CN107033385A - Scrap rubber regenerated environment protecting method - Google Patents
Scrap rubber regenerated environment protecting method Download PDFInfo
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- CN107033385A CN107033385A CN201710314758.6A CN201710314758A CN107033385A CN 107033385 A CN107033385 A CN 107033385A CN 201710314758 A CN201710314758 A CN 201710314758A CN 107033385 A CN107033385 A CN 107033385A
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- rubber
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- environment protecting
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2321/00—Characterised by the use of unspecified rubbers
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
The invention discloses scrap rubber regenerated environment protecting method, it is under nitrogen protection, low pressure, low-temperature condition, to carry out physics regeneration and chemical regeneration successively in closed stirring reaction equipment, produces reclaimed rubber.The scrap rubber regenerated environment protecting method of the present invention has that desulfurization condition is simple, easy operational control, scrap rubber desulfurization regeneration fully, environmental protection the advantages of.
Description
Technical field
The present invention relates to scrap rubber regenerated environment protecting method, belong to scrap rubber resource reclaim regeneration field.
Background technology
China is that rubber uses big country, and substantial amounts of rubber causes extremely serious environmental pollution after use, and is
To the serious waste of resource.The tire yield of only 2016 annual China has reached 9.4 hundred million, damaged tire more than 1.3 hundred million, plus
Effective recycling to scrap rubber resource by force, can obtain huge return in terms of environmental protection, resource, income, promote useless
Reasonable, the high-quality recovery of rubber is highly important.
Rubber regeneration method can generally be divided into three classes：Physics regeneration, chemical regeneration and microorganisms reproduction.
1st, physics regeneration techniques
Physics regeneration can be put using additional, and such as power, heating power, cold power, microwave, ultrasonic wave, radial energy make the three of crosslinking rubber
Tie up network to crush, form the reclaimed rubber with mobility.
(1) micro wave regeneration.Microwave desulfurization is a kind of non-chemical, non-mechanical step method of reproduction, and it is to utilize microwave energy
Put cut-out sulphur sulfide linkage（S-S), sulphur carbon key（S-C) without destroying carbon-carbon bond（C-C）, so as to reach the purpose of regeneration.Because microwave
Energy is controllable, and the bond energy of various chemical bonds is different, also different in the energy needed during fracture, so microwave energy scission of link is that have choosing
Selecting property, the reclaimed rubber performance produced in this way is close to virgin rubber.
(2) ultrasonic regeneration.Also optionally cross-bond can be destroyed using ultrasonic wave and retains molecular backbone, make vulcanization
Rubber reaches the purpose of regeneration.In the ultrasonic wave sweetening process of vulcanization rubber in addition to destroying tridimensional network, also cause
The fractures of part macromolecular chain C-C keys, therefore there is a need to further research, to improve the selectivity of ultrasonic wave desulfurization, only
Have and selectively destroy chemical bond, virgin rubber performance could be kept to greatest extent.
(3) electron beam regenerates.Electron beam irradiation renovation process is exclusive to radiation-sensitive using butyl rubber (IIR)
Feature, the high-power electron beam produced by electron accelerator produces the chemical depolymerization effect of scission of link one to it, is allowed to be regenerated.
(4) shear flow reaction technology.Shear flow reaction controlling technology is without using chemical agent, by rubber of giving up
Glue applies heat energy, pressure and shearing force, is broken the sulfide linkage of vulcanizate, so as to generate performance stabilization and have the regeneration of plasticity
Glue.
2nd, chemical regeneration technology
Chemical regeneration is exactly chemical assistant and sulphur-sulfide linkage in scrap rubber under the conditions of certain temperature and solvent atmosphere（S-s) make
With making sulfur bonds, reclaimed rubber of the generation with mobility.Conventional method is oil process, water/oil method and dynamic desulfurization, desulfurization
Effect is obvious.But under the high temperature conditions, sulphur-sulfide linkage（S-S) also easy fracture, often generates many small molecules fragments, makes regeneration
The hydraulic performance decline of glue.Plus the volatilization of Pintsch process and scrap rubber small molecular, greatly pollution can be caused to air and water source.It is vertical
The regeneration history of scrap rubber is seen, effective regenerative agent has following several：
(1) disulphide, mercaptan disulphide and mercaptan regenerative agent, mainly there is diphenyl disulfide, dibenzyl disulfide and butyl mercaptan
Deng.These materials contain active sulfur, in the presence of heat and mechanical energy, can catalytic cleavage S -- S, S-C keys, but also have fracture
The possibility of C-C keys, so with such regenerative agent reproducing waste rubber effect significantly, but property retention rate is not high, and disulphide and
Mercaptan etc. has niff, and to environment there is also certain pollution, application in recent years is gradually decreased.
