CN102167292B - Equipment and method for producing medium-grade insoluble sulfur with continuous ageing method - Google Patents
Equipment and method for producing medium-grade insoluble sulfur with continuous ageing method Download PDFInfo
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- CN102167292B CN102167292B CN2011100344496A CN201110034449A CN102167292B CN 102167292 B CN102167292 B CN 102167292B CN 2011100344496 A CN2011100344496 A CN 2011100344496A CN 201110034449 A CN201110034449 A CN 201110034449A CN 102167292 B CN102167292 B CN 102167292B
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Abstract
The invention provides equipment for producing medium-grade insoluble sulfur with a continuous ageing method. The equipment comprises a feeding unit, a gasifying unit, an ageing unit and a postprocessing unit, wherein the feeding unit is used for providing liquid sulfur raw materials; the gasifying unit is used for gasifying the liquid sulfur raw materials to obtain gaseous sulfur; the ageing unit is used for ageing the gaseous sulfur to prepare powder so as to obtain wet powdery medium-grade insoluble sulfur; and the postprocessing unit is used for postprocessing the wet powdery medium-grade insoluble sulfur to obtain the medium-grade insoluble sulfur. The invention also provides a method for producing the medium-grade insoluble sulfur. The invention provides the continuous ageing method and equipment for producing the medium-grade insoluble sulfur in a safety, low-consumption and high-quality way.
Description
Technical field
The present invention relates to a kind of middle grade insoluble sulphur production unit and preparation method, the production unit and the preparation method of grade insoluble sulphur in particularly a kind of continuous ageing method.
Background technology
Middle grade insoluble sulphur production; The existing high-temperature gasification method in home and abroad is continued to use the heat technical process of gasification, quenching chilling, compressing tablet, washing, dry solidification, pulverizing of liquid sulfur always; This flow operations environment is abominable, labor strength is big, production cost is high, unstable product quality, has seriously restricted the development of domestic insoluble sulfur.
Grade insoluble sulphur is well known by persons skilled in the art in said, and it describes visible Chinese patent publication number CN1986388 and CN101337659 etc.
In sum, this area lacks the continuous production method of grade insoluble sulphur in safety, low consumption, the production of high mass-energy.
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 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;
Said liquid-state sulfur raw material gasified obtain the gasification unit of gaseous sulfur;
Thereby said 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 said wet-milling shape is carried out the post-processing unit that aftertreatment obtains middle grade insoluble sulphur.
In an embodiment of the present invention, the said unit that feeds intake comprises liquid sulfur pit (1) that stores said liquid-state sulfur raw material and the volume pump (2) that said 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 when molten sulfur lacks, fuse solid sulphur (or being called solid-state sulphur).
In an embodiment of the present invention, said 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, said vapourizing furnace (3) is the tubular type vapourizing furnace.
In an embodiment of the present invention, said ageing unit comprises:
Ageing powder process tower (5), the middle part of said ageing powder process tower (5) be provided with quencher (6), top be provided with condensing surface (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), condensing surface (7), also be provided with optional liquidometer, tensimeter, TM.
In a preference, said 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 of the present invention, said post-processing unit comprises drying machine (12).
In a preference, described drying machine (12) can adopt Vacuumdrier.Said Vacuumdrier can be various types of Vacuumdriers.
In an embodiment of the present invention, said 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), condensing surface (7), suspension-s transferpump (8), ageing tank (9), ageing transferpump (10), solid-liquid separating machine (11), drying machine (12);
Its annexation is following:
The interior liquid sulfur of described liquid sulfur pit (1) is delivered to tubular type vapourizing furnace (3) through the quantitative level pressure of volume pump (2), and liquid sulfur is gasificated into gaseous sulfur in tubular type vapourizing furnace (3); Said gaseous sulfur is through quencher (6) inside at gaseous sulfur shower nozzle (4) side entering ageing powder process tower (5) middle part from ageing powder process tower (5) bottom; Accelerant suspension-s is delivered in the quencher (6), condensing surface (7) on ageing powder process tower (5) middle part and top through suspension-s transferpump (8); Another road accelerant suspension-s is delivered to ageing tank (9), and said 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-s evenly gets into ageing tank (9) continuously through suspension-s 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;
Through drying machine (12) drying treatment, obtain middle grade insoluble sulphur finished product again.
