CN103739873A - Process method for recycling rubber by utilizing light energy - Google Patents
Process method for recycling rubber by utilizing light energy Download PDFInfo
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- CN103739873A CN103739873A CN201310703240.3A CN201310703240A CN103739873A CN 103739873 A CN103739873 A CN 103739873A CN 201310703240 A CN201310703240 A CN 201310703240A CN 103739873 A CN103739873 A CN 103739873A
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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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Abstract
The invention relates to a method for recycling waste rubber and in particular relates to a process method for recycling rubber by utilizing light energy. According to the process method, the waste rubber is used as a raw material, and cross bond in the rubber is fractured to generate reclaimed rubber under the action of mechanical shearing, a photocatalyst and light. By utilizing the process method, the waste rubber is continuously regenerated to reused high-performance rubber by utilizing the light energy, the process is simple, the entire process can be completed at normal temperature and normal pressure, energy consumption is low, environment is protected, and safety index is high. By utilizing the process method, continuous production can be realized, and human spending can be reduced after automation control is introduced.
Description
Technical field
The present invention relates to a kind of method that waste rubber reclaims, particularly relate to a kind of processing method of utilizing luminous energy to reclaim rubber.
Background technology
After entering 21 century, the industrialization development in the whole world presents the trend of rising, and rubber industry has also accelerated the step of development, and the demand of the annual rubber in the whole world increases fast, therefore also produces a large amount of waste olds.Waste old, as macromolecular compound, is not easy degraded at occurring in nature, deals with improperly and will cause environmental pollution.So, promote the environmental protection of rubber sources to recycle, develop a circular economy, be the road of guaranteeing the certainty of Chinese rubber industry sound development.
In current society, process waste rubber and be one of exceptional hardship that people face.In order to meet the rubber performance requirement improving constantly, make rubber towards high-strength, wear-resisting, stabilising direction development, but caused the problem of waste old difficult degradation in nature simultaneously, a large amount of waste and old tires have caused than the more unmanageable black pollution of plastic pollution (white pollution): make environment be subject to serious infringement on the one hand, wasted on the other hand rubber sources.Reclaim waste old, the method by physics and chemistry makes their regeneration, so just can reduce environmental pollution, has also saved a large amount of rubber sourcess simultaneously.
Over nearest 50 years, the fast development of petrochemical complex, the utilization of rubber is increasing, and a large amount of waste rubbers is scattered socially, has polluted greatly physical environment, has occupied soil, has threatened the mankind's health.Past people bury waste and old rubber, pile up or burn, and such way can cause the pollution of environment, nourishes mosquito, has wasted valuable resource, make again society can not get progressive.In recent years, started to pay attention to the recovery of waste old abroad, advocated environmental protection treatment, realizing Sustainable development has become the target that countries in the world are pursued.
Waste old comprises doughnut, rubber waste, sole etc., automotive industry prosperity very now, therefore, the replacing of tire is very frequent, damaged tire need to be processed, if their are placed no matter, i.e. land occupation, waste again resource, long-term stacking, water resources that also can be to us, soil destroys, therefore, the recycling of waste old is extremely urgent.
People have had the method for several waste rubber recycles now, such as, waste rubber is carried out to modification recycling, or directly burning, heat energy reclaimed; Adopt Pintsch process technology, reclaim small molecules chemical; Utilize the method for chemistry and physics, make insoluble not molten cross-linked rubber again or obtain plasticity-, become the elastomer material that reprocessing utilizes; Manufacture rubber powder as high molecular equivalent material, for rubber and plastic processing industry, building trade, road traffic etc.
Patent CN200410066712.X discloses a kind of high-temperature continuous reproduction process of butyl rubber, this technique can realize the cyclic regeneration of rubber, but this technique need at high temperature be carried out, and need to add the multiple processing such as tenderizer and activator, be unfavorable for energy-conserving and environment-protective, increased the cost of waste rubber recycling and the risk of production.
