium oxide Cao (line d/n - 2,40 and others ).Was extracted and analyzed condensed after the restoration of phosphogypsum elemental sulfur. X-ray phase analysis showed that it is orthorhombic its modification (line d/n - 3,85, 3,21, 3,43, and others ). Transcript of diffraction patterns was carried out with the help of the American x-ray file cabinets ASTM.
FIELD: transportation of sulfur.
SUBSTANCE: according to proposed method of transportation of elemental sulfur, elemental sulfur is mixed with anhydrous ammonia and/or sulfur dioxide to form fluid mixture which is then transported in container. Method of extraction of elemental sulfur from sulfur containing geological formation, mainly water-free, includes blowing through of geological formation with anhydrous ammonia, obtaining liquid solution of elemental sulfur dissolved in anhydrous ammonia and extraction of elemental sulfur from liquid solution. Method of extraction of elements sulfur from sulfur-containing mineral formation, mainly water-free, includes blowing through of mineral formation with liquid anhydrous ammonia with obtaining liquid solution of elemental sulfur in anhydrous ammonia and extraction of elemental sulfur from liquid solution. Method of storing elements sulfur includes mixing of elemental sulfur and liquid anhydrous ammonia with obtaining liquid solution or suspension and forming deposts from solution or suspension in underground formation, mainly water-free. Composition consisting mainly of solution or suspension is essentially mixture of elemental sulfur with liquid sulfur dioxide.
EFFECT: improved economic characteristics of industrial chemical processes which include presence of sulfur either in elemental or chemically boded form.
32 cl, 9 ex, 4 dwg
FIELD: mechanics; heating.
SUBSTANCE: heater element comprises a set of spacing-separated melting tubes that form a heating plane, the upper collector tube and the lower collector tube attached to the relevant ends of the melting tubes and communicating with them. The upper collector tube has an inlet for steam delivery and distribution within the melting tubes system. The lower collector tube has an outlet for condensate collection and discharge. In addition the heater element is equipped with a hot-tipped tube positioned beside and before the lower collector tube. The hot-tipped tube has a steam inlet and a condensate outlet and is intended for sulphur melting before the lower collector. The heater elements may be controllable and modular. The device for solid sulphur melting consists of a support tower for the heater element transportation, a fixture for at least partial support of the heater element in the vertical position, a fixture for the heater element transfer from the vertical position to a basically horizontal one on a transportation truck, a fixture for the melting device travel across the ground surface in the direction of solid sulphur storage location. The latter fixture comprises a hydraulic cylinder, a directional distributing valve and a variable volume pressure compensation pump. The heater element for melting cross band contaminated sulphur consists of a set of spacing-separated melting tubes confining the melting plane and individual melting tubes having steam inlets and condensate outlets with the specified set of melting tubes performing cross band contaminated sulphur melting whenever the device comes in contact with a bulk of sulphur containing a cross band.
EFFECT: simplified and relatively inexpensive fabrication technique; possibility of onsite sulphur melting.
31 cl, 28 dwg
FIELD: oil and gas industry.
SUBSTANCE: invention refers to methods of hydrogen sulphide withdrawal from liquid sulphur and is designed for implementation at enterprisers of oil and gas processing industry at production of elemental sulphur. Liquid sulphur is de-gassed by means of mixing liquid sulphur with a catalyst. As the catalyst air is used; also sulphur extracted from a process equipment is mixed with air in a flask containing ferromagnetic mixing elements; the flask is installed in a space of a stator with three-phase coil connected to a source of alternate current. Fragments of magnets of 3-5 mm fraction are used as ferromagnetic elements.
EFFECT: invention facilitates reducing time of de-gassing without reduction of quality.
2 cl, 1 tbl
SUBSTANCE: method for separation of the elemental sulphur and sulphide concentrate from the intermediate products of the sulphide concentrates hydrometallurgy processing includes sulphur-sulphide flotation of the intermediate original pulp in order to separate the sulphur and sulphides from intermediate oxide components with forming of the sulphur-sulphide concentrate. Then the autoclave disintegration of the sulphur-sulphide concentrate pulp is carried out in the presence of reagent - sulphide hydrophilisator and at the temperature higher than melting point of the elemental sulphur. After that the sulphur flotation is carried out in order to separate the disintegrated pulp into sulphur and sulphide concentrates. Before the sulphur-sulphide and sulphur flotations the pulp undergoes the additive agitation with the reagents, the disintegration is carried out at the temperature 140-150°C.
