CN114367246A

CN114367246A - Continuous melting and multi-phase separation system

Info

Publication number: CN114367246A
Application number: CN202210036704.9A
Authority: CN
Inventors: 沈齐晖; 赵雅晶; 沈立嵩
Original assignee: Individual
Current assignee: Individual
Priority date: 2022-01-13
Filing date: 2022-01-13
Publication date: 2022-04-19

Abstract

The invention discloses a system and a method for continuous melting and multi-phase separation. The system is particularly suitable for the separation of stratified liquid-phase media after melting, preferably for the purification technology of water-containing sulphur particles in petrochemical, natural gas and metallurgical industries, and the related application of solvent recovery from sulphur solutions.

Description

Continuous melting and multi-phase separation system

Technical Field

The invention relates to a continuous melting and multi-phase separation system and a method, which are particularly suitable for the separation of stratified liquid-phase media after melting, preferably suitable for the purification technology of water-containing sulfur particles in petrochemical industry, natural gas and metallurgical industry, and the related application of recovering a solvent from a sulfur solution, and belong to the field of energy conservation and environmental protection.

Background

The hydrous sulfur pellets are a mixture mainly comprising sulfur pellets and a desulfurization solution (an aqueous ammonia solution or a sodium carbonate solution containing a secondary salt and a trace amount of a wet oxidation catalyst), and may contain a small amount of hydrocarbons or tar depending on the conditions of the sulfur pellet generation end.

The wet catalytic oxidation process is used in petrochemical, steel, coking and other industries to purify H₂When S is, H₂S is converted into fine sulfur particles and separated from the desulfurization solution; the sulphur particles separated are mixed with the desulphurisation liquor and possibly also with small amounts of hydrocarbons or tars, which the industry custom refers to as: a sulfur foam.

Typical composition and individual component characteristics of the sulfur foam can be found in table 1:

TABLE 1 typical composition and Individual component characteristics of Sulfur foams

The prior art is that sulfur foam is heated in a melting kettle, and the sulfur melting implementation process is as follows: charging sulfur foam → heating, separating clear liquid → reheating, transforming sulfur crystal form → continuing heating, melting sulfur particles into liquid sulfur → discharging sulfur slag and oil.

The current intermittent sulfur melting technology is characterized in that each step in the sulfur melting implementation process is sequentially operated in batches, the steps cannot be simultaneously operated in parallel, and the heat supply amount and the heating time need to be adjusted according to the temperature requirements of different steps.

The prior continuous sulfur melting technology is characterized in that: the steps of discharging liquid sulfur and exhausting sulfur slag and oil are carried out in sequence in batch operation in the process of melting sulfur, so that the operation condition of separating clear liquid is destroyed when discharging liquid sulfur and exhausting sulfur slag and oil, and the separating clear liquid cannot be continuously carried out. Essentially, the current continuous sulfur melting technology realizes that: 1) continuous "sulfur foam charge"; 2) when the operations of discharging liquid sulfur and discharging sulfur slag and oil are not carried out, the continuous operation of heating, separating clear liquid → reheating, sulfur crystal form conversion → continuously heating and melting sulfur particles into liquid sulfur can be realized; 3) when the operations of discharging liquid sulfur and discharging sulfur slag and oil are carried out, clear liquid can not be separated in equal amount; to prevent drainage difficulties due to increased viscosity of the liquid sulphur, it is also necessary to reduce or even stop the sulphur foam charge.

The current sulfur melting technology adopts a jacket kettle to melt sulfur particles into liquid sulfur. 1) Because the temperature gradient exists between the heating surface in the kettle and the center of the kettle, under the condition of no mechanical stirring, the sulfur particles in the central area of the kettle can not be reliably and completely melted, the discharged liquid sulfur mixed with the sulfur particles is a frequent phenomenon, and the heating time is prolonged or the heating intensity is improved after the state of the discharged liquid sulfur is observed manually; 2) because the density of the hydrocarbons or tar is lower than that of the liquid sulfur, the hydrocarbons or tar can be discharged out of the melting kettle only after the liquid sulfur is discharged; 3) the batch operation of the melting kettle and the need of manual direct observation of liquid sulfur medium and the like cause large field operation intensity and poor operation environment; 4) the temperature of discharged gas and clear liquid is high due to the high operating pressure of the melting kettle; in addition, the equipment temperature reduction-temperature rise process caused by batch operation of charging and discharging generates larger heating consumption and corresponding cooling consumption; as described in the relevant information, the lowest sulfur melt consumption is currently about 200Kg steam/t liquid sulfur.

At present, for sulfur melting technology of sulfur foam generated in the wet catalytic oxidation method, a melting kettle is operated under the pressure of more than 0.2MPa (g); the heating intensity of the sulfur-melted portion is low; the automation degree is low; the continuous operation is unstable.

So far, no continuous sulfur melting and multi-phase separation technology for hydrous sulfur particles, which has stable and continuous operation, low manual operation intensity, high operation efficiency and environmental friendliness, exists.

Disclosure of Invention

In view of the above, the present invention is directed to a continuous melting and multi-phase separation system and method for continuously dehydrating, deoiling, and melting sulfur from aqueous sulfur pellets that addresses the above-mentioned deficiencies in the treatment of aqueous sulfur pellets. According to the system and the method, the liquid-fusible solid mixed material can be continuously melted and subjected to multi-phase separation, such as continuous sulfur melting and multi-phase separation on the water-containing sulfur particles, so that non-condensable gas and solvent steam, clear liquid (the sulfur content is less than 1g/L), tar and liquid sulfur are obtained. The method has the outstanding advantages of improved liquid sulfur color, stable and continuous operation, environmental friendliness, low manual operation intensity and high operation efficiency, and greatly improves the treatment technical level of the water-containing sulfur particles.

In one aspect, the present invention relates to a continuous melting and multiple phase separation system, the system comprising:

the heat supply unit is used for enabling the heat medium to release energy so as to continuously provide driving force required by heating, evaporating and melting the liquid-meltable solid mixture;

a heat exchanger group for heating a liquid-soluble solid mixture, said heat exchanger group comprising a melting heater 5 for heating a meltable solid;

the multiphase separation tank is used for standing and layering the continuously added liquid-meltable solid mixed material; the multiphase separation tank comprises a multiphase separation tank 7, the multiphase separation tank 7 is connected with the melting heater 5 in the heat exchanger group in the vertical direction to form a melting-separation kettle body, and the melting-separation kettle body can completely melt soluble solid particles without mechanical stirring; and discharging the product of each phase out of the system; the products of each phase include gas-phase products and liquid-phase products (such as liquid-phase product YI, liquid-phase product YII, and liquid-phase product YIII);

the liquid level maintaining mechanism comprises a discharge system of each liquid-phase product, and is used for stably discharging each continuous liquid-phase product which is equal to the fed material and is continuously discharged out of the system under the condition that the adjusting mechanism is not arranged; and a control system for adjusting the temperature of the liquid-meltable solid mixture and the respective phase products, the pressure and level in the melting-separating vessel during operation of the system.

In another aspect, the present invention also relates to a method for continuous melt-in and multiphase separation using the above system, the method comprising:

s1, after heat exchange is carried out on a continuously added liquid-fusible solid mixed material and a heating medium for heating, evaporating and melting the liquid-fusible solid mixed material, completely melting fusible solid particles under the condition of no mechanical stirring;

s2, standing and layering the molten liquid-meltable solid mixed material in a multiphase separation tank 7 to form each phase product; the respective phase products include a gas phase product and a liquid phase product (liquid phase product YI, liquid phase product YII, and liquid phase product YIII);

s3, continuously discharging each liquid-phase product through the liquid level maintaining mechanism and keeping the thickness of the liquid layer of each layered product in the multiphase separation tank 7 unchanged;

s4, keeping the operating pressure of 0.01-0.8 MPa through a control system, and discharging a gas-phase product;

s5, continuously and automatically discharging a liquid-phase product YI with the minimum density, a liquid-phase product YII with the intermediate density and a liquid-phase product YII from top to bottom respectively through the liquid level keeping mechanism along the height direction;

s6, regulating the temperature T2 in the multi-phase separation tank 7 to be stably kept in a certain range lower than T1 through the control system; adjusting the outlet temperature T1 of the liquid-phase product YIIII to be stably kept higher than the melting point and the boiling point of the meltable solid medium;

and S7, depositing the solid slag with the density higher than that of the liquid-phase product YIIII at the bottom, gradually accumulating and intermittently discharging.

In another aspect, the present invention also relates to the use of the above-described continuous melting and multiple phase separation system in a continuous melting and multiple phase separation technique for aqueous sulphur particles.

In another aspect, the present invention also relates to a system for continuous melting and multiple phase separation of aqueous sulphur particles, the system comprising: a heat supply unit, a heat exchanger group, a multiphase separation tank, a liquid level maintaining mechanism and a control system,

the heat medium in the heat supply unit comprises a heat medium with the temperature higher than the melting point of the fusible solid, such as: steam F or heat transfer oil F'; the heat exchanger group is used for providing heating, evaporation and melting heat for the sulfur foam raw material A;

the heat exchanger group comprises a melting heater 5 and a heat conduction oil heater 4 'when heat conduction oil F' is used;

the multi-phase separation tank comprises a multi-phase separation tank 7 which is vertically and coaxially connected with the heat exchanger group to form a melting-separation kettle, and each phase product is stably discharged through the liquid level maintaining mechanism while the sulfur foam raw material A is continuously added, wherein each phase product comprises a gas phase product and a liquid phase product (such as a liquid phase product YI, a liquid phase product YII and a liquid phase product YIIII);

the liquid level maintaining mechanism is a discharge pipe system which is arranged on the melting-separating kettle according to the height difference of the pipe bottom of each liquid phase medium discharge pipe determined by the density difference of different liquid phase products, such as a discharge port I, a discharge port II and a discharge port III;

the control system comprises a material level meter L1 and a temperature meter T1 to E, which are arranged on the melting-separating kettle

T4, pressure gauge P1, regulating valve TV2 and heating regulator TC1 provided on the sulfur foam feed line, and pressure regulator PV1 on the gas phase QI discharge pipe.

In another aspect, the present invention relates to a method for continuous melting and multiple phase separation using the above system, the method comprising:

s1, continuously adding a sulfur foam raw material A, exchanging heat with a heating medium for heating, evaporating and melting the sulfur foam raw material A, and then feeding the sulfur foam raw material A into a multiphase separation tank 7 of a melting-separation kettle from the top of the melting-separation kettle; the sulfur particles descending from the multiple phase separation tank 7 to the melting heater 5 are completely melted in the liquid sulfur flow passage of the melting heater 5 without mechanical stirring; the heat medium comprises steam F or heat conducting oil F';

s2, the molten sulfur foam raw material A generates various phase products in the melting separation kettle, and the production comprises the following steps: gas phase QI, liquid phase product YI, liquid phase product YII, and liquid phase product YII;

s3, adjusting a loop by controlling the PC1, keeping the operation pressure of the melting-separating kettle at 0.01-0.8 MPa, and removing gas products QI; simultaneously, continuously discharging the liquid-phase product YI from the melt-separation tank through a discharge port I;

s4, adjusting the temperature T2 in the multi-phase separation tank 7 to be kept at 85-130 ℃ stably through TC 2; adjusting the outlet temperature T1 of the liquid sulfur E through TC1 to stably maintain 130-150 ℃;

s5, gradually accumulating the liquid layer of the liquid-phase product YI and the liquid layer of the liquid-phase product YII to form a YII liquid layer, wherein the liquid-phase product YI, the liquid-phase product YII and the liquid-phase product YII are automatically discharged through a liquid level maintaining mechanism; stably maintaining the interface of the YI, YII and YII liquid layers;

s6, depositing the sulfur slag with the density larger than that of the liquid-phase product YIIII at the bottom, gradually accumulating, and intermittently discharging.

