CN102816343A - Method for preparing reclaimed rubber by continuous low-temperature high shear - Google Patents
Method for preparing reclaimed rubber by continuous low-temperature high shear Download PDFInfo
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- CN102816343A CN102816343A CN2012103316721A CN201210331672A CN102816343A CN 102816343 A CN102816343 A CN 102816343A CN 2012103316721 A CN2012103316721 A CN 2012103316721A CN 201210331672 A CN201210331672 A CN 201210331672A CN 102816343 A CN102816343 A CN 102816343A
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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
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
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- Y02W30/62—Plastics recycling; Rubber recycling
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Abstract
The invention relates to a method for preparing reclaimed rubber by continuous low-temperature high shear and belongs to the field of waste rubber recycling. The preparation method includes that by means of two or more serially connected screw extruders, preprocessed waste rubber powders are subjected to continuous low-temperature high shear actions of a plurality of the screw extruders to crush a three-dimensional cross-linked network of the waste rubber so as to obtain the reclaimed rubber. According to the method for preparing the reclaimed rubber by continuous low-temperature high shear, used devices are the two or more serially connected screw extruders, the technological process is simple, desulfuration temperatures are low, and the method has the advantages of being energy-saving, environment-friendly, continuous and high in stability of product qualities.
Description
Technical field
The present invention relates to a kind of novel method of waste old desulfurization regeneration, relate in particular to a kind of novel method and technology of utilizing the high-shear of many series connection screw extrusion press continuous low temperatures to prepare shoddy, belong to waste old cycling and reutilization field.
Background technology
Along with rapid development of automobile industry, China is that main rubber consumption continues high growth with the tire, and meanwhile, the generation of waste old also grows with each passing day, and according to statistics, China's junked tire generation was 2.33 hundred million in 2009, and weight reaches 8,600,000 tons approximately.The comprehensive utilization of waste old is the core of rubber industry recycling economy, and for practicing thrift the petrochemical industry resource, the protection environment is alleviated the high present situation of the external interdependency of China's rubber sources and had huge economic and social benefit.
Utilization again for waste rubber mainly contains tyre rebuilding, produces rubber powder, produces shoddy, thermo-cracking, heat energy utilization.Wherein, China is main to produce shoddy mainly, and shoddy is as the 3rd rubber sources behind tree elastomer, viton, and the production of high-quality shoddy helps solving problems such as China's rubber sources scarcity.As reclaiming process, mainly be divided into: physics regeneration, chemical regeneration and bio-regeneration.
At present; The desulfurization regeneration method of waste rubber mostly need carry out under hot conditions, high temperature regeneration not only energy consumption high, be easy to produce waste gas, security is low, and makes a large amount of fracture of rubber backbone in the high temperature desulfurizing process; Reduced the performance of shoddy, the very big scope that must limit its application.
China mainly adopts the dynamic desulfurization pot process of HTHP, and its technical process is with shoddy, and desulfurizing assistant agent and water successively add in the digester; WP 2.2MPa; 220 ℃ of working temperatures, desulfurization time be about 2 hours, pressure release get expect the desulfurization rubber powder; Obtain shoddy through refiner then, the shoddy that utilizes this kind method to obtain demonstrates more excellent mechanical property.But pressure release is got material and refining process all has serious smoke pollution in the sweetening process, and production process is discontinuous.In order to solve high-temperature dynamic desulfurization serious smoke pollution when the desulfurization micelle releases from jar, recently, people change jar into continuous conduit again, implement the continuous desulfurization reaction and lower the temperature with the propulsive mode of duplex.But because this method top temperature can reach 300 ℃, make the thermal-oxidative degradation on micelle surface serious, the shoddy quality that therefore obtains receives bigger influence.
