CN106829877B - It is a kind of to prepare insoluble sulfur mist projection granulating tower - Google Patents

It is a kind of to prepare insoluble sulfur mist projection granulating tower Download PDF

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Publication number
CN106829877B
CN106829877B CN201710129232.0A CN201710129232A CN106829877B CN 106829877 B CN106829877 B CN 106829877B CN 201710129232 A CN201710129232 A CN 201710129232A CN 106829877 B CN106829877 B CN 106829877B
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liquid nitrogen
projection granulating
mist projection
insoluble sulfur
nozzle
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CN106829877A (en
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杨松
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Shandong Tiansheng cellulose 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
    • C01B17/12Insoluble sulfur (mu-sulfur)

Abstract

The present invention relates to insoluble sulfur technical fields, and in particular to and it is a kind of to prepare insoluble sulfur mist projection granulating tower, it is characterized in that:Including mist projection granulating tower assembly, material returning device, liquid nitrogen storage tank.Liquid nitrogen(Nitrogen)As a kind of technical process medium completion prepare rapid cooling needed for insoluble sulfur, 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

It is a kind of to prepare 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 insoluble sulfur mist projection granulating tower.
Background technology
Insoluble sulfur(IS)Also known as polymerised sulphur, also known as μ types sulphur, refer to the sulphur insoluble in carbon disulfide, are the long-chains of sulphur Polymer has chemically and physically inertia.Due to the use of common sulphur rubber solubility be 1%, common sulphur is in rubber Dosage be more than its dissolving part sizing material cooling after can spray surface, i.e. bloom.Bloom will influence 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 preparing insoluble sulfur)A kind of method 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)Atomization:Sulphur liquid after melting is through atomizer Centrifugal atomizing is at 10 μm~50 μm of sulphur droplet;3)Polymerization: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 is cooled to -40~0 DEG C and the nitrogen after gas distributor distributes mixes with through cooling device again, into tower body lower part, It was cooled to 60 DEG C or less 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)Disclose insoluble sulfur Preparation method, it is characterized in that:1. a kind of preparation method of non-oil-filled type insoluble sulfur, it is characterised in that non-oil-filled type is insoluble Sulfur product includes mainly following preparation process:(1) by the compound stabilizer of common sulphur and mass percent 0.01~0.2% It is added in heating, the container stirred, is filled with inert gas and protects, constant temperature 10- at a temperature of 250~350 DEG C 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 5~60min is stirred at a temperature of 45~80 DEG C, is filtered while hot, can Obtain the non-oil-filled type product of high content insoluble sulfur.
Conventional example one discloses a kind of method preparing insoluble sulfur, mainly prepare rubber tyre use it is insoluble Property sulphur, cooling medium is liquid nitrogen, and technological process is melting, atomization, polymerization, chilling, detaches and pack, and key is how to protect Sulphur liquid after card melting, at the sulphur droplet of 20 μm of average grain diameter, is wanted through atomizer centrifugal atomizing to reach the above technology It asks, needs to ensure that atomizer at high operating temperatures still being capable of reliably working(Centrifugal atomizing needs atomizer high-speed rotation), 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 Ensure 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.
Invention content
In view of the deficiencies of the prior art, insoluble sulfur mist projection granulating tower is prepared the object of the present invention is to provide a kind of, It is characterized in:Including mist projection granulating tower assembly, material returning device, liquid nitrogen storage tank.
The mist projection granulating tower assembly includes material blanking tube, air distribution plate, blast cap, air compartment, spray gun assembly, atomization comb component, spray Mist is granulated tower body.The spray gun assembly includes liquid nitrogen central nozzle, overheat sulphur steam jet, liquid nitrogen outer shroud nozzle, baffle ring, cone Shape comb, guide ring, the liquid nitrogen central nozzle, overheat sulphur steam jet, the casing that liquid nitrogen outer shroud nozzle is same central shaft, It is logical that the spray gun assembly is followed successively by liquid nitrogen central nozzle, overheat sulphur steam jet, the fluid of liquid nitrogen outer shroud nozzle from inside to outside Road converges in outlet end.The atomization comb component includes taper comb, baffle ring, guide ring, and the taper, which is combed, to be mounted on baffle ring, It can be moved along atomization comb component central axes, the guide ring is inverted cone-shaped structure, and expanded angle is identical as taper comb apex angle And same central shaft, taper is combed adjusts the gap with guide ring by mobile, and the atomization comb component is connect with spray gun assembly.
The material returning device includes refeed line, purging device, material returning device room, exhaust tube.
It is connect with material returning device room at the top of the mist projection granulating tower body, described refeed line one end connects with mist projection granulating tower body lower part It connects, one end is connect with material returning device room bottom.
The blast cap includes bell jar, air hose, casing, and the air hose and casing connection, casing are anchored at cloth wind by screw thread On plate, and the height of blast cap is adjusted by rotating, the air hose has along the circumferential direction opened row's ventilation hole, and the bell jar is set up On air hose top.
Liquid nitrogen central nozzle, the liquid nitrogen outer shroud nozzle of the spray gun assembly are connect with liquid nitrogen storage tank.
Inventor has found, liquid nitrogen is used so that overheat sulphur steam rapid cooling to 90 DEG C of temperature or less is made for rapid cooling agent Insoluble sulfur is taken, therefore it is liquid nitrogen runner to design the overheat sulphur steam flow channel internal and external casing in spray gun assembly, and 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.
Inventor has found that insoluble sulfur content is higher, preferably just insoluble sulfur processed produces high-temperature stability to obtain 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, rapid cooling effect is made to carry Height, and make just insoluble sulfur product yield raising processed.