In another aspect, the present invention relates to a system for continuous melting and multiple phase separation of aqueous sulfur granules, the system comprising: a heat supply unit, a heat exchanger group, a multiphase separation tank, a liquid level maintaining mechanism and a control system,

the heat exchanger group comprises a preheater 9, a heater 1, a melting heater 5 and a heat conduction oil heater 4 'when heat conduction oil F' is used;

the multiphase separation tank comprises a multiphase separation tank 7 which is vertically and coaxially connected with the melting heater 5 to form a melting-separating kettle, and each phase product is stably discharged through the liquid level maintaining mechanism while the sulfur foam raw material A is continuously added, wherein each phase product comprises: non-condensable gas B, clear liquid C, tar D, and liquid sulfur E;

the heat medium in the heat supply unit comprises steam F or heat conducting oil F'; when the heating medium of the heat supply unit is steam F, the heat supply unit comprises a steam trap 2, an outlet at the bottom of a cone below the melting heater 5 is connected with the steam trap 2, and generated steam condensate water G is discharged after heat exchange of the heater 1; or when the heat medium of the heat supply unit is heat conduction oil F ', the heat supply unit comprises a heat conduction oil expansion tank 2 ' and a heat conduction oil pump 3 '; the heat conduction oil pump 3 'is connected with the heat conduction oil heater 4'; the outlet of the heat-conducting oil heater 4 ' is connected with the inlet of the melting heater 5, the heat-conducting oil heater and the heat-conducting oil pump 3 ' form a circulation loop through the outlet of the multiphase separation tank 7 via the heater 1, and the heat-conducting oil expansion tank 2 is externally connected with the circulation loop and is arranged at the front end of the heat-conducting oil pump 3 ';

the liquid level maintaining mechanism comprises a discharge port I, a discharge port II and a discharge port III; determining the tube bottom height difference of the discharge port I, the discharge port II and the discharge port III through the density difference of different liquid phase products;

the control system comprises a material level meter L1, a temperature meter T1-T4, a pressure meter P1, a regulating valve TV2 and a heat supply regulating device TC1 which are arranged on a sulfur foam feeding pipeline, and a pressure regulating device PV1 on a non-condensable gas B discharge pipe, wherein the material level meter L1, the temperature meter T1-T4, the pressure meter P1, the regulating valve TV 3838 and the heat supply regulating device TC1 are arranged on the melting-separating kettle.

In another aspect, the present invention relates to a method for continuous phase separation using the above system, the method comprising:

s1, continuously adding a sulfur foam raw material A into a multi-phase separation tank 7 of a melting-separation kettle after heat exchange of a preheater 9 and a heater 1, and completely melting sulfur particles descending from the multi-phase separation tank 7 to a melting heater 5 in a liquid sulfur flow channel of the melting heater 5 under the condition of no mechanical stirring after the heat exchange of the sulfur foam raw material A and a heat medium for heating, evaporation and melting; the heat medium comprises steam F or heat conducting oil F'; when the heating medium is steam F, the steam F firstly enters a jacket of a multi-phase separation tank 7, the steam or steam-water mixture which is discharged from the jacket of the multi-phase separation tank 7 is sent to a melting heater 5, and steam condensate G discharged from the melting heater 5 enters a steam trap 2 and then is subjected to heat exchange by a heater 1 to discharge the generated steam condensate G; or when the heat medium is heat conducting oil F ', the heat conducting oil F ' is sent into the heat conducting oil heater 4 through the heat conducting oil pump 3, the heat conducting oil F ' in the heat conducting oil heater 4 is heated and then sent into the melting heater 5, the heat conducting oil F ' discharged out of the melting heater 5 enters a jacket of the multiphase separation tank 7, and the heat conducting oil F ' discharged out of the jacket of the multiphase separation tank 7 returns to an inlet of the heat conducting oil pump 3 through the heater 1;

s2. the molten sulfur foam feedstock A produces, in the melt-separation kettle, various phase products including:

non-condensable gas B, clear liquid C, tar D, and liquid sulfur E;

s3, adjusting a loop by controlling the PC1, keeping the operation pressure of the melting-separation kettle at 0.01-0.8 MPa, and removing gas phase products QI; simultaneously, the clear liquid C is continuously discharged from the melting-separating kettle through a discharge port I by gravity flow;

s5, gradually accumulating and forming tar D between the liquid layer of the clear liquid C and the liquid layer of the liquid sulfur E, wherein the tar D is discharged through a discharge port II in a self-flowing manner; the liquid sulfur E is discharged through a discharge port III in a self-flowing manner; keeping the interface of the clear liquid C, the tar D and the liquid sulfur E stable;

s6, depositing the sulfur slag with the density larger than that of the liquid sulfur E at the bottom, gradually accumulating, and intermittently discharging.

Compared with the prior art, the continuously operating multi-item separation system and the method have the following advantages:

1) the operating pressure of the continuously operating multi-item separation system is obviously reduced;

2) the operation pressure intensity, the temperature gradient and the interfaces of all material layers in the melting-separating kettle are continuously and stably maintained;

3) the adding amount of the heat supply medium corresponds to the feeding amount of the sulfur foam raw material and the components of the sulfur foam raw material are self-adaptively adjusted;

4) various media except sulfur slag separated by the melting-separating kettle can be continuously discharged, and the discharge amount of each medium is adaptively matched with the feeding amount and the components of the sulfur foam raw material;

5) because the melting heater adopts the dividing wall type heat exchanger except the jacket heat exchanger, the heat exchange area (tube bundle or multilayer/ring plate) of the melting heater is much larger than that of a melting-separating kettle of the single-layer inner wall of the jacket, the heating intensity is obviously improved, the distance between the heat transfer wall surface and the center of the flow channel is greatly reduced, the sulfur particles at the center of the flow channel can be reliably and completely melted under the condition of no mechanical stirring, and the discharged liquid sulfur is prevented from being mixed with the sulfur particles;

6) the measure of continuously separating and discharging tar and intermittently discharging sulfur slag improves the color of liquid sulfur and reduces organic matters and ash content; meanwhile, the temperature gradient in the melting-separating kettle of the system avoids the salt in the residual desulfurization solution from transferring to the melting-separating kettle in the prior art caused by temperature batch heating of the melting-separating kettleProblems in liquid sulfur, further reducing liquid sulfur ash; the system for continuously melting and multi-phase separating the water-containing sulfur particles avoids O brought into a melting-separating kettle in the charging and discharging processes of the intermittent sulfur melting technology₂So that the liquid sulfur acidity is reduced;

7) the continuously-operated multi-item separation system and the method have the advantages of high overall heat conductivity coefficient, low operation condition, high production efficiency and small equipment volume;

8) the material and energy consumption of the system is obviously reduced through the cascade heat exchange between the media;

9) the monitoring measures are indirect and complete, the operating conditions are good, the starting and stopping are convenient and fast, and the manual operation intensity is obviously reduced;

10) the closed continuous disposal mode avoids the volatilization and the dissipation of gas, and realizes the essential cleanness of the disposal process.

The continuous operation multiple separation system and method greatly improve the resource utilization level of the water-containing sulfur particles in the industries such as petrochemical industry, natural gas, metallurgy and the like, and have extremely high economic value and environmental protection value.

Drawings

FIG. 1 is a system flow chart of embodiments 1-2, 4-6 of the present invention.

FIG. 2 is a system flowchart of embodiments 3, 4 to 6 of the present invention.

Symbolic illustrations of the main devices, components and media:

the device comprises a heater 1, an expansion tank 2 ', a steam trap 2, a heat-conducting oil pump 3 ', a heat-conducting oil heater 4 ', a melting heater 5, a liquid collecting disc 6, a multiphase separation tank 7, a liquid collecting disc 8, a preheater 9, a distributor 10 and a valve 11.

Liquid-fusible solid mixture (preferably sulfur foam material A), non-condensable gas B, clear liquid C, tar D, liquid sulfur E, heating medium F and steam condensate G.

FIG. 3 is a bottom high differential view of the discharge piping of the system for continuous melting and multiple phase separation of aqueous sulfur granules according to the present invention.

Detailed Description

The present invention will be described in detail below with reference to specific embodiments and examples, and the advantages and various effects of the present invention will be more clearly apparent therefrom. It will be understood by those skilled in the art that these specific embodiments and examples are for the purpose of illustrating the invention and are not to be construed as limiting the invention.

Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. If there is a conflict, the present specification will control.

Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.

According to the continuous melting and multiphase separation system, the component devices/parts/heat transfer media can be combined into a plurality of integrated parts/devices or a set of integrated devices according to the medium flow direction sequence and the butt joint of process functions. Combinations and modifications of the above should be understood to be within the scope of the present application and its equivalents.

The "melting heater" in the invention refers to: a heat transfer member for indirectly heating the liquid-meltable solid mixture with the heat medium and melting the meltable solid.

The 'multiphase separation tank' in the invention refers to: and (3) a part for standing and layering multiple layers of liquid and non-condensable gas obtained after the liquid-meltable solid mixture is heated.

The melting-separating kettle is a combination of the heater and a multiphase separating tank in any operable mode, and the melting-separating kettle with the multiphase separating tank and the melting heater coaxially connected in the vertical direction is preferred.

The present invention provides a system for continuous melting and multiple phase separation, the system comprising:

the liquid level maintaining mechanism comprises a discharge system of each liquid-phase product, and is used for stably discharging each continuous liquid-phase product which is equal to the fed material and is continuously discharged out of the system under the condition that the adjusting mechanism is not arranged; and

and the control system is used for adjusting the temperature of the sulfur foam raw material A and each phase product, the pressure in the melting-separating kettle and the material level in the operation process of the system.

In certain embodiments of the present invention, the heat medium used in the heat supply unit is heat conducting oil or steam.

The heat medium is used in parallel in the components of the system, or used in series between the components of the system in a cascade manner.

In certain embodiments of the present invention, the heat exchanger group comprises a melting heater 5 and a conduction oil heater 4' when conduction oil is used as a heat medium, and the melting heater 5 is a cylinder-shaped, preferably cylindrical or rectangular cylinder. The liquid phase product YIIII and the meltable solid product vertically flow downwards in the cylinder and indirectly exchange heat with the heating medium, the liquid phase product YIIII reaches the bottom of the melting heater 5 and is completely melted, and the liquid phase product YIIII is discharged out of the system from the side part of the conical bottom of the melting heater 5.

Further, the conduction oil heater 4' is preferably a dividing wall type heat exchanger except for a jacket heat exchanger.

Further, the heat exchanger group also comprises a preheater 9 and a heater 1 for heating the liquid-meltable solid mixture, which are optional components of the system of the present invention, in order to further reduce the energy medium consumption of the system.

Furthermore, the preheater 9 and the heater 1 are arranged in series, according to different temperatures of inlet heat sources, the liquid-meltable solid mixed material fed into the system is subjected to indirect heat exchange with a liquid-phase product YI (such as supernatant) discharged from the melting-separating kettle with a lower temperature in the preheater 9 to heat up, and then is subjected to indirect heat exchange with steam condensate G or heat-conducting oil F' discharged from the melting-separating kettle with a higher temperature in the heater 1 to heat up, and then enters the multiphase separation tank 7 of the melting-separating kettle from the top of the melting-separating kettle; if the preheater 9 and the heater 1 are not arranged, the liquid-meltable solid mixed material fed into the system directly enters the multiphase separation tank 7 of the melting-separation kettle from the top of the melting-separation kettle at a lower temperature; the preheater 9 and the heater 1 of the system can also be integrated into an integrated heat exchanger for sectional heat exchange.