Twin screw extrusion molding desulfurization regeneration waste rubber is the shear extrusion effect that utilizes screw extrusion press, in the short period of time, makes a kind of method of waste rubber powder desulfurization regeneration.(the US6 such as Matsushita of Japan; 77; 453 B1.Aug.17,2004:Method of reclaiming crosslinked rubber and Molded article of reclaimed rubber.) adopt the twin screw extruder reproducing waste rubber, and in screw rod, introduce certain and take away degradation production except that gas carrier; Reach the effect of continuous production, purifying exhaust gas, its desulfurization temperature is at 100 ℃ ~ 520 ℃.Can find out, because higher desulfurization temperature has still produced waste gas, waste water.(CN 101508795A.Aug.19 such as the Zhang Liqun of China; 2009. a method that adopts the twin screw extruder desulfurization regeneration of vulcanized rubber) propose to adopt the method that physical chemistry links and twin screw links and combines; Utilize twin screw extruder to attach and make the fast rapid regeneration of waste or used vulcanized rubber, to replace the dynamic digester of conventional high-temperature high pressure with suitable desulfurization regeneration agent.Introduce the notion of two rank screw rod desulfurization first; To pass through pretreated rubber powder and add heating and pressurizing in first twin screw extruder; Temperature is at 200 ~ 230 ℃, and pressure is at 2 ~ 3Mpa, and side direction continues warming and pressurizing to inserting second forcing machine then; Make temperature reach 250 ~ 300 ℃, pressure reaches 3 ~ 5Mpa.Though this method can realize continuous, the environmental protection of technology, because too high desulfurization temperature possibly cause the excessive degradation of main chain, is unfavorable for guaranteeing mechanical property.
Adopting cold method to prepare aspect the shoddy; (CN 1778836 A.May.31 such as WU XIANGDONG; 2006: waste or used vulcanized rubber low temperature, desulfurization rapidly prepare the method for odorless shoddy) developed the composite regenerant that the agent of a kind of high reactivity regeneration reducing, reduction auxiliary agent, tenderizer are formed; Through change-Li chemical action, reach and make waste or used vulcanized rubber low temperature desulfurization rapidly regeneration.Its techniqueflow is that employing 20-80 purpose waste or used vulcanized rubber powder is a raw material; Above-mentioned composite regenerant is added the mixing tank thorough mixing; After treating that material is warming up to 50 ~ 80 ℃; Discharge is stacked the desulfurization regeneration rubber powder that slaking obtained mixing slaking in 2 ~ 3 hours, and the desulfurization regeneration rubber powder that will mix slaking again drops into to press in the rubber mixing machine produces sheet, obtains the odorless shoddy.Can find out that this method needs a large amount of chemical assistants, and desulfurization time is longer, and is discontinuous.In addition; A kind of De-link regenerator (Sekhar BC has been invented in Malaysia scientist doctor Sekhar and Russian scientist doctor Kormer joint research; Subramaniam A. EP0690091 [P]. Sep.15; 1995: Improvements in and relating to the reclaiming of natural and synthetic rubbers) its ultimate principle is to adopt De-link regenerator and the reaction of S-S key, and does not destroy the C-C key, makes the vulcanized network fracture.The De-link regenerator only is applicable to sulfur vulcanization rubber.The core of De-link is the mixing preparation thing of commercially available various promotor, and some researchs show it is that captax, ZDMC, Triple Pressed Stearic Acid, zinc oxide and sulphur are dispersed in the mixture that constitutes in the divalent alcohol.The program that De-link uses is that De-link regenerator and 100 part of 40 order shoddy of 2～6 parts are realized desulfurization regeneration in two roller mills; Therefore thisly be tantamount to increase greatly labour intensity in strong mechanical shearing effect; And the De-link regenerator costs an arm and a leg, and increased to realize industrialized difficulty.
Summary of the invention:
The objective of the invention is to overcome prior art pollute big, energy consumption is high, discontinuous, SF is low, the shortcoming of regenerability difference; Provide a kind of continuous low temperature high-shear to prepare the method for shoddy, utilize many placed in-line screw extrusion presss that shoddy is carried out effective desulphurization, disaggregation and regeneration.
The objective of the invention is to realize through following flow process: a kind of continuous low temperature high-shear prepares the method for shoddy; After it is characterized in that waste rubber and tenderizer mixed in stirrer; Add after placed in-line first screw extrusion press carry out preliminary desulfurization; Material is docked to second screw extrusion press through head under the effect of gravity; So continuously shear and be delivered to last screw extrusion press, and all placed in-line screw extrusion press temperature are 10 ℃～100 ℃, promptly get the shoddy for preparing after extruding by head.
