CN106829877A - One kind prepares insoluble sulfur mist projection granulating tower - Google Patents

One kind prepares insoluble sulfur mist projection granulating tower Download PDF

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Publication number
CN106829877A
CN106829877A CN201710129232.0A CN201710129232A CN106829877A CN 106829877 A CN106829877 A CN 106829877A CN 201710129232 A CN201710129232 A CN 201710129232A CN 106829877 A CN106829877 A CN 106829877A
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liquid nitrogen
mist projection
projection granulating
insoluble sulfur
granulating tower
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CN201710129232.0A
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CN106829877B (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 field, and in particular to one kind prepares 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)A kind of operational process of craft for rapidly cooling down, protecting, be atomized, granulate, convey, be separate needed for insoluble sulfur is prepared as technical process medium completion; so as to complete the whole technical process of insoluble sulfur mist projection granulating in tower, make it possible that batch is continuous and produce.

Description

One kind prepares insoluble sulfur mist projection granulating tower
Technical field
The present invention relates to insoluble sulfur technical field, and in particular to one kind prepares insoluble sulfur mist projection granulating tower.
Background technology
Insoluble sulfur(IS)Also known as polymerised sulphur, also known as μ types sulphur refers to the sulphur insoluble in carbon disulfide, is the long-chain of sulphur Polymer, with chemically and physically inertia.It is 1% in the solubility of rubber due to using common sulphur, common sulphur is in rubber Consumption exceed its dissolving part sizing material cooling after can spray surface, i.e. bloom.Bloom will be influenceed between semifinished part Stickiness simultaneously brings adverse effect to product vulcanization uniformity, therefore in sulfur consumption appropriate to the occasion use insoluble sulfur higher, it is insoluble Sulphur does not dissolve in rubber, only dispersed in elastomeric compound, and product vulcanization crosslinking point is uniform, has with its rubber for vulcanizing optimal No blooming, and can effectively prevent sizing material from occurring 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, it is melted;2)Atomization:Sulphur liquid after melting is through atomizer Centrifugal atomizing is into 10 μm~50 μm of sulphur droplet;3)Polymerization:Nitrogen at room is mixed with sulphur droplet after being distributed through gas distributor Close;Sulphur drop is stopped 2~25 seconds on tower body top, and nitrogen outlet temperature control is at 180~240 DEG C;4)Chilling:After polymerization Sulphur is cooled to -40~0 DEG C and mixes through the nitrogen after gas distributor distribution with through cooling device again, into tower body bottom, Less than 60 DEG C were cooled at 2~20 seconds;5)Separate packaging:Cyclonic separation, collects, and packaging obtains insoluble sulfur product.China Patent of invention(Patent No. 02157245.3, patent name is 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 mainly includes following preparation process:(1) by common sulphur and the compound stabilizer of mass percent 0.01~0.2% In adding with heating, the container of stirring, it is filled with inert gas and protects, the 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 obtain conversion ratio be 53~55% it is insoluble Sulphur crude product;Compound stabilizer is made up of I2 or Br2 with rubber accelerator DM or DZ;(2) by insoluble sulfur crude product with The solid-to-liquid ratio mixing of leaching agent in mass ratio 1: 15~20, stirs 5~60min at a temperature of 45~80 DEG C, 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, and mainly prepare that rubber tyre uses is insoluble Property sulphur, cooling medium is liquid nitrogen, technological process be melting, atomization, polymerization, chilling, separation pack, it is critical only that how to protect Sulphur liquid after card melting through atomizer centrifugal atomizing into 20 μm of average grain diameter sulphur droplet, will to reach above technology Ask, it is necessary to ensure that atomizer at high operating temperatures still being capable of reliably working(Centrifugal atomizing needs atomizer high-speed rotation), it is many It is well known, according to the 280-400 DEG C of production environment of high temperature, batch industrialization production it is difficult to ensure that atomizer can normal work and Ensure the Particle size requirements of sulphur droplet, while mention sulphur drop being had to go to the toilet cold polymerization in tower, be and immediate technology of the invention Scheme, but the details and its application method of process units are not disclosed;Conventional example two discloses the system of insoluble sulfur Preparation Method, main innovation point is to use normal pressure or low-voltage equipment to complete the preparation of insoluble sulfur, and main production plant is to add Heat, the container of stirring, superheater, spray gun, atomisation tower and heat exchanger, it is close with technical solution of the present invention, but life is not disclosed Produce the details and its application method of device.
The content of the invention
