CN1308084C - Method of preparation high surface activity rubber powder by waste tyre - Google Patents
Method of preparation high surface activity rubber powder by waste tyre Download PDFInfo
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Abstract
The present invention relates to a method for preparing high surface activity rubber powder by a waste tyre. The present invention is characterized in that a ' dynamic chemical reactor in the shape of an abrasive disc 'obtaining China invention patent (ZL95111258.9) by the inventor is used as a means; a waste rubber thread with the length of 0.1 to 50mm and the width of 0.1 to 5mm, or rough rubber particles or rough rubber powder with the particle diameter of 0.1 to 5mm is used as a raw material; the preparation of the rubber powder with high surface activity and less granularity by the ordinary temperature pulverization of a waste rubber is realized by grinding; a particle diameter range of the rubber powder is from 0.5 to 130 mu m, specific surface area is as high as 0.5 to 7.5m<2>/g, and the content of oxygen containing base groups is high. The rubber powder has favorable compatibility with polymeric materials, asphalt and concrete. After the rubber powder which is obtained by the grinding, the super fine rubber powder of which the primary particle diameter is smaller than 10 mu m is obtained. The rubber powder can be used for tyre manufacture, asphalt modificaeted by rubbers, polymer or rubber powder composite materials, thermoplastic elastic bodies, waterproof roll materials, runways, protection layers and the field laying of gymnasiums, and raw materials or auxiliary materials of insulation boards, insulating gaskets, sports shoes and rubber hoses.
Description
One, technical field
The present invention relates to a kind ofly prepare the method for high surface rubber powder, provide a kind of method for preparing the active colloidal powder that surface area is big, oxy radical content is high from thick waste old specifically from junked tire.Method provided by the invention is specially adapted to the recycling of waste tire rubber and waste rubber product, also can be used for the recovery of the rubber leftover pieces that produce in the production process and substandard products, waste product.
Two, background technology
With developing of automobile industry, the growing amount of junked tire is more and more.Junked tire and other waste rubber product are global problems to the severe contamination of environment, are that " black pollution " that main product is given birth to just causing people's attention with the waste tire rubber.
China's tire total output in 2003 reaches 1.34 hundred million, occupy third place in the world (being only second to the U.S., Japan), China has pending junked tire to reach more than 5,000 ten thousand every year at present, increase along with cars ' entry into family and car owning amount, junked tire quantity also will roll up, add sebific duct, adhesive tape, rubber overshoes and other rubber, the gross weight of waste old reaches 5,000,000 tons.How effective recycling is turned waste into wealth, prevents from environment is polluted, and be the new problem that China's utilization of the recycling of renewable resources faces.
Rubber for tire is a kind of macromolecular material of high crosslink density, have high resiliency and high energy storage, under less external force effect, can produce very big deformation, return to approximate original shape again very soon after allaying load, therefore it is generally acknowledged that rubber is difficult to pulverize, and adopts liquid nitrogen deep to pulverize usually under normal temperature condition; In addition, because its thermosetting characteristics can not resemble waste or used plastics and reduce volume or melt machine-shaping recycling by fusion or dissolving, adopt burning or landfill to reduce accumulating amount usually, but produce serious secondary pollution.The degree of depth utilization of waste tire rubber causes that people pay attention to, and makes rubber powder by rubber is pulverized, and directly uses then or use with other material blending to be considered to the optimal path that waste old is recycled, and the pulverizing of waste old is the basis of recycling.Over past ten years, waste old normal temperature crushing technology and technology obtain people's attention and make progress (Prog.Polym.Sci.2000,25:909; Environmental project, 2003 (1): 53).The production method of rubber powder mainly contains: (1) normal temperature crushing up: utilize mechanical shear stress that film is cut, pushes at normal temperatures, make it become the rubber powder with certain particle size.Can select for use the mill of wounded in the battle roller, the pulverizer that the band saw dentation revolves cutter to pulverize.The characteristics of this production rubber powder method are that equipment is simple, treating capacity is big, and rubber grain is stretched, tears under the mechanical shearing effect being subjected to, and is burr shape and strip, the rubber powder of acquisition, and the rubber powder particle diameter is bigger, and it is serious to reunite, and difficulties in dispersion is used restricted.(2) low-temperature grinding method: the damaged tire piece is refrigerated to below the rubber glass transition temperature, it is become fragile, carry out fragmentation again, produce rubber powder.Generally adopt liquid nitrogen refrigerating abroad, the domestic compressed air multistage segmentation refrigeration explained hereafter rubber powder that expands of also having developed, both common advantages are that technology is simple, pollution-free, the fine glue powder productive rate is higher, but shortcoming is that investment is big, energy consumption and cost height, produce every Kg rubber powder and need consume liquid nitrogen 1.5～5Kg, the rubber powder fineness that this method is produced is less than 500 μ m, but equipment has high input, the production process energy consumption is up to 1500kWh/t, and it is low that rubber powder specific activity normal temperature is pulverized.
