Continuous gasification sulfur purification device for oil-containing black sulfur and process method thereof

Abstract

The invention provides a continuous gasification sulfur purification device for oil-containing black sulfur and a process method thereof, and belongs to the field of gas desulfurization. The device comprises a melting gravity settling furnace, a liquid sulfur delivery pump, a high-temperature gasification furnace, an oil-gas heat exchanger, a water-oil separator, a sulfur heat exchanger, a slicing packaging machine and a nitrogen generator, the melting gravity settling furnace is connected with the liquid sulfur conveying pump; the upper half part of the high-temperature gasification furnace is of a double-layer jacket furnace structure, an oil-gas outlet is formed in the top of the high-temperature gasification furnace, the oil-gas outlet is connected with the oil-gas heat exchanger, and the oil-gas heat exchanger is connected with the water-oil separator; a jet orifice and an upper heating pipe are arranged at the upper part of the high-temperature gasification furnace; the jet orifice is connected with a liquid sulfur delivery pump; according to the method, the high-purity sulfur is extracted by continuous reduced pressure gasification by taking black sulfur which is produced by desulfurization of a wet oxidation method and contains sulfur, organic matters, trace moisture and other impurities in blast furnace gas (produced by coking) containing hydrogen sulfide as a raw material.

Description

Technical Field

[0001] The present invention belongs to the field of gas desulfurization, and particularly relates to an oil-containing black sulfur continuous gasification and purification sulfur device and its process method. Background Technique

[0003] Currently, in the mainstream wet desulfurization process, when the working efficiency of the purification system in the process system is low, in the sulfur foam obtained by the regeneration of the desulfurization liquid, in addition to the main component sulfur, there are also organic substances such as coal tar and aromatic hydrocarbons, as well as water and other trace impurities. According to environmental protection requirements and resource recycling, it is necessary to treat the sulfur foam to produce valuable sulfur products. However, the black sulfur produced by the coke oven has many impurities and cannot be directly used in the traditional single sulfur melting kettle in the sulfur melting process for continuous or intermittent sulfur melting production.

[0004] When adopting the continuous sulfur melting process, the liquid black sulfur containing molten sulfur, organic substances, water and other trace impurities is discharged from the bottom of the sulfur melting equipment and cooled to obtain black sulfur without commercial value. When adopting the intermittent sulfur melting process, the sulfur foam is treated by a filter press or a centrifuge and then enters the sulfur melting kettle. The sulfur melting kettle is heated to about 135 °C, and after 6 hours of heating, the sulfur foam becomes a molten state. The internal black sulfur is naturally stratified due to the fluid density difference. The lower layer is the crude sulfur containing coal tar, organic substances and other trace impurities. After stopping heating, the valve at the bottom of the sulfur melting kettle is opened to discharge the crude sulfur with low commercial value. From the above two processes, the intermittent sulfur melting process takes a long time, the working environment is harsh, and the purity of the sulfur product is not high; while the quality of the sulfur product extracted by the continuous sulfur melting process is extremely poor.

[0005] Based on the traditional sulfur melting process, in the existing gasification and refining sulfur process, the core is the gasification furnace. The black sulfur is sublimated by heating to extract sulfur, and the obtained sulfur has high purity and stable quality. However, the sulfur gasification temperature needs to be above 444.6 °C, which not only has high energy consumption but also has the problem of corroding equipment. The sulfur vapor will react with metals at temperatures above 350 °C, and the service life of the reaction furnace is basically within half a year, which will increase the production cost. At the same time, there is a leakage and combustion of sulfur vapor, causing environmental pollution and safety hazards. Summary of the Invention

[0006] The purpose of the present invention is to provide an oil-containing black sulfur continuous gasification and purification sulfur device and its process method. This method uses the black sulfur containing sulfur, organic substances, trace moisture and other impurities produced by the wet oxidation method for desulfurizing the gas containing hydrogen sulfide in blast furnace gas (coking production) as the raw material, and adopts continuous vacuum gasification to extract high-purity sulfur.