(2) inorganic compound.Metallic sodium can be regenerated vulcanizate.Rubber powder is suspended in toluene, hexamethylene etc. molten
In agent, in 300 DEG C of high temperature, trapping is handled under conditions of metallic sodium is present, and can make monosulfidic bond, cystine linkage and polysulfide bond fracture.But
It is that metallic sodium is active metal, fierce chemical reaction easily occurs at ambient conditions, and course of reaction is whard to control.At oxygen barrier
The reaction condition of reason is also harsher, in addition, the vulcanized sodium and remaining solvent of generation can be polluted to environment.
(3) RV reducing/regeneratings agent, RV rubber reclaiming agents are a kind of reclaimed rubber new technologies, and its general principle is to use one kindization
Learning agent makes it be reacted with S -- S, without destroying C-C keys, is broken vulcanized network.
(4) regenerated resources (RRM) regenerative agent, the researcher of India, which is developed using a kind of plant product, is used as regenerative agent
Technology, i.e., be used as regenerative agent by the use of renewable resource (RRM).At home, Liu Anhua etc. enters from the production of the plants such as garlic, orange peel
A kind of regeneration of the sub- scrap rubber of plant regeneration agent is extracted in product, preferable effect is also obtain.Natural plants regenerative agent profit
With renewable resource, possesses the condition of sustainable development, the recycling of improvement and rubber sources to black pollution
With far-reaching significance.
3rd, microorganisms reproduction technology
Bacterial desulfurization is exactly oxidation or the sulfur cross-linking for reducing sulphur, makes scrap rubber powder superficial degradation or modification.With
Bacterial desulfurization has the advantages that cost is low and free from environmental pollution.But, the commercialization road Stalk of bacterial desulfurization is also very long.
In addition, polymer coating to be used for the surface treatment or activation of rubber powder, it is possible to increase rubber powder and rubber or thermoplasticity
The bonding bran degree of matrix.Process of surface treatment can make rubber powder apply the occasion in high added value.Using containing crosslinking agent can
The process of surface treatment of cross-linked polymer cladding rubber powder in the U.S. and Dutch commercialization, be referred to as Tirecvle and
Surcrum.With reactant gas handle rubber powder, the table of spiral glue powder and aoxidize polarization group, can make rubber powder with it is gluing
Agent such as polyurethane has more preferable compatibility, the Vistamer commercializations in the U.S..
Chinese patent CN105860130A will vulcanize rubber and solution crosslinking coagent mixing after, by solvent swell and keep solution
Crosslinking temperature, solution crosslinking is carried out by solving the interaction of crosslinking coagent and coordinating to vulcanization rubber, can be in scrap rubber
Sulphur-sulfide linkage has selective abstriction well, and the significantly rupture of cross-linked network can be realized at relatively low temperature, is obtained
To reclaimed rubber.
Chinese patent CN106366342A is related to a kind of production method of reclaimed rubber, includes the preparation of rubber powder, then will
Rubber powder is layered on conveyer belt, below thickness 2cm, and in the hot-air environment of 80 150 DEG C of temperature, the retention time is 30 120
Minute prepares reclaimed rubber.
It is chemical desulfurization operation that Chinese patent CN104151660B, which discloses a kind of preparation method of tasteless reclaimed rubber, plus
Enter tread compound powder, environmental activator, vegetable oil softener and water；Wherein environmental activator is by persulfate and aliphatic acid, plant
Oily softening agent is each vegetable oil, and reclaimed rubber reaches country-level reclaimed rubber standard.
Chinese patent CN106313362A is related to a kind of method of a low temperature preparation reclaimed rubber, by vulcanized rubber powder,
Auxiliary agent and plasticizer are added in high shear banbury, and reclaimed rubber piece is discharged after banburying, and mixing temperature is maintained at 60-90 DEG C.
The method of this low temperature preparation reclaimed rubber does not influence the advantage of external environment when can either retain low temperature preparation, additionally it is possible to carry significantly
The efficiency of high/low temperature banburying and the quality of reclaimed rubber.