Placed in-line screw extrusion press platform number is advisable with two or three or four or five.
The placed in-line screw extrusion press of institute is single screw extrusion machine or parallel dual-screw extruding machine or taper counter rotation twin screw extruder preferably.
The used waste rubber of preparation liquid shoddy can be tire tread or carcass waste rubber, tailing, scrap rubber footwear, useless ethylene-propylene rubber(EPR), or a kind of in the waste butyl rubber.
Tenderizer is preferably coal tar, Stockholm tar, Yatall MA, NO, kautschin, Yellow Protopet 2A, oleic acid or rosin or several persons' mixture in the aforesaid method, and waste rubber and tenderizer weight ratio are advisable with 100:5～30.
The present invention adopts many placed in-line screw extrusion presss as the shoddy production unit, under coldcondition, connects the high continuous preparation shoddy of shearing, and with existing desulfurization regeneration compared with techniques following advantage is arranged:
1) from security standpoint, avoided necessary high temperature of traditional sulfur method and condition of high voltage, safe;
2) from energy point of view, many placed in-line screw extrusion press low temperature are sheared the preparation shoddy, and are more reasonable aspect the power consumption distribution, effectively utilized energy; Need not to obtain the high temperature desulfurizing condition as the extra energy that applies of traditional sulfur method; Material is extruded from the screw rod head and is promptly got required shoddy, need not flow processs such as follow-up refining, greatly reduces energy consumption;
3) from environmental angle, because sweetening process is accomplished, there is not the discharge of any waste gas waste water under coldcondition, production process does not have any smoke pollution yet, has improved the Working environment of factory greatly;
4) from the production efficiency angle, the finished product during material can be produced in one whole was operated have been realized the serialization of producing, and whole process flow less than 10 minutes, have improved production efficiency greatly; Level of automation is high, and labour intensity is low;
5) slave unit manufacturing and input angle, multistage placed in-line screw extruder length-to-diameter ratio is generally shorter, to mechanical workout convenience is provided, and occupation area of equipment is little, cost is low, can accomplish whole regenerative process in common workshop.
Therefore, adopt the high-shear of placed in-line multistage screw extrusion press continuous low temperature to prepare shoddy, realized whole process flow safety, energy-saving and environmental protection and efficient.
In addition, the use of shearing force that produces through several screw extrusion presss and mixing elements etc. makes shoddy realize sufficient compression, shunting, metathesis; Make the shoddy desulfurization even, guarantee the stability of product, when the mooney viscosity of extruded product is reduced to the shoddy national standard, obtain required shoddy product; Mooney viscosity＜95 such as the damaged tire shoddy; Mooney＜80 of scrap rubber footwear shoddy, Mooney＜70 of useless butyl reclaimed rubber, Mooney＜65 of useless second third shoddy.
In addition; Utilize multistage placed in-line screw extrusion press; Under coldcondition, let the pretreated shoddy cross-link bond that under the shearing action of screw rod, optionally ruptures, farthest avoided because the thermal destruction of the rubber backbone that high temperature causes; And then guaranteed performance of products all to have reached national superfine standard such as the shoddy performance index of utilizing tyre waste rubber powder to obtain; The butyl reclaimed rubber that and for example utilizes the desulfurization of the damaged tire inner tube of a tyre to obtain, resistance to air loss do not have too big variation.Therefore, economic benefit of the present invention and social benefit are obvious, have wide market application prospect.
Below in conjunction with embodiment the present invention is done further description.
Embodiment:
Embodiment 1: adopt 100 parts of the useless heavy load radial tire tyre surface rubber powders of 22 order particle diameters, add 10 parts of Yatall MAs, Stockholm tar is a tenderizer for 8 parts, in the interior 90 ℃ of following mixing and stirring of impeller (rotating speed 1000r/min).Adopt two placed in-line screw extrusion presss, at first through feeding device with pretreated shoddy add first parallel dual-screw extruding machine (D=71mm, L/D=32); Screw speed is 250 rev/mins, and extruder temperature is set at 10 ℃, material through first twin screw extruder shear extrude the back directly side direction to the access single screw extrusion machine; (D=150mm; L/D=7), screw speed is 60 rev/mins, and extruder temperature is set at 10 ℃.Material further shears plasticizing in single screw extrusion machine, mix after thus single screw extrusion machine mouth mould extrude and promptly get required shoddy.Gained shoddy performance is following: ash content=8.6%, acetone extract=16.5%, mooney viscosity ML100 ℃ of (1+4min)=89; According to the sulfuration of GB/T 13460-2008 shoddy revulcanization prescription, it is following to get mechanical property of vulcanized rubber: tensile strength=15.2Mpa, tensile yield=480%.
