CN106809806B - A kind of application method preparing insoluble sulfur mist projection granulating tower - Google Patents

A kind of application method preparing insoluble sulfur mist projection granulating tower Download PDF

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Publication number
CN106809806B
CN106809806B CN201710128820.2A CN201710128820A CN106809806B CN 106809806 B CN106809806 B CN 106809806B CN 201710128820 A CN201710128820 A CN 201710128820A CN 106809806 B CN106809806 B CN 106809806B
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nitrogen
insoluble sulfur
projection granulating
mist projection
granulating tower
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CN106809806A (en
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杨松
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Jiangsu duofushan Agricultural Development Co.,Ltd.
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杨松
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    • 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
    • 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
    • B01J2/04Processes 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 gaseous 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
    • C01B17/12Insoluble sulfur (mu-sulfur)

Abstract

The present invention relates to insoluble sulfur technical fields, and in particular to a kind of application method for preparing insoluble sulfur mist projection granulating tower, it is characterized in that: overheat sulphur steam is granulated through mist projection granulating tower chilling obtains insoluble sulfur.Rapid cooling needed for liquid nitrogen (nitrogen) prepares insoluble sulfur as a kind of technical process medium completion, protection, atomization, granulation, conveying, separation operational process of craft; to complete the entire technical process of insoluble sulfur mist projection granulating in tower, make it possible batch continuous production.