EFFECT: effective separation of the sulphur and sulphide concentrates.
5 cl, 3 dwg, 1 tbl
SUBSTANCE: invention relates to the oil and gas industry and is meant for use in degassing liquid sulphur. Sulphur is degassed in a column with a packed layer (2) in which the catalyst used is a support (3) on which cobalt disulfophthalocyanine is deposited. A packed catalyst is used in the packed layer of the column.
EFFECT: invention considerably shortens the duration of degassing sulphur.
2 cl, 1 ex, 1 tbl, 1 dwg
SUBSTANCE: invention can be used in the chemical industry. A method of separation of melted sulphur from a flowing medium includes isolation of a liquid mixture, which contains a redox solution and melted sulphur into a reservoir, which has an upper part, a lower part, a zone of a gaseous phase, a zone of the redox solution and a zone of melted sulphur. Melted sulphur subsides in the reservoir and forms a separating boundary between the zone of the redox solution and the zone of melted sulphur at some height of the reservoir. Control of pressure in the reservoir is performed and gas is added or discharged from the zone of the gaseous phase, located immediately above the zone of the redox solution in the reservoir. Pressure inside the reservoir is supported irrespective of the height of the phase separation boundary. Gas is added through a valve of gas supply and discharged through a valve of gas output. Control over the valves is performed by means of a controller. Melted sulphur is discharged from the reservoir and a level of the boundary of the phase separation is measured by means of a device for control of the boundary of the phase separation depending on intensity of the melted sulphur output from the reservoir.
EFFECT: invention makes it possible to increase quality of separated sulphur, prevent its carryover.
9 cl, 4 dwg
SUBSTANCE: disclosed is a method of producing granular sulphur by adding liquid sulphur to water. Liquid sulphur under pressure of 900 Pa to 9000 Pa flows from an opening with a diameter of 0.5 mm to 2.5 mm in form of a vertical solid jet and falls into water. The distance between the exit point of the jet of sulphur and the water surface is not more than 80 mm. The obtained spherical sulphur granules are the best geometric shape of solid sulphur, which is characterised by the best mass to volume ratio and the best mechanical strength. The uniformity of the grain-size composition and the spherical shape of the particles improve the accuracy of feeding granular sulphur with any type of feeder.
EFFECT: obtaining granular sulphur in the form of spherical particles of a given diameter.
SUBSTANCE: invention relates to use of polysiloxanes at granulation from melt. One proposes application of organic modified polysiloxanes, containing at least three different from each other simple polyester residues, wherein at least two of these simple polyester residues differ by content of ethylene oxide units, at least 9 wt% of total weight of simple polyester residues, as separation agent or separation agent component at granulation from melt.
EFFECT: technical result is providing not deforming separation of granulate from conveyor and lack of deposits on conveyor belt.
7 cl, 1 tbl
SUBSTANCE: invention relates to chemical industry. Device comprises cooling tank (4) storing a liquid, first sprayer (2), granulating drum (6), conveyor (20) for conveying sulphur seeds. First sprayer (2) is configured for spraying molten sulphur in liquid in cooling tank (4) to form sulphur seeds.
EFFECT: invention provides a more efficient process of producing sulphur seeds, which can be enlarged to sulphur granules.
21 cl, 19 dwg
SUBSTANCE: way to implement in different, not completely isolated cells, each of which is filled with liquid sulfur first zone and gas filled second zone. Liquid sulfur is pumped from the first zone of each of the chambers in the second zone of this same chamber and sprayed in the area. In the first zone of the first camera insufflated with oxygen-containing gas to remove the H2S, and in the first zone chamber, located after the first chamber, insufflated with inert gas to remove SO2. The device contains a container (1), split by partition (4) into two not completely isolated one from another chambers (a, b) filled with liquid sulfur first zone (2) and gas filled second zone (3). The first blowing device (12) is located in the first zone (2) of chamber (b) for oxygen-containing gas injection into liquid sulfur, the second blowing device (31)-in the first zone (2) of chamber (c) after the camera (b) for injection of inert gas into a liquid sulfur. Incoming into the second zone (3) of chamber (b) of the first device (25') for spraying liquid sulfur connected with pump (21'), suction liquid sulfur from the first zone (2) of chamber (b). Incoming into the second zone (3) of chamber (c) second device (25") for spraying liquid sulfur connected with pump (21"), suction liquid sulfur from the first zone (2) of chamber (c).
EFFECT: effective removal of gases contained in the liquid sulphur, low level of SO2 formation.
7 cl, 4 dwg