Summary of the invention
First purpose of the present invention is to obtain a kind of continuous maturing equipment of grade insoluble sulphur in a kind of safety, low consumption, the production of high mass-energy.
Second purpose of the present invention is to obtain a kind of continuous ageing method of grade insoluble sulphur in a kind of safety, low consumption, the production of high mass-energy.
In a first aspect of the present invention, the production unit of grade insoluble sulphur in a kind of continuous ageing method is provided, it comprises:
The unit that feeds intake of liquid-state sulfur raw material is provided;
Described liquid-state sulfur raw material gasified obtain the gasification unit of gaseous sulfur;
Thereby described gaseous sulfur is carried out the ageing unit that ageing powder process obtains grade insoluble sulphur in the wet-milling shape;
Grade insoluble sulphur in the described wet-milling shape is carried out the post-processing unit that aftertreatment obtains middle grade insoluble sulphur.
In a specific embodiment of the present invention, the described unit that feeds intake comprises liquid sulfur pit (1) that stores described liquid-state sulfur raw material and the volume pump (2) that described liquid-state sulfur raw material is measured.
In a preference, described liquid sulfur pit (1) is dual-purpose design, both can store molten sulfur (or being called liquid sulfur), also can fuse solid sulphur (or being called solid-state sulphur) when molten sulfur lacks.
In a specific embodiment of the present invention, described gasification unit comprises vapourizing furnace (3) that the liquid-state sulfur raw material is gasified and the gaseous sulfur shower nozzle (4) that gaseous sulfur is sprayed.
In a preference, described vapourizing furnace (3) is the tubular type vapourizing furnace.
In a specific embodiment of the present invention, described ageing unit comprises:
Ageing powder process tower (5), the middle part of described ageing powder process tower (5) be provided with quencher (6), top be provided with condenser (7) and
Ageing tank (9).
In a preference, described ageing tank (9) is provided with insulation, heating system, ageing tank (9) but the serial or parallel connection setting.
In a preference, described ageing powder process tower (5) is combined by horizontal stirred vessel and vertical stirred vessel, on horizontal stirred vessel, be provided with gaseous sulfur shower nozzle (4), quencher (6), condenser (7), also be provided with optional liquidometer, tensimeter, thermometer.
In a preference, described ageing unit also comprises solid-liquid separating machine (11); In a preference, described solid-liquid separating machine (11) can adopt separating centrifuge or vacuum filter.
In a specific embodiment of the present invention, described post-processing unit comprises drying machine (12).
In a preference, described drying machine (12) can adopt Vacuumdrier.Described Vacuumdrier can be various types of Vacuumdriers.
In a specific embodiment of the present invention, described production unit comprises:
Liquid sulfur pit (1), volume pump (2), tubular type vapourizing furnace (3), gaseous sulfur shower nozzle (4), ageing powder process tower (5), quencher (6), condenser (7), suspension transferpump (8), ageing tank (9), ageing transferpump (10), solid-liquid separating machine (11), drying machine (12);
Its annexation is as follows:
The interior liquid sulfur of described liquid sulfur pit (1) is delivered to tubular type vapourizing furnace (3) by the quantitative level pressure of volume pump (2), and liquid sulfur is gasificated into gaseous sulfur in tubular type vapourizing furnace (3); Described gaseous sulfur enters quencher (6) inside at ageing powder process tower (5) middle part from ageing powder process tower (5) bottom side through gaseous sulfur shower nozzle (4); Accelerant suspension is delivered in the quencher (6), condenser (7) on ageing powder process tower (5) middle part and top by suspension transferpump (8); Another road accelerant suspension is delivered to ageing tank (9), and described gaseous sulfur is converted into the plastic mixture of insoluble sulfur and soluble sulfur through chilling;
Accelerant evenly is added in the ageing powder process tower (5) continuously, accelerant suspension evenly enters ageing tank (9) continuously by suspension transferpump (8), in ageing tank (9), handle through the high temperature ageing, be delivered to solid-liquid separating machine (11) with ageing transferpump (10) and carry out solid-liquid separation and washing, promptly obtain containing grade insoluble sulphur in the wet-milling shape;
Drying machine (12) drying treatment obtains middle grade insoluble sulphur finished product again.