The superfine A1 standard of country: ash content≤10%, acetone extract≤18%, mooney viscosity ML100 ℃ of (1+4min)≤95, tensile strength>=14.0Mpa, tensile yield>=420%.
Embodiment 2: adopt 100 parts of the useless heavy load radial tire tyre surface rubber powders of 22 order particle diameters, add 15 parts in coal tar, Stockholm tar is a tenderizer for 5 parts, in the interior 90 ℃ of following mixing and stirring of impeller (rotating speed 1000r/min).Adopt five placed in-line screw extrusion presss, at first through feeding device with pretreated shoddy add first parallel dual-screw extruding machine (D=93mm, L/D=28); Screw speed is 250 rev/mins, and extruder temperature is set at 50 ℃, and material is tentatively sheared the back butt joint at first twin screw extruder and got into second parallel dual-screw extruding machine (D=93mm; L/D=28, built-in reverse thread original paper and mixing elements), screw speed is 250 rev/mins; Extruder temperature is set at 40 ℃; Material further receives stronger shearing and mixing effect in second twin screw extruder, shear continuously then get into the 3rd with the 4th parallel dual-screw extruding machine (the screw-rod structure parameter is all consistent with second forcing machine with the expressing technique parameter), side direction is to the access single screw extrusion machine at last; (D=180mm; L/D=7), screw speed is 55 rev/mins, and extruder temperature is set at 10 ℃.After fully shear, blended shoddy sample extrudes through last single-screw machine head.Gained shoddy performance is following: ash content=8.9%, acetone extract=17.8%, mooney viscosity ML100 ℃ of (1+4min)=45; According to the sulfuration of GB/T 13460-2008 shoddy revulcanization prescription, it is following to get mechanical property of vulcanized rubber: tensile strength=17.5Mpa, tensile yield=540%.
The superfine A1 standard of country: ash content≤10%, acetone extract≤18%, mooney viscosity ML100 ℃ of (1+4min)≤95, tensile strength>=14.0Mpa, tensile yield>=420%.
Embodiment 3: 100 parts of the damaged tire inner tube of a tyre butyl rubbers of employing 1mm, adding kautschin is tenderizer for 5 parts, in the interior 120 ℃ of following mixing and stirring of impeller (rotating speed 1500r/min).Adopt two placed in-line screw extrusion presss, at first through feeding device with pretreated shoddy add first parallel dual-screw extruding machine (D=71mm, L/D=32); Screw speed is 300 rev/mins, and extruder temperature is set at 100 ℃, material through first twin screw extruder shear extrude the back directly side direction to the access single screw extrusion machine; (D=150mm; L/D=7), screw speed is 65 rev/mins, and extruder temperature is set at 80 ℃.Material further shears plasticizing in single screw extrusion machine, mix after thus single screw extrusion machine mouth mould extrude and promptly get required shoddy.Gained shoddy performance is following: ash content=7.0%, acetone extract=8.5%, mooney viscosity ML100 ℃ of (1+4min)=65; According to the sulfuration of GB/T 13460-2008 shoddy revulcanization prescription, it is following to get mechanical property of vulcanized rubber: tensile strength=8.5Mpa, tensile yield=520%, gas-barrier coefficient 1.23.
Butyl reclaimed rubber national standard: ash content≤10%, acetone extract≤15%, mooney viscosity ML100 ℃ of (1+4min)≤70, tensile strength>=6.8Mpa, tensile yield>=460%; Original sizing material gas-barrier coefficient is 1.27.
