CN110639427A - Sulfur molten liquid spraying water-cooling medium granulation process - Google Patents

Sulfur molten liquid spraying water-cooling medium granulation process Download PDF

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Publication number
CN110639427A
CN110639427A CN201811504493.7A CN201811504493A CN110639427A CN 110639427 A CN110639427 A CN 110639427A CN 201811504493 A CN201811504493 A CN 201811504493A CN 110639427 A CN110639427 A CN 110639427A
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China
Prior art keywords
sulfur
water
cooling
cooling tower
liquid
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Pending
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CN201811504493.7A
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Chinese (zh)
Inventor
安鹏九
李东旺
王瑞
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Jinchang Zhengxu Industry And Trade Co Ltd
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Jinchang Zhengxu Industry And Trade Co Ltd
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Priority to CN201811504493.7A priority Critical patent/CN110639427A/en
Publication of CN110639427A publication Critical patent/CN110639427A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/02Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
    • B01J2/06Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a liquid medium
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00Sulfur; Compounds thereof
    • C01B17/02Preparation of sulfur; Purification
    • C01B17/0237Converting into particles, e.g. by granulation, milling

Abstract

The invention provides a sulfur melt spray water cooling medium granulation process, which comprises the following steps: (1) placing the sulfur solid in a sulfur melting kettle to prepare liquid sulfur, wherein the working temperature of the sulfur melting kettle is controlled at 120-150 ℃; (2) the prepared liquid sulfur is conveyed to an atomization cooling tower through a conveying pipeline, the liquid sulfur is atomized into a smoke gas state under normal pressure through a centrifugal atomizer in the atomization cooling tower to form sulfur fog drops with the purity of 99.99 percent and the temperature of 80-100 ℃, and nitrogen is added as protective gas in the atomization process; (3) the sulfur droplets fall into cooling water below the nozzle under the protection of nitrogen, form spherical droplets in the cooling water due to interfacial tension, sink or float in a cooling tower due to density difference, release heat in the movement process, are cooled to 15-30 ℃, and are solidified to form water-containing sulfur particles; (4) after being dried and dehydrated by a two-stage dehydration device, the sulfur particles with the purity of 99.9 percent, the fineness of 150-200 meshes and the shape of similar spherical shape are obtained.