In a preference, described suspension transferpump (8), ageing transferpump (10) adopt vertical or horizontal anticorrosive anti-wear shurry pump.
In a preference, all adopt corrosion resistant metallic substance, anti-corrosion of metal or nonmetal anticorrosive material with gas, liquid contacting part position in the described all devices.
A second aspect of the present invention provides the preparation method of grade insoluble sulphur in a kind of continuous ageing method, and it comprises the steps:
The unit provides liquid sulfur by feeding intake;
Adopt gasification unit liquid towards sulphur to carry out high-temperature gasification, obtain gaseous sulfur;
In the ageing unit, carry out chilling powder process, high temperature ageing, separating, washing, obtain grade insoluble sulphur in the wet-milling shape;
Grade insoluble sulphur in the described wet-milling shape is carried out drying, obtain middle grade insoluble sulphur.
In a specific embodiment of the present invention, in the unit that feeds intake, the interior liquid sulfur of liquid sulfur pit (1) is delivered in the tubular type vapourizing furnace (3) by the quantitative level pressure of volume pump (2), and its pressure-controlling is in 0.2 to 1.0MPa scope;
In gasification unit, described liquid sulfur changes into gaseous sulfur through tubular type vapourizing furnace (3) High Temperature Gas, and the gaseous sulfur temperature out is controlled between 450-750 ℃;
In the ageing unit, described gaseous sulfur enters quencher (6) inside at ageing powder process tower (5) middle part from ageing powder process tower (5) bottom side through gaseous sulfur shower nozzle (4), accelerant suspension is delivered to the quencher (6) on ageing powder process tower (5) middle part and top by suspension transferpump (8), in the condenser (7), its cloth liquid direction is: accelerant suspension is past decline from top, gaseous sulfur rises by the bottom is past, thereby reach gaseous sulfur and accelerant suspension is direct, fast, fully contact, make the gaseous sulfur chilling be converted into the plastic mixture of insoluble sulfur and soluble sulfur, the interior temperature of ageing powder process tower (5) is controlled between 35 to 90 ℃, and pressure-controlling is between 0.05 to 1.0MPa;
The interior accelerant suspension of ageing powder process tower (a 5) part is circulated to quencher (6), condenser (7); A part evenly enters ageing tank (9) continuously and carries out high temperature ageing processing, is 30 minutes to 4 hours in ageing tank (9) residence time, and temperature is controlled between 45-95 ℃, and pressure-controlling is between 0.05 to 1.0MPa;
Be delivered to solid-liquid separating machine (11) through the accelerant suspension of ageing tank (9) pyroprocessing with ageing transferpump (10) and carry out solid-liquid separation and washing, accelerant is recycled, and washings enters Sewage treatment systems;
In post-processing unit, grade insoluble sulphur enters drying machine (12) and carries out vacuum-drying in the wet-milling shape, and its dry water temperature is controlled between 40 to 95 ℃, and vacuum pressure is controlled between 0.02 to 0.08MPa, obtains middle grade insoluble sulphur.
In a specific embodiment of the present invention, described accelerant adopts water, nitric acid, iron trichloride, aluminum chloride, iodine, alcohol mixeding liquid.
In a specific embodiment of the present invention, the purity of described middle grade insoluble sulphur is between 40~65 weight %.
Embodiment
The inventor is through extensive and deep research, by improving preparation technology, two technical process of grade insoluble sulphur in the home and abroad high-temperature gasification manufactured have during the last ten years been changed, flow processs such as traditional compressing tablet depickling, drying and crushing have been cancelled, thereby improved operating environment, reduced labor strength, saved production cost, improve the high-temperature stability of product, obtained grade insoluble sulphur production unit and preparation method in a kind of ideal.Finished the present invention on this basis.
Technical conceive of the present invention is as follows:
The objective of the invention is for overcome existing in grade insoluble sulphur production unit and preparation method's shortcoming, and provide a kind of safety, low consumption, high mass-energy produce in grade insoluble sulphur production unit and preparation method in a kind of continuous ageing method of grade insoluble sulphur.