Patent CN201110053062.5 discloses a kind of method that water photocatalyst is prepared chlorinated rubber, the method be take water purification as medium, and need to carry out the complicated processing step such as acidifying, deacidification, obviously have the problem of the wasting of resources, increase cost, and the poor continuity of producing.12-20h is carried out in its light-catalyzed reaction under the illumination of 300-380nm, and the synergy of photocatalyst and photochemical catalysis promotor is grown and needed to the time, and formula complexity and time are long, and are unfavorable for using in the large production of industrialization.
Summary of the invention
The object of the present invention is to provide a kind of formula simple, consuming time short, can be continuously produced and gained reclaimed rubber performance is good utilizes luminous energy to reclaim the processing method of rubber.
The technical solution adopted in the present invention is as follows:
Processing method of the present invention is to take waste rubber as starting material, under the effect of mechanical shearing, photocatalyst and illumination, makes the cross-link bond in rubber that the method that fracture generates reclaimed rubber occur.
Further, the waste rubber described in processing method of the present invention is waste Crumb rubber; Described photocatalyst is zinc oxide, titanium dioxide or Cadmium Sulfide; The add-on of described photocatalyst is 10% ~ 15% of waste Crumb rubber weight; Described illumination is the UV-light of wavelength 300-400nm; The time of described illumination is 10 ~ 60 minutes; Described mechanical shearing is provided by twin screw extruder, mill or refiner.
Further, the photocatalyst described in processing method of the present invention is nano zine oxide.
Further, the illumination described in processing method of the present invention is the UV-light of wavelength 365nm.
Further, processing method of the present invention comprises the steps:
Step 1: by a certain amount of waste Crumb rubber and photocatalyst mixing and stirring, the add-on of wherein said photocatalyst is 10% ~ 15% of waste Crumb rubber weight, 800 ~ 1200rpm continues stirring until when temperature is not less than 90 ℃ and stops stirring, be discharged in cooling and stirring machine, adjust rotating speed to 20 ~ 50rpm, when temperature discharging during not higher than 35 ℃;
Step 2: the material being stirred in step 1 is put into agitator, the uviolizing of 300-400nm wavelength 10 ~ 30 minutes;
Step 3: obtain reclaimed rubber after the material powder of step 2 gained is placed in to mill roller-compaction;
Or step 3: obtain reclaimed rubber after being placed in again refiner roller-compaction after the material powder of step 2 gained is placed in to twin screw extruder and rolls.
Further, in processing method step 2 of the present invention, the ultraviolet ray of 300-400nm wavelength is provided by high voltage mercury lamp.
Further, in processing method step 1 of the present invention, the rotating speed of 800 ~ 1200rpm is provided by high speed plastication machine, and in step 1, the rotating speed of 20 ~ 50rpm is provided by cooling unit.
Further, the rotating speed of the twin screw extruder described in processing method of the present invention is 220rpm, and the temperature of each heating or cooled region is no more than 100 ℃.
The positively effect of technical scheme that the present invention adopts is:
It is the high-performance rubber that can again utilize that the present invention utilizes the continuous regenerating waste or used rubber that makes of luminous energy, and technical process is simple, only can complete whole process at normal temperatures and pressures, and energy waste is low, environmental friendliness, and safety index is high.The present invention can realize serialization and produce, and introduces after automatization is controlled and can reduce manpower expenditure.
Embodiment
Waste Crumb rubber of the present invention is the granular or meal that waste rubber obtains after fragmentation, for the size of rubber powder, there is no special requirement, can not be as restriction condition of the present invention.Particle diameter is less still can increase pretreated cost for follow-up light-catalyzed reaction is more fully more efficient, and the rubber powder that preferred various embodiments of the present invention adopt is 50-60 object rubber powder.