In view of the shortcomings of the prior art, insoluble sulfur mist projection granulating tower is prepared it is an object of the invention to provide one kind, its 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 granulates tower body.The spray gun assembly includes liquid nitrogen central nozzle, overheat sulphur steam jet, liquid nitrogen outer shroud nozzle, baffle ring, cone Shape is combed, guide ring, the liquid nitrogen central nozzle, overheat sulphur steam jet, the sleeve pipe that liquid nitrogen outer shroud nozzle is same central shaft, The spray gun assembly is followed successively by liquid nitrogen central nozzle, overheat sulphur steam jet, the fluid of liquid nitrogen outer shroud nozzle and leads to from inside to outside Road, converges in the port of export.The atomization comb component includes taper comb, baffle ring, guide ring, and the taper is combed and is arranged on baffle ring, Can be moved along atomization comb component axis, the guide ring is inverted cone-shaped structure, and its expanded angle is identical with taper comb drift angle And same central shaft, taper combs by mobile to adjust the gap with guide ring, and the atomization comb component is connected with spray gun assembly.
The material returning device includes refeed line, purging device, material returning device room, aiutage.
The mist projection granulating tower body top is connected with material returning device room, and described refeed line one end connects with mist projection granulating tower body bottom Connect, one end is connected with material returning device room bottom.
The blast cap includes bell jar, airduct, sleeve pipe, the airduct and sleeve pipe connection, and sleeve pipe is anchored at cloth wind by screw thread On plate, and the height of blast cap is adjusted by rotating, the airduct has along the circumferential direction opened row's air vent, the bell jar sets up On airduct top.
The liquid nitrogen central nozzle of the spray gun assembly, liquid nitrogen outer shroud nozzle are connected with liquid nitrogen storage tank.
Inventor has found, uses liquid nitrogen overheat sulphur steam is rapidly cooled to system below 90 DEG C of temperature for rapidly cooling agent It is liquid nitrogen runner to take the overheat sulphur steam flow channel internal and external casing in insoluble sulfur, therefore design spray gun assembly, and in outlet End mixing, can effective observing and controlling process conditions such as temperature, flow, pressure etc., and protect lance driving device to work under the high temperature conditions just Often.
Inventor has found that insoluble sulfur content is higher, preferably just insoluble sulfur processed is produced high-temperature stability to obtain Product, atomization is critical process, by adjusting the gap that guide ring is combed with taper, makes insoluble sulfur with nitrogen fluid-mixing at a high speed Injection, runs into the rough surface of taper comb, agitates the drop for being separated into and being suspended in nitrogen, carries rapidly cooling effect Height, and improve just insoluble sulfur product yield processed.
Inventor has found that granulation is conducive to preventing insoluble sulfur to the conversion of common sulphur, improves its stability.Using The 20-22 DEG C of recovery nitrogen of temperature is cooled down as insoluble sulfur, protected, granulating, separating, the technological operation medium of conveying is excellent The technical scheme of choosing, is conducive to recovery nitrogen circulation to utilize reduces cost.Nitrogen is from atomization granulation tower bottom air distribution plate purging Come, can be formed along the atomization granulation spiralling air-flow of tower wall, observed from air-flow cross section transverse, air-flow has periphery flow velocity Hurry up, center flow velocity it is slow, the periphery feature big compared with center pressure can order about the insoluble sulfur particle constantly grown up and throw to tower wall Frictional impact loses kinetic energy whereabouts, and assembles to center, and insoluble sulfur particle diameter is grown up to after certain diameter in gravity Lower and nitrogen separation is acted on, subsequent processing is entered 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 is necessary to passing through to design the structure of blast cap, height, arrangement goes solve problem, the present invention preferably bell-type windshield, nitrogen is through airduct Air vent purged to air distribution plate from the gap of bell jar and airduct again, then flowed to atomization granulation tower top through the stop of air distribution plate, The navigation designing for unifying direction perforate by the air vent on the exhaust duct of material blanking tube periphery 3~4 is oriented to nitrogen spiral, It is exactly actually the width for adjusting nitrogen spiral wind band by adjusting bell jar with a distance from air distribution plate, substantially have adjusted nitrogen spiral shell The time that whirlwind band rises along atomization granulation tower spiral inner wall, so as to ensure that the technique in atomization granulation tower of insoluble sulfur is stopped Stay(Granulation)Time.