In some embodiments of the present invention, when the heating medium of the heating unit is steam F, the heating unit includes a steam trap 2, and an outlet below the melting heater 5 is connected to the steam trap 2 for discharging the generated steam condensate G.

In other embodiments of the present invention, when the heat medium of the heat supply unit is heat transfer oil F ', the heat supply unit includes a heat transfer oil expansion tank 2', a heat transfer oil pump 3 ', and a heat transfer oil heater 4'; the heat conduction oil pump 3 'is connected with the heat conduction oil heater 4'; the outlet of the heat conduction oil heater 4 'is connected with the inlet of the melting heater 5, and forms a circulation loop with the heat conduction oil pump 3' through the outlet of the multiphase separation tank 7. The heat conducting oil expansion tank 2 is externally connected with the circulation loop and is arranged at the front end of the heat conducting oil pump 3'.

In some embodiments of the present invention, the multi-phase separation tank 7 is a liquid containing tank body provided with a distributor 10, a liquid collecting tray 8 and a liquid collecting tray 6, and the multi-phase separation tank 7 is coaxially connected with the melting heater 5 in the heat exchanger group in the vertical direction.

Further, the liquid-meltable solid mixture entering the multiphase separation tank 7 is in direct countercurrent contact with rising gas in the multiphase separation tank 7 in the upper space of the distributor 10, so that gas phase QII serving as condensable gas in the rising gas is condensed and cooled, and the gas phase QI serving as non-condensable gas B is discharged out of the system; the liquid-phase product YI is collected by the liquid collecting tray 8 and then is continuously discharged through the discharge port I; the liquid-phase product YII is collected from the liquid collecting tray 6 and then continuously discharged; the liquid-phase product YIII and meltable solid product flow vertically downward into the melt heater 5.

In some embodiments of the present invention, the liquid level maintaining mechanism is a height difference of tube bottoms of the liquid phase medium discharge tubes determined according to density differences of different liquid phase products.

Further, the level maintenance mechanism includes a plurality of discharge ports, such as discharge port I, discharge port II, and discharge port III, for discharging the separation medium out of the system.

Further, taking the three-phase separation shown in fig. 3 as an example, the height difference of the tube bottom of each liquid-phase medium discharge tube can be calculated by the following formula:

h4 ═ H1+ H2+ H3 (formula I)

H5H 4-H1 + ρ 1 ÷ ρ 2 XH 1 (formula II)

H6 ═ H3+ ρ 1 ÷ ρ 3 × H1+ ρ 2 ÷ ρ 3 × H2 (formula III)

Wherein H1 is the liquid layer thickness of liquid phase I; h2 is the liquid layer thickness of liquid phase II; h3 is the liquid layer thickness of liquid phase III; h4 is the height of the discharge pipe I (corresponding to the total liquid layer height); h5 is the height of discharge pipe II; h6 is the height of discharge pipe III; ρ 1 is the density of the liquid phase I; ρ 2 is the density of the liquid phase II; ρ 3 is the liquid phase III density.

In certain embodiments of the invention, the discharge piping may be either fixedly or movably disposed.

In certain embodiments of the invention, the control system comprises instrumentation points on the melting-separation vessel for monitoring level, temperature and pressure, and regulating valves and heating regulators on the feed lines.

The present invention also provides a method for continuous melting and multiple phase separation using a system as described above, the method comprising:

In certain embodiments of the present invention, the heat medium is a heat medium having a temperature above the melting point of the meltable solid, such as: heat conducting oil or steam; preferably, the heat medium is used in parallel in the constituent devices of the system or used in series and in cascade between the constituent devices of the system.

In some embodiments of the present invention, when the heating medium is steam F, the steam F enters the jacket of the multi-phase separation tank 7, the steam or steam-water mixture exiting the jacket of the multi-phase separation tank 7 is sent to the melting heater 5, and the steam condensate G exiting the melting heater 5 is discharged after passing through the steam trap 2.

In some embodiments of the present invention, when the heat medium is heat transfer oil F ', the heat transfer oil F ' is sent into the heat transfer oil heater 4 through the heat transfer oil pump 3, the heat transfer oil F ' in the heat transfer oil heater 4 is heated and then sent into the melting heater 5, the heat transfer oil F ' discharged from the melting heater 5 enters the jacket of the multiphase separation tank 7, and the heat transfer oil F ' discharged from the jacket of the multiphase separation tank 7 returns to the inlet of the heat transfer oil pump 3.

In certain embodiments of the invention, the liquid-meltable solid mixture continuously fed into the system enters the multiphase knockout drum 7 of the melting-knockout drum directly from the top of the melting-knockout drum at a relatively low temperature; meanwhile, a heat medium (steam/heat conduction oil) is sent into a melting heater 5 of the melting-separating kettle and/or a jacket of a multiphase separating tank 7, and the heat medium F or steam condensate G with reduced enthalpy value after heat exchange is equivalently discharged out of the melting-separating kettle.

In certain embodiments of the invention, the liquid-meltable solid mixture continuously fed in S3 is heated in the multiphase knockout drum 7; because each medium liquid phase, such as the liquid phase product YI, the liquid phase product YI and the liquid phase product YIIII, are mutually insoluble and have density difference, the medium liquid phase is continuously discharged out of the multiphase separation tank 7 at a set position after being layered in the multiphase separation tank 7, wherein the gas phase product, the liquid phase product YI and the liquid phase product YII are cooled by heat exchange condensation or directly discharged out of a system through the liquid level keeping mechanism, and solid particles are discharged into the melting heater 5 through the liquid phase product YII between the multiphase separation tank 7 and the melting heater 5.

Alternatively, in other embodiments of the present invention, when the preheater 9 and the heater 1 are provided in the present system, the liquid-meltable solid mixture fed into the present system is first heated by indirect heat exchange with the liquid-phase product YI (such as clear liquid C) discharged from the lower-temperature melting-separating kettle in the preheater 9, and then heated by indirect heat exchange with the steam condensate G or heat transfer oil F' discharged from the higher-temperature melting-separating kettle in the heater 1, and then fed into the multiphase separation tank 7 of the melting-separating kettle from the top of the melting-separating kettle.

In certain embodiments of the invention, the temperature of the heat medium entering the melt-separation tank of the system of the invention is greater than 120 ℃.

In some embodiments of the present invention, the upper limit of the operation pressure of the melting-separating vessel is not limited theoretically, the lower limit of the operation pressure is higher than 85kpa (a), and the operation pressure of the present invention is determined to be 0.01 to 0.8MPa according to the system pressure of the absorption end of the gas phase product (non-condensable gas B), so that the gas phase product (non-condensable gas B) saturated by the solvent vapor in the system is discharged and the system is kept stable.

Preferably, the absolute pressure is 0.09-0.18 MPa (a).

In certain embodiments of the invention, 85 ℃ < T2<95 ℃; 135 < T1<142 ℃.

In certain embodiments of the present invention, a liquid layer of YII is gradually formed by accumulating between a liquid layer of the liquid-phase product YI having the smallest density and a liquid layer of the liquid-phase product YII having the largest density, wherein the liquid-phase product YI, the liquid-phase product YII, and the liquid-phase product YII are each self-flowing discharged via a liquid level maintaining mechanism; liquid level holding mechanism the liquid level holding mechanism stably holds the interfaces of the YI liquid layer, the YII liquid layer, and the YII liquid layer.

In certain embodiments of the present invention, the liquid level maintaining mechanism is only a combination of the respective separated medium discharging pipes, and the height difference between the respective separated medium discharging pipes is designed by considering the density difference of the respective separated media and the thickness of the liquid layer of the respective separated media stably held in the multi-phase separation tank. The liquid level maintaining mechanism of the invention can have the following functions: 1) continuously discharging the corresponding separated media with equal raw material liquid addition amount at the liquid layer position of each separated media in the multi-phase separation tank; 2) the continuous addition of the raw material liquid and the continuous discharge of each separated medium in equal amounts allows each separated medium to continuously maintain a liquid layer thickness at a determined liquid layer position.

In certain embodiments of the present invention, the continuous melting and multiple phase separation systems of the present invention can be used for emulsion separation. For example, emulsion a formed by mixing media b, c and d generally cannot be separated by standing, and can be broken only by heating. With the system of the present invention, it is possible to heat the emulsion a continuously → stratify statically → discharge the separated media b, c and d continuously through the discharge piping. If the multiphase separation tank top temperature T4 is higher than the boiling point of separation medium b, the separated media c and d are continuously discharged through a liquid phase discharge piping.

The present invention also provides a system for continuous melting and multiple phase separation of aqueous sulphur particles, the system comprising: a heat supply unit, a heat exchanger group, a multiphase separation tank, a liquid level maintaining mechanism and a control system,

the heat medium in the heat supply unit comprises steam F or heat conducting oil F'; the heat exchanger group is used for providing heating, evaporation and melting heat for the sulfur foam raw material A;

the liquid level maintaining mechanism is a discharge port I, a discharge port II and a discharge port III which are arranged on the melting-separating kettle according to the height difference of the tube bottoms of the liquid phase medium discharge tubes determined by the density difference of different liquid phase products;

the control system comprises a material level meter L1, a temperature meter T1-T4, a pressure meter P1, a regulating valve TV2 and a heat supply regulating device TC1 which are arranged on a sulfur foam feeding pipeline, and a pressure regulating device PV1 on a gas-phase product discharge pipe, wherein the material level meter L1, the temperature meter T1-T4 and the pressure meter P1 are arranged on the melting-separation kettle.

In certain embodiments of the present invention, the heat medium is heat transfer oil or steam; preferably, the heat medium is used in parallel in the constituent devices of the system or used in series and in cascade between the constituent devices of the system.

In certain embodiments of the invention, the melting heater 5 is a multi-plate parallel or multi-tube parallel dividing wall heater with a jacketed conical bottom; preferably, the melting heater 5 is a cylindrical heater. The heat exchange area (tube bundle or multilayer/ring plate) of the melting heater 5 is much larger than that of the melting-separating kettle of the single-layer inner wall of the jacket, the heating intensity is obviously improved, and the distance between the heat transfer wall surface and the center of the flow channel is greatly reduced. The liquid phase product YIIII (such as liquid sulfur E) and sulfur particles flow vertically downwards in the cylinder and indirectly exchange heat with a heating medium to reach the bottom of the melting heater 5 to be completely melted, and the liquid phase product YIIII is discharged out of the system from the side part of the conical bottom of the melting heater 5.

Further, the heat exchanger group also comprises a preheater 9 and a heater 1 which are optional components of the system, and the aim is to further reduce the energy medium consumption of the system.

Furthermore, the preheater 9 and the heater 1 are arranged in series, according to different temperatures of inlet heat sources, the sulfur foam raw material A sent into the system is subjected to indirect heat exchange with a liquid-phase product YI (clear liquid C) discharged from the melting-separating kettle with a lower temperature in the preheater 9 to heat up, and then is subjected to indirect heat exchange with steam condensate G or heat-conducting oil F' discharged from the melting-separating kettle with a higher temperature in the heater 1 to heat up, and then enters the multiphase separation tank 7 of the melting-separating kettle from the top of the melting-separating kettle; if the preheater 9 and the heater 1 are not arranged, the sulfur foam raw material A fed into the system directly enters the multiphase separation tank 7 of the melting-separation kettle from the top of the melting-separation kettle at a lower temperature; the preheater 9 and the heater 1 of the system can also be integrated into an integrated heat exchanger for sectional heat exchange.

In some embodiments of the present invention, when the heating medium of the heating unit is steam F, the heating unit comprises a steam trap 2, and the bottom outlet of the lower cone of the melting heater 5 is connected to the steam trap 2 for discharging the generated steam condensate G.