For this reason, the invention provides grade insoluble sulphur production unit and preparation method in a kind of continuous ageing method.Be characterized in that equipment comprises: liquid sulfur pit, volume pump, tubular type vapourizing furnace, gaseous sulfur shower nozzle, ageing powder process tower, quencher, condenser, suspension transferpump, ageing tank, ageing transferpump, solid-liquid separating machine, drying machine; Liquid sulfur is delivered to the tubular type vapourizing furnace by the quantitative level pressure of volume pump in the liquid sulfur pit, and liquid sulfur High Temperature Gas in the tubular type vapourizing furnace changes into gaseous sulfur; Gaseous sulfur enters the quencher inside at ageing powder process tower middle part from ageing powder process tower bottom side through the gaseous sulfur shower nozzle; Accelerant suspension is delivered in the quencher, condenser on ageing powder process tower middle part and top by the suspension transferpump; Another road accelerant suspension is delivered to ageing tank, and gaseous sulfur is converted into the plastic mixture of insoluble sulfur and soluble sulfur through chilling.Accelerant evenly is added in the ageing powder process tower continuously, accelerant suspension evenly enters ageing tank continuously by the suspension transferpump, in ageing tank, handle through the high temperature ageing, be delivered to solid-liquid separating machine with the ageing transferpump and carry out solid-liquid separation and washing, promptly obtain containing grade insoluble sulphur in the wet-milling shape; Drying machine drying treatment obtains middle grade high temperature stability insoluble sulfur finished product again.
Below describe in detail to various aspects of the present invention:
Production unit
The production unit of grade insoluble sulphur in a kind of continuous ageing method, it comprises:
The unit that feeds intake of liquid-state sulfur raw material is provided;
Described liquid-state sulfur raw material gasified obtain the gasification unit of gaseous sulfur;
Thereby described gaseous sulfur is carried out the ageing unit that ageing powder process obtains grade insoluble sulphur in the wet-milling shape;
Grade insoluble sulphur in the described wet-milling shape is carried out the post-processing unit that aftertreatment obtains middle grade insoluble sulphur.
In an embodiment, the described unit that feeds intake comprises liquid sulfur pit (1) that stores described liquid-state sulfur raw material and the volume pump (2) that described liquid-state sulfur raw material is measured.
In a preference, described liquid sulfur pit (1) is dual-purpose design, both can store molten sulfur (or being called liquid sulfur), also can fuse solid sulphur (or being called solid-state sulphur) when molten sulfur lacks.
In an embodiment, described gasification unit comprises vapourizing furnace (3) that the liquid-state sulfur raw material is gasified and the gaseous sulfur shower nozzle (4) that gaseous sulfur is sprayed.
In a preference, described vapourizing furnace (3) is the tubular type vapourizing furnace.
In an embodiment, described ageing unit comprises:
Ageing powder process tower (5), the middle part of described ageing powder process tower (5) be provided with quencher (6), top be provided with condenser (7) and
Ageing tank (9).
In a preference, described ageing tank (9) is provided with insulation, heating system, ageing tank (9) but the serial or parallel connection setting.
In a preference, described ageing powder process tower (5) is combined by horizontal stirred vessel and vertical stirred vessel, on horizontal stirred vessel, be provided with gaseous sulfur shower nozzle (4), quencher (6), condenser (7), also be provided with optional liquidometer, tensimeter, thermometer.
In a preference, described ageing unit also comprises solid-liquid separating machine (11); In a preference, described solid-liquid separating machine (11) can adopt separating centrifuge or vacuum filter.
In an embodiment, described post-processing unit comprises drying machine (12).
In a preference, described drying machine (12) can adopt Vacuumdrier.Described Vacuumdrier can be various types of Vacuumdriers.