In a preference, described suspension-s 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.
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 through 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 said wet-milling shape is carried out drying, obtain middle grade insoluble sulphur.
In an 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) through the quantitative level pressure of volume pump (2), and its pressure-controlling is in 0.2 to 1.0MPa scope;
In gasification unit, said 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; Said gaseous sulfur is through quencher (6) inside at gaseous sulfur shower nozzle (4) side entering ageing powder process tower (5) middle part from ageing powder process tower (5) bottom; Accelerant suspension-s is delivered in the quencher (6), condensing surface (7) on ageing powder process tower (5) middle part and top through suspension-s transferpump (8); Its cloth liquid direction is: accelerant suspension-s is past decline from top; Gaseous sulfur by the bottom toward rising, thereby reach gaseous sulfur and accelerant suspension-s directly, quick, 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-s of ageing powder process tower (a 5) part is circulated to quencher (6), condensing surface (7); A part evenly gets into 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-s of ageing tank (9) pyroprocessing with ageing transferpump (10) and carry out solid-liquid separation and washing, accelerant is recycled, and washings gets into Sewage treatment systems;
In post-processing unit, grade insoluble sulphur entering drying machine (12) 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 of the present invention, said accelerant adopts water, nitric acid, iron trichloride, aluminum chloride, iodine, alcohol mixeding liquid.
In an embodiment of the present invention, the purity of said middle grade insoluble sulphur is between 40～65 weight %.
Description of drawings
Fig. 1 is the connection synoptic diagram of an embodiment of the present invention.
Embodiment
The inventor is through extensive and deep research, through improving preparation technology, changed two technical process of grade insoluble sulphur in the home and abroad high-temperature gasification manufactured during the last ten years; Flow processs such as traditional compressing tablet depickling, drying and crushing have been cancelled; Thereby improved operating environment, reduced labor strength, practiced thrift production cost; Improve the high-temperature stability of product, obtained grade insoluble sulphur production unit and preparation method in a kind of ideal.Accomplished the present invention on this basis.
Technical conceive of the present invention is following:
The objective of the invention is for overcome existing in grade insoluble sulphur production unit and preparing 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 present 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, condensing surface, suspension-s transferpump, ageing tank, ageing transferpump, solid-liquid separating machine, drying machine; Liquid sulfur is delivered to the tubular type vapourizing furnace through 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 is inner through the quencher at gaseous sulfur shower nozzle side entering ageing powder process tower middle part from ageing powder process tower bottom; Accelerant suspension-s is delivered in the quencher, condensing surface on ageing powder process tower middle part and top through the suspension-s transferpump; Another road accelerant suspension-s 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-s evenly gets into ageing tank continuously through the suspension-s 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; Through the drying machine drying treatment, obtain middle grade high temperature stability insoluble sulfur finished product again.
Below 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;
Said liquid-state sulfur raw material gasified obtain the gasification unit of gaseous sulfur;
Thereby said 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 said wet-milling shape is carried out the post-processing unit that aftertreatment obtains middle grade insoluble sulphur.
In an embodiment, the said unit that feeds intake comprises liquid sulfur pit (1) that stores said liquid-state sulfur raw material and the volume pump (2) that said 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 when molten sulfur lacks, fuse solid sulphur (or being called solid-state sulphur).
In an embodiment, said 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, said vapourizing furnace (3) is the tubular type vapourizing furnace.