In other embodiments of the present invention, when the heat medium of the heat supply unit is heat transfer oil F ', the heat supply unit includes a heat transfer oil expansion tank 2 ' and a heat transfer oil pump 3 '; the heat conduction oil pump 3 'is connected with the heat conduction oil heater 4'; the outlet of the heat-conducting oil heater 4 ' is connected with the inlet of the melting heater 5, and forms a circulation loop with the heat-conducting oil pump 3 ' through the outlet of the multiphase separation tank 7, and the heat-conducting oil expansion tank 2 is externally connected with the circulation loop and is arranged at the front end of the heat-conducting oil pump 3 '.

In some embodiments of the present invention, the multi-phase separation tank 7 is a liquid containing tank body provided with a distributor 10, a liquid collecting tray 8 and a liquid collecting tray 6. The multiphase separation tank 7 is coaxially connected with the melting heater 5 in the heat exchanger group in the vertical direction. The heat required by the temperature rise of each medium in the multi-phase separation tank 7 is conducted from bottom to top in a heat conduction mode between each medium layer and a convection mode in each layer, and the efficiency of the direct heat exchange mode is improved compared with the efficiency of the indirect heat exchange mode.

In certain embodiments of the present invention, the liquid level maintaining mechanism is a drain piping having a difference in height of bottom of each liquid phase medium drain pipe determined according to a difference in density of different liquid phase products.

h4 ═ H1+ H2+ H3 (formula I)

H5H 4-H1 + ρ 1 ÷ ρ 2 XH 1 (formula II)

H6 ═ H3+ ρ 1 ÷ ρ 3 × H1+ ρ 2 ÷ ρ 3 × H2 (formula III)

In certain embodiments of the invention, the gas phase product is non-condensable gas B, the liquid phase product YI is clear liquid C, the liquid phase product YII is tar D, and the liquid phase product YIII is liquid sulfur E.

The present invention also provides a method for continuous melting and multiple phase separation using the above system, the method comprising:

In certain embodiments of the present invention, the amount of the heat medium added in S1 is adaptively adjusted by the TC1 regulation loop in relation to the amount of the sulfur foam raw material a fed and the water content therein.

In certain embodiments of the present invention, wherein the temperature of the heat medium entering the melt-separation tank in the system of the present invention is greater than 130 ℃.

According to some embodiments of the present invention, preferably, the two heat media are used in parallel in the constituent devices of the system or in series and in cascade between the constituent devices of the system.

According to some embodiments of the present invention, when the heating medium is steam F, the steam F is first fed into the jacket of the multiple phase separation tank 7, the steam or steam-water mixture discharged from the jacket of the multiple phase separation tank 7 is fed into the melting heater 5, and the steam condensate G discharged from the melting heater 5 is discharged through the steam trap 2.

According to other embodiments of the present invention, when the heat medium is heat transfer oil F ', the heat transfer oil F ' is fed into the heat transfer oil heater 4 through the heat transfer oil pump 3, the heat transfer oil F ' in the heat transfer oil heater 4 is heated and then fed into the melting heater 5, the heat transfer oil F ' discharged from the melting heater 5 enters the jacket of the multiphase separation tank 7, and the heat transfer oil F ' discharged from the jacket of the multiphase separation tank 7 returns to the inlet of the heat transfer oil pump 3.

According to certain embodiments of the present invention, the sulfur foam feed a fed to the present system enters the multiphase knockout drum 7 of the melting-knockout drum directly from the top of the melting-knockout drum at a lower temperature; meanwhile, a heat medium (steam/heat conduction oil) is sent into a melting heater 5 of the melting-separating kettle and/or a jacket of a multiphase separating tank 7, and the heat medium F or steam condensate G with reduced enthalpy value after heat exchange is equivalently discharged out of the melting-separating kettle.

In some embodiments of the present invention, the upper limit of the operation pressure of the melting-separating vessel is not limited theoretically, the lower limit of the operation pressure is higher than 85kpa (a), and the operation pressure of the present invention is determined to be 0.01 to 0.8MPa according to the system pressure of the absorption end of the gas phase product (non-condensable gas B), so that the gas phase product (non-condensable gas B) saturated by the solvent vapor in the system is discharged and the system is kept stable. Since the operating pressure of the multi-phase separator tank 7 according to the invention is lower than in the prior art, less heat is required for the temperature rise of the media.

Preferably, the absolute pressure is 0.09-0.18 MPa (a). The operating pressure of the melting-separating kettle is maintained by adjusting a loop through PC 1;

in certain embodiments of the invention, the temperature T2 at the bottom of the multiphase separation tank 7 of the melt-separation kettle is maintained constantly at a value between 85 and 130 ℃ by means of a TC2 regulation loop in S4; meanwhile, the temperature T1 of liquid sulfur at the outlet of the melting heater 5 of the melting-separating kettle is stably maintained between 130 ℃ and 150 ℃ through a TC1 regulating loop.

In certain embodiments of the invention, 85 ℃ < T2<95 ℃; 135 < T1<142 ℃.

The liquid phase product YIII and solid sulfur particles vertically flow downwards in the cylinder of the melting heater 5 and indirectly exchange heat with a heating medium F, the liquid phase product YIII reaches the bottom of the melting heater 5 and is completely melted, and the liquid phase product YIII is discharged out of the system through a discharge port III at the side part of the conical bottom of the melting heater 5.

Specifically, a distributor 10, a liquid collecting tray 8 and a liquid collecting tray 6 are arranged in the multiphase separation tank 7; the sulfur foam raw material A entering the multiphase separation tank 7 is in direct countercurrent contact with ascending steam in the multiphase separation tank 7 in the upper space of the distributor 10, a gas-phase product serving as condensable steam in the ascending steam is condensed and cooled, and the gas-phase product serving as non-condensable gas B is discharged out of the system; the sulfur foam raw material a dropped by the distributor 10 is dropped to a lower position of the liquid collecting tray 8; the liquid-phase product YI is collected by the liquid collecting tray 8 and then is continuously discharged through the discharge port I; the liquid-phase product YII is collected by the liquid collecting tray 6 and then is continuously discharged through the discharge port II; the liquid-phase product YIII and sulfur particles flow vertically downward into the melting heater 5.

In certain embodiments of the present invention, a heat medium is continuously added to the melting heater 5 of the melting-separating kettle to indirectly heat the liquid sulfur and sulfur particles entering the melting heater 5 to 130-150 ℃; the liquid phase product YIII (liquid sulfur) and sulfur particles reach the bottom of the melting heater 5 and are completely melted, and the liquid phase product YIII is continuously discharged from the system from the side part of the conical bottom of the melting heater 5; the material with the density higher than that of the liquid sulfur is deposited at the bottom of the cone bottom of the melting heater 5 and is discharged intermittently according to the situation; the material having a density lower than that of the liquid-phase product YIIII floats on the liquid layer of the liquid-phase product YIIII. The liquid phase product YIIII and the sulfur particles transfer heat in a heat conduction mode, and meanwhile, due to the density difference caused by the temperature difference of the upper end and the lower end in the liquid sulfur layer, the liquid phase product YIIII generates convection in a heat exchange tube bundle of the melting heater 5 or among heat exchange plates, so that the stirring effect is achieved, namely: by utilizing the thermal stirring effect in the heat exchange tube bundle or among the heat exchange plates, the sulfur particles at the center of the flow channel can be reliably and completely melted under the condition of no mechanical stirring, and the sulfur particles reach the bottom of the melting heater 5 and are completely melted, so that the discharged liquid-phase product YIIII is prevented from being mixed with the sulfur particles.

In certain embodiments of the present invention, the upper material of the liquid layer of the liquid-phase product YII is the liquid-phase product YII having a density between the liquid-phase product YII and the liquid-phase product YII, the liquid-phase temperature of the liquid-phase product YII is between 85 and 130 ℃, the height of the liquid layer of the liquid-phase product YII at the lower edge of the liquid collecting tray 6 is continuously pressed out of the multiphase separation tank 7 of the melting-separation kettle, and the discharge amount of the liquid-phase product YII is equal to the intake amount of the liquid-phase product YII into the melting-separation kettle.

The continuous melting and multi-phase separation system of the water-containing sulfur particles is characterized in that the preheater 9, the heater 1, the melting heater 5 and the heat conducting oil heater 4 are divided wall type heat exchangers except a jacket heat exchanger.

The present invention also provides a system for continuous melting and multiple phase separation of aqueous sulphur particles, the system comprising: the heat supply unit consists of a heat exchanger group, a multiphase separating tank, a liquid level maintaining mechanism and a control system,

the liquid level maintaining mechanism comprises a discharge port I, a discharge port II and a discharge port III, and the height difference of the bottom of the pipe is determined according to the density difference of different liquid phase products;

In certain embodiments of the invention, the melting heater 5 is a multi-plate parallel or multi-tube parallel dividing wall heater with a jacketed conical bottom; preferably, the melting heater 5 is a cylindrical heater. The heat exchange area of the fusion heater 5 (tube bundle or multi-layer/ring plate) is much larger than that of the multi-phase separation tank 7 (jacket single-layer inner wall), and the fusion heater 5 can be understood as the heat-transferring 'heart' component in the system of the present invention.

In some embodiments of the present invention, the heat transfer oil or steam as the heat transfer medium may be used in parallel in the constituent devices of the system or in cascade between the constituent devices of the system.

In certain embodiments of the invention, the melting heater 5 is a multi-plate parallel or multi-tube parallel dividing wall heater with a jacketed conical bottom; preferably, the melting heater 5 is a cylindrical heater. The heat exchange area (tube bundle or multilayer/ring plate) of the melting heater 5 is much larger than that of the melting-separating kettle of the single-layer inner wall of the jacket, the heating intensity is obviously improved, and the distance between the heat transfer wall surface and the center of the flow channel is greatly reduced. The liquid phase product YIIII (liquid sulfur E) and sulfur particles vertically flow downwards in the cylinder and indirectly exchange heat with a heating medium to reach the bottom of the melting heater 5 to be completely melted, and the liquid sulfur E is discharged out of the system from the side part of the conical bottom of the melting heater 5.

In certain embodiments of the invention, the discharge piping may be a fixed height setting or a height adjustable setting.

s2. the molten sulfur foam feedstock A produces, in the melt-separation kettle, various phase products including: non-condensable gas B, clear liquid C, tar D, and liquid sulfur E;

s4, adjusting the temperature T2 in the multi-phase separation tank 7 to be kept at 85-130 ℃ stably through TC 2;

adjusting the outlet temperature T1 of the liquid sulfur E through TC1 to stably maintain 130-150 ℃;

Preferably, the absolute pressure is 0.09-0.18 MPa (a).

In certain embodiments of the invention, the temperature T2 at the bottom of the multiphase separation tank 7 of the melt-separation kettle is maintained stably between 85 and 130 ℃ by a TC2 regulation loop in S3, namely: controlling the feeding amount of the sulfur foam raw material A of the melting-separating kettle according to the temperature; meanwhile, the temperature T1 of liquid sulfur at the outlet of the melting heater 5 of the melting-separating kettle is stably maintained between 130 ℃ and 150 ℃ by a TC1 regulating loop, namely: the feeding amount of the heat medium of the melting-separating kettle is controlled according to the temperature.

In certain embodiments of the invention, 85 ℃ < T2<95 ℃; 135 < T1<142 ℃.

The liquid sulfur E and the solid sulfur particles vertically flow downwards in the cylinder of the melting heater 5 and indirectly exchange heat with a heating medium F, the liquid sulfur E reaches the bottom of the melting heater 5 and is completely melted, and the liquid sulfur E is discharged out of the system through a discharge opening III on the side part of the conical bottom of the melting heater 5.