Three, summary of the invention
Order of the present invention is to provide a kind of method for preparing the high surface rubber powder from junked tire at the prior art deficiency.Be characterized in utilizing the normal temperature solid state shear and the triaxiality field action of pan type physico chemical reactor, to the pulverizing of milling of thick waste-tyre rubber-powder, the preparation particle diameter is little, surface area is big, the active colloidal powder that surface active groups content is high.
The present inventor finds by increasing speed of grinding plate, can effectively alleviate the rubber powder that particle size is little after pulverizing and reunite, and obtains dispersiveness rubber powder preferably; The slow-speed of revolution, mill and cause granule easily and close, reunite for a long time, contrary crushing phenomenon is serious.Suitable speed of grinding plate is 30～150 rev/mins.
Purpose of the present invention is realized by following technical measures.
The method for preparing the high surface rubber powder from waste tire rubber:
(1) with waste and old rubber particle, collodion silk, oddments or thick rubber powder, add pan type physico chemical reactor (ZL95111258.9), material enters mill by the central feeding mouth, mill then, feed the recirculated water cooling simultaneously, the control circulating water temperature is at 5～35 ℃, by screw press system controlled pressure, the flour milling static pressure is 12000～22000kN, 30～150 rev/mins of rotating speeds, material after milling by the discharging of mill edge, finish once and mill, the product that obtains is entered mill by charge door once more, mill to death is pulverized 5～15 times, at shear pressure, under pressure and the frictional force acting in conjunction, the thin rubber powder after pulverizing is agglomerated into fine strip shape.
(2) reduce pressure, increase abrasive disk space by the screw press system, make the flour milling static pressure keep 4000～12000kN, 30～150 rev/mins of rotating speeds, the rubber of above-mentioned one-tenth fine strip shape is entered mill by the central feeding mouth once more, mill then 3～10 times, the recirculated water cooling, the fine strip shape rubber that forms is ground into rubber powder until reuniting.
The raw material that adopts is waste and old rubber particle, collodion silk, oddments or thick rubber powder, and wherein collodion silk is of a size of long 0.1～50mm, wide 0.1～5mm; The particle diameter of thick micelle or thick rubber powder is 0.1～5mm; And this waste old can contain the dirt of fiber, metal and sand, earth, and wherein material is composed as follows:
Waste and old rubber particle or rubber thread 60～100%
Dirt 20～0%
The rubber powder specific area of the present invention's preparation is 0.5～7.5m
2/ g (BET method mensuration); Particle size distribution range is 20～130 μ m (aggregates, the laser particle size distribution instrument is measured); The particle size distribution range of separating the primary particle of the back rubber powder of reuniting is 0.5～30 μ m.The vulcanized rubber powder oxygen content has improved 30～65% before pulverizing.
Figure 1 shows that SEM (SEM) pattern of junked tire collodion silk change of shape in mill processes.Before the pulverizing, the scrap gum major part is strip (shown in Fig. 1-a), than high-amplification-factor the time, observes its surface comparatively level and smooth (shown in Fig. 1-b); Mill after 20 times, form the fluffy particle of rough surface, particle size distribution is wide, ((shown in Fig. 1-c) than high-amplification-factor the time, finds that particle is made up of numerous fine particle adhesion between particle, granule adsorbs or sticks in large particle surface, seemingly reads spherical (shown in Fig. 1-d).Mill after 25 times, rubber grain has the change main trend, and illustrating with grinding times increases, and rubber grain is reunited, surface more coarse (shown in Fig. 1-e and Fig. 1-f).