A kind of scrap rubber sulfur method disclosed in Chinese patent CN1085224C, is by by monocyclic fragrant footpath, organic acid, metal
The desulfurizing agent that oxide is constituted with inorganic acid, closes uniform with scrap rubber rod according to a certain ratio, 0.1- is reacted at 10 ~ 150 DEG C
200 hours, you can make the effective desulfurization of useless rafter glue.
Chinese patent CN100486789C is continuously to handle surface of waste rubber powder by microwave device, so as to can connect
Surface that is continuous and more effectively handling waste Crumb rubber, reclaimed rubber has good surface roughness and processability, product
Physical and chemical properties are obtained for improvement；Have the disadvantage that desulfurized effect is poor, produce large quantity of exhaust gas.
Chinese patent CN101418082B discloses a kind of green desulfurization technique of waste rubber, by waste rubber grain through charging
Area is added in double-screw rubber devulcanizing reaction unit, high temperature, high pressure and the shearing energy collective effect of compressed shear zone, makes rubber
Crosslinking it is strong be broken, then exhaust gas purification, then knead by double-screw rubber devulcanizing reaction unit the mixing in area, generative nature
The stable new resurgent crude rubber of energy.Advantage is that whole technical process is the shearing desulfurization work under continuous, closed, rubber powder flow regime
Skill, in the feeding section of double-screw rubber devulcanizing reaction unit | using continuous conveying mode is forced, further to glue | powder particles enter
Row dispersion and fining, improves desulfuration efficiency.Shortcoming pyroreaction, processing are uneven, produce waste gas.
Chinese patent 201110031880.5 discloses a kind of waste old automatic microwave cracking reaction device, by controlling automatically
System processed, variable-frequency motor, screw-pushing type microwave cracking reaction warehouse, pneumatic closed automatic feed valve combination and it is pneumatic it is closed go out
Slag valve combination is constituted, and microwave magnetron is uniformly located at the outer of screw-pushing type microwave cracking reaction warehouse inside spin propeller both sides
On wall, pneumatic closed automatic feed valve combination is located at the feed end of screw-pushing type microwave cracking reaction warehouse, it is pneumatic it is closed go out
Slag valve combination is located at the discharge end of screw-pushing type microwave cracking reaction warehouse, and stock distributor is located at pneumatic closed automatic feed
On the charging aperture of valve combination.
Chinese patent 201120034422.2 discloses a kind of waste rubber microwave desulfuration regenerating device, including stir storehouse, stirs
Device and drive mechanism are mixed, drive mechanism is connected with agitator.Flex point is provided with blade, the radian of blade is axially carried out
It is covert, the resistance being subject in whipping process is reduced, energy consumption is reduced, mixing effect is good.
Chinese patent 201320815701.1 discloses new type rubber microwave desulfurization device, including the rotation of feeding mechanism, material
Rotation mechanism and microwave cavity, feeding mechanism include feed pipe and helical blade, and material rotating mechanism includes raw material rotation and managed, again
Rubber rotation pipe and microwave desulfurization pipe, raw material rotation pipe, reclaimed rubber rotation pipe use stainless steel or carbon steel, and microwave desulfurization pipe is used
Ceramics or glass.Have the disadvantage that equipment complexity, desulfurized effect are poor, produce large quantity of exhaust gas.
Chinese patent 201521109962.7 discloses a kind of rubber microwave desulfurizer, including at least two groups rubber microwaves
Desulfurization heating arrangements；Every group of rubber microwave desulfurization heating arrangements include microwave cavity, feeding screw and entering of being sequentially connected with
Expects pipe, Ceramic desulfation pipe, discharge nozzle, Ceramic desulfation pipe are located at microwave resonance intracavitary, and feeding screw is extended transversely through in feed pipe, pottery
In porcelain desulfurization pipe, discharge nozzle.Chinese patent 2016103883215.5 discloses the automatic cracking reaction device of waste old microwave,
Including control unit, reducing agent feeding unit, catalytic reduction unit, micro particle catching unit and temperature sensor, catalysis reduction is single
Member is connected with micro particle catching unit by connecting pipe, and connecting pipe connects the reducing agent feeding unit provided with branch road.
Have the disadvantage that equipment is complicated, desulfurization is insufficient, effect is poor, produce large quantity of exhaust gas.
The content of the invention
In order to solve the above problems, the present invention proposes multi-functional plastic cement processing unit (plant), with advanced design, compact, makes
With environmental protection, conveniently, it is ensured that production safety, energy consumption is saved, reduces production cost.