Specifically, a distributor 10, a liquid collecting tray 8 and a liquid collecting tray 6 are arranged in the multiphase separation tank 7; the sulfur foam raw material A entering the multiphase separation tank 7 is in direct countercurrent contact with rising steam in the multiphase separation tank 7 in the upper space of the distributor 10, the rising steam is condensed and cooled as condensable steam, and the condensable steam is discharged out of the system as a gas-phase product of non-condensable gas B; the sulfur foam raw material a dropped by the distributor 10 is dropped to a lower position of the liquid collecting tray 8; the clear liquid C is collected by the liquid collecting disc 8 and then is continuously discharged through the discharge port I; the tar D is collected from the liquid collecting disc 6 and then is continuously discharged through the discharge port II; the liquid sulfur E and sulfur particles flow vertically downward into the melting heater 5.

In certain embodiments of the invention, a heat medium is continuously added to the melting heater 5 of the melting-separating kettle to indirectly heat the liquid sulfur E and the sulfur particles entering the melting heater 5 to 130-150 ℃; the liquid sulfur E and the sulfur particles reach the bottom of the melting heater 5 and are completely melted, and the liquid sulfur E is continuously discharged out of the system from the side part of the conical bottom of the melting heater 5; the material with the density larger than that of the liquid sulfur E is deposited at the bottom of the cone bottom of the melting heater 5 and is discharged intermittently according to the situation; the material with density less than that of the liquid sulfur E floats on the liquid layer of the liquid sulfur E.

In some embodiments of the invention, the upper material of the liquid layer of the liquid sulfur E is tar D with the density between that of the liquid sulfur E and that of the clear liquid C, the temperature of the liquid layer of the tar D is between 85 and 130 ℃, the height of the liquid layer of the tar D is continuously pressed out of the multiphase separation tank 7 of the melting-separation kettle at the lower edge of the liquid collecting tray 6, and the discharge amount of the tar D is equal to the entering amount of the tar D entering the melting-separation kettle.

In some embodiments of the present invention, the upper layer material of the tar D is a lower density clear liquid C, the liquid layer temperature of the clear liquid C is between 85 and 95 ℃, the height of the clear liquid C is continuously discharged from the multiphase separation tank 7 of the melting-separation kettle at the upper edge of the liquid collecting tray 8, and the discharge amount of the clear liquid C is slightly less than that of the clear liquid C entering the melting-separation kettle (wherein the difference is the discharge amount of gas phase products).

In certain embodiments of the invention, the preheater 9, heater 1, melting heater 5, and conduction oil heater 4 are in the form of dividing wall heat exchangers other than jacket heat exchangers.

Specifically, the system heats the sulfur foam raw material A with lower temperature into non-condensable gas B with higher temperature, clear liquid C, tar D and liquid sulfur E, and the non-condensable gas B, the clear liquid C, the tar D and the liquid sulfur E are separated at different positions of the melting-separating kettle, and the required heat is provided by a heat medium; under the heat transfer and heat exchange effects of the melting heater 5, the preheater 9 and the heater 1, the clear liquid C, the tar D and the liquid sulfur E are in direct liquid-liquid contact in the multiphase separation tank 7, heat is transferred among layers in a heat conduction mode, and heat is transferred in layers in a convection mode; due to the density difference between the non-condensable gas B, the clear liquid C, the tar D and the liquid sulfur E, the continuous sulfur foam raw material A added from the top of the multiphase separation tank 7 and the continuous phase change heat absorption of the sulfur particles, an obvious temperature gradient is formed in the melting-separation kettle of the invention, namely: the temperature is gradually increased from top to bottom.

Continuously adding a heat medium into a melting heater 5 of the melting-separating kettle to indirectly heat liquid sulfur E and sulfur particles entering the melting heater 5 to 130-150 ℃; the liquid sulfur and the sulfur particles reach the bottom of the melting heater 5 and are completely melted, and the liquid sulfur is continuously discharged from the system from the side part of the conical bottom of the melting heater 5; depositing the material with the density higher than that of the liquid sulfur on the bottom of the conical bottom of the melting heater 5, and intermittently discharging the material according to the situation; the material with density less than that of the liquid sulfur floats on the liquid sulfur layer. Heat is conducted between liquid sulfur and the sulfur particles in a heat conduction mode, and meanwhile, due to the density difference caused by the temperature difference between the upper end and the lower end in the liquid sulfur layer, convection occurs between the liquid sulfur and the heat exchange tube bundle or the heat exchange plates of the melting heater 5, so that the stirring effect is achieved, namely: by utilizing the thermal stirring effect in the heat exchange tube bundle or among the heat exchange plates, the sulfur particles at the center of the flow channel can be reliably and completely melted under the condition of no mechanical stirring, and the sulfur particles reach the bottom of the melting heater 5 and are completely melted, so that the discharged liquid sulfur is prevented from being mixed with the sulfur particles.

With the gradual melting of the sulphur particles, at the bottom of the multiphase separation tank 7 is a layer of liquid sulphur mixing moisture, tar and sulphur particles: when the sulfur particles are melted, moisture adhering to the surfaces and micropores of the sulfur particles vaporizes and rises due to a density difference with the sulfur particles; tar attached to the surface of the sulfur particles and in the micropores also rises up in a floating manner due to a density difference between the sulfur particles and the liquid sulfur; the moisture and tar adhered to the surfaces of the sulfur particles and in the micropores are separated from the liquid sulfur layer below the middle part of the melting heater 5, so that the color of the discharged liquid sulfur E is improved; the materials (non-melting ash) with density higher than that of the liquid sulfur are deposited at the bottom of the cone of the melting heater 5 and gradually accumulated.

The liquid sulfur E is continuously discharged from the system from the side part of the conical bottom of the melting heater 5; the material with density less than that of the liquid sulfur floats on the liquid sulfur layer.

The tar D can be gradually accumulated between the clear liquid layer and the liquid sulfur layer to form a tar layer, and the tar D can be discharged from the melting-separating kettle in a self-flowing manner; the liquid sulfur E will be discharged from the melting-separating vessel by gravity flow; so far, the interfaces of the clear liquid layer, the tar layer and the liquid sulfur layer can be stably maintained, and the feeding amount of the heat medium can be adaptively adjusted according to the feeding amount of the sulfur foam raw material A and the water content in the sulfur foam raw material A, so that the temperature gradient in the melting-separating kettle is stably maintained.

Materials (such as unfused ash and salts insoluble in sulfur) with density higher than that of liquid sulfur are deposited at the bottom of the cone bottom of the melting heater 5, gradually accumulated and intermittently discharged through a valve 11 according to circumstances, because of being mixed with sulfur, the materials are called sulfur slag and waste; when the sulfur slag is discharged intermittently, other valves and the feeding amount of the sulfur foam raw material A do not need to be adjusted manually.

In some embodiments of the present invention, in order to avoid the adverse effect of the precipitation of tar droplets and sulfur particles due to "convection" in the melt-separation kettle, the upflow in the layer is designed to have a flow velocity of less than 0.2m/s and a tar standing time of more than 20 min.

In some specific embodiments of the invention, in order to avoid the discharged liquid sulfur from being mixed with sulfur particles, the temperature of 95-150 ℃ is designed, the heating time of the sulfur particles is more than 40min, and the sulfur particles are fully ensured to realize crystal form transformation and complete melting.

In some embodiments of the present invention, since the temperature gradient in the multiphase separation tank 7 is gradually increased from top to bottom, the clear liquid C, the tar D, and the liquid sulfur E in the tank are all liquids, the upper limit of the operation pressure of the multiphase separation tank 7 of the melting-separation kettle is theoretically not limited, and the lower limit of the operation pressure should be higher than 85kpa (a); the operating pressure of the melting-separating vessel of the present invention can then be determined in view of the system pressure at the digestion end of the non-condensable gas B.

In certain embodiments of the invention, sulfur color is improved and impurities are reduced by continuous heating of tar, stratification by density difference, and continuous drainage, as tar is mixed into liquid sulfur, which results in a blackening of sulfur color and an increase in char content.

In some embodiments of the invention, the temperature of the supernatant layer is between 85 and 95 ℃, the temperature is lower than the melting point of sulfur, and the upflow velocity in the layer is less than 0.2m/s, so that the discharged supernatant C can be reliably prevented from carrying sulfur particles.

According to the method for continuously melting and multi-phase separating the water-containing sulfur particles, the upper limit of the operation pressure of the melting-separating kettle is not limited theoretically, the lower limit of the operation pressure is higher than 85KPa (a), and the operation pressure of the melting-separating kettle is determined according to the system pressure of the absorption end of the non-condensable gas B; the S1-S4 is generally carried out under a lower absolute pressure ranging from 0.01 to 0.8MPa (a).

Preferably, the absolute pressure is 0.09-0.18 MPa (a).

According to the continuous melting and multi-phase separation method of the water-containing sulfur particles, the adding amount of the heat medium F of S1 is related to the feeding amount of the sulfur foam raw material A and the water content thereof, and the self-adaptive adjustment is realized through a TC1 adjusting loop.

According to the continuous melting and multi-phase separation method of the water-containing sulfur particles, a loop is adjusted through TC2 in S3, and the temperature T2 at the bottom of a multi-phase separation tank 7 of a melting-separation kettle is stably maintained at a certain value between 85 and 130 ℃; meanwhile, the temperature T1 of liquid sulfur at the outlet of the melting heater 5 of the melting-separating kettle is stably maintained at a certain value between 130 and 150 ℃ through a TC1 regulating loop. Preferably, 85 ℃ < T2<95 ℃; 135 < T1<142 ℃.

According to the continuous melting and multi-phase separation method of aqueous sulfur granules, in S2, the non-condensable gas B saturated by the solvent vapor in the system is discharged, and the operation pressure of the melting-separating kettle is stably maintained.

Examples

Example 1 initial feeding of the System and establishment of Normal conditions

The raw material liquid is sulfur foam after filter pressing or centrifugal separation, and the desulfurization liquid is ammonia solution with the proportion of 30 percent (wt/%); the sulfur particle proportion was 30% (wt/%); tar < 1% (wt/%); the temperature was 25 ℃.

The system comprises: the device comprises a heat supply unit, a heat exchanger group, a multiphase separation tank, a liquid level retaining mechanism and a control system.

Wherein the heat exchanger group comprises a heater 1, a melting heater 5 and a preheater 9; the heat supply unit comprises a steam trap 2; an outlet below the melting heater 5 is connected with the steam trap 2, and the generated steam condensate G is discharged after heat exchange of the heater 1.

The multiphase separation tank comprises a multiphase separation tank 7, and a distributor 10, a liquid collecting tray 8 and a liquid collecting tray 6 are arranged in the multiphase separation tank 7; the multiphase separation tank 7 is coaxially connected with the melting heater 5 in the vertical direction to form a melting-separation kettle body; the preheater 9 and the heater 1 are arranged in series along the feeding route of the sulfur foam raw material A, and the heater 1 is connected with the top of the melting-separating kettle, so that the heat-exchanged material enters the multiphase separating tank 7 of the melting-separating kettle from the top of the melting-separating kettle.

The liquid level keeping mechanism comprises a discharge port I, and the height of the discharge port I is 2000 mm; a discharge outlet II having a height of 1948 mm; and a discharge port III having a height of 1671 mm.

The control system comprises an instrument measuring point arranged on the melting-separating kettle, and a regulating valve 11 and a heat supply regulating device which are arranged on a sulfur foam feeding pipeline. A spare port 12 is left on the sulfur discharge pipe for adding liquid sulfur or solid sulfur particles during initial feeding. The melting heater 5 is a vertical tube type heat exchanger, and steam passes through the shell pass; the throughput of the system was 1t feed solution/h.

The normal working pressure of the melting-separating kettle of the system is 55KPa (g); the heat medium is saturated steam of 0.45MPa (g).