In an embodiment, said ageing unit comprises:
Ageing powder process tower (5), the middle part of said ageing powder process tower (5) be provided with quencher (6), top be provided with condensing surface (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), condensing surface (7), also be provided with optional liquidometer, tensimeter, TM.
In a preference, said 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, said post-processing unit comprises drying machine (12).
In a preference, described drying machine (12) can adopt Vacuumdrier.Said Vacuumdrier can be various types of Vacuumdriers.
In an embodiment, said 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), condensing surface (7), suspension-s transferpump (8), ageing tank (9), ageing transferpump (10), solid-liquid separating machine (11), drying machine (12);
Its annexation is following:
The interior liquid sulfur of described liquid sulfur pit (1) is delivered to tubular type vapourizing furnace (3) through the quantitative level pressure of volume pump (2), and liquid sulfur is gasificated into gaseous sulfur in tubular type vapourizing furnace (3); One tunnel quencher (6) inside of said gaseous sulfur through gaseous sulfur shower nozzle (4) side entering ageing powder process tower (5) middle part from ageing powder process tower (5) bottom; Accelerant suspension-s is delivered in the quencher (6), condensing surface (7) on ageing powder process tower (5) middle part and top through suspension-s transferpump (8); Another road accelerant suspension-s is delivered to ageing tank (9), and said 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-s evenly gets into ageing tank (9) continuously through suspension-s 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;
Through drying machine (12) drying treatment, obtain middle grade insoluble sulphur finished product again.
In a preference, described suspension-s 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 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 through 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 said 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) through the quantitative level pressure of volume pump (2), and its pressure-controlling is in 0.2 to 1.0MPa scope;
In gasification unit, said 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; Said gaseous sulfur is through quencher (6) inside at gaseous sulfur shower nozzle (4) side entering ageing powder process tower (5) middle part from ageing powder process tower (5) bottom; Accelerant suspension-s is delivered in the quencher (6), condensing surface (7) on ageing powder process tower (5) middle part and top through suspension-s transferpump (8); Its cloth liquid direction is: accelerant suspension-s is past decline from top; Gaseous sulfur by the bottom toward rising, thereby reach gaseous sulfur and accelerant suspension-s directly, quick, 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-s of ageing powder process tower (a 5) part is circulated to quencher (6), condensing surface (7); A part evenly gets into 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-s of ageing tank (9) pyroprocessing with ageing transferpump (10) and carry out solid-liquid separation and washing, accelerant is recycled, and washings gets into Sewage treatment systems;
In post-processing unit, grade insoluble sulphur entering drying machine (12) 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, said accelerant adopts water, nitric acid, iron trichloride, aluminum chloride, iodine, alcohol mixeding liquid.
In an embodiment, the purity of said middle grade insoluble sulphur is between 40～65 weight %.
The invention has the advantages that:
Because the present invention has adopted above technical scheme; Changed two traditional technologys of grade insoluble sulphur in the home and abroad high-temperature gasification manufactured during the last ten years, cancelled flow processs such as compressing tablet, depickling, dry solidification pulverizing, thereby improved operating environment; Reduced labor strength; Having practiced thrift production cost, improved the high-temperature stability of product, is grade insoluble sulphur production unit and preparation method in a kind of ideal.
Specify like nothing, various raw materials of the present invention all can obtain through commercially available; Or prepare according to the ordinary method of this area.Only if definition or explanation are arranged in addition, the same meaning that all specialties used herein and scientific words and those skilled in the art are familiar with.Any in addition with the institute similar content of putting down in writing or the equalization method 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 the restriction scope of the present 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.
Only if definition or explanation are arranged in addition, the same meaning that all specialties used herein and scientific words and those skilled in the art are familiar with.Any in addition with the institute similar content of putting down in writing or the equalization method and material all can be applicable in the inventive method.