Description

Sulfur molten liquid spraying water-cooling medium granulation process
Technical Field
The invention relates to the field of sulfur production, in particular to a process for granulating a sulfur melt by spraying a water cooling medium.
Background
The preparation method of the sulfur particles mainly comprises a crushing method. The demand of sulfur particles in some chemical industries and rubber industries is increasing year by year, and the requirement on the quality is increasing day by year, but the sulfur production industry has three major problems up to now, namely, the explosion of the sulfur particles in the production process, the improvement of the quality of the sulfur particles and the reduction of dust pollution under the condition of increasing daily output. Of which the solution to the problem of explosion of sulphur particles is most important and most urgent. It is known that lump sulfur is light yellow crystal, the combustion temperature is generally between 240 ℃ and 260 ℃, while powdered sulfur is only about 190 ℃, and if the sulfur-containing yellow particles reach 35 g per cubic meter in the processing process, the explosion is very easy to occur. The physical reason is that when the sulfur is crushed, the sulfur micro-particles collide with each other, and a large amount of static electricity and heat are generated by friction, and when the sulfur particles reach a certain concentration and temperature, explosion is caused. Therefore, it is urgent to design and produce a preparation process for producing sulfur particles with explosion prevention, high quality, high yield and no pollution.
Disclosure of Invention
Technical problem to be solved
In view of the above, the present invention aims to provide a process for granulating a sulfur melt by spraying a water cooling medium, so as to achieve the purposes of safely producing sulfur particles and improving the purity of the sulfur particles.
(II) technical scheme
In order to solve the technical problem, the invention provides a sulfur melt spraying water cooling medium granulation process,
the method is characterized by comprising the following steps:
(1) placing the sulfur solid in a sulfur melting kettle to prepare liquid sulfur, wherein the working temperature of the sulfur melting kettle is controlled at 120-150 ℃;
(2) the prepared liquid sulfur is conveyed to an atomization cooling tower through a conveying pipeline, the liquid sulfur is atomized into a smoke gas state under normal pressure through a centrifugal atomizer in the atomization cooling tower to form sulfur fog drops with the purity of 99.99 percent and the temperature of 80-100 ℃, and nitrogen is added as protective gas in the atomization process;
(3) the sulfur droplets fall into cooling water below the nozzle under the protection of nitrogen, form spherical droplets in the cooling water due to interfacial tension, sink or float in a cooling tower due to density difference, release heat in the movement process, are cooled to 15-30 ℃, and are solidified to form water-containing sulfur particles;
(4) after being dried and dehydrated by a two-stage dehydration device, the sulfur particles with the purity of 99.9 percent, the fineness of 150-200 meshes and the shape of similar spherical shape are obtained.
The sulphur melt spray water cooling medium granulation process provided by the invention can be further set in such a way that the atomization cooling tower in the step (2) is of a hollow structure, a plurality of spray heads are arranged above the inside of the atomization cooling tower, and cooling liquid is contained below the atomization cooling tower.
The sulphur melt spray water-cooling medium granulation process provided by the invention can be further set in such a way that the operation temperature of the atomization cooling tower in the step (2) is less than 30 degrees, and the pressure intensity in the atomization cooling tower is one atmospheric pressure.
The sulphur melt spray water-cooling medium granulation process provided by the invention can be further set in the step (3) that the cooling liquid adopts circulating water as the cooling liquid to form a matrix, the working temperature of the circulating water is less than 30 ℃, the circulating water is tap water, and the cooling time is controlled to be 5-8 seconds.
The sulphur melt liquid spray water-cooling medium granulation process provided by the invention can be further set in such a way that a first-stage dehydration device in the two-stage dehydration device is a solid-liquid separator, and a second-stage dehydration mode is a horizontal centrifuge; the solid-liquid separator is arranged behind the heat exchanger and used for removing the large-volume water drops in the water-containing sulfur, and the horizontal centrifuge is arranged behind the solid-liquid separator and used for centrifugally dewatering the water-containing sulfur particles.
The sulphur melt spraying water-cooling medium granulation process provided by the invention can be further set to ensure that the cooling liquid separated by the two-stage dehydration device returns to the cooling tower again through a pipeline.
The sulphur melt spray water cooling medium granulation process provided by the invention can be further set in such a way that the temperature of nitrogen in the step (3) is always kept within 30 ℃.
(III) advantageous effects
The invention provides a sulphur melt spray water cooling medium granulation process, which obtains good results, firstly, the process is simple, the used process equipment is less, and the preparation cost is saved; secondly, when preparing sulfur particles, the sulfur fog drops form spherical drops in cooling water due to interfacial tension, and the process is finished in a cooling medium, so that the explosion condition of the sulfur particles is reduced, and the production safety is improved; and thirdly, the product produced by the method does not need to be crushed again, so that the production cost is reduced, the production environment is optimized, and the method belongs to a green environment-friendly process.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
The following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1:
a sulphur melt spray water cooling medium granulation process comprises the following steps:
(1) putting the sulfur solid into a sulfur melting kettle to prepare liquid sulfur, wherein the working temperature of the sulfur melting kettle is controlled at 150 ℃;