Figure 2 shows that the specific area of rubber powder and the relation of grinding times.Analysis result shows that the specific area of rubber powder increases with grinding times, and 25 (each time is 30～40 seconds) specific areas of milling are from 0.0073m
2It is 7.23m that/g increases
2/ g (the BET method is measured, down together), the scrap rubber powder of acquisition high surface.Close with particle diameter pulverized and compared through the room temperature scrap rubber that alligatoring obtains of milling by cryogenic freezing, its specific area is 0.15m
2/ g, the specific area of the rubber powder that the present invention obtains improves nearly 50 times, also extrudes than solid state shear and pulverizes the close rubber powder height of particle diameter that obtains, and the process solid state shear is extruded and pulverized the rubber powder specific area that obtains for 6 times is 0.47m
2/ g.
The rubber powder that the present invention obtains can be separated to reunite and disperse by the mixed solution that water soluble alcohols-water-surfactant-slaine constitutes, and process disperses the size of the primary particle of back rubber powder can reach below the 10 μ m.Waste old is milled and obtained the primary particle particle diameter is micron-sized ultra-fine rubber powder.Fig. 3 is the SEM pattern of rubber powder powder after isopropyl alcohol-water-softex kw-NaCl mixed solution is separated reunion, process disperses the size majority of back WTR primary particle below 10 μ m, coating of particles is irregular, exist reuniting between the small size particles and close, mainly is that mill powerful shear stress and pressure effect causes.
The content of the vulcanized rubber powder oxy radical that the present invention obtains increases with grinding times, and analysis result shows that the stress effect that the pulverizing of milling is induced causes rubber powder to produce oxidation reaction, obtains the chemically active rubber powder that has of functionalisation of surfaces.Table 1 is the influence to the vulcanized rubber powder constituent content of the different grinding times that obtain by the chemical analysis photoelectron spectroscopy, finds to mill after 25 times, and the vulcanized rubber powder oxygen content increases to 5.10% from 3.17%, has improved about 61%.Oxy radical is mainly-O-CH
2-,-CO-or-groups such as COO-, promptly mill and introduce hydroxyl, carboxyl and carbonyl isoreactivity group at vulcanized rubber powder.
Fig. 4-a is depicted as the intermingling material cross-section morphology that interpolation is mixed with without the waste old meal of milling altogether and PP, has big crackle and cavity, and the bonding of thick rubber powder and PP is bad, and a little less than the interface interaction, compatibility is bad; Fig. 4-b is the intermingling material cross-section morphology that rubber powder and PP make of milling, and rubber powder combines well with the PP interface, and the rubber powder particulate is interspersed in the PP matrix, and the compatibility of rubber powder and PP is largely improved.The present invention can effectively improve waste old dispersed in polypropylene matrix and improve rubber powder and polyacrylic interfacial bond property and compatibility, improves polyacrylic impact strength.
High surface waste-tyre rubber-powder and other polymeric materials, pitch and the concrete of the present invention's preparation have good compatibility, can be used for the tire manufacturing; Rubber modified asphalt; Polymer/rubber powder composite; Thermoplastic elastomer (TPE); Waterproof roll; Lay in the runway of stadiums, protective layer, place; Sound panel, felt pad; Sport footwear, rubber hose.
The present invention has following advantage:
1, pan type physico chemical reactor is a kind of disintegrating apparatus that has solid state shear and triaxiality effect characteristics concurrently, and the normal temperature that can be used for degree of cross linking height, waste old that elasticity is big is pulverized the efficient height.
2, do not need in advance with metal, fiber (as steel wire and the cord fabric thread that contains in the junked tire) and other impurity such as sand grains and the earth removal that contain in thick scrap rubber silk and the micelle, can directly pulverize, reduced by the cleaning of comminuting matter and separation circuit, can not influence crushing effect of the present invention, effectively reduce the cost recovery of waste old.