Introducing the steam F into the melting-separating kettle, and discharging steam condensate G out of the system after passing through a jacket of a multiphase separating tank 7 → a melting heater 5 → a steam trap 2 → a heater 1;

when the temperature of the liquid sulfur measuring point T1 and the temperature of the bottom T2 of the multiphase separation tank 7 are both higher than 130 ℃, adding the liquid sulfur to half of the height of the heat exchange tube bundle of the immersion melting heater 5 through the standby port 12 on the sulfur discharge tube, or adding solid sulfur particles, and after melting, adding the solid sulfur particles to half of the height of the heat exchange tube bundle of the immersion melting heater 5; closing the standby port 12;

opening a valve of a clear liquid discharge pipeline to ensure that the clear liquid can be discharged out of the melting-separation kettle when the liquid level in the melting-separation kettle reaches the upper edge of the liquid collecting tray 8, so as to form a route of discharging of the melting-separation kettle → a preheater 9 → a discharge system, and then;

the sulfur foam raw material A of about 0.2t/h and 25 ℃ enters a multiphase separation tank 7 of the melting-separation kettle from the top of the melting-separation kettle through a preheater 9 → a heater 1 → the pressure in the melting-separation kettle rises due to the evaporation of liquid in the sulfur foam raw material A, the pressure in the melting-separation kettle is kept at 55KPa (g) through PC1, and non-condensable gas B is discharged out of the system; meanwhile, the temperature T2 at the bottom of the multiphase separation tank 7 is rapidly reduced, the temperature T2 at the bottom of the multiphase separation tank 7 is lower than 130 ℃, and steam with the maximum flow can be introduced into the melting-separation kettle; at this stage, the addition ratio of "steam F/sulfur foam feedstock a" is several times higher than in normal operation, thereby establishing a temperature gradient deviating from the normal operation state;

after the temperature measuring point T2 at the bottom of the multiphase separation tank 7 is higher than 100 ℃, gradually increasing the feeding amount of the sulfur foam raw material A according to the temperature rising speed of the temperature until the normal feeding amount (0.2T/h) is reached, and stably controlling the temperature at 112 ℃; simultaneously, the feeding amount of the steam F is regulated according to a liquid sulfur temperature measuring point T1, and the temperature is stably controlled at 138 ℃; namely: gradually adjusting the adding ratio of the steam F/sulfur foam raw material A which is several times higher than that of the normal running to the adding ratio of the steam F/sulfur foam raw material A in the normal running;

when the liquid level in the melting-separating kettle reaches the liquid collecting tray 8, the heated clear liquid is discharged out of the melting-separating kettle in a self-flowing manner and is discharged out of the system through the sulfur preheater 9, and the thickness H of the clear liquid layer₁700mm, specific gravity 1.

Heating the sulfur foam raw material A to 85 ℃ in a melting-separation kettle, naturally layering sulfur particles, tar and desulfurization liquid according to density difference, settling the sulfur particles to the bottom of a multiple phase separation tank 7, feeding the sulfur particles into a melting heater 5, heating and melting the sulfur particles into liquid sulfur, and accumulating a tar layer between a liquid sulfur layer and a desulfurization liquid layer; the liquid sulfur layer has the specific gravity of 1.8 and can automatically flow out of the system when reaching 1255 mm; opening a discharge valve of a tar pipeline, closing the valve if the discharged material is desulfurization clear liquid, continuously waiting for the accumulation of tar in material layers in the melting-separating kettle, if the discharged material is tar, self-maintaining each material layer (a liquid sulfur layer, a tar layer and a desulfurization liquid layer), automatically discharging the tar layer from a system when the specific gravity of the tar layer is 1.08 and reaches 45mm, wherein the total liquid layer is 2000mm thick, and various media (non-condensable gas B, desulfurization liquid C, tar D and liquid sulfur E) separated by the melting-separating kettle can be continuously discharged according to the self-adaptive matching of the feeding amount and the components thereof;

so far, a temperature system, a pressure system and a liquid layer thickness are stably established in the system, and the separation performance of discharging materials in the same amount as the sulfur foam raw material A is realized.

Example 2:continuous feeding of system and realization of continuous sulfur melting and multi-phase separationSeparation device

The system consists of a heater 1, a steam trap 2, a melting heater 5, a liquid collecting tray 6, a multiphase separation tank 7, a liquid collecting tray 8, a preheater 9, a distributor 10 and a valve 11, wherein a standby port 12 is reserved on a sulfur discharge pipe, the melting heater 5 is a vertical pipe type heat exchanger, and steam passes through a shell pass; the processing capacity of the system is 1t of raw material liquid/h, and the initial feeding and the establishment of normal working conditions of the system are completed.

The heat medium is saturated steam of 0.45MPa (g).

The steam F is introduced into the melting-separating kettle and passes through a jacket of the multiphase separating tank 7 → the melting heater 5 → the steam trap 2 → the heater 1, and then the steam condensate G is discharged out of the system; the working pressure of the melting-separating kettle of the system is kept at 55KPa (g) by PC1, and the non-condensable gas B is discharged out of the system;

the temperature measuring point T2 at the bottom of the multiphase separation tank 7 is maintained at 112 +/-2 ℃, and the temperature measuring point T1 of liquid sulfur is maintained at 138 +/-2 ℃;

1t/h and 25 ℃ of the sulfur foam raw material A enter a multiphase separation tank 7 of the melting-separation kettle from the top of the melting-separation kettle through a preheater 9 → a heater 1 → the temperature of the sulfur foam raw material A entering the multiphase separation tank 7 is 39.8 ℃; the non-condensable gas B (saturated by solvent vapor in the system) is continuously discharged out of the system at 0.3kg/h through PC1, the working pressure of a melting-separation kettle of the system is kept at 55KPa (g), the solvent vapor amount in the non-condensable gas B is 8g/h, and the temperature of the non-condensable gas B discharged out of the multiphase separation tank 7 (namely the upper temperature T4 of the multiphase separation tank 7) is about 52 ℃; the clear liquid C is discharged out of the melting-separation kettle from a liquid collecting tray 8 in the multiphase separation tank 7 in a self-flowing manner, the temperature of the discharged clear liquid (namely the temperature T3 in the middle of the multiphase separation tank 7) is 92 ℃, the clear liquid C is discharged out of the system after heat exchange with the sulfur foam raw material A at the temperature of 25 ℃ by a preheater 9, and the temperature and the flow rate of the clear liquid C discharged out of the system are about 60 ℃ and 300 kg/h; the tar D is discharged from a liquid collecting disc 6 in the multiphase separation tank 7 to the melting-separation kettle in a self-flowing manner, the discharge temperature is 95-112 ℃ (namely, the discharge value between the middle temperature T3 and the bottom temperature T2 of the multiphase separation tank 7), and the tar D flow discharged from the system is less than 10 kg/h; when the sulfur foam raw material A is heated to 85-95 ℃ in a melting-separating kettle, sulfur particles, tar and desulfurization liquid are naturally layered according to density difference, the sulfur particles are settled in a liquid sulfur layer at the bottom of a multi-phase separating tank 7, the sulfur particles float in the liquid sulfur layer and sink into a heat exchange tube bundle of a melting heater 5 of the melting-separating kettle and are heated and melted due to the density difference between the sulfur particles and the liquid sulfur, when the liquid sulfur discharge temperature T1 (namely the bottom temperature of the melting heater 5) is 138 +/-2 ℃, the sulfur particles are discharged out of a system through a U-shaped liquid sulfur discharge pipe, and the discharge amount of the liquid sulfur E is about 700 kg/h;

the flow rate of steam F added into the system is about 71 kg/h; the temperature of the steam condensate G discharged from the system is 60 ℃;

with the gradual melting of the sulphur particles, at the bottom of the multiphase separation tank 7 is a layer of liquid sulphur mixing moisture, tar and sulphur particles: moisture attached to the surface of the sulfur particles and in the micropores is vaporized and rises up in a floating manner due to a density difference with the sulfur particles; tar attached to the surface of the sulfur particles and in the micropores also rises up in a floating manner due to a density difference between the sulfur particles and the liquid sulfur; the moisture and tar adhered to the surfaces of the sulfur particles and in the micropores are separated from the liquid sulfur layer below the middle part of the melting heater 5, so that the color of the discharged liquid sulfur E is improved; the materials (non-molten ash and slag) with the density higher than that of the liquid sulfur are deposited at the bottom of the cone of the melting heater 5, gradually accumulated and intermittently discharged through a valve 11 according to the situation, and the discharged sulfur slag is discarded.

Therefore, the system realizes the improvement of the color of the liquid sulfur E and the separation performance of discharging each material in the same amount as the sulfur foam raw material A through a stable temperature system, a pressure system and the thickness of a liquid layer.

Example 3:initial feeding of system and establishment of normal working condition

The system comprises: the device comprises a heat supply unit, a heat exchanger group, a liquid level retaining mechanism of a multiphase separation tank and a control system.

Wherein the heat exchanger group comprises a heater 1, a melting heater 5, a preheater 9 and a heat conducting oil heater 4'; the heat supply unit comprises a steam trap 2; an outlet below the melting heater 5 is connected with the steam trap 2, and the generated steam condensate G is discharged after heat exchange of the heater 1.

The heat supply unit comprises a heat-conducting oil expansion tank 2 'and a heat-conducting oil pump 3'; the heat conduction oil pump 3 'is connected with the heat conduction oil heater 4'; the outlet of the heat-conducting oil heater 4 'is connected with the inlet of the melting heater 5, the outlet of the multiphase separation tank 7 forms a circulation loop with the heat-conducting oil pump 3' through the heater 1, and the heat-conducting oil expansion tank 2 'is externally connected with the circulation loop and is arranged at the front end of the heat-conducting oil pump 3'.

The multiphase separation tank comprises a multiphase separation tank 7, and a distributor 10, a liquid collecting tray 8 and a liquid collecting tray 6 are arranged in the multiphase separation tank 7; the multiphase separation tank 7 is coaxially connected with the melting heater 5 in the vertical direction to form a melting-separation kettle body; the preheater 9 and the heater 1 are arranged in series along a feeding route of the sulfur foam raw material A, and the heater 1 is connected with the top of the melting-separating kettle, so that the heat-exchanged material enters the multiphase separating tank 7 of the melting-separating kettle from the top of the melting-separating kettle of the sulfur melting kettle.

The liquid level keeping mechanism comprises a discharge port I, and the height of the discharge port I is 2000 mm; a discharge outlet II having a height of 1948 mm; and a discharge port III having a height of 1732 mm.

The control system comprises a material level meter L1, temperature meters T1-T4, a pressure meter P1, a regulating valve TV2 and heat supply regulating devices TC 1-TC 2 which are arranged on a sulfur foam feeding pipeline, and a pressure regulating device PV1 on a gas phase QI discharge pipe, wherein the material level meter L1, the temperature meters T1-T4, the pressure meter P1, the regulating valve TV2 and the heat supply regulating devices TC 1-TC 2 are arranged on the melting-separating kettle.

A spare port 12 is left on the sulfur discharge pipe for adding liquid sulfur or solid sulfur particles during initial feeding. The melting heater 5 is a vertical tube type heat exchanger, and shell pass through heat conducting oil; the heat conducting oil heater 4' is an electric heater; the throughput of the system was 1t feed solution/h.

The normal working pressure of the melting-separating kettle of the system is 55KPa (g); the heat medium is heat conducting oil.