In an embodiment, described production unit comprises:
Liquid sulfur pit (1), volume pump (2), tubular type vapourizing furnace (3), gaseous sulfur shower nozzle (4), ageing powder process tower (5), quencher (6), condenser (7), suspension transferpump (8), ageing tank (9), ageing transferpump (10), solid-liquid separating machine (11), drying machine (12);
Its annexation is as follows:
The interior liquid sulfur of described liquid sulfur pit (1) is delivered to tubular type vapourizing furnace (3) by the quantitative level pressure of volume pump (2), and liquid sulfur is gasificated into gaseous sulfur in tubular type vapourizing furnace (3); A road of described gaseous sulfur enters quencher (6) inside at ageing powder process tower (5) middle part through gaseous sulfur shower nozzle (4) from ageing powder process tower (5) bottom side; Accelerant suspension is delivered in the quencher (6), condenser (7) on ageing powder process tower (5) middle part and top by suspension transferpump (8); Another road accelerant suspension is delivered to ageing tank (9), and described gaseous sulfur is converted into the plastic mixture of insoluble sulfur and soluble sulfur through chilling;
Accelerant evenly is added in the ageing powder process tower (5) continuously, accelerant suspension evenly enters ageing tank (9) continuously by suspension transferpump (8), in ageing tank (9), handle through the high temperature ageing, be delivered to solid-liquid separating machine (11) with ageing transferpump (10) and carry out solid-liquid separation and washing, promptly obtain containing grade insoluble sulphur in the wet-milling shape;
Drying machine (12) drying treatment obtains middle grade insoluble sulphur finished product again.
In a preference, described suspension transferpump (8), ageing transferpump (10) adopt vertical or horizontal anticorrosive anti-wear shurry pump.
In a preference, all adopt corrosion resistant metallic substance, anti-corrosion of metal or nonmetal anticorrosive material with gas, liquid contacting part position in the described all devices.
The preparation method
The invention provides the preparation method of grade insoluble sulphur in a kind of continuous ageing method, it comprises the steps:
The unit provides liquid sulfur by feeding intake;
Adopt gasification unit liquid towards sulphur to carry out high-temperature gasification, obtain gaseous sulfur;
In the ageing unit, carry out chilling powder process, high temperature ageing, separating, washing, obtain grade insoluble sulphur in the wet-milling shape;
Grade insoluble sulphur in the described wet-milling shape is carried out drying, obtain middle grade insoluble sulphur.
In an embodiment, in the unit that feeds intake, the interior liquid sulfur of liquid sulfur pit (1) is delivered in the tubular type vapourizing furnace (3) by the quantitative level pressure of volume pump (2), and its pressure-controlling is in 0.2 to 1.0MPa scope;
In gasification unit, described liquid sulfur changes into gaseous sulfur through tubular type vapourizing furnace (3) High Temperature Gas, and the gaseous sulfur temperature out is controlled between 450-750 ℃;
In the ageing unit, described gaseous sulfur enters quencher (6) inside at ageing powder process tower (5) middle part from ageing powder process tower (5) bottom side through gaseous sulfur shower nozzle (4), accelerant suspension is delivered to the quencher (6) on ageing powder process tower (5) middle part and top by suspension transferpump (8), in the condenser (7), its cloth liquid direction is: accelerant suspension is past decline from top, gaseous sulfur rises by the bottom is past, thereby reach gaseous sulfur and accelerant suspension is direct, fast, fully contact, make the gaseous sulfur chilling be converted into the plastic mixture of insoluble sulfur and soluble sulfur, the interior temperature of ageing powder process tower (5) is controlled between 35 to 90 ℃, and pressure-controlling is between 0.05 to 1.0MPa;
The interior accelerant suspension of ageing powder process tower (a 5) part is circulated to quencher (6), condenser (7); A part evenly enters ageing tank (9) continuously and carries out high temperature ageing processing, is 30 minutes to 4 hours in ageing tank (9) residence time, and temperature is controlled between 45-95 ℃, and pressure-controlling is between 0.05 to 1.0MPa;
Be delivered to solid-liquid separating machine (11) through the accelerant suspension of ageing tank (9) pyroprocessing with ageing transferpump (10) and carry out solid-liquid separation and washing, accelerant is recycled, and washings enters Sewage treatment systems;
In post-processing unit, grade insoluble sulphur enters drying machine (12) and carries out vacuum-drying in the wet-milling shape, and its dry water temperature is controlled between 40 to 95 ℃, and vacuum pressure is controlled between 0.02 to 0.08MPa, obtains middle grade insoluble sulphur.