Photocatalyst of the present invention refers to the chemical substance that can play katalysis under the exciting of photon, can be for any one now known photocatalyst, as titanium dioxide (TiO
2), zinc oxide (ZnO), stannic oxide (SnO
2), zirconium dioxide (ZrO
2) or Cadmium Sulfide (CdS) etc.Because light-catalyzed reaction is mainly that rubber absorbs ultraviolet luminous energy and makes its inner chemical bond rupture, so in theory, as long as can accelerate the photocatalyst of this process, can be applied to processing method of the present invention.Preferably, photocatalyst of the present invention is nano zine oxide, nano titanium oxide or Cadmium Sulfide.Further preferred, photocatalyst of the present invention is nano zine oxide, because nano zine oxide is a kind of effective inorganic active agent and vulcanization accelerator in rubber industry, in rubber, to have vulcanization rate fast in application, be converted into the transformation efficiency high of zinc sulphide, can greatly improve smooth finish, physical strength, the heat resistance, particularly wear resisting property of rubber item.Therefore when the photocatalyst of selecting is nano zine oxide, when the reclaimed rubber of gained is carried out to follow-up sulfidizing, can directly carry out vulcanization reaction.Same, can not as inorganic active agent or vulcanization accelerator use, negate novelty of the present invention or creativeness in the prior art due to zinc sulphide.
The preparation of embodiment 1 rubber powder
At normal temperatures, by mechanical shear stress, waste and old tyre film is cut and roll final powder and be broken into powder, rubber powder of the present invention is prepared by following steps:
(1) with rubber breaker waste and old tyre film fragmentation into about the square fritter of 5cm.
(2) use primary crusher the square fritter of 5cm to be broken into the thick micelle of 2cm size, finally use the impurity such as steel wire in separated these the thick micelles of magnetic separator, use winnowing machine to remove those useless fibers.
(3) the above-mentioned thick micelle that filters steel wire and fiber is sent in rubber fine crusher, obtained 50-60 object rubber powder after further grinding screening and separating.
Embodiment 2
With high speed plastication unit, 100 parts of rubber powders and 15 parts of nano zine oxides are uniformly mixed, first the rotating speed of reaction unit is transferred to 1000 revs/min, when temperature reaches 90 ℃ (in stirring storeroom frictional heat and without the process of heating), stop stirring, material is put in cooling and stirring machine, rotating speed is 35 revs/min, and temperature is carried out discharging about 30 ℃ of left and right greatly.The material being stirred is put into agitator, with ultraviolet lamp, this material is irradiated to different durations.The ultraviolet lamp using is 3KW high voltage mercury lamp, and ultraviolet wavelength is 365nm.
The roll spacing of mill is transferred to minimum, puts into rubber powder, after approximately rolling 7-8 minute, rubber powder is no longer loose, forms a thin slice, then, tunes up the roll spacing of mill, and the thin slice pressing is put in, and presses more than 10 all over go out sheet moulding later, to obtain reclaimed rubber.
In order to detect the physicals of reclaimed rubber, the reclaimed rubber of gained is carried out detecting after sulfidizing.The step of sulfuration is: to adding vulcanizing agent (formula is in Table 1) in the reclaimed rubber of gained, carry out mixingly, make it mixing evenly, 5 minutes later lower sheets are placed material 24 hours under the condition of room temperature.Secondly, in temperature, be 145 ℃ ± 1 ℃, under the condition that pressure is 25MPa, material is inserted in vulcanizing press, vulcanize 10 minutes, hot-forming, at room temperature place 24 hours, then test its physicals, testing standard adopts GB/T 13460-2008, and experimental result is in Table 2.
Table 1 vulcanizing agent
The physicals detected result of table 2 embodiment 1
According to the data in table 2, the present embodiment carries out illumination to rubber powder and has used respectively 10 minutes, and 15 minutes, 20 minutes, 30 minutes, 60 minutes, their tensile strength was respectively 8.96MPA, 9.39MPA, 10.47MPA, 9.54MPA, 8.22MPA; Tensile yield is 256.97%, 282.33%, 301.37%, 283.53%, 267.2%.By data analysis, the waste rubber that uses ultra violet lamp to cross, rolls by mill, and the physicals that is sulfided into built-in testing is up to state standards substantially.When illumination is in the time of 20 minutes, the brute force of rubber has reached maximum, and elongation is also best, and swelling capacity and cross-linking density are also best, along with the time increase of ultra violet lamp, its deterioration in physical properties.