Relative to prior art, the present invention is at least containing having the advantage that:First, liquid nitrogen(Nitrogen)As a kind of technical process Medium completion prepares rapidly cooling down needed for insoluble sulfur, protection, atomization, granulation, conveying, separate operational process of craft, It is optimal technical process medium;Second, nitrogen makes the possibility that sulphur is fired extremely low as protection gas, beneficial to safe life Produce;3rd, the overheat sulphur steam flow channel internal and external casing in spray gun assembly is liquid nitrogen runner, and in port of export mixing, 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, by adjusting The gap that whole guide ring and taper are combed, makes insoluble sulfur be sprayed at a high speed with nitrogen fluid-mixing, runs into taper comb uneven Surface, agitate the drop for being separated into and being suspended in nitrogen, make rapidly cooling effect improve, and make just insoluble sulfur product processed Yield is improved;5th, granulation is conducive to preventing insoluble sulfur to the conversion of common sulphur, improves its stability.Using 20-25 The recycle and reuse nitrogen of DEG C temperature as insoluble sulfur cooling, protection, granulation, separate, the technological operation medium of conveying It is preferred technical scheme, and nitrogen carries insoluble sulfur particle spiral, insoluble sulfur in granulation tower is atomized Grain diameter grow up to after certain diameter under gravity with nitrogen separation, enter subsequent processing through material blanking tube, make batch produce Industry metaplasia is produced and is possibly realized;6th, atomization granulation tower is obturator, and atomization prilling operating process is in closed production Carried out in device, making the probability of pollution environment becomes extremely low.
Brief description of the drawings
Fig. 1 is a kind of main structure diagram for preparing insoluble sulfur mist projection granulating tower of the present invention.
Fig. 2 is a kind of overlooking the structure diagram for preparing insoluble sulfur mist projection granulating tower of the present invention.
Fig. 3 is a kind of A rotation mplifying structure schematic diagrams for preparing insoluble sulfur mist projection granulating tower of the present invention.
Fig. 4 is a kind of B partial enlargement structural representations for preparing insoluble sulfur mist projection granulating tower of the present invention.
Fig. 5 is a kind of C for preparing insoluble sulfur mist projection granulating tower of the present invention to structural representation.
Fig. 6 is a kind of D full-page proof structural representations for preparing insoluble sulfur mist projection granulating tower of the present invention.
Fig. 7 is a kind of E partial enlargement structural representations for preparing insoluble sulfur mist projection granulating tower of the present invention.
Fig. 8 is a kind of F-F cross section structure diagrams 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 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- aiutages
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- air vent 23- sleeve pipe 24- airducts.
Specific embodiment
The present apparatus is described further with specific embodiment below in conjunction with the accompanying drawings.
As shown in accompanying drawing 1, Fig. 2, Fig. 3, Fig. 4, Fig. 5, Fig. 6, Fig. 7, Fig. 8, one kind prepares insoluble sulfur spraying to the present invention 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 that material blanking tube 5, air distribution plate 4, blast cap 20, air compartment 6, spray gun assembly 7, atomization are combed 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 sleeve pipe 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 passage of sulphur steam jet 14, liquid nitrogen outer shroud nozzle 15, converges in the port of export.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 the axis of atomization comb component 16, The guide ring 19 is inverted cone-shaped structure, and its expanded angle and taper are combed, and 18 drift angles are identical and same central shaft, and taper is combed 18 logical Cross to move and adjust the gap with guide ring 19, the atomization comb component 16 is connected with spray gun assembly 7.
The material returning device 2 includes refeed line 8, purging device 9, material returning device room 11, aiutage 12.
The top of the mist projection granulating tower body 10 is connected with material returning device room 11, the one end of the refeed line 8 and mist projection granulating tower body 10 bottoms connect, and one end is connected with the bottom of material returning device room 11.
The blast cap 20 includes bell jar 21, airduct 24, sleeve pipe 23, and the airduct 24 is connected with sleeve pipe 23, and sleeve pipe 23 passes through Screw thread is anchored on air distribution plate 4, and the height of blast cap 20 is adjusted by rotating, and the airduct 24 has along the circumferential direction opened a row Air vent, the bell jar 21 is erected on the top of airduct 24.
The liquid nitrogen central nozzle 13 of the spray gun assembly 7, liquid nitrogen outer shroud nozzle 15 are connected with liquid nitrogen storage tank 3.
The announcement and teaching of book according to the above description, those skilled in the art in the invention can also be to above-mentioned embodiment party Formula is changed and changed.Therefore, the invention is not limited in specific embodiment disclosed and described above, to of the invention Some modifications and changes should also be as falling into scope of the claims of the invention.Although additionally, being used in this specification Some specific terms, but these terms are merely for convenience of description, do not constitute any limitation to the present invention.