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), condensing surface (7), suspension-s 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) through 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 is through quencher (6) inside at gaseous sulfur shower nozzle (4) side entering ageing powder process tower (5) middle part from ageing powder process tower (5) bottom; Accelerant suspension-s is delivered in the quencher (6), condensing surface (7) on ageing powder process tower (5) middle part and top through suspension-s 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-s evenly gets into ageing tank (9) continuously through suspension-s 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; Through drying machine (12) drying treatment, obtain 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), condensing surface (7), also be provided with liquidometer, tensimeter, TM.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-s 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 when molten sulfur lacks, fuse solid sulphur, and its material is a stainless steel for the molten sulfur contact site.
Preparing 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 following:
A, the interior liquid sulfur of liquid sulfur pit (1) are delivered in the tubular type vapourizing furnace (3) through 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 ℃.
Side gets into quencher (6) inside at ageing powder process tower (5) middle part from ageing powder process tower (5) bottom through gaseous sulfur shower nozzle (4) for c, gaseous sulfur; Accelerant suspension-s is delivered in the quencher (6), condensing surface (7) on ageing powder process tower (5) middle part and top through suspension-s transferpump (8); Its cloth liquid direction is: accelerant suspension-s is past decline from top; Gaseous sulfur by the bottom toward rising, thereby reach gaseous sulfur and accelerant suspension-s directly, quick, 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-s of ageing powder process tower (a 5) part are circulated to quencher (6), condensing surface (7); A part evenly gets into 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-s of ageing tank (9) pyroprocessing with ageing transferpump (10) and carry out solid-liquid separation and washing, accelerant is recycled, and washings gets into Sewage treatment systems.
F, contain in the wet-milling shape grade insoluble sulphur and get into 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 practiced thrift 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 is merely 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, and if any technological entity or method that other people accomplish are defined identical with the claim scope of application; Also or a kind of change of equivalence, all will be regarded as and be covered by among this claim scope.
All documents in that the present invention mentions are all quoted as a reference in this application, are just quoted such as a reference separately as each piece document.Should be understood that in addition that after having read foregoing of the present invention those skilled in the art can do various changes or modification to the present invention, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Claims (2)
1. the production unit of grade insoluble sulphur in the continuous ageing method is characterized in that, comprising:
The unit that feeds intake of liquid-state sulfur raw material is provided; The said unit that feeds intake comprises liquid sulfur pit (1) that stores said liquid-state sulfur raw material and the volume pump (2) that said liquid-state sulfur raw material is measured,
Said liquid-state sulfur raw material gasified obtain the gasification unit of gaseous sulfur; Said gasification unit comprises tubular type vapourizing furnace (3) that the liquid-state sulfur raw material is gasified and the gaseous sulfur shower nozzle (4) that gaseous sulfur is sprayed,
Thereby said gaseous sulfur is carried out the ageing unit that ageing powder process obtains grade insoluble sulphur in the wet-milling shape; Said ageing unit comprises: ageing powder process tower (5), the middle part of said ageing powder process tower (5) are provided with quencher (6), top is provided with condensing surface (7) and ageing tank (9),
Grade insoluble sulphur in the said wet-milling shape is carried out the post-processing unit that aftertreatment obtains middle grade insoluble sulphur; Said post-processing unit comprises drying machine (12);
Wherein, said production unit also comprises:
Suspension-s transferpump (8), ageing transferpump (10) and solid-liquid separating machine (11);
Its annexation is following:
The interior liquid sulfur of described liquid sulfur pit (1) is delivered to tubular type vapourizing furnace (3) through the quantitative level pressure of volume pump (2), and liquid sulfur is gasificated into gaseous sulfur in tubular type vapourizing furnace (3); Said gaseous sulfur is through quencher (6) inside at gaseous sulfur shower nozzle (4) side entering ageing powder process tower (5) middle part from ageing powder process tower (5) bottom; The suspension-s transferpump (8) of leading up to of accelerant suspension-s is delivered in the quencher (6), condensing surface (7) on ageing powder process tower (5) middle part and top; Another road accelerant suspension-s is delivered to ageing tank (9), and said 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-s evenly gets into ageing tank (9) continuously through suspension-s 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;
Through drying machine (12) drying treatment, obtain middle grade insoluble sulphur again.