3, the rubber powder particle diameter of Huo Deing is little, surface area is big, and surface active groups content height has good compatibility with other polymeric materials, pitch and concrete.
4, the present invention need not add other auxiliary agents, environmental friendliness in normal-temperature operation; Realizing large-scale industrialization production easily, is the new way that waste old is recycled, normal temperature is pulverized the preparation fine glue powder.
Four, description of drawings
The SEM pattern of Fig. 1 rubber powder change of shape in mill processes
Before 1-a, 1-b-milled, 1-c, 1-d-milled 20 times, and 1-e, 1-f-mill 25 times
The specific area of Fig. 2 rubber powder and the relation of grinding times.
Fig. 3 rubber powder of milling is separated ESEM pattern after the reunion.
3-a, mill 10 times, 3-b, mill 14 times, 3-c, mill 25 times
Fig. 4 polypropylene/rubber powder intermingling material impacts the ESEM pattern of section
The thick rubber powder of 4-a, PP/ (not milling) intermingling material, 4-b, PP/ rubber powder (milling 10 times) intermingling material
Five, the specific embodiment
Below by embodiment the present invention is specifically described; be necessary to be pointed out that at this following examples only are used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment to the present invention according to the invention described above content.
Embodiment:
1, feed recirculated water at pan type physico chemical reactor static cutting disk lateral surface cavity, 25 ± 2 ℃ of water temperatures start pan type physico chemical reactor, 30～35 rev/mins of control rotating speeds.Pass through charge door, add to remove cord fabric thread, strengthen steel wire and silt, and the clean tread rubber collodion silk that obtains from waste tire (long 3～15mm, wide by 0.5～1mm), the pulverizing of milling, the control charging rate makes the time of staying of material in mill between 30～40 seconds.Mill processes is as follows: (1) is under 16000～18000kN in the flour milling static pressure, mills after 15 times, and rubber powder begins to reunite; (2) the flour milling static pressure is reduced to 4000～10000kN, mills after 10 times, rubber powder is separated reunion, obtains thin rubber powder.The specific area of the rubber powder that obtains is from the preceding 0.0073m that mills
2It is 7.23m that/g increases
2/ g (the BET method is measured, down together); Particle size distribution range is 20～130 μ m (not depolymerization, the laser particle size distribution instrument is measured); The particle size distribution range of the primary particle of rubber powder is 0.8～30 μ m after isopropyl alcohol-water-softex kw-NaCl mixed solution is separated reunion.The vulcanized rubber powder oxygen content increases to 5.10% from 3.17%, has improved approximately 61%, and oxy radical is mainly-O-CH
2-,-CO-or-groups such as COO-, promptly mill and introduce hydroxyl, carboxyl and carbonyl isoreactivity group at vulcanized rubber powder.
2, feed recirculated water at pan type physico chemical reactor static cutting disk lateral surface cavity, 13 ± 2 ℃ of water temperatures start pan type physico chemical reactor, 50～55 rev/mins of control rotating speeds.By charge door, add without the rubber powder that separates, contains impurity, it consists of cord fabric thread, and (main component is a nylon 6, content 8%), strengthen steel wire (fines, particle diameter 0.3～1.8mm, content 3%), silt (particle diameter 0.5～2mm, content 9%), tread rubber collodion silk (long 5～20mm, wide 0.3～3mm, content 80%), the pulverizing of milling, the control charging rate makes the time of staying of material in mill between 15～20 seconds.Mill processes is as follows: (1) is under 18000～20000kN in the flour milling static pressure, mills after 12 times, and rubber powder begins to reunite; (2) the flour milling static pressure is reduced to 6000～9000kN, mills after 3 times, rubber powder is separated reunion, obtains thin rubber powder.Repeat (1) (2) process, according to the grinding times under the rubber powder reunion situation change different pressures.After total grinding times reached 20 times, the specific area of the rubber powder of acquisition was from the preceding 0.015m that mills
2It is 5.60m that/g increases
2/ g (the BET method is measured, down together); Particle size distribution range is 5.8～90.2 μ m (not depolymerization, the laser particle size distribution instrument is measured).