[0007] In order to achieve the above purpose, the present invention adopts the following technical solutions:

[0008] The present invention discloses an oil-containing black sulfur continuous gasification and purification sulfur device, including a molten gravity sedimentation furnace, a liquid sulfur transfer pump, a high-temperature vaporization furnace, an oil-gas heat exchanger, a water-oil separator, a sulfur heat exchanger, a slicing and packaging machine, and a nitrogen generator;

[0009] The molten gravity sedimentation furnace is connected to the liquid sulfur transfer pump;

[0010] The upper half of the high-temperature vaporization furnace is a double-layer sleeve furnace structure, with an oil-gas outlet arranged at the top. The oil-gas outlet is connected to the oil-gas heat exchanger, and the oil-gas heat exchanger is connected to the water-oil separator;

[0011] The upper part of the high-temperature vaporization furnace is provided with a spray port and upper heating tubes. The spray port is connected to the liquid sulfur transfer pump;

[0012] The middle part of the high-temperature vaporization furnace is provided with a liquid sulfur outlet. The liquid sulfur outlet is connected to the sulfur heat exchanger, and the sulfur heat exchanger is connected to the slicing and packaging machine;

[0013] The lower part of the high-temperature vaporization furnace is provided with lower heating tubes, mechanical stirring paddles, and a nitrogen interface. The nitrogen interface is connected to the nitrogen generator;

[0014] Sulfur raw materials enter the molten gravity sedimentation furnace for impurity separation. After obtaining liquid crude sulfur, it is transported to the inside of the high-temperature liquefaction furnace through the liquid sulfur transfer pump. The inside of the high-temperature vaporization furnace is evacuated, and it is sprayed out through the spray port. Part of the sprayed sulfur is vaporized by heat during the descending process. After vaporization, the sulfur is liquefied into liquid sulfur, passes through the sulfur heat exchanger, and then is sent to the slicing and packaging machine to be cooled to solid sulfur and sliced and packaged; Another part of the crude sulfur containing sulfur slag falls to the bottom of the furnace and is evenly heated by the mechanical stirring paddles at the bottom of the furnace, so that the sulfur in the crude sulfur continues to be vaporized, leaving sulfur slag. The sulfur vapor moves upward under the push of the nitrogen transported by the nitrogen generator, is liquefied into liquid sulfur, and then is discharged to the sulfur heat exchanger through the liquid sulfur outlet, and is sent to the slicing and packaging machine to be cooled to solid sulfur and sliced and packaged; The waste gas remaining after the high-temperature vaporization furnace liquefies the sulfur vapor is transported to the oil-gas heat exchanger through the oil-gas outlet, cooled to room temperature with cold water, and then transported to the water-oil separator to form organic by-products.

[0015] Preferably, the device further includes a reciprocating vacuum pump. The upper part of the high-temperature vaporization furnace is provided with a vacuum pump interface, and the vacuum pump interface is connected to the reciprocating vacuum pump.

[0016] Preferably, the lower part of the high-temperature vaporization furnace is further provided with a slag discharge interface.

[0017] Preferably, both the molten sedimentation separator and the water-oil separator adopt vertical conical bottom furnace bodies.

[0018] The present invention also provides a process method for continuously gasifying and purifying oil-containing black sulfur into sulfur, including:

[0019] The sulfur raw material enters the molten gravity sedimentation furnace for sedimentation to form liquid crude sulfur;

[0020] The obtained liquid crude sulfur is transported to the inside of the high-temperature liquefaction furnace by a liquid sulfur transfer pump. The high-temperature vaporization furnace is evacuated. During the descent of the liquid crude sulfur, a part of it is heated and vaporized by the upper heating tubes. After vaporization, the sulfur is liquefied into liquid sulfur and enriched in the collection tanks on the outer and inner layers of the high-temperature vaporization furnace. After passing through the sulfur heat exchanger, it is then sent to the slicing and packaging machine to be cooled to solid sulfur and sliced and packaged;