Description

A kind of application method preparing insoluble sulfur mist projection granulating tower
Technical field
The present invention relates to insoluble sulfur technical fields, and in particular to a kind of to prepare making for insoluble sulfur mist projection granulating tower Use method.
Background technique
Insoluble sulfur (IS) is also known as polymerised sulphur, also known as μ type sulphur, refers to the sulphur insoluble in carbon disulfide, is the long-chain of sulphur Polymer has chemically and physically inertia.Due to use common sulphur rubber solubility be 1%, common sulphur is in rubber Dosage be more than that its dissolution part can spray surface, i.e. bloom after sizing material is cooling.Bloom will affect between semifinished part Stickiness simultaneously brings adverse effect to product vulcanization uniformity, therefore higher appropriate to the occasion using insoluble sulfur in sulfur consumption, insoluble Sulphur does not dissolve in rubber, and only evenly dispersed in rubber compound, product vulcanization crosslinking point is uniform, has with the rubber of its vulcanization best No blooming, and sizing material can be effectively prevented and occur early stage incipient scorch in process and promote rubber and steel wire or chemical fibre curtain The bonding of sub-line is the dedicated vulcanization agent of radial tyre production.Chinese invention patent (Patent No. 201310511371.1, Patent name is a kind of method for preparing insoluble sulfur) a kind of method for preparing insoluble sulfur is disclosed, it is characterized in that: 1) Melting: raw material sulphur is directly heated to 280~400 DEG C, its melting is made;2) be atomized: the sulphur liquid after melting is through atomizer Centrifugal atomizing is at 10 μm~50 μm of sulphur droplet;3) polymerize: nitrogen at room is mixed with sulphur droplet after gas distributor distributes It closes;Sulphur drop stops 2~25 seconds on tower body top, and nitrogen outlet temperature is controlled at 180~240 DEG C;4) chilling: after polymerization Sulphur again be cooled to -40~0 DEG C through cooling device and the nitrogen after gas distributor distributes mixes, into tower body lower part, 60 DEG C or less were cooled at 2~20 seconds;5) separation packaging: cyclonic separation is collected, and packaging obtains insoluble sulfur product.China Patent of invention (Patent No. 02157245.3, patent name are the preparation method of insoluble sulfur) discloses insoluble sulfur Preparation method, it is characterized in that: a kind of 1. preparation methods of non-oil-filled type insoluble sulfur, it is characterised in that non-oil-filled type is insoluble Sulfur product mainly includes following preparation step: (1) by the compound stabilizer of common sulphur and mass percent 0.01~0.2% Be added with heating, stirring container in, be filled with inert gas and protect, in 250~350 DEG C of at a temperature of constant temperature 10- 90min, after the cooling via superheater, spray gun, atomisation tower and heat exchanger, can be obtained conversion ratio be 53~55% it is insoluble Sulphur crude product;Compound stabilizer is made of I2 or Br2 and rubber accelerator DM or DZ;(2) by insoluble sulfur crude product with The solid-to-liquid ratio of leaching agent in mass ratio 1: 15~20 mixes, and in 45~80 DEG C of at a temperature of 5~60min of stirring, filters while hot, can Obtain the non-oil-filled type product of high content insoluble sulfur.
Conventional example one discloses a kind of method for preparing insoluble sulfur, mainly prepare rubber tyre use it is insoluble Property sulphur, cooling medium is liquid nitrogen, and process flow is melting, atomization, polymerization, chilling, separates and pack, and key is how to protect Sulphur liquid after card melting, at 20 μm of average grain diameter of sulphur droplet, is wanted through atomizer centrifugal atomizing to reach the above technology Ask, need to guarantee atomizer at high operating temperatures still can reliably working (centrifugal atomizing needs atomizer high-speed rotation), it is many It is well known, according to the production environment of 280-400 DEG C of high temperature, batch industrialization production it is difficult to ensure that atomizer can work normally and Guarantee the Particle size requirements of sulphur droplet, while mentioning sulphur drop and having to go to the toilet cold polymerization in tower, is and the immediate technology of the present invention Scheme, but without the details and its application method of open process units;Conventional example two discloses the system of insoluble sulfur Preparation Method, main innovation point are the preparation using normal pressure or low-voltage equipment completion insoluble sulfur, and main production plant is to add Heat, container, superheater, spray gun, atomisation tower and the heat exchanger stirred, it is close with technical solution of the present invention, but without open life Produce the details and its application method of device.
Summary of the invention
In view of the deficiencies of the prior art, making for insoluble sulfur mist projection granulating tower is prepared the object of the present invention is to provide a kind of With method, it is characterized in that: including mist projection granulating tower assembly, material returning device, liquid nitrogen storage tank.
Step 1, first starting liquid nitrogen storage tank purge mist projection granulating tower assembly, material returning device using liquid nitrogen, the time 5 ~6 minutes, mist projection granulating tower assembly, material returning device oxygen amount is made to be down to 1~2%, mist projection granulating tower component temperature is down to 20~22 DEG C, Purpose is to prevent overheat sulphur from firing and providing cooler environment temperature.Then start to recycle nitrogen, and protected after heat exchanger is cooling Holding recycling nitrogen temperature is 20~22 DEG C.