3, feed recirculated water at pan type physico chemical reactor static cutting disk lateral surface cavity, 15 ± 2 ℃ of water temperatures start pan type physico chemical reactor, 100～105 rev/mins of control rotating speeds.By charge door, add and remove cord fabric thread, enhancing steel wire and silt, (particle diameter is 0.3～0.8mm) to the thick rubber powder that obtains from junked tire, and the pulverizing of milling is controlled charging rate and made the time of staying of material in mill between 10～12 seconds.Mill processes is as follows: (1) is under 16000～18000kN in the flour milling static pressure, mills after 18 times, and rubber powder begins to reunite; (2) the flour milling static pressure is reduced to 4000～10000kN, mills after 5 times, rubber powder is separated reunion, obtains thin rubber powder.The rubber powder specific area that obtains is from the preceding 0.08m that mills
2It is 3.5m that/g increases
2/ g (the BET method is measured, down together); Particle size distribution range is 10～86 μ m (not depolymerization, the laser particle size distribution instrument is measured); The particle size distribution range of the primary particle of rubber powder is 2.2～25 μ m after isopropyl alcohol-water-softex kw-NaCl mixed solution is separated reunion.The vulcanized rubber powder oxygen content increases to 7.8% from 3.6%, has improved about 117%.
4, application example: respectively with polypropylene (PP, the trade mark: F401, Lanzhou Petrochemical Company is produced) with without the thick rubber powder of milling and the rubber powder of milling and obtaining after 10 times, after 80/20 (percentage by weight) mixing, add Haake RC90 torque rheometer plasticizing (rotating speed 30rpm, fusion time 10min) down at 190 ℃.With the PP/ rubber powder compound that obtains, at vulcanizing press hot-forming (190 ℃ of temperature, time 10min, pressure 8MPa), the cooling back makes batten, the mechanical property of test material and impact cross-section morphology.Discover the waste old meal that blending is not milled in PP, the shock strength of material drops to 1.9kJ/m from 3.0
2, and the shock strength that adds the intermingling material that 10 times the rubber powder of milling makes in PP is increased to 4.2kJ/m by 3.0
2Result of study shows, the present invention can effectively improve waste old dispersed in polypropylene matrix and improve rubber powder and polyacrylic interfacial bond property and compatibility, improves polyacrylic impact strength.
Table 1 is milled to the influence of vulcanized rubber powder element relative amount (C, O, S)
| Grinding times | Element relative amount (%) | ||
| | O | S | |
| 0 14 25 | 96.46 94.82 94.43 | 3.17 4.74 5.10 | 0.37 0.44 0.47 |
Claims (3)
1, a kind ofly prepare the method for high surface rubber powder, it is characterized in that from junked tire:
(1) with waste and old rubber particle, collodion silk, oddments or thick rubber powder, add pan type physico chemical reactor, material enters mill by the central feeding mouth, mill then, feed the recirculated water cooling simultaneously, the control circulating water temperature is at 5～35 ℃, and by screw press system controlled pressure, the flour milling static pressure is 12000～22000kN, 30～150 rev/mins of rotating speeds, material by the discharging of mill edge, is finished once and is milled after milling, and the product that obtains is entered mill by charge door once more, mill to death is pulverized 5～15 times, rubber powder after pulverizing is at shear pressure, under pressure and the frictional force acting in conjunction, thin rubber powder is agglomerated into fine strip shape
(2) reduce pressure, increase abrasive disk space by the screw press system, make the flour milling static pressure keep 4000～12000kN, 30～150 rev/mins of rotating speeds, the rubber of above-mentioned one-tenth fine strip shape is entered mill by the central feeding mouth once more, mill then 3～10 times, the recirculated water cooling, the fine strip shape rubber that forms is ground into rubber powder until reuniting
The specific area of the rubber powder of gained is 0.5～7.5m
2/ g, particle size distribution range are 20～130 μ m, and the particle diameter of separating the primary particle of the back rubber powder of reuniting is 0.5～30 μ m.