2. the preparation method of grade insoluble sulphur in the continuous ageing method is characterized in that, comprises the steps:
The unit provides liquid sulfur through feeding intake; In the unit that feeds intake, the interior liquid sulfur of liquid sulfur pit (1) is delivered in the tubular type vapourizing furnace (3) through the quantitative level pressure of volume pump (2), and its pressure-controlling is in 0.2 to 1.0MPa scope;
Adopt gasification unit liquid towards sulphur to carry out high-temperature gasification, obtain gaseous sulfur; In gasification unit, said 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, carry out chilling powder process, high temperature ageing, separating, washing, obtain grade insoluble sulphur in the wet-milling shape; In the ageing unit; Said gaseous sulfur is through quencher (6) inside at gaseous sulfur shower nozzle (4) side entering ageing powder process tower (5) middle part from ageing powder process tower (5) bottom; Accelerant suspension-s is delivered in the quencher (6), condensing surface (7) on ageing powder process tower (5) middle part and top through suspension-s transferpump (8); Its cloth liquid direction is: accelerant suspension-s is past decline from top; Gaseous sulfur by the bottom toward rising, thereby reach gaseous sulfur and accelerant suspension-s directly, quick, 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-s of ageing powder process tower (a 5) part is circulated to quencher (6), condensing surface (7); A part evenly gets into 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-s of ageing tank (9) pyroprocessing with ageing transferpump (10) and carry out solid-liquid separation and washing, accelerant is recycled, and washings gets into Sewage treatment systems;
Grade insoluble sulphur in the said wet-milling shape is carried out drying, obtain middle grade insoluble sulphur; Wherein, grade insoluble sulphur gets into drying machine (12) and carries out vacuum-drying in the said wet-milling shape in post-processing unit, 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.
Priority Applications (1)
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| CN102424363B (en) * | 2011-09-16 | 2013-05-22 | 无锡华盛橡胶新材料科技股份有限公司 | Processing unit for recovering sulphur from insoluble sulphur solvent |
| CN103552989A (en) * | 2013-11-07 | 2014-02-05 | 无锡华盛橡胶新材料科技股份有限公司 | Production equipment for continuously producing medium content insoluble sulfur |
| CN103539080A (en) * | 2013-11-07 | 2014-01-29 | 无锡华盛橡胶新材料科技股份有限公司 | Continuous preparation method of medium-content insoluble sulfur |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1424247A (en) * | 2002-12-25 | 2003-06-18 | 南化集团研究院 | Insoluble sulfur preparation |
| CN101066753A (en) * | 2007-05-29 | 2007-11-07 | 谭建中 | Continuous one-step process for producing insoluble sulphur |
| CN101486447A (en) * | 2008-12-15 | 2009-07-22 | 吴勇 | Method for preparing insoluble sulfur and common sulfur powder by gasification continuous one-step water method |
| CN101708824A (en) * | 2009-11-27 | 2010-05-19 | 江苏宏泰橡胶助剂有限公司 | Preparation method of high-thermostability insoluble sulfur |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1424247A (en) * | 2002-12-25 | 2003-06-18 | 南化集团研究院 | Insoluble sulfur preparation |
| CN101066753A (en) * | 2007-05-29 | 2007-11-07 | 谭建中 | Continuous one-step process for producing insoluble sulphur |
| CN101486447A (en) * | 2008-12-15 | 2009-07-22 | 吴勇 | Method for preparing insoluble sulfur and common sulfur powder by gasification continuous one-step water method |
| CN101708824A (en) * | 2009-11-27 | 2010-05-19 | 江苏宏泰橡胶助剂有限公司 | Preparation method of high-thermostability insoluble sulfur |
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