Step 2, overheat sulphur steam is through overheat sulphur steam jet, liquid nitrogen through liquid nitrogen central nozzle, liquid nitrogen outer ring nozzle Into in spray gun assembly, overheat sulphur steam forms nitrogen and sulphur mixed with polymers fluid with liquid nitrogen mixing chilling, through spray gun The outlet end of component sprays, and adjusts guide ring and taper comb gap, and nitrogen and sulphur mixed with polymers fluid high-speed wash away taper Comb convex-concave surface agitates to form insoluble sulfur mist, and the baffle ring for being atomized comb component stops and guiding, sprays in baffle ring two sides, side To tangent with mist projection granulating tower body.The recycling nitrogen to come up in mist projection granulating tower body with air compartment, air distribution plate, blast cap purging is mixed It closes, adjusts bell jar at a distance from air distribution plate by casing spinning in and out, and on 3~4 air-exhausting duct of material blanking tube periphery Ventilation hole unifies the navigation designing of direction aperture, and nitrogen can form spiralling wind band along mist projection granulating tower body inner wall, carries Insoluble sulfur mist realizes technical process that is cooling, being granulated, separate, convey: insoluble sulfur mist is with nitrogen along mist projection granulating tower During internal wall spiral, form the particle constantly grown up and mutually collide, rubbing loses kinetic energy, and to mist projection granulating Tower body center is assembled, and after particle growth to certain diameter, is fallen under gravity into material blanking tube and is entered next procedure.
Step 3, the nitrogen after separating with insoluble sulfur particle continue upwardly into material returning device room, and thin in nitrogen Grain cyclonic separation again, returns in mist projection granulating tower body with the help of purging device, nitrogen is after exhaust tube is discharged through refeed line Recycling is recycled after heat exchanger is cooling.
Inventors have found that liquid nitrogen is used to make overheat sulphur steam rapid cooling to 90 DEG C of temperature or less can for rapid cooling agent Insoluble sulfur is produced, production practices prove, the content of rapid cooling to 60 DEG C of insoluble sulfurs continues to drop up to 78~80% Although low cooling technique temperature can be improved the content of insoluble sulfur, but production cost greatly improves, therefore preferably rapidly cold But technological temperature is 60 DEG C, and the overheat sulphur steam flow channel internal and external casing designed in spray gun assembly is liquid nitrogen runner, and is being exported End mixing, can effective observing and controlling process conditions such as temperature, flow, pressure etc., and lance driving device is protected to work under the high temperature conditions just Often.
Inventors have found that obtain, insoluble sulfur content is higher, preferably just insoluble sulfur processed produces high-temperature stability Product, atomization are critical processes, by adjusting the gap that guide ring and taper are combed, make insoluble sulfur and nitrogen fluid-mixing high speed Injection, encounters the rough surface of taper comb, and surge is separated into the drop being suspended in nitrogen, proposes rapid cooling effect Height, and make just insoluble sulfur product yield raising processed.
It is beneficial to prevent conversion of the insoluble sulfur to common sulphur inventors have found that being granulated, improves its stability.Using The recycling nitrogen of 20-22 DEG C of temperature is cooling as insoluble sulfur, protection, is granulated, separates, the technological operation medium of conveying is excellent The technical solution of choosing, being conducive to recycling nitrogen circulation utilization reduces cost.Nitrogen is granulated on tower bottom air distribution plate purging from atomization Come, will form and be granulated the spiralling air-flow of tower wall along atomization, from coming from air-flow cross section transverse, air-flow has periphery flow velocity Fastly, center flow velocity is slow, and the periphery feature big compared with center pressure can drive the insoluble sulfur particle constantly grown up to throw to tower wall Frictional impact lose kinetic energy whereabouts, and to center assemble, insoluble sulfur particle diameter grow up to certain diameter after in gravity Lower and nitrogen separation is acted on, enters subsequent processing through material blanking tube.
Inventors have found that nitrogen can be by design requirement when atomization granulation tower inside spin rises and guarantees the stop of material Between, it needs to go to solve the problems, such as by the structure of design blast cap, height, arrangement, the preferred bell-type windshield of the present invention, nitrogen is through air hose Ventilation hole purge again from the gap of bell jar and air hose to air distribution plate, then the blocking through air distribution plate to atomization be granulated tower top flowing, It is oriented to nitrogen spiral by the navigation designing that the ventilation hole on 3~4 air-exhausting duct of material blanking tube periphery unifies direction aperture, By adjusting bell jar with a distance from air distribution plate, actually it is exactly the width for adjusting nitrogen spiral wind band, substantially has adjusted nitrogen spiral shell The time that whirlwind band rises along atomization granulation tower spiral inner wall, to guarantee stopping in the technique of atomization granulation tower for insoluble sulfur Stay (granulation) time.
Compared with the existing technology, the present invention, which at least contains, has the advantage that first, and liquid nitrogen (nitrogen) is used as a kind of technical process Rapid cooling needed for medium completion prepares insoluble sulfur, protection, atomization, granulation, conveying, separation operational process of craft, It is optimal technical process medium;Second, nitrogen is used as a possibility that protecting gas to fire sulphur extremely low, and it is raw to be conducive to safety It produces;Third, the overheat sulphur steam flow channel internal and external casing in spray gun assembly are liquid nitrogen runner, and are mixed in outlet end, can be effective Observing and controlling process conditions such as temperature, flow, pressure etc., and protect lance driving device working properly under the high temperature conditions;4th, pass through tune The gap that whole guide ring is combed with taper sprays insoluble sulfur and nitrogen fluid-mixing high speed, it is uneven to encounter taper comb Surface, surge be separated into the drop being suspended in nitrogen, make rapid cooling effect improve, and make just insoluble sulfur product processed Yield improves;5th, granulation is beneficial to prevent conversion of the insoluble sulfur to common sulphur, improves its stability.Using 20-25 The recycling nitrogen of DEG C temperature is cooling as insoluble sulfur, protection, is granulated, separation, the technological operation medium conveyed It is preferred technical solution, and nitrogen carries insoluble sulfur particle spiral in atomization granulation tower, insoluble sulfur Grain diameter grow up to certain diameter after under gravity with nitrogen separation, enter subsequent processing through material blanking tube, make batch produce The production of industry metaplasia is possibly realized;6th, atomization granulation tower is obturator, is atomized prilling operating process in closed production It is carried out in device, the probability for polluting environment is made to become extremely low.