Inventor has found that granulation is conducive to the conversion for preventing insoluble sulfur to common sulphur, improves its stability.Using The recycling nitrogen of 20-22 DEG C of temperature is cooling as insoluble sulfur, protection, is granulated, detaches, 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 from atomization on tower bottom air distribution plate purging Come, can be formed 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 Soon, 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.
Inventor has found that nitrogen can be by design requirement when atomization granulation tower inside spin rises and ensures 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 purged 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, The navigation designing for unifying direction trepanning by the ventilation hole on 3~4 exhaust duct of material blanking tube periphery is oriented to nitrogen spiral, By adjusting bell jar with a distance from air distribution plate, it is exactly actually 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 ensure stopping in the technique of atomization granulation tower for insoluble sulfur It stays(It is granulated)Time.
Compared with the existing technology, the present invention at least contains and has the advantage that:First, liquid nitrogen(Nitrogen)As a kind of technical process Medium completion prepare rapid cooling needed for insoluble sulfur, protection, atomization, granulation, conveying, separation operational process of craft, It is optimal technical process medium;Second, nitrogen is extremely low as the possibility that protection gas makes sulphur fire, and it is raw to be conducive to safety Production;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 and taper are combed makes insoluble sulfur be sprayed with 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 conducive to the conversion for preventing insoluble sulfur to common sulphur, improves its stability.Using 20-25 The recycling nitrogen of DEG C temperature is cooling as insoluble sulfur, protection, be granulated, separation, the technological operation medium conveyed It is preferred technical solution, and nitrogen carries insoluble sulfur particle spiral in being atomized 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, and atomization prilling operating process is in closed production It is carried out in device, the probability of pollution environment is made to become extremely low.
Description of the drawings
Fig. 1 is a kind of main structure diagram preparing insoluble sulfur mist projection granulating tower of the present invention.
Fig. 2 is a kind of overlooking structure diagram preparing insoluble sulfur mist projection granulating tower of the present invention.
Fig. 3 is that a kind of A preparing insoluble sulfur mist projection granulating tower of the present invention rotates enlarged structure schematic diagram.
Fig. 4 is a kind of B partial enlargement structural representations preparing insoluble sulfur mist projection granulating tower of the present invention.
Fig. 5 is a kind of C 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 diagrams preparing insoluble sulfur mist projection granulating tower of the present invention.
Fig. 7 is a kind of E partial enlargement structural representations preparing insoluble sulfur mist projection granulating tower of the present invention.
Fig. 8 is a kind of F-F schematic cross-sectional views 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 plates
5- material blanking tube 6- air compartment 7- spray gun assembly 8- refeed line 9- purging devices
10- mist projection granulating tower body 11- material returning devices room 12- exhaust tubes
13- liquid nitrogen central nozzles 14- overheats sulphur steam jet 15- liquid nitrogen outer shroud nozzles
16- is atomized comb component 17- baffle ring 18- taper comb 19- guide rings
20- blast cap 21- bell jar 22- ventilation hole 23- casing 24- air hoses.
Specific implementation mode
The present apparatus is described further with specific embodiment below in conjunction with the accompanying drawings.
The present invention is a kind of to prepare insoluble sulfur spraying as shown in attached drawing 1, Fig. 2, Fig. 3, Fig. 4, Fig. 5, Fig. 6, Fig. 7, Fig. 8 Granulation tower, it is characterized in that:Including mist projection granulating tower assembly 1, material returning device 2, liquid nitrogen storage tank 3.
The mist projection granulating tower assembly 1 includes material blanking tube 5, air distribution plate 4, blast cap 20, air compartment 6, spray gun assembly 7, atomization comb Component 16, mist projection granulating tower body 10.The spray gun assembly 7 includes liquid nitrogen central nozzle 13, overheat sulphur steam jet 14, liquid nitrogen Outer shroud nozzle 15, baffle ring 17, taper comb 18, guide ring 19, the liquid nitrogen central nozzle 13, overheat sulphur steam jet 14, liquid Nitrogen outer shroud nozzle 15 is the casing of same central shaft, and the spray gun assembly 7 is followed successively by liquid nitrogen central nozzle 13, overheat from inside to outside The fluid channel of sulphur steam jet 14, liquid nitrogen outer shroud nozzle 15, converges in outlet end.The atomization comb component 16 includes taper Comb 18, baffle ring 17, guide ring 19, the taper comb 18 on baffle ring 17, can be moved along 16 central axes of atomization comb component, The guide ring 19 is inverted cone-shaped structure, and expanded angle and taper are combed, and 18 apex angles are identical and same central shaft, and taper, which is combed, 18 leads to It crosses and moves to adjust the gap with guide ring 19, the atomization comb component 16 is connect with spray gun assembly 7.
The material returning device 2 includes refeed line 8, purging device 9, material returning device room 11, exhaust tube 12.
10 top of the mist projection granulating tower body is connect with material returning device room 11,8 one end of the refeed line and mist projection granulating tower body 10 lower parts connect, and one end is connect with 11 bottom of material returning device room.
The blast cap 20 includes bell jar 21, air hose 24, casing 23, and the air hose 24 is connect with casing 23, and casing 23 passes through Screw thread is anchored on air distribution plate 4, and adjusts the height of blast cap 20 by rotating, and the air hose 24 has along the circumferential direction opened a row Ventilation hole, the bell jar 21 are erected on the top of air hose 24.
Liquid nitrogen central nozzle 13, the liquid nitrogen outer shroud nozzle 15 of the spray gun assembly 7 are connect with liquid nitrogen storage tank 3.
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 changed.Therefore, the invention is not limited in specific implementation modes disclosed and described above, to the present invention's 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 (1)

