CN86101191A - Useless synthetic rubber sulfur removal technology and equipment thereof - Google Patents

Useless synthetic rubber sulfur removal technology and equipment thereof Download PDF

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Publication number
CN86101191A
CN86101191A CN86101191.0A CN86101191A CN86101191A CN 86101191 A CN86101191 A CN 86101191A CN 86101191 A CN86101191 A CN 86101191A CN 86101191 A CN86101191 A CN 86101191A
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China
Prior art keywords
rubber
digester
chuck
thermal oil
inner core
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CN86101191.0A
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CN1012067B (en
Inventor
黄世钰
张谱香
吕春源
楼润初
贾生圭
刘显武
颜长贵
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SHANGHAI SCRAPED MATERIAL RECOVERY CO
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SHANGHAI SCRAPED MATERIAL RECOVERY CO
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Priority to CN86101191A priority Critical patent/CN1012067B/en
Publication of CN86101191A publication Critical patent/CN86101191A/en
Publication of CN1012067B publication Critical patent/CN1012067B/en
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/141Feedstock
    • Y02P20/143Feedstock the feedstock being recycled material, e.g. plastics
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/62Plastics recycling; Rubber recycling

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  • Processing Of Solid Wastes (AREA)

Abstract

The present invention relates to waste rubber regeneration, particularly waste rubber sulfur removal technology and equipment.It is waste Crumb rubber to be broken into rubber powder contact stirring desulphurization with regenerator with the water mixing or with saturated vapo(u)r, it is characterized in that adopting thermal oil in chuck material to be carried out conduction heating, controls desulfurization reaction temperature, pressure etc.; Its sweetening process is carried out in the jacketed type digester, and this jar comprises inner core, chuck and feed inlet and outlet, constitutes sealed can by inner core and chuck, and the thermophore in the chuck is a thermal oil, and the two-way agitator that revolves direction about relative is arranged in the inner core.It can handle useless synthetical glue, can handle useless natural gum again.

