CS263599B1 - Connection of apparatus for the production of hydrogen sulphide - Google Patents

Abstract

Engagement is made so technological part of the apparatus made up of a reservoir for liquid sulfur, metering pump and reactor catalytic hydrogen sulfide synthesis the hydrogen and sulfur inlet route is sulfur separation from hydrogen sulfide, the condenser and the system two parallel branches of heat exchangers with the possibility of Sulfur smelting and removal; part of the sulfur separation is preceded by parts of the compression and liquefaction of hydrogen sulfide formed gas tank system, compressor, condensers and reservoirs of liquid hydrogen sulphide.

Description

263599

BACKGROUND OF THE INVENTION The present invention relates to the incorporation of sulfur-free liquid hydrogen sulfide converting apparatus.

Hydrogen sulfide can be prepared by direct hydrogenation of sulfur vapors with a molar ratio of 1 to 1 to 6 when the mixture of Η2 (8) and S (g) is a lead catalyst tube filled with known catalysts whose mainly components are tungsten, nickel, vanadium sulfurics , or their combination. There is conversion to the catalytic contact! of hydrogen and sulfur with the release of heat. A reactor of this type is described in Chem. Engineering 24, 62 (1958), respectively, for laboratory preparation in Chemische Technik 9, (8) 50.3 (1967) and Neftepererabotka ineftechimija 1, 42 (1976). According to British Patent No. 1193,040, for example, increasing the hydrogen saturation of sulfur vapors utilizes a carbonation column scrubbed with sulfur in a hydrogen stream. At the same time, it is heated to the reaction temperature. The catalyst in this arrangement is located above the carbonation column. Podlá čs. AO No. 190 79'2 is agitated at 180 to 400 ° C with sulfur vapors at 180 to 350 ° C. Podfa čs. AOC. 190 793, 1 to 6 parts of the circulating hydrogen sulfide produced are added to one hydrogen at 20-400 ° C, which allows to reduce the temperature of the nitrogen to 180 ° C while maintaining a quantitative conversion. hydrogen to hydrogen sulfide.

By the above processes, it is possible to obtain dry gas hydrogen sulfide in high yields without the formation of by-products.

A disadvantage of the hitherto known processes for the production of hydrogen sulfide is that they do not interfere with the sulfur separation system which is entrained into the stream of hydrogen sulfide formed under the hydrogen and sulfur conversion conditions of the catalytic contact. A particular disadvantage is the special requirement for the construction of a reactor for the removal of heat from the exothermic reaction of hydrogen sulfide formation.

Today's equipment described in the literature for the production of hydrogen sulphide mainly deals with the hydrogen saturation of sulfur vapors at temperatures of 180 to 400 ° C and the construction of the reactor itself with a sulphide-based catalyst chargeNi, W, V. In the hydrogen saturation process, the paramisir produces a mixture of a pair of sulfur and hydrogen with a higher vapor content the sulfur equivalent to hydrogen equivalence, especially at a heating temperature regime of 400 ° C. This also causes vv-sokei, respectively. quantitatively converting hydrogen hydrogen sulfide to a high vapor content and / or vaporization of hydrogen sulfide reactor causing difficulties such as hydrogen sulfide liquefaction.

The aforementioned disadvantages are solved by the invention, which is essentially connected with apparatuses for the production of liquid sulfur free sulfur hydrogen, a reactor for catalytic sulfur dioxide synthesis, a liquid sulfur storage tank (with the function of providing temperature regime in the reactor) and a pump connected to a circulating circuit to which the liquid storage tank is preceded sulfur and the circulating circuit is preceded by a sulfur separator system, followed by a filter unit, which is preceded by the hydrogen sulfide technology part.

The sulfur-filled capacitor reservoir, equipped with a sulfur melt inlet pipe and a sulfur return pipe, is connected via a sulfur pipe to a sulfur feed pump with a sulfur outlet pipe to a sulfur feed pump connected to a hydrogen sulfide reactor equipped with a water inlet pipe. , a return hydrogen sulphide conduit, a sulfur return conduit to a sulfur service reservoir, a sulfur return conduit from a sulfur condenser, a sulfur discharge conduit, which is connected to a sulfur pump discharge conduit by a sulfur conduit and a sulfur reservoir. at the same time, the hydrogen sulfide reactor is provided with a hydrogen sulphide outlet pipe to the sulfur condenser cooled by boiling water evaporation.