1. a kind of preparing insoluble sulfur mist projection granulating tower, it is characterized in that:Including mist projection granulating tower assembly, material returning device, liquid nitrogen storage Tank;Mist projection granulating tower assembly includes material blanking tube, air distribution plate, blast cap, air compartment, spray gun assembly, atomization comb component, mist projection granulating tower Body;Spray gun assembly includes liquid nitrogen central nozzle, overheat sulphur steam jet, liquid nitrogen outer shroud nozzle, baffle ring, taper comb, guide ring; Atomization comb component includes taper comb, baffle ring, guide ring, and taper, which is combed, to be mounted on baffle ring, can be moved along atomization comb component central axes Dynamic, atomization comb component is connect with spray gun assembly;Material returning device includes refeed line, purging device, material returning device room, exhaust tube, mist projection granulating It is connect with material returning device room at the top of tower body, refeed line one end is connect with mist projection granulating tower body lower part, and one end connects with material returning device room bottom It connects;Liquid nitrogen central nozzle, the liquid nitrogen outer shroud nozzle of spray gun assembly are connect with liquid nitrogen storage tank;Liquid nitrogen central nozzle, overheat sulphur steam Vapour nozzle, the casing that liquid nitrogen outer shroud nozzle is same central shaft, spray gun assembly are followed successively by liquid nitrogen central nozzle, overheat from inside to outside The fluid channel of sulphur steam jet, liquid nitrogen outer shroud nozzle, converges in outlet end;Guide ring is inverted cone-shaped structure, the angle of spread Identical as taper comb apex angle and same central shaft is spent, taper is combed adjusts the gap with guide ring by mobile;Blast cap includes clock Cover, air hose, casing, air hose and casing connection, casing are anchored at by screw thread on air distribution plate, and adjust blast cap by rotating Just, air hose has along the circumferential direction opened row's ventilation hole, and bell jar is erected on air hose top.
CN201710129232.0A 2017-03-06 2017-03-06 It is a kind of to prepare insoluble sulfur mist projection granulating tower Active CN106829877B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103539078A (en) * 2013-10-25 2014-01-29 北京化工大学 Method for preparation of insoluble sulfur
CN103539079A (en) * 2013-10-25 2014-01-29 北京化工大学 Method for one-step preparation of insoluble sulfur
CN104174326A (en) * 2014-07-21 2014-12-03 江苏凯茂石化科技有限公司 Spray granulating drying tower
CN104843651A (en) * 2014-02-18 2015-08-19 中国石油化工股份有限公司 Production process for preparing insoluble sulphur through low temperature method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103539078A (en) * 2013-10-25 2014-01-29 北京化工大学 Method for preparation of insoluble sulfur
CN103539079A (en) * 2013-10-25 2014-01-29 北京化工大学 Method for one-step preparation of insoluble sulfur
CN104843651A (en) * 2014-02-18 2015-08-19 中国石油化工股份有限公司 Production process for preparing insoluble sulphur through low temperature method
CN104174326A (en) * 2014-07-21 2014-12-03 江苏凯茂石化科技有限公司 Spray granulating drying tower

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Address after: 362000 the 2 floor of 32 new gate Street and 1916 Creative Industrial Park, Licheng District, Quanzhou, Fujian, China, 1916

Applicant after: Yang Song

Address before: 362000 No. 135 Cui Hu Road, Hu tou Town, Anxi County, Fujian, Quanzhou, Fujian

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Application publication date: 20170613

Assignee: Quanzhou green low carbon Research Institute

Assignor: Yang Song

Contract record no.: 2019350000001

Denomination of invention: Use method for preparing insoluble sulfur spray granulation tower

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Address after: 274000 coal electricity chemical industry park, Mudan District, Heze City, Shandong Province

Patentee after: Shandong Tiansheng cellulose Co., Ltd

Address before: 362000 Yuanyuan, 610 Xinmen Street, Licheng District, Quanzhou City, Fujian Province, and 32 buildings and 2 floors of 1916 Creative Industry Park

Patentee before: Yang Song

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