[0021] Another part of the liquid crude sulfur, which contains sulfur slag, falls to the furnace bottom. It is evenly heated by the mechanical stirring paddle at the furnace bottom, so that the sulfur in the crude sulfur is vaporized and the sulfur slag is left. The sulfur slag is transported to the slag discharge system through the slag discharge interface; the vaporized sulfur forms sulfur vapor. The sulfur vapor moves upward under the push of the nitrogen gas transported by the nitrogen generator. When it contacts the upper wall of the high-temperature vaporization furnace, it is liquefied into liquid sulfur. The liquid sulfur slides down along the furnace wall into the liquid sulfur storage tank between the inner and outer walls, and is discharged to the sulfur heat exchanger through the liquid sulfur outlet, and then sent to the slicing and packaging machine to be cooled to solid sulfur and sliced and packaged; the water and organic vapor generated during the vaporization process are transported to the oil and gas heat exchanger and cooled to room temperature with cold water, and then transported to the water and oil separator to form organic by-products.

[0022] Preferably, the sedimentation time is 3 - 6 hours.

[0023] Preferably, the heating temperature of the upper heating tubes is 250 - 270 °C, and the heating temperature of the lower heating tubes is 300 - 320 °C.

[0024] Advantages of the present invention

[0025] Compared with the prior art, the present invention first separates crude sulfur from black sulfur by the gravity method. The high-temperature vaporization furnace adopts an internal suspended heating method, with high heat conduction efficiency. The crude sulfur is quickly vaporized after spraying, and the impurities flow to the bottom without deposition. Moreover, a vacuum pump is provided in the upper section of the furnace body, which reduces the vaporization temperature of sulfur and extends the service life. At the same time, the vaporization waste gas of the crude sulfur is further separated to obtain organic by-products. Brief description of the drawings

[0026] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings required to be used in the embodiments. Obviously, the drawings described below are only some embodiments recorded in the present invention. For those of ordinary skill in the art, other drawings can also be obtained based on these drawings.

[0027] Figure 1 It is a structural schematic diagram of a device and process for continuously purifying sulfur by vacuum gasification of oil-containing black sulfur provided by an embodiment of the present invention;

[0028] In the figure, 10 is a melting gravity sedimentation furnace;

[0029] 20 is a liquid sulfur transfer pump;

[0030] 30 is a high-temperature vaporization furnace; 31 is an oil and gas outlet; 32 is a jet port; 33 is an upper heating pipe; 34 is a lower heating pipe; 35 is a mechanical stirring paddle; 36 is a vacuum pump interface; 37 is a liquid sulfur outlet; 38 is a nitrogen interface; 39 is a slag discharge interface;

[0031] 40 is an oil and gas heat exchanger;

[0032] 50 is a water-oil separator;

[0033] 60 is a reciprocating vacuum pump;

[0034] 70 is a sulfur heat exchanger;

[0035] 80 is a slicing and packaging machine;

[0036] 90 is a nitrogen generator. Detailed implementation manner

[0037] In order to enable those skilled in the art to better understand the technical solution of the present invention, the present invention will be further introduced in detail below in conjunction with the accompanying drawings.