Description

Useless synthetic rubber sulfur removal technology and equipment thereof
The present invention relates to waste rubber regeneration, particularly all kinds of a kind of sulfur removal technologies of useless synthetic rubber regenerated and equipment thereof.
Rubber has purposes widely, and along with the rubber process development, the consumption of rubber has reached promptly and increased.Especially the expansion of synthetic rubber articles turnout and usage quantity has produced the dead meal of a large amount of synthetical glue goods.How to make full use of a large amount of useless natural rubber and the synthetic rubber that produce thereupon and caused people's attention.
The known waste rubber regenerated of people key is " desulfurization ", so-called " desulfurization " is meant and uses mechanical energy and regenerator in vulcanized rubber, open and cut off sulphur one sulphur in the cross-linked rubber, sulphur one carbon cross-link bond selectively, and preserve the base key structure, make backbone tear fracture fully, separate.Obtain uneven in lengthly at last, the assorted molecular structure of in disorder inequality becomes the desulfurization rubber of desulfurization, and this desulfurization rubber is exactly well-known " regenerated rubber ".
Produce the regenerated rubber sulfur removal technology at present, mainly be regeneration to useless natural rubber, generally be earlier waste rubber to be cut into 18~24 order rubber particles through mechanical shear, mix with a certain proportion of regenerator again, under the condition of outside a part of saturation steam reaches, heating, permeate desulfurization, used desulfurization cylinder temperature can only reach about 150 ℃, and in-cylinder pressure also only reaches 5kg/cm 2About, and the synthetic rubber structure is different with natural rubber with performance, different synthetical glues has property separately again, therefore the useless synthetical glue of this class is to be difficult to regenerated in above-mentioned known technology and equipment, sometimes can only burn as fuel in order to handle, part resource, contaminate environment had again so both been wasted.
Though useless elastomeric regeneration has the research report, but their technology and equipment all are more complicated.What have need be supporting with high pressure steam and boiler, and condition is difficult with control and realization, production cost height.
An object of the present invention is to provide the sulfur removal technology of a simple and easy enforcement for the useless synthetic rubber of regenerating for this reason.
Another purpose is can handle useless natural rubber for regenerated rubber provides a kind of, can handle useless elastomeric sweetener again.
Also having a purpose is to be the shortening desulfurization cycle, improves the quality of reclaimed rubber, and convenient accurately control desulfurization condition provides a kind of technology and equipment.
The present invention realizes like this, earlier rubber powder is sheared or be ground into to useless synthetical glue or useless natural rubber, mix with regenerator and water by proportioning again or carry out stirring desulphurization with part steam, it is characterized in that adopting thermal oil in the chuck of digester, material to be carried out the mode of conduction heating, control the regeneration condition such as temperature, pressure of desulphurization reaction; Its sweetening process is carried out in a kind of jacketed type digester.
This digester is a kind of horizontal digester of belt stirrer, it is the sealed can that constitutes by inner core and chuck, inner core is that two is arc garden, garden column-shaped barrel, has the bidirectional screw agitator that revolves direction about relative in the inner core, and inner core has assembled the chuck of one deck closed at both ends outward; The thermophore that passes through in the chuck is a thermal oil, has the thermal oil that connects the outer heating of thermal oil system to import and export pipeline on the chuck, is equipped with the insertion pipe box that inserts electric heater and temperature regulator in chuck; Pass chuck outward by digester and in inner core, have able to turn on or off feed inlet and outlet.
Above-mentioned feed inlet and outlet can be offered a mouth in the middle part of digester, so not only reduced technical difficulty from the sealed can manufacturing, and helps rubber powder is fully carried out permeable reactive in jar; Tank body is wanted 180 ° of rotations during discharging, and this rotation is to getting rid of because high temperature causes that the carbide buildup also is favourable.If will rotate, digester is outer will set up wheelwork, the two ends steam inlet pipeline of digester and the thermal oil inlet and outlet piping of chuck will adopt in the machinofacture and pressure-vessel in existing union device or hose connection, make the digester rotation unaffected.
Digester also can above establish an able to turn on or off opening for feed, establish an able to turn on or off discharge port below, the digester discharging does not just need to rotate like this, and the thermal oil of digester two ends steam inlet pipe and chuck is imported and exported pipeline and can be connected as routine, and digester is set up wheelwork outward and also can be saved.