The closed circulation of the heat transfer oil F is formed by the heat transfer oil pump 3 ' → the heat transfer oil heater 4 ' → the melting heater 5 ' → the jacket of the multiphase separation tank 7 → the heater 1 ' → the heat transfer oil pump 3 '; starting an electric heater of the heat conducting oil heater 4'; the heat conducting oil expansion tank 2' balances the volume expansion of the heat conducting oil from the normal temperature to the working temperature;

when the temperature of the liquid sulfur measuring point T1 and the temperature of the bottom T2 of the multiphase separation tank 7 'are both higher than 130 ℃, adding the liquid sulfur to half of the height of the heat exchange tube bundle of the submerged melting heater 5' through a standby port 12 'on the sulfur discharge pipe, or adding solid sulfur particles, and after melting, adding the solid sulfur particles to half of the height of the heat exchange tube bundle of the submerged melting heater 5'; closing the spare port 12';

opening a valve of a clear liquid discharge pipeline to ensure that the clear liquid can be discharged out of the melting-separating kettle when the liquid level in the melting-separating kettle reaches the upper edge of the liquid collecting tray 8 ', so as to form a route of discharging from the melting-separating kettle → a preheater 9' → discharging system, and then;

the sulfur foam raw material A at 25 ℃ of about 0.2t/h enters a multiphase separation tank 7 'of a melting-separation kettle from the top of the melting-separation kettle through a preheater 9' → a heater 1 '→ due to evaporation of liquid in the sulfur foam raw material A, the pressure in the melting-separation kettle rises, the pressure in the kettle is maintained at 55KPa (g) through PC 1', and non-condensable gas B is discharged out of the system; meanwhile, the temperature T2 at the bottom of the multiphase separation tank 7 is rapidly reduced, the temperature T2 at the bottom of the multiphase separation tank 7' is lower than 130 ℃, and heat conduction oil with the maximum flow and the highest allowable temperature can be introduced into the melting-separation kettle; at this stage, the addition ratio of the heat-conducting hot oil F/the sulfur foam raw material A is several times higher than that in normal operation, and the melting-separating kettle can quickly establish a temperature gradient deviating from the normal operation state;

after the temperature measuring point T2 at the bottom of the multiphase separation tank 7' is higher than 100 ℃, gradually increasing the feeding amount of the sulfur foam raw material A according to the temperature rising speed of the temperature until the normal feeding amount is reached, and stably controlling the temperature at 112 ℃; simultaneously, the temperature of the hot thermal conductive oil F entering the melting-separating kettle is regulated according to a liquid sulfur temperature measuring point T1, and the liquid sulfur temperature measuring point T1 is stably controlled at 138 ℃; namely: gradually adjusting the adding ratio of the heat conduction hot oil F/sulfur foam raw material A which is several times higher than that of the heat conduction hot oil F/sulfur foam raw material A in normal operation to the adding ratio of the heat conduction hot oil F/sulfur foam raw material A in normal operation;

when the liquid level in the melting-separating kettle reaches the liquid collecting tray 8 ', the heated clear liquid is discharged out of the melting-separating kettle in a self-flowing manner and is discharged out of the system through the preheater 9', and the thickness H of the clear liquid layer₁570mm, specific gravity 1.

When the sulfur foam raw material A is heated to 95 ℃ in a melting-separation kettle, sulfur particles, tar and desulfurization liquid in the sulfur foam raw material A are naturally layered according to density difference, the sulfur particles are settled at the bottom of a multiple phase separation tank 7 'and enter a melting heater 5' to be heated and melted into liquid sulfur, and a tar layer is accumulated between a liquid sulfur layer and a desulfurization liquid layer; the liquid sulfur layer has the specific gravity of 1.6 and can automatically flow out of the system when reaching 1255 mm; opening a discharge valve of a tar pipeline, closing the valve if the discharge is observed to be desulfurized clear liquid, and continuing to wait for the accumulation of tar in a material layer in the melting-separating kettle; if the discharged material is tar, the material layers (a liquid sulfur layer, a tar layer and a desulfurization liquid layer) can be self-maintained, the specific gravity of the tar layer is 1.1 at the moment, the tar layer can automatically flow out of the system when reaching 175mm, the total liquid layer is 2000mm thick, the total liquid layer can be self-adaptively matched according to the feeding amount and the components thereof, and various media (non-condensable gas B, desulfurization liquid C, tar D and liquid sulfur E) separated by the melting-separating kettle are continuously discharged;

Finish makingInitial feeding of system and establishment of normal working conditionAfter that time, the user can use the device,

the bottom temperature measuring point T2 of the multiphase separation tank 7' is kept at 112 +/-2 ℃, and the liquid sulfur temperature measuring point T1 is kept at 138 +/-2 ℃;

1t/h and 25 ℃ of the sulfur foam raw material A enter a multiphase separation tank 7 'of the melting-separation kettle from the top of the melting-separation kettle through a preheater 9' → a heater 1 '→ and the temperature of the sulfur foam raw material A entering the multiphase separation tank 7' is 39.8 ℃; the non-condensable gas B (saturated by solvent vapor in the system) is continuously discharged out of the system at 0.3kg/h through PC1, the working pressure of a melting-separation kettle of the system is kept at 55KPa (g), the solvent vapor amount in the non-condensable gas B is 8g/h, and the temperature of the non-condensable gas B discharged out of the multi-phase separation tank 7' (namely the upper temperature T4 of the multi-phase separation tank 7) is about 52 ℃; the clear liquid C is discharged out of the melting-separation kettle from a liquid collecting disc 8 ' in the multiphase separation tank 7 ' in a self-flowing manner, the temperature of the discharged clear liquid (namely the temperature T3 in the middle of the multiphase separation tank 7) is 92 ℃, the clear liquid C is discharged out of the system after heat exchange with the sulfur foam raw material A at 25 ℃ by a preheater 9 ', and the temperature of the clear liquid C discharged out of the system is about 60 ℃ and the flow rate is 300 kg/h; the tar D is discharged from a liquid collecting disc 6 ' in the multiphase separation tank 7 ' to the melting-separation kettle in a self-flowing manner, the discharge temperature is 95-112 ℃ (namely, the temperature is between the display values of the middle temperature T3 and the bottom temperature T2 of the multiphase separation tank 7 '), and the tar D flow discharged from the system is less than 10 kg/h; when the sulfur foam raw material A is heated to 85-95 ℃ in a melting-separating kettle, sulfur particles, tar and desulfurization liquid therein are naturally layered according to density difference, the sulfur particles are settled in a liquid sulfur layer at the bottom of a multi-phase separating tank 7 ', and due to the density difference between the sulfur particles and the liquid sulfur, the sulfur particles float in the liquid sulfur layer and sink into a heat exchange tube bundle of a melting heater 5' of the melting-separating kettle and are heated and melted, when the liquid sulfur discharge temperature T1 (namely the temperature at the bottom of the melting heater 5) is 138 +/-2 ℃, the sulfur particles are discharged out of a system through a U-shaped liquid sulfur discharge pipe, and the discharge amount of the liquid sulfur E is about 700 kg/h;

the temperature of the heat transfer oil F entering the melting-separating kettle is 242 ℃, the temperature of the heat transfer oil F discharged from the melting-separating kettle is 120 ℃, the temperature of the heat transfer oil F discharged from the heater 1' is 60 ℃, and the circulation quantity of the heat transfer oil F in the system is about 117 kg/h; the consumed power of the heat-conducting oil pump 3' is 0.01 Kw: the consumption power of the electric heater of the conduction oil heater 4' is 49.33 Kw;

accompanying the gradual melting of the sulphur particles, at the bottom of the multiphase separation tank 7' is a layer of liquid sulphur mixing moisture, tar and sulphur particles: moisture attached to the surface of the sulfur particles and in the micropores is vaporized and rises up in a floating manner due to a density difference with the sulfur particles; tar attached to the surface of the sulfur particles and in the micropores also rises up in a floating manner due to a density difference between the sulfur particles and the liquid sulfur; the moisture and tar adhered to the surfaces of the sulfur particles and in micropores are separated from the liquid sulfur layer below the middle part of the melting heater 5', so that the color of the discharged liquid sulfur E is improved; the materials (non-molten ash and slag) with the density higher than that of the liquid sulfur are deposited at the bottom of the cone bottom of the melting heater 5', gradually accumulated, intermittently discharged through a valve 11 according to the situation, and discarded.

Example 4:when the composition of the raw material liquid of the system changes:

the raw material liquid is sulfur foam from a sulfur foam tank, and the desulfurization liquid is ammonia solution with the proportion of 95% (wt/%); sulfur particle ratio was 5% (wt/%); tar < 1% (wt/%); the temperature was 25 ℃. The system feeding amount is 1 t/h.

The changes compared to example 2 were: the flow rate of the discharged clear liquid C is 950 kg/h; the discharge amount of the liquid sulfur E is about 50 kg/h; the flow rate of steam F fed into the system was about 66 kg/h.

Compared to example 3, the changes are: the flow rate of the discharged clear liquid C is 950 kg/h; the discharge amount of the liquid sulfur E is about 50 kg/h; the circulation quantity of the heat conducting oil F in the system is about 108 kg/h; the consumed power of the heat-conducting oil pump 3' is 0.01 Kw: the consumption power of the electric heater of the conduction oil heater 4' is 45.86 Kw.

Therefore, the system realizes self-adaption of composition change of the raw material liquid, improvement of color of the liquid sulfur E and separation performance of discharging materials in the same amount as the sulfur foam raw material A through a stable temperature system, a stable pressure system and a stable liquid layer thickness.

Example 5:

the noncondensable gas B (saturated by the solvent vapor in the system) discharged from the system is sent to wet catalytic oxidation desulfurization (H)₂S) in an unpurified gas pipeline before the unit; the discharged clear liquid C is sent to the wet catalytic oxidation method for desulfurization (H)₂S) a desulfurization liquid circulation tank of the unit; the tar D is sent to a wet catalytic oxidation method for desulfurization (H)₂S) a tar ammonia water separation unit before the unit.

Example 6:

if there is no need to improve the color and purity of the liquid sulfur E, the system may be provided without a drip pan 6 in the multi-phase separation tank 7, as compared with examples 1 to 5.

Example 7: height adjustment of discharge piping system

For a solid-liquid mixture system, when three layers are separated in terms of mutual density differences in a melt-separation tank, it can be derived by known conditions and common knowledge: liquid layer thickness H of liquid 1₁700mm, specific gravity of 1.1; liquid layer thickness H of liquid 2₂50mm, specific gravity of 1.5; liquid layer thickness H of liquid 3₃1250mm and the specific gravity of 2; total liquid level height H₄Is 2000 mm.

The height of the discharge pipe, which can be determined from the density difference, is then: discharge pipe C (corresponding to liquid 1) H₄2000mm, discharge pipe D (corresponding to liquid 2) H₅1813mm, discharge tube E (corresponding to liquid 3) H₆1673 mm.

If the specific gravity of the liquid 2 becomes 1.6 and the specific gravity of the liquid 3 becomes 1.8, that is, if the density difference between the liquid 2 and the liquid 3 becomes small, then the positions of the discharge pipes are not changed, and H is only required to be changed₆Adjusted to 1735mm, the liquid layer thickness of each liquid medium can be adaptively changed into: h₁Is 645mm and H₂Is 105mm, H₃1250 mm.

While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.

It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.

Claims

1. A continuous melting and multiple phase separation system, the system comprising:

the multiphase separation tank is used for standing and layering the continuously added liquid-meltable solid mixed material; the multiphase separation tank comprises a multiphase separation tank 7, the multiphase separation tank 7 is connected with the melting heater 5 in the heat exchanger group in the vertical direction to form a melting-separation kettle body, and the melting-separation kettle body can completely melt soluble solid particles without mechanical stirring; and discharging the product of each phase out of the system; the products of each phase include gas-phase products and liquid-phase products (such as liquid-phase product YI, liquid-phase product YII, and liquid-phase product YIII); the liquid level maintaining mechanism comprises a discharge system of each liquid-phase product, and is used for stably discharging each continuous liquid-phase product which is equal to the fed material and is continuously discharged out of the system under the condition that the adjusting mechanism is not arranged; and

a control system for regulating the temperature of the liquid-meltable solid mixture and the respective phase products, the pressure and level in the melting-separation vessel during operation of the system.