[0038] The present invention first provides an oil-containing black sulfur continuous gasification and purification sulfur device, including a melting gravity sedimentation furnace 10, a liquid sulfur transfer pump 20, a high-temperature vaporization furnace 30, an oil and gas heat exchanger 40, a water-oil separator 50, a sulfur heat exchanger 70, a slicing and packaging machine 80, and a nitrogen generator 90;

[0039] The melting gravity sedimentation furnace 10 is connected to the liquid sulfur transfer pump 20;

[0040] The upper half of the high-temperature vaporization furnace 30 is a double-layer sleeve furnace structure, and an oil and gas outlet 31 is provided at the top. The oil and gas outlet 31 is connected to the oil and gas heat exchanger 40, and the oil and gas heat exchanger 40 is connected to the water-oil separator 50;

[0041] The upper part of the high-temperature gasification furnace 30 is provided with a jet port 32 and an upper heating pipe 33, and the jet port 32 is connected to the liquid sulfur transfer pump 20;

[0042] The middle part of the high-temperature gasification furnace 30 is provided with a liquid sulfur outlet 37. The liquid sulfur outlet 37 is connected to the sulfur heat exchanger 70, and the sulfur heat exchanger 70 is connected to the BKQ4 type slicing and packaging machine 80;

[0043] The lower part of the high-temperature gasification furnace 30 is provided with a lower heating pipe 34, a mechanical stirring paddle 35, and a nitrogen interface 38. The nitrogen interface 38 is connected to the nitrogen generator 90;

[0044] The device described in this embodiment further includes a reciprocating vacuum pump 60 . A vacuum pump interface 36 is provided on the upper portion of the high-temperature gasification furnace, and the vacuum pump interface 36 is connected to the reciprocating vacuum pump 60 .

[0045] The high temperature gasification furnace 30 described in this embodiment is further provided with a slag discharge interface 39 at the lower part.

[0046] The molten gravity settling furnace 10 and the water-oil separator 50 described in this embodiment both adopt a vertical conical bottom furnace body.

[0047] The model of the slice packaging machine 80 described in this embodiment is BKQ4.

[0048] The present invention also provides a process for continuously gasifying and purifying sulfur from oil-containing black sulfur, such as Figure 1 As shown, including:

[0049] The sulfur foam produced by the desulfurization system is processed by a filter press or a centrifuge to obtain black sulfur. Black sulfur is fed into the melting gravity settling furnace 10 through the feeding port at the upper end of the melting gravity settling furnace 10 as a sulfur raw material. The melting gravity settling furnace 10 is heated to about 135°C with superheated steam all year round (the specific temperature is appropriately adjusted according to the phenomenon), and settles for 3-6 hours (obvious page stratification can be seen from the observation window). Crude sulfur containing sulfur, organic matter and other impurities is obtained at the bottom of the melting gravity settling furnace 10. Liquid crude sulfur is transported to the high-temperature vaporization furnace 30 through the liquid sulfur delivery pump 20 through the insulation pipeline.

[0050] The high temperature vaporization furnace 30 is evacuated by a reciprocating vacuum pump 60. At the same time, an upper heating tube 33 and a lower heating tube 34 are arranged in the furnace to control the temperature of different spaces in the furnace in sections. The heating temperature of the upper heating tube is set to 250-270°C, and the heating temperature of the lower heating tube is set to 300-320°C.

[0051] The liquid crude sulfur sent to the vaporizer is sprayed into the vaporizer through the injection port 32. During the descent process, a part of it is heated and vaporized (under vacuum conditions, the boiling point of sulfur decreases from 444.6°C to about 300°C). After vaporization, the sulfur is liquefied into liquid sulfur and is accumulated in the collecting tanks of the outer and inner layers of the high-temperature vaporizer. After passing through the sulfur heat exchanger 70, it is sent to the slice packer 80 to be cooled into solid sulfur and sliced ​​and packaged.