Claims (4)

1. one kind prepares 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 is combed and is arranged on baffle ring, can be moved along atomization comb component axis Dynamic, atomization comb component is connected with spray gun assembly;Material returning device includes refeed line, purging device, material returning device room, aiutage, mist projection granulating Tower body top is connected with material returning device room, and refeed line one end is connected with mist projection granulating tower body bottom, and one end connects with material returning device room bottom Connect;The liquid nitrogen central nozzle of spray gun assembly, liquid nitrogen outer shroud nozzle are connected with liquid nitrogen storage tank.
2. one kind according to claim 1 prepares insoluble sulfur mist projection granulating tower, it is characterized in that:Liquid nitrogen central nozzle, Overheat sulphur steam jet, the sleeve pipe that liquid nitrogen outer shroud nozzle is same central shaft, spray gun assembly are followed successively by liquid nitrogen from inside to outside Heart nozzle, overheat sulphur steam jet, the fluid passage of liquid nitrogen outer shroud nozzle, converge in the port of export.
3. one kind according to claim 1 prepares insoluble sulfur mist projection granulating tower, it is characterized in that:Guide ring is back taper Structure, its expanded angle is identical with taper comb drift angle and same central shaft, and taper combs by mobile to adjust and between guide ring Gap.
4. one kind according to claim 1 prepares insoluble sulfur mist projection granulating tower, it is characterized in that:Blast cap include bell jar, Airduct, sleeve pipe, airduct and sleeve pipe connection, sleeve pipe are anchored on air distribution plate by screw thread, and the height of blast cap is adjusted by rotating Low, airduct has along the circumferential direction opened row's air vent, and bell jar is erected on airduct 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

Applicant before: Yang Song

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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

Granted publication date: 20181023

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Record date: 20190116

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Assignee: QUANZHOU GREEN LOW CARBON Research Institute

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Effective date of registration: 20201125

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