Embodiment 3
With high speed plastication unit, 100 parts of rubber powders and 15 parts of nano zine oxides are uniformly mixed, first the rotating speed of reaction unit is transferred to 1000 revs/min, when temperature reaches 90 ℃ (after stirring, material is from heat release and without the process of heating), stop stirring, material is put in cooling unit, rotating speed is 35 revs/min, and temperature is carried out discharging about 30 ℃ of left and right greatly.The material being stirred is put into agitator, with ultraviolet lamp, this material is irradiated to different durations.The ultraviolet lamp using is 3KW high voltage mercury lamp, and ultraviolet wavelength is 365nm.
The speed of adjusting the main frame rotation of twin screw extruder is adjusted to 220 and turns, charging rotation speed is made as 15 and turns, the region that has 7 heating and cooling in twin screw extruder, temperature is respectively 55 ℃-68 ℃-76 ℃-75 ℃-78 ℃-75 ℃-41 ℃, the temperature in each region, not higher than 100 ℃, realizes normal temperature and pressure production status.
Rubber powder from twin screw extruder out after, according to the method for embodiment 2, gained reclaimed rubber is vulcanized and detects its performance, experimental result is in Table 3.
The physicals detected result of table 3 embodiment 2
Rubber powder through ultra violet lamp, when extruding by twin screw extruder, presented plastic state, rubber powder becomes bulk, illustrate that illumination waste old has played conclusive effect, those cross-link bonds in waste rubber powder have effectively been broken, and do not destroy its main chain, and kept the physicals that rubber is higher, make it recover original activity.Twin screw has also played some effects to rubber powder, and it can make rubber powder inside react, and suitable opens some cross-link bonds in rubber powder, but effect is not clearly.
This experiment is carried out illumination to rubber powder and has been used respectively 10 minutes, and 15 minutes, 20 minutes, 30 minutes, within 60 minutes, by table 2, we found out, their tensile strength is respectively 9.25MPa, 9.4MPa, 11.47MPa, 10.54MPa, 9.22MPa; Tensile yield is 266.97%, 282.8%, 311.33%, 293.5%, 277.3%.By data analysis, the waste rubber that uses ultra violet lamp to cross, rolls by mill, and the physicals that is sulfided into built-in testing is up to state standards substantially.When illumination is in the time of 20 minutes, the brute force of rubber has reached maximum, and elongation is also best, and swelling capacity and cross-linking density are also best, along with the time increase of ultra violet lamp, its deterioration in physical properties.
Further, compared embodiment 2 and adopted mill and embodiment 3 to adopt twin screw extruder for the impact of waste rubber regeneration, the performance of illumination gained reclaimed rubber in the time of 20 minutes is compared, experimental data is in Table 4.
The comparison of table 4 embodiment 2 and embodiment 3
By above-mentioned data analysis, in illumination in 20 minutes, the physicals of the revulcanization rubber that use twin screw renovation process is worked it out is better than the film that mill renovation process is made, illustrate that photochemical catalysis has destroyed the tridimensional network of waste rubber, interrupted most cross-link bond, used the method for twin screw regeneration, can make waste rubber and machine contact surface become large, be conducive to mechanical shear stress and act on the of waste rubber own, the cross-link bond of part in waste rubber is opened.
Embodiment 4
With high speed plastication unit, 100 parts of rubber powders and 20 parts of nano titanium oxides are uniformly mixed, first the rotating speed of reaction unit is transferred to 800 revs/min, when temperature reaches 90 ℃ (after stirring, material is from heat release and without the process of heating), stop stirring, material is put in cooling unit, rotating speed is 20 revs/min, and temperature is carried out discharging about 30 ℃ of left and right greatly.The material being stirred is put into agitator, with ultraviolet lamp, this material is irradiated to different durations.The ultraviolet lamp using is 3KW high voltage mercury lamp, and ultraviolet wavelength is 365nm.
The speed of adjusting the main frame rotation of twin screw extruder is adjusted to 220 and turns, charging rotation speed is made as 15 and turns, the region that has 7 heating and cooling in twin screw extruder, temperature is respectively 50 ℃-73 ℃-71 ℃-70 ℃-73 ℃-70 ℃-46 ℃, the temperature in each region, not higher than 100 ℃, realizes normal temperature and pressure production status.
Rubber powder from twin screw extruder out after, according to the method for embodiment 2, gained reclaimed rubber is vulcanized and detects its performance, experimental result is in Table 5.