[0052] Another part of the liquid crude sulfur, which contains sulfur slag, falls to the bottom of the furnace and is evenly heated through the mechanical stirring paddle 35 at the bottom of the furnace, causing the sulfur in the crude sulfur to vaporize and leaving the sulfur slag behind. The sulfur slag is transferred to the slag discharge system through the slag discharge interface 39; the vaporized sulfur forms sulfur vapor, and the sulfur vapor moves upward under the push of the nitrogen gas transported by the nitrogen gas generator 90. When it reaches the upper wall of the high-temperature vaporization furnace 30 at a relatively low temperature (about 200 - 250 °C), it liquefies into liquid sulfur. The liquid sulfur slides down along the furnace wall into the liquid sulfur storage tank between the inner and outer walls, and is discharged through the liquid sulfur outlet 37 to the sulfur heat exchanger 70, where it is cooled to about 135 °C with relatively stable chemical properties by superheated water, and then sent to the slicing and packaging machine 80 to be cooled into solid sulfur and sliced and packaged;

[0053] The waste gas remaining after the high-temperature vaporization furnace 30 liquefies the sulfur vapor is organic matter and trace water vapor, which is transported to the oil-gas heat exchanger 40 through the oil-gas outlet 31, cooled to room temperature with cold water, and then transported to the water-oil separator 50. Due to the different densities of oil and water, they naturally separate into layers. The water returns to the reaction system, and the oil forms an organic by-product.

[0054] In the device of this embodiment, the bottom of the high-temperature vaporization furnace 30 has a slag discharge port 39, which is connected to the slag discharge system and can discharge the sulfur slag after sulfur sublimation treatment.

[0055] In the device of this embodiment, the bottom of the high-temperature vaporization furnace 30 is connected to the nitrogen gas generator 90, which uses nitrogen to assist the vaporization and volatilization of sulfur, and at the same time avoids the reaction between sulfur and oxygen in the air to ensure the purity of the sulfur product.

[0056] In the device of this embodiment, the bottom of the high-temperature vaporization furnace 30 has a mechanical stirring paddle, which is driven by an electric motor to stir the liquid crude sulfur to make the heating more uniform.

[0057] In this embodiment, the sulfur heat exchanger 70 is connected to the slicing and packaging machine 80 to slice, collect, and package the high-purity solid sulfur.

[0058] In this embodiment, the sulfur heat exchanger 70, the water-oil separator 50, and the reciprocating vacuum pump 60 are all connected to the waste gas treatment system to collect and treat the waste gas generated during each stage of the gasification process.

[0059] Those skilled in the art of this industry should understand that the present invention is not limited by the above embodiments. What is described in the above embodiments and the specification only illustrates the principle of the present invention. Without departing from the spirit and scope of the present invention, the present invention will have various changes and improvements, and these changes and improvements all fall within the scope of the present invention claimed. The scope of protection claimed by the present invention is defined by the appended claims and their equivalents.

Claims

1. An oil-containing black sulfur continuous gasification and purification sulfur device, characterized in that It includes a melting gravity settling furnace, a liquid sulfur transfer pump, a high-temperature vaporization furnace, an oil-gas heat exchanger, a water-oil separator, a sulfur heat exchanger, a slicing and packaging machine, and a nitrogen generator; The melting gravity settling furnace is connected to the liquid sulfur transfer pump; The upper half of the high-temperature vaporization furnace is of a double-layer sleeve furnace structure, and an oil-gas outlet is arranged at the top. The oil-gas outlet is connected to the oil-gas heat exchanger, and the oil-gas heat exchanger is connected to the water-oil separator; The upper part of the high-temperature gasification furnace is provided with a spray port and an upper heating pipe, and the spray port is connected to the liquid sulfur transfer pump; The middle part of the high-temperature gasification furnace is provided with a liquid sulfur outlet, and the liquid sulfur outlet is connected to the sulfur heat exchanger, and the sulfur heat exchanger is connected to the slicing and packaging machine; The lower part of the high-temperature gasification furnace is provided with a lower heating pipe, a mechanical stirring paddle and a nitrogen interface, and the nitrogen interface is connected to the nitrogen generator; Sulfur raw materials enter the melting gravity settling furnace for impurity separation. After obtaining liquid crude sulfur, it is transported to the inside of the high-temperature liquefaction furnace through the liquid sulfur transfer pump. The inside of the high-temperature vaporization furnace is evacuated and sprayed through the spray port. Part of the sprayed sulfur is vaporized by heat during the falling process. After vaporization, the sulfur is liquefied into liquid sulfur. After passing through the sulfur heat exchanger, it is sent to the slicing and packaging machine to be cooled to solid sulfur and sliced and packaged; Another part of the crude sulfur containing sulfur slag falls to the furnace bottom, and is stirred evenly by the mechanical stirring paddle at the furnace bottom, so that the sulfur in the crude sulfur continues to vaporize and leave the sulfur slag. The sulfur vapor moves upward under the push of the nitrogen transported by the nitrogen generator, is liquefied into liquid sulfur, and then is discharged to the sulfur heat exchanger through the liquid sulfur outlet, and is sent to the slicing and packaging machine to be cooled to solid sulfur and sliced and packaged; The waste gas remaining after the high-temperature vaporization furnace liquefies the sulfur vapor is transmitted to the oil-gas heat exchanger, cooled to room temperature with cold water, and then transmitted to the water-oil separator to form organic by-products.