The condenser is connected by a conduit to the parallel connected condensers cooled by hot water with the possibility of fused-condensed sulfur, which are connected to the condensers cooled by cold water, and which are again connected by a sulfur-dioxide conduit to the condensers cooled by the cooling medium which they are jointly connected with a charcoal filter pipe. At the same time, the sulfur condensers are cooled with hot water, cold water, and glycol combined with sulfur piping with the operating coupler. The sulfur outlet pipe from a parallel pair of charcoal filters is connected to a pair of parallel-connected filters (with a paper insert), which are connected by pipeline to a gasholder provided with return hydrogen sulphide inlet pipes, such as thiol, return pipes and hydrogen sulfide. the hydrogen sulfide reservoir and the hydrogen sulfide outlet pipe connected to the hydrogen sulfide compressor.

The compressor is connected to the outlet via a hydrogen sulfide condenser, which is directly connected to a hydrogen sulfide stack, with the sulfur-hydrogen reservoir being provided with a return hydrogen sulfide inlet (from thiol production), an inert-deflector discharge pipe and an outlet. hydrogen sulphide to the hydrogen sulphide dosing pump. The deflegmator is a coupled conduit with a liquid hydrogen sulphide binder and also a gas tank duct.

Involvement under. of the invention has the following advantages over the known circuits and devices. It allows to continuously produce hydrogen sulphide in high or low. quantitative yields without the formation of (co-) ballast substances. The connection of the apparatus for the production of hydrogen sulfide allows the separation of sulfur in the form of vapor and / or mist in the

Claims (2)