(2) the prepared liquid sulfur is conveyed to an atomization cooling tower through a conveying pipeline, the working temperature of the atomization cooling tower is 25 ℃, the liquid sulfur is atomized into a smoke gas state under normal pressure through a centrifugal atomizer in the atomization cooling tower, sulfur fog drops with the purity of 99.99 percent and the temperature of 98 ℃ are formed, and nitrogen is added as protective gas in the atomization process;
(3) the sulfur droplets fall into cooling water below the nozzle under the protection of nitrogen, form spherical droplets in the cooling water due to interfacial tension, sink or float in a cooling tower due to density difference, release heat in the movement process, are cooled to 28 ℃, are cooled for 8 seconds, and are solidified to form water-containing sulfur particles;
(4) the sulfur particles with the purity of 99.9 percent, the fineness of 190-200 meshes and the shape of sphere-like are obtained after two-stage dehydration by a solid-liquid separator and a horizontal centrifuge which are arranged below the atomizing cooling tower.
Example 2:
a sulphur melt spray water cooling medium granulation process comprises the following steps:
(1) putting the sulfur solid into a sulfur melting kettle to prepare liquid sulfur, wherein the working temperature of the sulfur melting kettle is controlled at 140 ℃;
(2) the prepared liquid sulfur is conveyed to an atomization cooling tower through a conveying pipeline, the working temperature of the atomization cooling tower is 26 ℃, the liquid sulfur is atomized into a smoke gas state under normal pressure through a centrifugal atomizer in the atomization cooling tower, sulfur fog drops with the purity of 99.99 percent and the temperature of 90 ℃ are formed, and nitrogen is added as protective gas in the atomization process;
(3) the sulfur droplets fall into cooling water below the nozzle under the protection of nitrogen, form spherical droplets in the cooling water due to interfacial tension, sink or float in a cooling tower due to density difference, release heat in the movement process, are cooled to 23 ℃ for 7 seconds, and are solidified to form water-containing sulfur particles;
(4) the sulfur particles with the purity of 99.9 percent, the fineness of 170-190 meshes and the shape of sphere-like are obtained after two-stage dehydration by a solid-liquid separator and a horizontal centrifuge which are arranged below the atomizing cooling tower.
Example 3:
a sulphur melt spray water cooling medium granulation process comprises the following steps:
(1) putting the sulfur solid into a sulfur melting kettle to prepare liquid sulfur, wherein the working temperature of the sulfur melting kettle is controlled at 130 ℃;
(2) the prepared liquid sulfur is conveyed to an atomization cooling tower through a conveying pipeline, the working temperature of the atomization cooling tower is 27 ℃, the liquid sulfur is atomized into a smoke gas state under normal pressure through a centrifugal atomizer in the atomization cooling tower, sulfur fog drops with the purity of 99.99 percent and the temperature of 85 ℃ are formed, and nitrogen is added as protective gas in the atomization process;
(3) the sulfur droplets fall into cooling water below the nozzle under the protection of nitrogen, form spherical droplets in the cooling water due to interfacial tension, sink or float in a cooling tower due to density difference, release heat in the movement process, are cooled to 20 ℃, are cooled for 6 seconds, and are solidified to form water-containing sulfur particles;
(4) the sulfur particles with the purity of 99.9 percent, the fineness of 160-170 meshes and the shape of spheroidal are obtained after two-stage dehydration by a solid-liquid separator and a horizontal centrifuge which are arranged below the atomizing cooling tower.
Example 4:
a sulphur melt spray water cooling medium granulation process comprises the following steps:
(1) putting the sulfur solid into a sulfur melting kettle to prepare liquid sulfur, wherein the working temperature of the sulfur melting kettle is controlled at 120 ℃;
(2) the prepared liquid sulfur is conveyed to an atomization cooling tower through a conveying pipeline, the working temperature of the atomization cooling tower is 28 ℃, the liquid sulfur is atomized into a smoke gas state under normal pressure through a centrifugal atomizer in the atomization cooling tower, sulfur fog drops with the purity of 99.99 percent and the temperature of 80 ℃ are formed, and nitrogen is added as protective gas in the atomization process;
(3) the sulfur droplets fall into cooling water below the nozzle under the protection of nitrogen, form spherical droplets in the cooling water due to interfacial tension, sink or float in a cooling tower due to density difference, release heat in the movement process, are cooled to 16 ℃, are cooled for 5 seconds, and are solidified to form water-containing sulfur particles;
(4) the sulfur particles with the purity of 99.9 percent, the fineness of 150-160 meshes and the shape of sphere-like are obtained after two-stage dehydration by a solid-liquid separator and a horizontal centrifuge which are arranged below the atomizing cooling tower.
In all of the above examples:
the atomization cooling tower in the step (2) is of a hollow structure, a plurality of spray heads are arranged above the atomization cooling tower, and cooling liquid is contained below the atomization cooling tower.
And (3) the operating temperature of the atomization cooling tower in the step (2) is less than 30 degrees, and the pressure intensity in the atomization cooling tower is one atmospheric pressure.
In the step (3), the cooling liquid adopts circulating water as the cooling liquid to form a matrix, the working temperature of the circulating water is less than 30 ℃, the circulating water is composed of tap water, and the cooling time is controlled to be 5-8 seconds.
The first stage dehydration device in the two-stage dehydration device is a solid-liquid separator, and the second stage dehydration mode is a horizontal centrifuge; the solid-liquid separator is arranged behind the heat exchanger and used for removing the large-volume water drops in the water-containing sulfur, and the horizontal centrifuge is arranged behind the solid-liquid separator and used for centrifugally dewatering the water-containing sulfur particles.
The cooling liquid separated from the two-stage dehydration device is returned to the cooling tower through a pipeline.
The temperature of the nitrogen in the step (3) is always kept within 30 ℃.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.