Desulfurization or the quality of the regenerative response control of mainly putting to death selection, Formula Design and regeneration condition in regenerator of waste rubber in above-mentioned digester.The rubber item kind is a lot, generally should select suitable regenerator for use according to the rubber kind.Regenerator mainly comprises tenderizer and activator.Tenderizer claims swelling agent and softening agent again.Swelling agent has been meant the low-boiling point material of pre-plastification, for example kautschin, di-terpene etc.Softening agent has been meant the high boiling material of plastification, for example the last running in coumarone, Stockholm tar, oxidation pine oar oil (Yatall MA), the refining of petroleum byproduct.The tenderizer kind can be divided into: vegetables oil system, coal tar are, oil is and synthesize system.Activator is can shorten the recovery time greatly in the waste rubber regenerative process, reduce the consumption of tenderizer, improve reclaimed rubber performance of technical process material, with reference to " rubber industry handbook " first fascicle rubber and framework material, " rubber industry handbook " group of writing writes, the P380-P391 of Chemical Industry Press.The regenerator Formula Design also changes according to waste rubber kind difference.The regenerator that for example useless synthetic rubber butyronitrile is selected and the proportioning of regenerator are: coumarone 5-10%, Stockholm tar are 45-65%, and rosin is 2.5-7% and 420 activators (being polyalkylbenzene phenol disulphide) 3-8%; The regenerator and the proportioning thereof of useless synthetic rubber butylbenzene are: coumarone 5-10%, Stockholm tar are 20-40%, 420 activators (being polyalkylbenzene phenol disulphide) 2-5%; The useless general regenerator proportioning of natural rubber is: coumarone 1.1%, Stockholm tar are 8.3%, 420 activator (being polyalkylbenzene phenol disulphide) 0.6%.Above proportioning all based on rubber powder 100% heavily and calculated weight per-cent.Regenerant consumption is generally 15-75%, adds entry to be: 10-25%(or logical fractional saturation steam) more than also be heavily to calculate regenerator and water consumption with 100% rubber powder.Principal feature of the present invention is the control of waste rubber desulfurization condition.Batching is in above-mentioned digester, and heating is undertaken by thermophore conduction heat in chuck.The thermophore that the present invention uses is the high boiling point thermal oil of selecting for use according to industrial requirements, the thermal oil kind is a lot, reasonable is to adopt the byproduct of petrochemical complex such as locomotive oil, steam turbine oils, high boiling alkyl benzene, three-way arylhydrocarbon in diesel oil hydrogenation, washing oil etc., and best is the thermal oil of three-way diesel oil hydrogenation class.They are harmless on nontoxic and the physiology, do not have uncomfortable smell and sensation, do not cause environmental pollution, normal pressure uses, and is appropriate to the use range more than 200 ℃, homogeneous heating, easily control, the may command desulfurization temperature from more than 150 ℃ near about 300 ℃.Because digester provided by the invention is the sealed can that inner core and chuck constitute, by material desulphurization reaction pressure in the temp controlling tank of thermal oil in the chuck from zero to 20 kilograms per centimeter 2About, relatively good is the 11-20 kilograms per centimeter 2In addition, in jar two-way agitator is arranged, can carry out the M type to material and stir, energy thorough mixing rubber powder and regenerator make them obtain the excellent contact reaction.According to temperature, pressure, how many stirring state and materials come to determine the suitable reaction times.Therefore this technology and equipment can not only be handled the desulfurization of useless natural rubber, and make complex structure and special useless synthetic rubber has been realized payable regeneration.By measuring the quality and the existing technology natural gum quality comparison sheet of its regeneration synthetical glue and regeneration natural gum: attached behind the A()
Calculate mean value from last table, this technology and the equipment useless synthetic rubber of not only can regenerating, and handle useless natural rubber and improve 25% than former handicraft product quality.Type of heating provided by the invention not only produces high heat effect, and thermal oil can use repeatedly, heats evenly, and warm-up time is short, can shorten the desulfurization cycle greatly, the more important thing is waste rubber desulfurization temperature and pressure can be controlled easily with more accurately.The bidirectional screw agitator is provided in the digester that is provided, and agitation condition is good, and the material contact evenly react completely, and occupation area of equipment is little, can realize mechanize and automated operation, implements easily, and facility investment is few, and production cost is low.
Further specify the present invention below in conjunction with accompanying drawing and embodiment.
Accompanying drawing is the structure iron that the invention provides the jacketed type digester of embodiment.