Embodiment 4: 100 parts of useless second third rubber powders of employing 2mm particle diameter, 15 parts of Yellow Protopet 2As of adding, NO are tenderizer for 10 parts, in the interior 100 ℃ of mixing and stirring of impeller (rotating speed 1200r/min).Adopt three placed in-line screw extrusion presss, at first through feeding device with pretreated shoddy add first parallel dual-screw extruding machine (D=71mm, L/D=32); Screw speed is 150 rev/mins, and extruder temperature is set at 80 ℃, and material is tentatively sheared the back butt joint at first twin screw extruder and got into second parallel dual-screw extruding machine (D=71mm; L/D=32, built-in reverse thread original paper and mixing elements), screw speed is 150 rev/mins; Extruder temperature is set at 60 ℃; Material further receives stronger shearing and mixing effect in second twin screw extruder, material through second twin screw extruder shear extrude the back directly side direction to the access single screw extrusion machine (D=150mm, L/D=7); Screw speed is 30 rev/mins, and extruder temperature is set at 40 ℃.Material further shears plasticizing in single screw extrusion machine, mix after thus single screw extrusion machine mouth mould extrude and promptly get required shoddy.In 20 parts of pure ethylene-propylene rubber(EPR) and usefulness, performance is following with it: tensile strength 12.8Mpa, and elongation at break 350%, hot air aging (80 ℃ * 168h) tensile strength velocity of variation-25%, tensile yield velocity of variation-20%.
Original properties of rubber: tensile strength 14.5Mpa, elongation at break 385%, the ageing-resistant performance hot air aging (80 ℃ * 168h) tensile strength velocity of variation-23%, tensile yield velocity of variation-18%.
Embodiment 5: 100 parts of useless second third rubber powders of employing 2mm particle diameter, adding Yellow Protopet 2A is tenderizer for 30 parts, in the interior 100 ℃ of mixing and stirring of impeller (rotating speed 1200r/min).Adopt three placed in-line screw extrusion presss, at first through feeding device with pretreated shoddy add first conical double screw extruder (D=80mm, L/D=35); Screw speed is 180 rev/mins, and extruder temperature is set at 100 ℃, and material is tentatively sheared the back butt joint at first conical double screw extruder and got into second parallel dual-screw extruding machine (D=71mm; L/D=32, built-in reverse thread original paper and mixing elements), screw speed is 180 rev/mins; Extruder temperature is set at 80 ℃; Material further receives stronger shearing and mixing effect in second twin screw extruder, material through second twin screw extruder shear extrude the back directly side direction to the access conical double screw extruder (D=80mm, L/D=35); Screw speed is 180 rev/mins, and extruder temperature is set at 80 ℃.Material further shears plasticizing in conical double screw extruder, mix after thus single screw extrusion machine mouth mould extrude and promptly get required shoddy.Gained shoddy performance is following: ash content=15.0%, acetone extract=27.5%, mooney viscosity ML100 ℃ of (1+4min)=55; According to the sulfuration of GB/T 13460-2008 revulcanization prescription, it is following to get mechanical property of vulcanized rubber: tensile strength=8.0Mpa, tensile yield=300%.
The second third shoddy national standard: ash content≤20%, acetone extract≤30%, mooney viscosity ML100 ℃ of (1+4min)≤65, tensile strength>=5.5Mpa, tensile yield>=260%.
Claims (5)
1. a continuous low temperature high-shear prepares the method for shoddy; After it is characterized in that waste rubber and tenderizer mixed in stirrer; Add after placed in-line first screw extrusion press carry out preliminary desulfurization, material is docked to second screw extrusion press through head under the effect of gravity, shear so continuously and be delivered to last screw extrusion press; And all placed in-line screw extrusion press temperature are 10 ℃～100 ℃, promptly get the shoddy for preparing after being extruded by head.
2. method according to claim 1 is characterized in that placed in-line screw extrusion press platform number is two to five.
3. method according to claim 1 is characterized in that placed in-line screw extrusion press is single screw extrusion machine or parallel dual-screw extruding machine or taper counter rotation twin screw extruder.
4. method according to claim 1 is characterized in that used waste rubber is tire tread or carcass shoddy, tailing, scrap rubber footwear, useless ethylene-propylene rubber(EPR), a kind of in the waste butyl rubber.