Technical solution of the present invention description is following：
1st, scrap rubber regenerated environment protecting method, it is characterised in that：Under nitrogen protection, low pressure, low-temperature condition, in closed stirring reaction
Scrap rubber is preheated in equipment, stirred, physics regeneration is carried out under stirring；After physics regeneration, it is directly added into chemistry and helps
Proceed chemical regeneration under agent, stirring, produce reclaimed rubber.
2nd, scrap rubber regenerated environment protecting method according to claim 1, it is characterised in that：Physics regeneration is microwave desulfurization
Method.
3rd, scrap rubber regenerated environment protecting method according to claim 1, it is characterised in that：Nitrogen protection is to use high-purity
Nitrogen is sufficiently displaced from air in consersion unit, and supplements nitrogen.
4th, scrap rubber regenerated environment protecting method according to claim 1, it is characterised in that：The pressure of low-pressure state is table
Press as -0.095MPa to 0.1MPa.
5th, scrap rubber regenerated environment protecting method according to claim 1, it is characterised in that：The temperature of low-temperature condition is 50
DEG C to 160 DEG C.
6th, scrap rubber regenerated environment protecting method according to claim 1, it is characterised in that：Closed stirring reaction equipment is
Kneader with microwave generator.
7th, scrap rubber regenerated environment protecting method according to claim 1, it is characterised in that：The preheating temperature of microwave desulfurization
It is 50 DEG C to 130 DEG C.
Due to above-mentioned technical proposal, the invention has the advantages that:
1st, nitrogen protection can prevent the reclaimed rubber of production from further aoxidizing, degrading.
2nd, low pressure, low-temperature condition can substantially reduce the exhaust gas production of scrap rubber regenerative process.
3rd, the microwave energy of microwave desulfurization is controllable, and the bond energy of various chemical bonds is different, in the energy needed during fracture
Also it is different, so microwave energy scission of link is selective, can according to different scrap rubber species, model, adjust reaction temperature and
Time is produced and processed.
4th, chemical regeneration method combination microwave desulfurization, can produce the reclaimed rubber close to virgin rubber performance.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Described embodiment is only schematical section Example of the invention, and is not used to limit the scope of the present invention, Ren Heben
The technical staff in field, made equivalent variations and modification on the premise of the design of the present invention and principle is not departed from, all should
It is included within this patent protection domain.
Embodiment
Closed stirring reaction equipment is to have 7 preformed holes on 500L screw rod bottom discharge kneaders, kneader cylinder cap, is connected respectively
Connect DN20 nitrogen pipelines, DN25 vacuum pipes, 4 DN50 mouthfuls of installations 4 1KW microwave generators, 1 DN500 charging aperture；Mediate
Machine cylinder body swept volume is 250L；It is to have heating agent in heat exchange jacket, chuck outside cylinder body, connects heat medium system.
The first step：30 200 kilograms of mesh pells powder are added to kneader, vacuum system is then turned on.
Second step：When pressure reaches -0.08MPa in kneader, vacuum valve is closed；Open nitrogen charging air valve, inflated with nitrogen displacement；
Repeat three times.
3rd step：Open heat medium system to heat to material in kneader cylinder body, temperature of charge is reached 80 DEG C.
4th step：Start kneader stirring, when temperature reaches 120 DEG C, stop heating medium for heating；Under stirring, open micro-
Wave producer, microwave physics regeneration is carried out to pells powder, while it is left kneader cylinder interior pressure is maintained at -0.03MPa
It is right；Temperature of charge reaches 130-145 DEG C, closes microwave generator, stops micro wave regeneration.
4th step：Close after microwave generator, vacuum adds chemically composited 4.5 kilograms or so of reclaiming aid；Stirring
Under, proceed chemical regeneration 10-30 minutes, complete the regeneration production of this batch pells powder.
The reclaimed rubber product analysis data that following table produces for the scrap rubber regenerated environment protecting method of the present invention：
Claims (7)
1. scrap rubber regenerated environment protecting method, it is characterised in that：Under nitrogen protection, low pressure, low-temperature condition, in closed stirring reaction
Scrap rubber is preheated in equipment, stirred, physics regeneration is carried out under stirring；After physics regeneration, it is directly added into chemistry and helps
Proceed chemical regeneration under agent, stirring, produce reclaimed rubber.