Claims (7)

1. A process for granulating a sulfur molten liquid by spraying a water cooling medium,
the method is characterized by comprising the following steps:
(1) placing the sulfur solid in a sulfur melting kettle to prepare liquid sulfur, wherein the working temperature of the sulfur melting kettle is controlled at 120-150 ℃;
(2) the prepared liquid sulfur is conveyed to an atomization cooling tower through a conveying pipeline, the liquid sulfur is atomized into a smoke gas state under normal pressure through a centrifugal atomizer in the atomization cooling tower to form sulfur fog drops with the purity of 99.99 percent and the temperature of 80-100 ℃, and nitrogen is added as protective gas in the atomization process;
(3) the sulfur droplets fall into cooling water below the nozzle under the protection of nitrogen, form spherical droplets in the cooling water due to interfacial tension, sink or float in a cooling tower due to density difference, release heat in the movement process, are cooled to 15-30 ℃, and are solidified to form water-containing sulfur particles;
(4) after being dried and dehydrated by a two-stage dehydration device, the sulfur particles with the purity of 99.9 percent, the fineness of 150-200 meshes and the shape of similar spherical shape are obtained.
2. The process according to claim 1, wherein the atomizing and cooling tower in step (2) is hollow, and has several nozzles at the upper part and cooling liquid at the lower part.
3. The process according to claim 1, wherein the atomizing cooling tower used in step (2) is operated at a temperature of less than 30 ° and the pressure inside the atomizing cooling tower is one atmosphere.
4. The process according to claim 1, wherein the cooling liquid in step (3) is a matrix composed of circulating water as the cooling liquid, the working temperature of the circulating water is less than 30 ℃, the circulating water is tap water, and the cooling time is controlled to be 5-8 seconds.
5. The process according to claim 1, wherein the first stage of the two-stage dehydration apparatus is a solid-liquid separator, and the second stage of the two-stage dehydration apparatus is a horizontal centrifuge; the solid-liquid separator is arranged behind the heat exchanger and used for removing the large-volume water drops in the water-containing sulfur, and the horizontal centrifuge is arranged behind the solid-liquid separator and used for centrifugally dewatering the water-containing sulfur particles.
6. A sulphur melt spray water cooling medium granulation process according to claim 5, wherein the cooling liquid exiting from the two stage dehydration unit is returned to the cooling tower via a pipeline.
7. The process according to claim 1, wherein the temperature of the nitrogen gas in step (3) is always kept within 30 ℃.
CN201811504493.7A 2018-12-10 2018-12-10 Sulfur molten liquid spraying water-cooling medium granulation process Pending CN110639427A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115400687A (en) * 2022-09-22 2022-11-29 河北林格环保科技有限公司 A forming device for deamination material production

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1136901A (en) * 1964-09-17 1968-12-18 Elliott Assoc Dev Improvements in or relating to the treatment of sulphur
CA2450779A1 (en) * 2003-12-22 2005-06-22 Warren H. Finlay Powder formation by atmospheric spray-freeze drying
CN102059073A (en) * 2010-11-15 2011-05-18 南京三普造粒装备有限公司 Tumbler sulfur granulator with two discharging ends
CN102083517A (en) * 2008-06-27 2011-06-01 茵舒尔股份有限公司 Sulphur granulation apparatus and process
CN106809806A (en) * 2017-03-06 2017-06-09 杨松 A kind of application method for preparing insoluble sulfur mist projection granulating tower

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1136901A (en) * 1964-09-17 1968-12-18 Elliott Assoc Dev Improvements in or relating to the treatment of sulphur
CA2450779A1 (en) * 2003-12-22 2005-06-22 Warren H. Finlay Powder formation by atmospheric spray-freeze drying
CN102083517A (en) * 2008-06-27 2011-06-01 茵舒尔股份有限公司 Sulphur granulation apparatus and process
CN102059073A (en) * 2010-11-15 2011-05-18 南京三普造粒装备有限公司 Tumbler sulfur granulator with two discharging ends
CN106809806A (en) * 2017-03-06 2017-06-09 杨松 A kind of application method for preparing insoluble sulfur mist projection granulating tower

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余本水主编: "《原药供应手册 (2007-2008年版)》", 31 October 2007, 中国农业出版社 *
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115400687A (en) * 2022-09-22 2022-11-29 河北林格环保科技有限公司 A forming device for deamination material production

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