Referring to accompanying drawing, this digester is made of inner core [1] and chuck [2]; The diameter of inner core [1] is selected according to treatment capacity, the two ends end socket, preferably adopt the standard circular end socket, because it is a pressure-vessel, need according to being subjected to peak pressure to come select materials, its material preferably selects the 20g boiler steel, outside inner core [1], be equipped with chuck [2] two ends end socket, be preferably the conical head of 45 ° of cone angles,, can select general steel plate materials for use because it does not bear elevated pressures.Feed inlet and outlet [3] is a mouth, this feed inlet and outlet is positioned at the digester central part, pass chuck, be not connected with chuck [2], its aperture can be gone into hole dimension by standard and selects for use, and able to turn on or off lamina tecti is arranged on feed inlet and outlet, lamina tecti covers can adopt existing multiple mode of connection on the feed inlet and outlet, it is convenient to require to open, and for example the clamping hoop type structure is equipped with exhaust body adapter [a] and connects security device and operating pressure table on top cover.The digester two ends, one end is that steam inlet [e], [d] the other end are oil-in [b], oil outlet [c], oil outlet pipe [4], oil inlet pipe [5], heated oil passage [6], steam and the waste gas exhaust pipe [f] of heated oil, because the tank body rotation is adopted existing union device in machinofacture and the pressure-vessel so import and export pipe, make the digester rotation unaffected, the square weave asbestos packing is adopted in its sealing.
Rolling ring [7] and master wheel [8] are housed on chuck [2], trundle [9] is equipped with in corresponding rolling ring [7] on support [11], trundle [9] links to each other with support [11] by sliding surface bearing [10], master wheel [8] drives by pinion(gear) [12], and above member has been formed the wheelwork part that digester is set up outward.Digester only rotates when discharging, and rotating speed is 13 rev/mins, and speed reduction unit [13] is selected Wxy18-37-II type for use.
In inner core [1], stir shaft [14] is housed, on stir shaft [14], be equipped with the bracing frame [16] of spiral leaf slurry, they can be connected on the stir shaft [14] by bolt connecting mode commonly used, stir shaft [14] can be the 20g steel pipe, double paddle is respectively the leaf slurry of left and right sides helicoidal surface, direction relatively is fixed on each side of stir shaft [14] two ends separately, their other end is starched support [16] by leaf and is fixed on stir shaft [14] middle part, constitutes in this way to revolve direction bidirectional screw leaf slurry about relative.In addition because two of jar is the loose joint device, so two of stir shaft [14] connects one section axle and bearing [17] respectively, whole agitator is supporting with this bearings at both ends [17], end at stir shaft, can be by the sprocket wheel (not shown) that links to each other with power set, rotate so that drive agitator, its rotating speed is chosen as 10~13 rev/mins.
Temperature regulator [18] also is housed on the jacketed type digester in addition, and this temperature regulator [18] has chain circuit assembly with thermal oil high tank heating system so that control thermal oil temperature (not shown).Temperature regulator [18] and electric heater [19] broadcast the hole and pipe all is contained in the chuck [2].
Also thermal insulation layer will be arranged outside chuck [2], its thermal insulation layer material can be selected Calucium Silicate powder for use.
The operating process of desulfurization is: feed inlet and outlet [3] the upper top cover plate of at first opening digester, waste rubber 300~400 kilogram weight rubber powders of crossing through mechanical workout, granularity 8~24 orders add in the jar, restart agitator, be metered into regenerator and moisture content while stirring, regenerator weight is 15%~75%, and moisture content is 10~25% all to weigh 100% with rubber powder and calculate, then the closed roof plate.Can or preheat from steam inlet [e] and the additional moisture content of [d] logical a small amount of saturation steam subsequently, also can be obstructed.Meanwhile thermal oil is warmed to the temperature of requirement in advance in the system with support equipments such as high tank and high temperature circulation pumps, the thermal oil that heated flows in the chuck [2] through oil pipe [5] by oil-in [b] material is heated, carry out heat exchange in this heated oil and material, the thermal oil that exchanged heat is got back to the thermal oil heating system (not shown) from oil outlet [c] through oil outlet pipe [4].Agitator carries out the M type to material and fully stirs when heating.The temperature of main admittance deep fat is controlled the pressure of digester internal reaction.After temperature and pressure reaches processing requirement, start the interior electric heater of chuck [2] [19] and be incubated.About 0.5~3 hour, reacting completely stopped to stir.Opening exhaust outlet [f] again scavenges.Then open feed inlet and outlet [3] upper top cover plate, start the digester wheelwork, drive pinion(gear) [12] by electric motor through speed reduction unit [13], pinion(gear) [12] drives master wheel [8], and master wheel [8] drives digester and rolls on the track of rolling ring [7] and roller [9] formation, and digester rotates 180 ° of angles during discharging, make feed inlet and outlet [3] down, restart the stirring discharging, unsnatch material and stop to stir, make digester reinstatement attitude again so that next operation.
Below provide the design and the desulfurization condition control embodiment table look-up of useless synthetic rubber butyronitrile, butylbenzene and useless natural rubber regenerator and its proportioning: attached behind the B()
Figure 86101191_IMG2
Figure 86101191_IMG3