Detailed description of the invention
Fig. 1 is a kind of schematic view of the front view for the application method for preparing insoluble sulfur mist projection granulating tower of the present invention.
Fig. 2 is a kind of overlooking structure diagram for the application method for preparing insoluble sulfur mist projection granulating tower of the present invention.
Fig. 3 is that a kind of A for the application method for preparing insoluble sulfur mist projection granulating tower of the present invention rotates enlarged structure signal Figure.
Fig. 4 is a kind of B partial enlargement structural representation for the application method for preparing insoluble sulfur mist projection granulating tower of the present invention Figure.
Fig. 5 is a kind of C for the application method for preparing insoluble sulfur mist projection granulating tower of the present invention to structural schematic diagram.
Fig. 6 is a kind of D full-page proof structural schematic diagram for the application method for preparing insoluble sulfur mist projection granulating tower of the present invention.
Fig. 7 is a kind of E partial enlargement structural representation for the application method for preparing insoluble sulfur mist projection granulating tower of the present invention Figure.
Fig. 8 is a kind of F-F schematic cross-sectional view for the application method for preparing insoluble sulfur mist projection granulating tower of the present invention.
1- mist projection granulating tower assembly 2- material returning device 3- liquid nitrogen storage tank 4- air distribution plate
5- material blanking tube 6- air compartment 7- spray gun assembly 8- refeed line 9- purging device
10- mist projection granulating tower body 11- material returning device room 12- exhaust tube
13- liquid nitrogen central nozzle 14- overheats sulphur steam jet 15- liquid nitrogen outer ring nozzle
16- is atomized comb component 17- baffle ring 18- taper comb 19- guide ring
20- blast cap 21- bell jar 22- ventilation hole 23- casing 24- air hose.
Specific embodiment
The present apparatus is described further with specific embodiment with reference to the accompanying drawing.
For the present invention as shown in attached drawing 1, Fig. 2, Fig. 3, Fig. 4, Fig. 5, Fig. 6, Fig. 7, Fig. 8, a kind of insoluble sulfur for preparing is spraying The application method of granulation tower, it is characterized in that: step 1, first starting liquid nitrogen storage tank 3 using liquid nitrogen to mist projection granulating tower assembly 1, Material returning device 2 is purged, and the time 5~6 minutes, so that mist projection granulating tower assembly 1,2 oxygen amount of material returning device is down to 1~2%, mist projection granulating 1 temperature of tower assembly is down to 20~22 DEG C, it is therefore an objective to prevent overheat sulphur from firing and providing cooler environment temperature.Then start to recycle Nitrogen, and holding recycling nitrogen temperature is 20~22 DEG C after heat exchanger is cooling.
Step 2, overheat sulphur steam is through overheat sulphur steam jet 14, liquid nitrogen through liquid nitrogen central nozzle 13, liquid nitrogen outer ring Nozzle 15 enters in spray gun assembly 7, and overheat sulphur steam is mixed with liquid nitrogen to be chilled to form nitrogen and sulphur mixed with polymers stream Body, the outlet end through spray gun assembly 7 spray, and adjust 18 gaps of guide ring 19 and taper comb, nitrogen and sulphur mixed with polymers stream Body high speed washes away taper 18 convex-concave surfaces of comb and agitates to form insoluble sulfur mist, and the baffle ring 17 for being atomized comb component 16 stops and leads To in the ejection of 17 two sides of baffle ring, direction and mist projection granulating tower body 10 are tangent.In mist projection granulating tower body 10 with air compartment 6, air distribution plate 4, blast cap 20 purges the recycling nitrogen mixing to come up, adjusts bell jar 21 at a distance from air distribution plate 4 by 23 spinning in and out of casing, And the navigation designing of the unified direction aperture of ventilation hole 22 on 5 periphery of material blanking tube, 3~4 air-exhausting duct 24, nitrogen can be along sprays Mist is granulated 10 inner wall of tower body and forms spiralling wind band, carry insoluble sulfur mist realize it is cooling, be granulated, separation, conveying Technical process: insoluble sulfur mist with nitrogen along 10 spiral inner wall of mist projection granulating tower body rise during, formation constantly grow up Particle and mutually collide, rubbing loses kinetic energy, and assemble to 10 center of mist projection granulating tower body, particle growth to certain diameter Afterwards, material blanking tube 5 is fallen under gravity into next procedure.
Step 3, the nitrogen after separating with insoluble sulfur particle continues upwardly into material returning device room 11, thin in nitrogen Particle cyclonic separation again, returns in mist projection granulating tower body 10 with the help of purging device 9, nitrogen is through exhaust tube through refeed line 5 Recycling is recycled after heat exchanger is cooling after 12 discharges.
According to the disclosure and teachings of the above specification, those skilled in the art in the invention can also be to above-mentioned embodiment party Formula is changed and is modified.Therefore, the invention is not limited to the specific embodiments disclosed and described above, to of the invention Some modifications and changes should also be as falling into the scope of the claims of the present invention.In addition, although being used in this specification Some specific terms, these terms are merely for convenience of description, does not limit the present invention in any way.