In an embodiment, described accelerant adopts water, nitric acid, iron trichloride, aluminum chloride, iodine, alcohol mixeding liquid.
In an embodiment, the purity of described middle grade insoluble sulphur is between 40~65 weight %.
The invention has the advantages that:
Because the present invention has adopted above technical scheme, two traditional technologys of grade insoluble sulphur in the home and abroad high-temperature gasification manufactured have during the last ten years been changed, flow processs such as compressing tablet, depickling, dry solidification pulverizing have been cancelled, thereby improved operating environment, reduced labor strength, having saved production cost, improved the high-temperature stability of product, is grade insoluble sulphur production unit and preparation method in a kind of ideal.
Specify as nothing, various raw materials of the present invention all can obtain by commercially available; Or prepare according to the ordinary method of this area.Unless otherwise defined or explanation, same meanings of being familiar with of all specialties used herein and scientific words and those skilled in the art.Any in addition method similar or impartial to described content and material all can be applicable in the inventive method.
Other aspects of the present invention are because the disclosure of this paper is conspicuous to those skilled in the art.
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.The experimental technique of unreceipted actual conditions in the following example usually according to normal condition, or carries out according to the condition that manufacturer advises.Unless otherwise indicated, otherwise all umbers are weight part, and all per-cents are weight percentage, and described polymericular weight is a number-average molecular weight.
Unless otherwise defined or explanation, same meanings of being familiar with of all specialties used herein and scientific words and those skilled in the art.Any in addition method similar or impartial to described content and material all can be applicable in the inventive method.
Embodiment 1
Fig. 1 is the schematic flow sheet of present device.
The production unit of grade insoluble sulphur in a kind of continuous ageing method of the present invention, be characterized in, comprise: liquid sulfur pit (1), volume pump (2), tubular type vapourizing furnace (3), gaseous sulfur shower nozzle (4), ageing powder process tower (5), quencher (6), condenser (7), suspension transferpump (8), ageing tank (9), ageing transferpump (10), solid-liquid separating machine (11), drying machine (12);
The interior liquid sulfur of described liquid sulfur pit (1) is delivered to tubular type vapourizing furnace (3) by the quantitative level pressure of volume pump (2), and liquid sulfur High Temperature Gas in tubular type vapourizing furnace (3) changes into gaseous sulfur; Gaseous sulfur enters quencher (6) inside at ageing powder process tower (5) middle part from ageing powder process tower (5) bottom side through gaseous sulfur shower nozzle (4); Accelerant suspension is delivered in the quencher (6), condenser (7) on ageing powder process tower (5) middle part and top by suspension transferpump (8); Another road is delivered to ageing tank (9), and gaseous sulfur is converted into the plastic mixture of insoluble sulfur and soluble sulfur through chilling.Accelerant evenly is added in the ageing powder process tower (5) continuously, accelerant suspension evenly enters ageing tank (9) continuously by suspension transferpump (8), in ageing tank (9), handle through the high temperature ageing, be delivered to solid-liquid separating machine (11) with ageing transferpump (10) and carry out solid-liquid separation and washing, promptly obtain containing grade insoluble sulphur in the wet-milling shape; Drying machine (12) drying treatment obtains middle grade high temperature stability insoluble sulfur finished product again.
Grade insoluble sulphur production unit in the above-mentioned continuous ageing method, wherein said ageing powder process tower (5) is combined by horizontal stirred vessel and vertical stirred vessel, on horizontal stirred vessel, be provided with gaseous sulfur shower nozzle (4), quencher (6), condenser (7), also be provided with liquidometer, tensimeter, thermometer.Ageing powder process tower (5) is corrosion resistant metallic substance, anti-corrosion of metal or nonmetal anticorrosive material with material contact site material.
Grade insoluble sulphur production unit in the above-mentioned continuous ageing method, wherein said suspension transferpump (8), ageing transferpump (10) adopt vertical or horizontal anticorrosive anti-wear shurry pump, and material is corrosion resistant metallic substance or corrosion resistant non-metallic material.