2. The sulfur continuous gasification and purification device for oil-containing black sulfur according to claim 1, wherein The device also includes a reciprocating vacuum pump. A vacuum pump interface is arranged at the upper part of the high-temperature gasification furnace, and the vacuum pump interface is connected to the reciprocating vacuum pump.

3. The sulfur continuous gasification and purification device for oil-containing black sulfur according to claim 1, characterized in that, The lower part of the high-temperature gasification furnace is also provided with a slag discharge interface.

4. The continuous gasification and purification sulfur device containing oily black sulfur according to claim 1, characterized in that, Both the melting and settling separation furnace and the water-oil separator adopt vertical conical bottom furnace bodies.

5. A process for continuously gasifying and purifying sulfur from oil-containing black sulfur according to claim 1, characterized in that, Including: Sulfur raw materials enter the melting gravity settling furnace for settling to form liquid crude sulfur; The obtained liquid crude sulfur is transported to the inside of the high-temperature liquefaction furnace through the liquid sulfur transfer pump. The inside of the high-temperature vaporization furnace is evacuated. During the falling process, part of the liquid crude sulfur is heated and vaporized by passing through the upper heating pipe. After vaporization, the sulfur is liquefied into liquid sulfur, enriched in the collection tanks on the outer layer and the inner layer of the high-temperature vaporization furnace. After passing through the sulfur heat exchanger, it is sent to the slicing and packaging machine to be cooled to solid sulfur and sliced and packaged; Another part of the liquid crude sulfur and the crude sulfur containing sulfur slag fall to the furnace bottom, where they are evenly heated by the mechanical stirring paddles at the furnace bottom, so that the sulfur in the crude sulfur is vaporized and the sulfur slag is left. The sulfur slag is transported to the slag discharge system through the slag discharge interface; the vaporized sulfur forms sulfur vapor, which moves upward under the push of the nitrogen gas transported by the nitrogen gas generator. When it contacts the upper wall of the high-temperature vaporizer, it liquefies into liquid sulfur, and the liquid sulfur slides down along the furnace wall into the liquid sulfur storage tank between the inner and outer walls, and is discharged to the sulfur heat exchanger through the liquid sulfur outlet, and then sent to the slicing and packaging machine to be cooled to solid sulfur and sliced and packaged; the water and organic vapor generated during the vaporization process are transported into the oil and gas heat exchanger, cooled to room temperature with cold water, and then transported into the water-oil separator to form organic by-products.

6. The process method for continuously gasifying and purifying sulfur from oil-containing black sulfur according to claim 5, characterized in that, The sedimentation time is 3 - 6 hours.

7. A process for continuously gasifying and purifying sulfur from oil-containing black sulfur according to claim 5, characterized in that, The heating temperature of the upper heating tube is 250 - 270 °C, and the heating temperature of the lower heating tube is 300 - 320 °C.

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