2. scrap rubber regenerated environment protecting method according to claim 1, it is characterised in that：Physics regeneration is microwave desulfurization.
3. scrap rubber regenerated environment protecting method according to claim 1, it is characterised in that：Nitrogen protection is to use high-purity nitrogen
Air in consersion unit is sufficiently displaced from, and supplements nitrogen.
4. scrap rubber regenerated environment protecting method according to claim 1, it is characterised in that：The pressure of low-pressure state is gauge pressure
For -0.095MPa to 0.1MPa.
5. scrap rubber regenerated environment protecting method according to claim 1, it is characterised in that：The temperature of low-temperature condition be 50 DEG C extremely
160℃。
6. scrap rubber regenerated environment protecting method according to claim 1, it is characterised in that：Closed stirring reaction equipment is with micro-
The kneader of wave producer.
7. scrap rubber regenerated environment protecting method according to claim 1, it is characterised in that：The preheating temperature of microwave desulfurization is 50
DEG C to 130 DEG C.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107602910A (en) * | 2017-10-19 | 2018-01-19 | 洛阳和梦科技有限公司 | Non-odor generated rubber production method |
| CN108948276A (en) * | 2018-08-11 | 2018-12-07 | 洛阳和梦科技有限公司 | The production method of cis-butenedioic anhydride graft type whole tire reclaim rubber powder |
| CN108976349A (en) * | 2018-08-11 | 2018-12-11 | 洛阳和梦科技有限公司 | The production method of cis-butenedioic anhydride graft type butyl reclaimed rubber powder |
| CN109160979A (en) * | 2018-08-11 | 2019-01-08 | 洛阳和梦科技有限公司 | The production method of cis-butenedioic anhydride graft type butylbenzene ground rubber |
| CN109160978A (en) * | 2018-08-11 | 2019-01-08 | 洛阳和梦科技有限公司 | The production method of cis-butenedioic anhydride graft type regeneration natural rubber powder |
| CN109180868A (en) * | 2018-08-11 | 2019-01-11 | 洛阳和梦科技有限公司 | The production method of cis-butenedioic anhydride graft type the third ground rubber of second |
| CN109694496A (en) * | 2018-04-17 | 2019-04-30 | 福建省邵武市恒晖橡胶再生有限公司 | A kind of scrap rubber sulfur method |
| CN111647198A (en) * | 2020-06-22 | 2020-09-11 | 北京克林泰尔环保科技有限公司 | Directional desulfurization regeneration method of tire rubber |
| CN113321847A (en) * | 2021-07-01 | 2021-08-31 | 青岛科技大学 | Waste rubber regeneration device and regeneration method |
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| CN107602910A (en) * | 2017-10-19 | 2018-01-19 | 洛阳和梦科技有限公司 | Non-odor generated rubber production method |
| CN109694496A (en) * | 2018-04-17 | 2019-04-30 | 福建省邵武市恒晖橡胶再生有限公司 | A kind of scrap rubber sulfur method |
| CN108948276A (en) * | 2018-08-11 | 2018-12-07 | 洛阳和梦科技有限公司 | The production method of cis-butenedioic anhydride graft type whole tire reclaim rubber powder |
| CN108976349A (en) * | 2018-08-11 | 2018-12-11 | 洛阳和梦科技有限公司 | The production method of cis-butenedioic anhydride graft type butyl reclaimed rubber powder |
| CN109160979A (en) * | 2018-08-11 | 2019-01-08 | 洛阳和梦科技有限公司 | The production method of cis-butenedioic anhydride graft type butylbenzene ground rubber |
| CN109160978A (en) * | 2018-08-11 | 2019-01-08 | 洛阳和梦科技有限公司 | The production method of cis-butenedioic anhydride graft type regeneration natural rubber powder |
| CN109180868A (en) * | 2018-08-11 | 2019-01-11 | 洛阳和梦科技有限公司 | The production method of cis-butenedioic anhydride graft type the third ground rubber of second |
| CN111647198A (en) * | 2020-06-22 | 2020-09-11 | 北京克林泰尔环保科技有限公司 | Directional desulfurization regeneration method of tire rubber |
| CN113321847A (en) * | 2021-07-01 | 2021-08-31 | 青岛科技大学 | Waste rubber regeneration device and regeneration method |
| CN113321847B (en) * | 2021-07-01 | 2022-07-26 | 青岛科技大学 | Waste rubber regeneration device and regeneration method |
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