Claims (2)

1. a kind of application method for preparing insoluble sulfur mist projection granulating tower, it is characterized in that: step 1, first starting liquid nitrogen storage tank Mist projection granulating tower assembly, material returning device are purged using liquid nitrogen, the time 5~6 minutes, make mist projection granulating tower assembly, material returning device Oxygen amount is down to 1~2%, and mist projection granulating tower component temperature is down to 20~22 DEG C, it is therefore an objective to prevent overheat sulphur from firing and providing cooling Environment temperature;Step 2, overheat sulphur steam is through overheat sulphur steam jet, liquid nitrogen through ring spray outside liquid nitrogen central nozzle, liquid nitrogen Mouth enters in spray gun assembly, and overheat sulphur steam forms nitrogen and sulphur mixed with polymers fluid with liquid nitrogen mixing chilling, through spraying The outlet end of rifle component sprays, and atomization is critical process, by adjusting the gap that guide ring and taper are combed, make insoluble sulfur with Nitrogen fluid-mixing high speed is sprayed, and the rough surface of taper comb is encountered, and surge is separated into the drop being suspended in nitrogen, passes through The baffle ring for being atomized comb component stops and guiding, sprays in baffle ring two sides, direction and mist projection granulating tower body are tangent, in mist projection granulating tower The recycling nitrogen to come up in vivo with air compartment, air distribution plate, blast cap purging mixes, and adjusts bell jar and cloth wind by casing spinning in and out The distance of plate, and the ventilation hole on 3~4 air-exhausting duct of material blanking tube periphery unifies the navigation designing of direction aperture, nitrogen meeting Spiralling wind band is formed along mist projection granulating tower body inner wall, insoluble sulfur mist is carried and realizes cooling, granulation, separation, conveying Technical process: insoluble sulfur mist with nitrogen during the mist projection granulating tower body inner wall spiral, constantly grow up by formation Particle and mutually collide, rubbing loses kinetic energy, and assemble to mist projection granulating tower body center, after particle growth to certain diameter, It falls under gravity into material blanking tube and enters next procedure;Step 3, the nitrogen after separating with insoluble sulfur particle continue It is upwardly into material returning device room, the cyclonic separation again of the fine grained in nitrogen returns with the help of purging device spraying through refeed line In granulation tower body, nitrogen recycles after exhaust tube is discharged to be recycled after heat exchanger is cooling.
2. a kind of application method for preparing insoluble sulfur mist projection granulating tower according to claim 1, it is characterized in that: using Liquid nitrogen is that rapid cooling agent makes overheat sulphur steam rapid cooling produce insoluble sulfur, and the technological temperature of rapid cooling is 60 ℃。
CN201710128820.2A 2017-03-06 2017-03-06 A kind of application method preparing insoluble sulfur mist projection granulating tower Active CN106809806B (en)

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Publication number Priority date Publication date Assignee Title
CN110639427A (en) * 2018-12-10 2020-01-03 金昌正旭工贸有限责任公司 Sulfur molten liquid spraying water-cooling medium granulation process
CN111804239A (en) * 2020-06-11 2020-10-23 盐城市锦东液压机械有限公司 Sealed rotary joint of reactor

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4234318A (en) * 1977-02-04 1980-11-18 Cominco Ltd. Process for granulation of sulfur
US4705467A (en) * 1984-11-28 1987-11-10 Shell Oil Company Method and apparatus for filtering the air outlet of a solid sulphur particle production apparatus
CN2897989Y (en) * 2005-08-10 2007-05-09 中国石油化工集团公司 Insoluble sulfur spray cooling tower
CN202687954U (en) * 2012-06-28 2013-01-23 山东尚舜化工有限公司 Liquid sulfur atomizing device for preparing insoluble sulfur
CN103043619A (en) * 2011-10-17 2013-04-17 江苏圣奥化学科技有限公司 Double-fluid quenching device

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4234318A (en) * 1977-02-04 1980-11-18 Cominco Ltd. Process for granulation of sulfur
US4705467A (en) * 1984-11-28 1987-11-10 Shell Oil Company Method and apparatus for filtering the air outlet of a solid sulphur particle production apparatus
CN2897989Y (en) * 2005-08-10 2007-05-09 中国石油化工集团公司 Insoluble sulfur spray cooling tower
CN103043619A (en) * 2011-10-17 2013-04-17 江苏圣奥化学科技有限公司 Double-fluid quenching device
CN202687954U (en) * 2012-06-28 2013-01-23 山东尚舜化工有限公司 Liquid sulfur atomizing device for preparing insoluble sulfur

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