Grade insoluble sulphur production unit in the above-mentioned continuous ageing method, wherein said solid-liquid separating machine (11) can adopt separating centrifuge or vacuum filter, and material is selected the corrosion resistant metallic substance for use.
Grade insoluble sulphur production unit in the above-mentioned continuous ageing method, wherein said ageing tank (9) is provided with whipping appts, be provided with insulation, heating system according to the high temperature ageing residence time, ageing tank (9) but the serial or parallel connection setting, its material is corrosion resistant metallic substance, anti-corrosion of metal or nonmetal anticorrosive material.
Grade insoluble sulphur production unit in the above-mentioned continuous ageing method, wherein said drying machine (12) can adopt various types of Vacuumdriers, and its material is the corrosion resistant metallic substance with material gas contact site.
Grade insoluble sulphur production unit in the above-mentioned continuous ageing method, wherein said liquid sulfur pit (1) can be dual-purpose, both can store molten sulfur, also can fuse solid sulphur when molten sulfur lacks, and its material is a stainless steel for the molten sulfur contact site.
Preparation method of the present invention is: adopt aforesaid device, and flow settings such as liquid sulfur high-temperature gasification, chilling powder process, high temperature ageing, separating, washing, drying, its step is as follows:
A, the interior liquid sulfur of liquid sulfur pit (1) are delivered in the tubular type vapourizing furnace (3) by the quantitative level pressure of volume pump (2), and its pressure-controlling is in 0.2 to 1.0MPa scope.
B, liquid sulfur change into gaseous sulfur through tubular type vapourizing furnace (3) High Temperature Gas, and the gaseous sulfur temperature out is controlled between 450-750 ℃.
C, gaseous sulfur enters quencher (6) inside at ageing powder process tower (5) middle part from ageing powder process tower (5) bottom side through gaseous sulfur shower nozzle (4), accelerant suspension is delivered to the quencher (6) on ageing powder process tower (5) middle part and top by suspension transferpump (8), in the condenser (7), its cloth liquid direction is: accelerant suspension is past decline from top, gaseous sulfur rises by the bottom is past, thereby reach gaseous sulfur and accelerant suspension is direct, fast, fully contact, make the gaseous sulfur chilling be converted into the plastic mixture of insoluble sulfur and soluble sulfur, the interior temperature of ageing powder process tower (5) is controlled between 35 to 90 ℃, and pressure-controlling is between 0.05 to 1.0MPa.
D, the interior accelerant suspension of ageing powder process tower (a 5) part are circulated to quencher (6), condenser (7); A part evenly enters ageing tank (9) continuously and carries out high temperature ageing processing, is 30 minutes to 4 hours in ageing tank (9) residence time, and temperature is controlled between 45-95 ℃, and pressure-controlling is between 0.05 to 1.0MPa.
E, be delivered to solid-liquid separating machine (11) through the accelerant suspension of ageing tank (9) pyroprocessing with ageing transferpump (10) and carry out solid-liquid separation and washing, accelerant is recycled, and washings enters Sewage treatment systems.
F, contain in the wet-milling shape grade insoluble sulphur and enter drying machine (12) and carry out vacuum-drying, its dry water temperature is controlled between 40 to 95 ℃, and vacuum pressure is controlled between 0.02 to 0.08MPa.
G, accelerant adopt water, nitric acid, iron trichloride, aluminum chloride, iodine, alcohol mixeding liquid.
The present invention has improved operating environment, has reduced labor strength, has saved production cost, has improved the high-temperature stability of product, is grade insoluble sulphur production unit and preparation method in a kind of ideal.
The above only is preferred embodiment of the present invention, be not in order to limit essence technology contents scope of the present invention, essence technology contents of the present invention is broadly to be defined in the claim scope of application, any technology entity or method that other people finish, if it is defined identical with the claim scope of application, also or a kind of change of equivalence, all will be regarded as being covered by among this claim scope.
All quote in this application as a reference at all documents that the present invention mentions, just quoted as a reference separately as each piece document.Should be understood that in addition after having read foregoing of the present invention, those skilled in the art can make various changes or modifications the present invention, these equivalent form of values fall within the application's appended claims institute restricted portion equally.