The physicals detected result of table 5 embodiment 4
In the present embodiment, the performance of illumination reclaimed rubber of gained in the time of 15 minutes is best.
Embodiment 5
With high speed plastication unit, 100 parts of rubber powders and 10 parts of Nano cadmium sulphides are uniformly mixed, first the rotating speed of reaction unit is transferred to 1200 revs/min, when temperature reaches 90 ℃ (after stirring, material is from heat release and without the process of heating), stop stirring, material is put in cooling unit, rotating speed is 50 revs/min, and temperature is carried out discharging about 30 ℃ of left and right greatly.The material being stirred is put into agitator, with ultraviolet lamp, this material is irradiated to different durations.The ultraviolet lamp using is 3KW high voltage mercury lamp, and ultraviolet wavelength is 365nm.
The speed of adjusting the main frame rotation of twin screw extruder is adjusted to 220 and turns, charging rotation speed is made as 15 and turns, the region that has 7 heating and cooling in twin screw extruder, temperature is respectively 54 ℃-67 ℃-77 ℃-76 ℃-79 ℃-73 ℃-42 ℃, the temperature in each region, not higher than 100 ℃, realizes normal temperature and pressure production status.
Rubber powder from twin screw extruder out after, according to the method for embodiment 2, gained reclaimed rubber is vulcanized and detects its performance, experimental result is in Table 6.
The physicals detected result of table 6 embodiment 5
In the present embodiment, the performance of illumination reclaimed rubber of gained in the time of 30 minutes is best.
Embodiment 6
With high speed plastication unit, 100 parts of rubber powders and 20 parts of nano titanium oxides are uniformly mixed, first the rotating speed of reaction unit is transferred to 1000 revs/min, when temperature reaches 90 ℃ (after stirring, material is from heat release and without the process of heating), stop stirring, material is put in cooling unit, rotating speed is 35 revs/min, and temperature is carried out discharging about 30 ℃ of left and right greatly.The material being stirred is put into agitator, with ultraviolet lamp, this material is irradiated to different durations.The ultraviolet lamp using is 3KW high voltage mercury lamp, and ultraviolet wavelength is 365nm.
The roll spacing of mill is transferred to minimum, puts into rubber powder, after approximately rolling 7-8 minute, rubber powder is no longer loose, forms a thin slice, then, tunes up the roll spacing of mill, and the thin slice pressing is put in, and presses more than 10 all over go out sheet later, to obtain reclaimed rubber.Method according to embodiment 2 is vulcanized gained reclaimed rubber and detects its performance, and experimental result is in Table 7.
The physicals detected result of table 7 embodiment 6
In the present embodiment, the performance of illumination reclaimed rubber of gained in the time of 15 minutes is best.
Embodiment 7
High speed plastication unit is uniformly mixed 100 parts of rubber powders and 10 parts of nano titanium oxides, first the rotating speed of reaction unit is transferred to 1100 revs/min, when temperature reaches 90 ℃ (after stirring, material is from heat release and without the process of heating), stop stirring, material is put in cooling unit, rotating speed is 40 revs/min, and temperature is carried out discharging about 30 ℃ of left and right greatly.The material being stirred is put into agitator, with ultraviolet lamp, this material is irradiated to different durations.The ultraviolet lamp using is 3KW high voltage mercury lamp, and ultraviolet wavelength is 365nm.
The roll spacing of mill is transferred to minimum, puts into rubber powder, after approximately rolling 7-8 minute, rubber powder is no longer loose, forms a thin slice, then, tunes up the roll spacing of mill, and the thin slice pressing is put in, and presses more than 10 all over go out sheet later, to obtain reclaimed rubber.Method according to embodiment 2 is vulcanized gained reclaimed rubber and detects its performance, and experimental result is in Table 7.
The physicals detected result of table 8 embodiment 7
In the present embodiment, the performance of illumination reclaimed rubber of gained in the time of 30 minutes is best.
Claims (8)
1. utilize luminous energy to reclaim a processing method for rubber, it is characterized in that it is to take waste rubber as starting material, under the effect of photocatalyst and illumination and mechanical shearing, make the cross-link bond in rubber that the method that fracture generates reclaimed rubber occur.