2, prepare the method for high surface rubber powder according to claim 1 is described from junked tire, it is characterized in that the raw material that adopts is waste and old rubber particle, collodion silk, oddments or thick rubber powder, wherein collodion silk is of a size of long 0.1～50mm, wide 0.1～5mm; The particle diameter of thick micelle or thick rubber powder is 0.1～5mm; And this waste old can contain the dirt of fiber, metal and sand, earth, and wherein material is composed as follows:
Waste and old rubber particle or rubber thread 60～100%
Fibrous impurity 10～0%
Metal impurities 10～0%
Dirt 20～0%.
3, according to the described method for preparing the high surface rubber powder from junked tire of claim 1; it is characterized in that; can be used for the tire manufacturing with the prepared rubber powder of this method; rubber modified asphalt; polymer/rubber powder composite, thermoplastic elastomer (TPE), waterproof roll; sound panel, felt pad, sport footwear and rubber hose are laid in the runway of stadiums, protective layer, place.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2143758A1 (en) * | 2008-07-11 | 2010-01-13 | Rohm and Haas Company | Process for Making Polymer Composites Having Thermoplastic Properties |
| CN101747527B (en) * | 2008-12-16 | 2011-12-28 | 安徽中鼎密封件股份有限公司 | High-activity vulcanized rubber powder and preparation method thereof |
| CN101831012B (en) * | 2010-05-07 | 2012-05-23 | 四川大学 | Preparation method of polyamide-amine dendrimer modified waste rubber micropowder |
| CN103601984B (en) * | 2013-11-08 | 2015-10-14 | 四川大学 | A kind of desulfurization Ethylene Propylene Terpolymer rubber powder/polypropene blended method preparing thermoplastic sulfurized rubber |
| CN106519171A (en) * | 2016-11-17 | 2017-03-22 | 无锡市长安曙光手套厂 | Low-density micropore polyurethane sole material |
| CN106380571A (en) * | 2016-11-17 | 2017-02-08 | 无锡市长安曙光手套厂 | Low-density microcellular polyurethane wear-resisting sole material |
| CN111533978A (en) * | 2020-05-26 | 2020-08-14 | 四川大学 | High-value composite material for automobile broken residues and preparation method thereof |
| CN114031636A (en) * | 2021-11-12 | 2022-02-11 | 福建师范大学 | Mechanical force chemical grinding assisted waste silicon rubber thermal cracking recovery method |
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|---|---|---|---|---|
| CN1191498A (en) * | 1995-06-07 | 1998-08-26 | 肯尼思F·帕菲多 | Process and apparatus for making crumb rubber from vehicle tires |
| CN1212921A (en) * | 1998-10-15 | 1999-04-07 | 陈耀池 | Quasi-low-temp. crushing technology or waste and used rubber tyre |
| CN1262987A (en) * | 1999-02-12 | 2000-08-16 | 中国科学院低温技术实验中心 | Preparation method of rubber powder by using waste and old tyre |
| CN1302231A (en) * | 1999-03-08 | 2001-07-04 | 株式会社森制作所 | Method and device for crushing waste tire |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1191498A (en) * | 1995-06-07 | 1998-08-26 | 肯尼思F·帕菲多 | Process and apparatus for making crumb rubber from vehicle tires |
| CN1212921A (en) * | 1998-10-15 | 1999-04-07 | 陈耀池 | Quasi-low-temp. crushing technology or waste and used rubber tyre |
| CN1262987A (en) * | 1999-02-12 | 2000-08-16 | 中国科学院低温技术实验中心 | Preparation method of rubber powder by using waste and old tyre |
| CN1302231A (en) * | 1999-03-08 | 2001-07-04 | 株式会社森制作所 | Method and device for crushing waste tire |
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Assignee: Jiangsu Mei Ya plastic cement Science and Technology Ltd. Assignor: Sichuan University Contract record no.: 2011320000529 Denomination of invention: Method of preparation high surface activity rubber powder by waste tyre Granted publication date: 20070404 License type: Exclusive License Open date: 20050323 Record date: 20110406 |