5 high purity hydrogen sulphide suitable for liquefaction or for further direct use, e.g. in the manufacture of mercaptosulphides, sulphides or sulphides. (The actual production process is such that the sulfur reservoir capacitor 1 provided by the sulfur inlet pipe 26 is fed with sulfur through line 27 with the sulfur pump 71 to the liquid sulfur reservoir 2, from which it passes through line 28, by the dosing pump 6, further by route 29. The sulfur excess of the hydrogen sulfide reactor 4 is returned to the sulfur sulfur storage tank 2. The hydrogen sulfide reactor 4 enters hydrogen through the line 25, which, after conversion to hydrogen sulfide, exits the hydrogen sulfide reactor 4 into the condenser 5 via the sulfur 31 line. Alternatively, recycled sulfur hydrogen may be returned to the hydrogen sulfide reactor 4 from the production line, e.g., thiol, via line 70. The condensed sulfur flows from the condenser 5 through the hydrogen sulfide reactor 4, and the hydrogen sulfide from the condenser 5 passes through line 36 to the heat exchanger 6 from which it then proceeds through the path 37 of the exchanger 10 and travels therefrom through the path 39to From the exchanger 12, the path 41 and the path 43 go to a filter with a charcoal 14 and / or 15. When sulfur is condensed in the exchangers 8, 10 and 12, the condenser 5 is led through the path 36 to the exchanger 9, from which hydrogen sulphide passes through line 38 to exchanger 11, then to line 40 to exchanger 13, from which route 42 and further to line 43, goes to the filter with charcoal 14 and / or 15. Smoked sulfur from exchangers 8, 9, 10, 11 12 and 13, it travels through paths 44, 45, 46, 47, 48 and 49 to route 50 from which it passes to the liquid sulfur storage tank 2. The hydrogen sulfide proceeds from the charcoal filter 14 and / or 15 through the line 51 to the liner filters 16 and / or 17, from which the retention path 52 to the gas reservoir 18, to which hydrogen sulphide is returned via line 53 of, for example, thiol. Hydrogen sulfide proceeds with gas 18 through line 54 to the hydrogen sulfide compressor 19 from which hydrogen sulfide under pressure is passed through line 55 to condenser 20 where, after 6 cooling, it is liquid. From the condenser 20, the liquid hydrogen sulfide passes through the line 56 to the liquid hydrogen sulfide reservoir 22 connected to the line 63 and the line 64 to the second liquid hydrogen sulfide reservoir 23. Gaseous hydrogen sulphide inserts flow into the condenser 21 from reservoirs 22 and 23 of liquid sulfur-hydrogen through line 61, and optionally condensed hydrogen sulphide is passed through line 60 to sleep in the hydrogen sulphide reservoir 23 and the inerts are conducted through line 62 to the gas reservoir 18 , where a constant pressure is maintained by the control circuit. The flow of the increased inert content together with the hydrogen sulfide gas into the alkaline absorption is ensured by the control circuit 67 through the line 65. The hydrogen sulfide gas recycled, for example, from the production line, is condensed into the exchanger 68. The hydrogenated hydrogen sulfide flows into the hydrogen sulfide reservoir 23 via the line 59. The liquified hydrogen sulfide from the reservoirs 22 and / or 23 passes through the line 57, e.g. 1 and 2). The invention is described in more detail below with reference to a specific embodiment. EXAMPLE Sulfur from a liquid sulfur storage tank was metered into the hydrogen sulfide reactor at a steady state (592.5 kg / hr). Overflow from the reactor returned 505.9 kg / h. molten sulfur. The sulfur temperature in the process vessel was 140 ° C, the reactor temperature was 370 to 375 degrees Celsius. Pre-heated hydrogen was introduced into the reactor at 5.66 kg / h. purity 98.7% (w / w). Hydrogen sulfide exiting the reactor at 550-575 ° C was fed to a sulfur condenser. After condensation of sulfur, hydrogen sulfide was passed through a system of exchangers and filters to a gas reservoir in front of a compressor where an overpressure of 0.01 MPa was maintained by the control circuit. Hydrogen sulfide gas compressed to a pressure of 2.1 MPa. Liquid hydrogen sulfide was collected in 8 h 736 kg of liquid hydrogen sulfide, representing 97.5% conversion. OBJECT 1. Connection of apparatuses for the production of liquid hydrogen sulphide, characterized in that the technological part of the apparatus consisting of the liquid sulfur reservoir, the metering pump and the catalytic synthesis reactor of hydrogen sulphide, provided with a hydrogen and sulfur inlet line, is a part of the sulfur separation from the sulfur dioxide formed by the condenser and the two parallel systems the heat exchange of the exchangers by the sulfur smelting and dewatering capability, while part of the sulfur separation is preceded by the hydrogen sulphide hydrogenation, liquefaction and liquefaction system of the hydrogen sulphide formed by the gas reservoir system. 2. Apparatus connection according to claim 1, characterized in that the liquid sulfur reservoir (1) provided by the sulfur inlet conduit (26), the sulfur return conduit (35) and the outlet conduit (27) via the sulfur pump (71) is preceded by an operating reservoir ( 2) sulfur connected by a sulfur inlet pipe (28) to a sulfur metering pump (6) with an outlet (29) to a hydrogen sulfide reactor (4) with a sulfur return (30) to a sulfur storage facility (2), the outlet (33) to the liquid sulfur master (3) provided with an outlet (34) of the sulfur pump (7) connected to the sulfur reservoir (35) with the sulfur reservoir (1) and the hydrogen sulfide reactor (4) being provided with the hydrogen inlet duct (25); (70) a reversible hydrogen sulphide and a outlet pipe (31) of a mixture of sulfur and sulfur-hydrogen in a condenser (5) provided with a sulfur outlet (32) to the hydrogen sulphide reactor (4) and the hydrogen sulphide outlet pipe (36) of the connected exchangers (8); (9) Op with the sulfur-hydrogen outlet pipe (37) from the exchanger (8) to the exchanger (10) and the hydrogen sulfide outlet pipe (38) of the exchanger (9) to the exchanger (11), wherein the exchanger (10) is provided with an outlet pipe (39) to the exchanger (12) and the exchanger (11) are provided with an outlet conduit (40) into the exchanger (13) and at the same time the exchanger (8, 9, 10, 11, 12, 13) are in the same direction as the sulfur outlet ducts (45, 44, 47, 46, 49, 48) connected to the route (50) raised to the sulfur storage tank (2) and at the same time the exchanger (12) is provided with an outlet pipe (41) of hydrogen sulfide and exchanger (13) ) is provided with a hydrogen sulphide outlet pipe (42), the paths (41, 42) being connected to a conduit (43) connected by charcoal-connected sparged filters (14, 15), and an outlet pipe (51) of charcoal filters coupled to parallel wired liner filters (16, 17) provided with a hydrogen sulphide outlet pipe (52) with a hydrogen sulfide gas reservoir (18) provided with a return hydrogen sulphide inlet conduit (53), for example, a thiol outlet, a return conduit (62) of a mixture of inerts and hydrogen sulphide provided with a pressure control circuit (66) and a hydrogen sulphide outlet conduit (54) to a compressor (19) with an outlet (55) coupled to a condenser (20) provided with a liquefied hydrogen sulphide outlet conduit (56) to a liquid hydrogen sulphide reservoir (22) connected to a conduit (64) and (63) with a reservoir (23) the hydrogen sulphide, wherein the reservoir (23) is provided with a hydrogen sulphide inlet conduit (59) from a condenser (68) with a hydrogen sulphide return (69), for example from a polyethylene, and at the same time a liquid hydrogen sulphide reservoir (23) is provided with a return conduit. (60) hydrogen sulfide from the condenser (21) and the outlet conduit (61) to the condenser (21) through the hydrogen sulfide discharge conduit (67) and at the same time liquid sulfur reservoirs (22, 23) are provided a common outlet conduit (57) of a liquid hydrogen sulfide supply pump (24) provided with an outlet conduit (58), for example, for the production of a thiol. 2 sheets of drawings