Claims (10)

1, relating to a kind of waste rubber sulfur removal technology of waste rubber regenerated comprises: waste Crumb rubber is broken into rubber powder, again the regenerator of rubber powder and certain proportioning and water are being sealed the desulfurization in-tank mixing, this batching is under agitation carried out desulfurization, it is characterized in that adopting thermal oil in chuck, batching to be carried out conduction heating, control the temperature and pressure of desulphurization reaction by the thermal oil temperature.
2, sulfur removal technology according to claim 1 is characterized in that used thermal oil is the byproduct of petrochemical complex, and best is the thermal oil of three-way diesel oil hydrogenation class.
3, sulfur removal technology according to claim 1 is characterized in that the proportioning of useless natural rubber powder and regenerator and water is: weigh 100% based on rubber powder, coumarone 1.1%, Stockholm tar 8.3%, 420 activator 0.6%, water 10~15%.
4, sulfur removal technology according to claim 1 is characterized in that the proportioning of useless synthetic rubber nitrile rubber powder and regenerator and water is: weigh 100% based on rubber powder, coumarone 5-10%, Stockholm tar 45~65%, 420 activator 3-8%, rosin 2.5-7%, water 10~25%.
5, sulfur removal technology according to claim 1 is characterized in that the proportioning of useless synthetic rubber sbr powder and regenerator and water is: weigh 100% based on rubber powder, coumarone 5.~10%, Stockholm tar 20~40%, 420 activators 2~5%, water 10~25%.
6, a kind of jacketed type digester is the horizontal digester of belt stirrer, it is characterized in that this digester comprises inner core, chuck and able to turn on or off feed inlet and outlet, constitute sealed can by inner core and chuck, the thermophore in the chuck is a thermal oil, has the bidirectional screw agitator in the inner core.
7, digester according to claim 6 is characterized in that two-way revolving stirrer comprises stir shaft, two-way pivoting leaf oar and support thereof.
8, digester according to claim 6 is characterized in that two-way pivoting leaf oar is left dextral plane of rotation, and direction is relative.
9, digester according to claim 1 is characterized in that feed inlet and outlet [3] is a mouth, and digester is furnished with wheelwork outward, and the Pipe moveable joint device is equipped with at the digester two ends.
10, digester according to claim 1 is characterized in that being equipped with in the chuck [2] electric heater [19], temperature regulator [18].
CN86101191A 1986-02-28 1986-02-28 Desulfurizing processing and its equipment of scraped synthetic rubber Expired CN1012067B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN86101191A CN1012067B (en) 1986-02-28 1986-02-28 Desulfurizing processing and its equipment of scraped synthetic rubber

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Application Number Priority Date Filing Date Title
CN86101191A CN1012067B (en) 1986-02-28 1986-02-28 Desulfurizing processing and its equipment of scraped synthetic rubber

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CN86101191A true CN86101191A (en) 1987-09-09
CN1012067B CN1012067B (en) 1991-03-20

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1056631C (en) * 1996-04-26 2000-09-20 秦国祥 Process of technique transformation for producing reclaimed rubber by dynamic desulfating
CN1056863C (en) * 1995-05-05 2000-09-27 李莲香 Method for preparing regenerated rubber by decomposition method
WO2010057444A1 (en) * 2008-11-21 2010-05-27 东莞市松山科技集团有限公司 Sealed dissociation and desulfurization reactor and system thereof
CN105752920A (en) * 2016-05-20 2016-07-13 广西梧州日成林产化工股份有限公司 Conveying method for hot rosin

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1056863C (en) * 1995-05-05 2000-09-27 李莲香 Method for preparing regenerated rubber by decomposition method
CN1056631C (en) * 1996-04-26 2000-09-20 秦国祥 Process of technique transformation for producing reclaimed rubber by dynamic desulfating
WO2010057444A1 (en) * 2008-11-21 2010-05-27 东莞市松山科技集团有限公司 Sealed dissociation and desulfurization reactor and system thereof
CN105752920A (en) * 2016-05-20 2016-07-13 广西梧州日成林产化工股份有限公司 Conveying method for hot rosin
CN105752920B (en) * 2016-05-20 2019-02-15 广西梧州日成林产化工股份有限公司 The delivery method of hot rosin

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Publication number Publication date
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