5. method according to claim 1 is characterized in that used tenderizer is coal tar, Stockholm tar, Yatall MA, NO, kautschin, Yellow Protopet 2A, oleic acid, rosin is a kind of or several persons' mixture, and the weight ratio of waste rubber and tenderizer is 100:5 ~ 30.
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| CN104892972A (en) * | 2014-03-06 | 2015-09-09 | 青岛科技大学 | Single screw extrusion desulphurization and post-treatment system, and reclaimed rubber preparation method |
| CN107936331A (en) * | 2017-11-10 | 2018-04-20 | 北京化工大学 | A kind of method that multistage screw rod continuous desulfurization prepares reclaimed rubber |
| CN108395571A (en) * | 2017-02-07 | 2018-08-14 | 北京合众建业机电科技有限公司 | A method of reclaimed rubber is produced using multistage extruder desulfurization |
| CN109957141A (en) * | 2017-12-14 | 2019-07-02 | 李云成 | A kind of reclaimed rubber and preparation method thereof |
| CN110157037A (en) * | 2018-03-12 | 2019-08-23 | 江苏强维橡塑科技有限公司 | A kind of Waste rubber desulfurization new process |
| CN110483837A (en) * | 2019-08-20 | 2019-11-22 | 江苏睿博环保设备有限公司 | The environmental friendly regenerated glue of novel desulphurization and preparation method |
| CN111647210A (en) * | 2020-07-06 | 2020-09-11 | 安徽丰运高分子材料有限公司 | Formula and preparation method of butyronitrile acid ester reclaimed rubber |
| CN115073807A (en) * | 2022-07-08 | 2022-09-20 | 青岛科技大学 | Regeneration process and regeneration device for waste rubber |
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| WO2015131526A1 (en) * | 2014-03-06 | 2015-09-11 | 青岛科技大学 | Single screw extrusion desulfurization and post-processing system, and method for preparing reclaimed rubber |
| US9969857B2 (en) | 2014-03-06 | 2018-05-15 | Baiyuan Lv | Single-screw extrusion desulfurization and post-processing system, and method for preparing reclaimed rubber |
| CN104892972A (en) * | 2014-03-06 | 2015-09-09 | 青岛科技大学 | Single screw extrusion desulphurization and post-treatment system, and reclaimed rubber preparation method |
| CN104892972B (en) * | 2014-03-06 | 2023-02-28 | 青岛高机科技有限公司 | Single-screw extrusion desulfurization and post-treatment system and method for preparing reclaimed rubber |
| CN108395571A (en) * | 2017-02-07 | 2018-08-14 | 北京合众建业机电科技有限公司 | A method of reclaimed rubber is produced using multistage extruder desulfurization |
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| CN107936331A (en) * | 2017-11-10 | 2018-04-20 | 北京化工大学 | A kind of method that multistage screw rod continuous desulfurization prepares reclaimed rubber |
| WO2019090938A1 (en) * | 2017-11-10 | 2019-05-16 | 北京化工大学 | Method for preparing regenerated rubber by multi-stage screw-based continuous desulfurization |
| US11453758B2 (en) | 2017-11-10 | 2022-09-27 | Nanjing Green Gold Giant Rubber & Plastic Hi-Tech Co., Ltd. | Method of continuous preparation of reclaimed rubber using multi-stage screw extruders |
| CN109957141A (en) * | 2017-12-14 | 2019-07-02 | 李云成 | A kind of reclaimed rubber and preparation method thereof |
| CN110157037A (en) * | 2018-03-12 | 2019-08-23 | 江苏强维橡塑科技有限公司 | A kind of Waste rubber desulfurization new process |
| CN110483837A (en) * | 2019-08-20 | 2019-11-22 | 江苏睿博环保设备有限公司 | The environmental friendly regenerated glue of novel desulphurization and preparation method |
| CN111647210A (en) * | 2020-07-06 | 2020-09-11 | 安徽丰运高分子材料有限公司 | Formula and preparation method of butyronitrile acid ester reclaimed rubber |
| CN115073807A (en) * | 2022-07-08 | 2022-09-20 | 青岛科技大学 | Regeneration process and regeneration device for waste rubber |
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