2. a kind of processing method of utilizing luminous energy to reclaim rubber according to claim 1, is characterized in that described waste rubber is waste Crumb rubber;
Described photocatalyst is zinc oxide, titanium dioxide or Cadmium Sulfide;
The add-on of described photocatalyst is 10% ~ 15% of waste Crumb rubber weight;
Described illumination is the UV-light of wavelength 300-400nm;
The time of described illumination is 10 ~ 60 minutes;
Described mechanical shearing is provided by twin screw extruder, mill or refiner.
3. a kind of processing method of utilizing luminous energy to reclaim rubber according to claim 2, is characterized in that described photocatalyst is nano zine oxide.
4. a kind of processing method of utilizing luminous energy to reclaim rubber according to claim 2, is characterized in that described illumination is the UV-light of wavelength 365nm.
5. according to a kind of processing method of utilizing luminous energy to reclaim rubber described in any one of claim 1 ~ 3, it is characterized in that it comprises the steps:
Step 1: by a certain amount of waste Crumb rubber and photocatalyst mixing and stirring, the add-on of wherein said photocatalyst is 10% ~ 15% of waste Crumb rubber weight, 800 ~ 1200rpm continues stirring until when temperature is not less than 90 ℃ and stops stirring, be discharged in cooling and stirring machine, adjust rotating speed to 20 ~ 50rpm, when temperature discharging during not higher than 35 ℃;
Step 2: the material being stirred in step 1 is put into agitator, the uviolizing of 300-400nm wavelength 10 ~ 30 minutes;
Step 3: obtain reclaimed rubber after the material powder of step 2 gained is placed in to mill roller-compaction;
Or step 3: obtain reclaimed rubber after being placed in again refiner roller-compaction after the material powder of step 2 gained is placed in to twin screw extruder and rolls.
6. a kind of processing method of utilizing luminous energy to reclaim rubber according to claim 5, is characterized in that the ultraviolet ray of 300-400nm wavelength in step 2 is provided by high voltage mercury lamp.
7. a kind of processing method of utilizing luminous energy to reclaim rubber according to claim 5, is characterized in that the rotating speed of 800 ~ 1200rpm in step 1 is provided by high speed plastication machine, and in step 1, the rotating speed of 20 ~ 50rpm is provided by cooling unit.
8. a kind of processing method of utilizing luminous energy to reclaim rubber according to claim 5, is characterized in that the rotating speed of described twin screw extruder is 220rpm, and the temperature of each heating or cooled region is no more than 100 ℃.
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| CN110723928A (en) * | 2018-07-17 | 2020-01-24 | 北京路德永泰环保科技有限公司 | High-performance rubber asphalt mixture, preparation method and application thereof |
| CN110724386A (en) * | 2018-07-17 | 2020-01-24 | 北京路德永泰环保科技有限公司 | High-viscosity rubber asphalt and preparation method thereof |
| CN110724385B (en) * | 2018-07-17 | 2022-03-11 | 北京路德永泰环保科技有限公司 | High-viscosity rubber asphalt modifier and preparation method thereof |
| CN110724386B (en) * | 2018-07-17 | 2022-05-03 | 北京路德永泰环保科技有限公司 | High-viscosity rubber asphalt and preparation method thereof |
| CN111607239A (en) * | 2019-02-26 | 2020-09-01 | 北京路德永泰环保科技有限公司 | Cold-patch rubber asphalt mixed solution and preparation method thereof |
| CN111606602A (en) * | 2019-02-26 | 2020-09-01 | 北京路德永泰环保科技有限公司 | Cold-patch rubber asphalt mixture and preparation method thereof |
| CN111606602B (en) * | 2019-02-26 | 2022-07-15 | 北京路德永泰环保科技有限公司 | Cold-patch rubber asphalt mixture and preparation method thereof |
| CN111607239B (en) * | 2019-02-26 | 2022-08-16 | 北京路德永泰环保科技有限公司 | Cold-patch rubber asphalt mixed solution and preparation method thereof |
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