2. A continuous melting and multiphase separation system as recited in claim 1, wherein the heat medium used in the heat supply unit is a heat medium having a temperature higher than the melting point of the meltable solid, such as: heat conducting oil or steam; preferably, the heat medium is used in parallel in the constituent devices of the system or used in series and in cascade between the constituent devices of the system.

3. The continuous melting and multiphase separation system as recited in claim 1 or 2, wherein when the heating medium of the heating unit is steam F, the heating unit includes a steam trap 2, and an outlet below the melting heater 5 is connected to the steam trap 2 for discharging steam condensate G.

4. The continuous melting and multiphase separation system as recited in claim 1 or 2, wherein when the heating medium of the heating unit is a conduction oil F ', the heating unit includes a conduction oil expansion tank 2 ' and a conduction oil pump 3 '; the heat exchanger group also comprises a heat conducting oil heater 4'; the heat conduction oil pump 3 'is connected with the heat conduction oil heater 4'; the outlet of the heat-conducting oil heater 4 'is connected with the inlet of the melting heater 5, and forms a circulation loop with the heat-conducting oil pump 3' through the heat-conducting oil outlet of the multiphase separation tank 7.

5. A continuous melting and multiphase separation system according to any of claims 1-4, wherein the multiphase separation tank 7 is a liquid containing tank body provided with a distributor 10, a drip pan 8, a drip pan 6; the multiphase separation tank 7 is coaxially connected with the melting heater 5 in the heat exchanger group in the vertical direction.

6. A continuous melting and multiphase separation system according to any of claims 1-5, wherein the heat exchanger group further comprises a preheater 9 for heating a liquid-meltable solid mixture, a heater 1, the preheater 9 being arranged in series with the heater 1, the liquid-soluble solid mixture outlet of the heater 1 being connected to the multiphase separation tank 7 via the top of the melting-separation tank.

7. A continuous melting and multiphase separation system according to any one of claims 1-6, wherein the level maintenance mechanism is a discharge piping system having a height difference of bottom of each liquid phase medium discharge pipe determined according to a difference in density of different liquid phase products.

8. The continuous melting and multiphase separation system of any one of claims 1-7, wherein in case of a three liquid phase product continuous separation system, the level maintenance mechanism comprises a drain I, a drain II, and a drain III; the height difference of the tube bottom of each liquid phase medium discharge tube can be calculated by the following formula:

h4 ═ H1+ H2+ H3 (formula I)

H5H 4-H1 + ρ 1 ÷ ρ 2 XH 1 (formula II)

H6 ═ H3+ ρ 1 ÷ ρ 3 × H1+ ρ 2 ÷ ρ 3 × H2 (formula III)

Wherein H1 is the liquid layer thickness of liquid phase I; h2 is the liquid layer thickness of liquid phase II; h3 is the liquid layer thickness of liquid phase III; h4 is the height of the bottom of the discharge pipe I; h5 is the height of discharge pipe II; h6 is the height of discharge pipe III; ρ 1 is the density of the liquid phase I; ρ 2 is the density of the liquid phase II; ρ 3 is the liquid phase III density.

9. A continuous melting and multiphase separation system according to any of claims 1-8, wherein the control system comprises instrumentation points on the melting-separation vessel for monitoring level, temperature and pressure, and regulating valves and heating regulating devices on the feed lines.

10. A method for continuous melting and multiple phase separation using the system of any one of claims 1-9, the method comprising:

11. The method as claimed in claim 10, wherein the heat medium is a heat medium having a temperature higher than the melting point of the meltable solid, such as: heat conducting oil or steam; preferably, the heat medium is used in parallel in the constituent devices of the system or used in series and in cascade between the constituent devices of the system.

12. The method according to claim 11, wherein when the heating medium is steam F, the steam F is first introduced into a jacket of the multiple phase separation tank 7, the steam or steam-water mixture discharged from the jacket of the multiple phase separation tank 7 is introduced into the melting heater 5, and the steam condensate G discharged from the melting heater 5 is discharged through the steam trap 2.

13. The method according to claim 11, wherein when the heat medium is a conduction oil F ', the conduction oil F ' is fed into the conduction oil heater 4 ' through the conduction oil pump 3 ', the conduction oil F ' heated in the conduction oil heater 4 ' is fed into the melting heater 5, the conduction oil F ' discharged from the melting heater 5 is fed into a jacket of the multiphase separation tank 7, and the conduction oil F ' discharged from the jacket of the multiphase separation tank 7 is returned to an inlet of the conduction oil pump 3 '.

14. The method according to any one of claims 10 to 13, wherein a liquid layer of the liquid-phase product YI is formed by gradually accumulating between a liquid layer of the liquid-phase product YI having the smallest density and a liquid layer of the liquid-phase product YII having the largest density, wherein the liquid-phase product YI, the liquid-phase product YII, and the liquid-phase product YII are each self-discharged via a liquid level maintaining mechanism; the liquid level holding mechanism stably holds the interface of the liquid-phase product YI liquid layer, the YII liquid layer, and the yiiii liquid layer.

15. Use of a continuous melting and multiple phase separation system according to any of claims 1-9 in a continuous melting and multiple phase separation technique for aqueous sulphur particles.

16. A system for continuous melting and multiple phase separation of aqueous sulfur granules, the system comprising: a heat supply unit, a heat exchanger group, a multiphase separation tank, a liquid level maintaining mechanism and a control system,

the multi-phase separation tank 7 is vertically and coaxially connected with the heat exchanger group to form a melting-separation kettle, and each phase product is stably discharged through the liquid level maintaining mechanism while the sulfur foam raw material A is continuously added, wherein each phase product comprises a gas phase product and a liquid phase product (such as a liquid phase product YI, a liquid phase product YII and a liquid phase product YII);

the control system comprises a material level meter L1, a temperature meter T1-T4, a pressure meter P1, a regulating valve TV2 and a heat supply regulating device TC1 which are arranged on a sulfur foam feeding pipeline, and a pressure regulating device PV1 on a gas phase QI discharge pipe, wherein the material level meter L1, the temperature meter T1-T4, the pressure meter P1, the regulating valve TV 3838 and the heat supply regulating device TC1 are arranged on the melting-separating kettle.

17. The continuous melt and multiphase separation system of claim 16, wherein the heat medium is used in parallel within the system components or in series and in stages between the system components.

18. A continuous melting and multiphase separation system according to claim 16 or 17, wherein the melting heater 5 is a multi-plate parallel or multi-tube parallel dividing wall heater with a jacketed conical bottom; preferably, the melting heater 5 is a cylindrical heater.

19. A continuous melting and multiphase separation system according to any of claims 16 to 18, wherein when the heating medium of the heating unit is steam F, the heating unit comprises a steam trap 2, and a jacket outlet of the conical bottom below the melting heater 5 is connected to the steam trap 2 for discharging the generated steam condensate water G.

20. The continuous melting and multiphase separation system according to any one of claims 16 to 19, wherein when the heating medium of the heating unit is a conduction oil F ', the heating unit further comprises a conduction oil expansion tank 2 ' and a conduction oil pump 3 '; the heat conduction oil pump 3 'is connected with the heat conduction oil heater 4'; the outlet of the heat conduction oil heater 4 'is connected with the inlet of the melting heater 5, and forms a circulation loop with the heat conduction oil pump 3' through the outlet of the multiphase separation tank 7.

21. The continuous melting and multiphase separation system of any one of claims 16 to 20, wherein the heat exchanger group further comprises a preheater 9 for heating the sulfur foam raw material a, a heater 1, the preheater 9 and the heater 1 being arranged in series along a sulfur foam raw material a feed route, a sulfur foam raw material outlet of the heater 1 being connected to the multiphase separation tank 7 through a top of the melting-separation tank.

22. The continuous melt and multiphase separation system of any one of claims 16-21, wherein the liquid phase product YI is serum C, the liquid phase product YII is tar D, and the liquid phase product YIII is liquid sulfur E.

23. A method for continuous melting and multiple phase separation using the system of any one of claims 16-22, the method comprising:

24. The method of claim 23, wherein the heat medium is used in parallel in the components of the system or in series and in steps between the components of the system.

25. The method according to claim 23 or 24, wherein when the heating medium is steam F, the steam F is first introduced into the jacket of the multiple phase separation tank 7, the steam or steam-water mixture discharged from the jacket of the multiple phase separation tank 7 is introduced into the melting heater 5, and the steam condensate G discharged from the melting heater 5 is discharged after passing through the steam trap 2.

26. The method according to claim 23 or 24, wherein when the heat medium is a thermal oil F ', the thermal oil F ' is fed into the thermal oil heater 4 through the thermal oil pump 3, the thermal oil F ' heated in the thermal oil heater 4 is fed into the melting heater 5, the thermal oil F ' discharged from the melting heater 5 is fed into a jacket of the multiphase separation tank 7, and the thermal oil F ' discharged from the jacket of the multiphase separation tank 7 is returned to an inlet of the thermal oil pump 3.

27. The method according to any one of claims 23 to 26, wherein a distributor 10, a drip pan 8, a drip pan 6; the sulfur foam raw material A entering the multiphase separation tank 7 is in direct countercurrent contact with rising steam in the multiphase separation tank 7 in the upper space of the distributor 10, gas phase QII serving as condensable steam in the rising steam is condensed and cooled, and the gas phase QI serving as non-condensable gas B is discharged out of the system; the liquid-phase product YI is collected by the liquid collecting tray 8 and then is continuously discharged through the discharge port I; the liquid-phase product YII is collected by the liquid collecting tray 6 and then is continuously discharged through the discharge port II; the liquid-phase product YIII and sulfur particles flow vertically downward into the melting heater 5.

28. The method as claimed in any one of claims 23 to 27, wherein the liquid phase product YIII and solid sulfur particles flow vertically downward in the barrel of the melting heater 5 and indirectly exchange heat with the heating medium F to reach the bottom of the melting heater 5 to be completely melted, and the liquid phase product YIII is discharged from the system through a discharge outlet III on the side of the conical bottom of the melting heater 5.

29. The method according to any one of claims 23 to 28, wherein the liquid-phase product YI is serum C, the liquid-phase product YII is tar D, and the liquid-phase product YIII is liquid sulfur E.

30. A system for continuous melting and multi-phase separation of aqueous sulfur granules, the system comprising: a heat supply unit, a heat exchanger group, a multiphase separation tank, a liquid level maintaining mechanism and a control system,

the heat exchanger group comprises a preheater 9 and a heater 1 which are used for heating the sulfur foam raw material A; a melting heater 5; and a conduction oil heater 4 'when using the conduction oil F';

the heat medium in the heat supply unit comprises steam F or heat conducting oil F'; when the heating medium of the heat supply unit is steam F, the heat supply unit comprises a steam trap 2, a condensed water outlet of a jacket at the lower part of the melting heater 5 is connected with the steam trap 2, and the generated steam condensed water G is discharged after heat exchange of the heater 1; or

When the heat medium of the heat supply unit is heat conduction oil F ', the heat supply unit comprises a heat conduction oil expansion tank 2 ' and a heat conduction oil pump 3 '; the heat conduction oil pump 3 'is connected with the heat conduction oil heater 4'; the outlet of the heat-conducting oil heater 4 ' is connected with the inlet of the melting heater 5, the heat-conducting oil heater and the heat-conducting oil pump 3 ' form a circulation loop through the outlet of the multiphase separation tank 7 via the heater 1, and the heat-conducting oil expansion tank 2 is externally connected with the circulation loop and is arranged at the front end of the heat-conducting oil pump 3 ';

31. A method for continuous phase separation using the above system, the method comprising: