CN101948578B - Waste rubber powder regenerant and preparation method thereof - Google Patents
Waste rubber powder regenerant and preparation method thereof Download PDFInfo
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Abstract
一种废旧橡胶粉再生剂各部分原材料所占质量份数为：A部分：再生组分80～100份；胶粉10～50份；防焦剂0.1-5份。B部分：溶剂油80-100份；硫化剂0.1-10份；促进剂0.1-10份；活化剂1-10份。在使用时A∶B的重量比为1∶1。其加工步骤包括：a、预热反应釜，将按比例称取的再生组分缓慢投入反应釜内，逐渐加热至80-130℃并不断搅拌，将按比例称取的橡胶粉投入到反应釜内，改为快速搅拌并维持30-60min，然后逐渐降温至60-100℃再投入按比例称取的防焦剂和防老剂，搅拌至均匀即得到A部分；b、预热反应釜，将按比例称取的溶剂油缓慢投入反应釜内，逐渐加热至30-70℃并不断搅拌，再将按比例称取的硫化剂、促进剂和活化剂依次投入反应釜内，快速搅拌至均匀即得到B部分。The parts by mass of the raw materials of each part of the waste rubber powder regeneration agent are as follows: part A: 80-100 parts of regeneration components; 10-50 parts of rubber powder; 0.1-5 parts of anti-scorch agent. Part B: 80-100 parts of solvent oil; 0.1-10 parts of vulcanizing agent; 0.1-10 parts of accelerator; 1-10 parts of activator. The weight ratio of A:B is 1:1 when used. The processing steps include: a. Preheating the reactor, slowly putting the regenerated components weighed in proportion into the reactor, gradually heating to 80-130°C and stirring continuously, putting the rubber powder weighed in proportion into the reactor Change to rapid stirring and maintain for 30-60min, then gradually cool down to 60-100°C and then put in the anti-scorch agent and anti-aging agent weighed in proportion, and stir until uniform to obtain part A; b. Preheat the reaction kettle, put The solvent oil weighed in proportion is slowly put into the reaction kettle, gradually heated to 30-70°C and stirred continuously, then the vulcanizing agent, accelerator and activator weighed in proportion are put into the reaction kettle in turn, and stirred quickly until uniform. Get Part B.
Description
Technical field
The present invention relates to the road pavement material, particularly be a kind of road waste rubber powder regenerator of reclaiming waste asphalt and preparation method thereof.
Background technology
Premium propertiess such as the road surface of asphalt paving is a kind of jointless continuous pavement, and it is strong with holding capacity, no airborne dust, the anti-cunning of wafing, noise are low have obtained widespread use in worldwide.But, bituminous pavement in use engenders diseases such as ageing of asphalt, pavement cracking, damage by water evil, rut owing to influence of various factors such as being subjected to carload, rainwater, ultraviolet ray, high temperature, low temperature, and causes the pavement performance of bituminous pavement to reduce greatly even can't use.At present, the annual bituminous pavement above 10% of China need be overhauled, waste asphalt mixture surpasses 2,000,000 t, not only cause data waste and environmental pollution, also need the virgin material of same quantity to re-lay simultaneously, virgin material need be exploited a large amount of ore deposits and crude oil when producing, simultaneously when production of resources, also need a large amount of energy to process, therefore cause double resource, energy dissipation, and discharge a large amount of greenhouse gases, this makes the matter worse to the global climate that has warmed beyond doubt, therefore to aging, the bituminous pavement that disease is serious is regenerated and is all paid much attention to both at home and abroad, a kind of maintenance method of energy-conserving and environment-protective.
Simultaneously, along with the quick growth of China's automobile pollution, the output of China's tire and the quantity of junked tire increase year by year.Data shows that 2006, China's tire output was up to 2.8 hundred million, and junked tire quantity also reaches more than 1.4 hundred million, about 3,600,000 tons, occupies first place in the world.Junked tire belongs to deleterious solid waste, and its natural decomposition need reach the time in hundreds of years.Do not recycle if do not adopt an effective measure, not only can cause the wasting of resources, and can bring serious environmental to pollute.
Lot of domestic and international scholar thinks that through a large amount of research the useless broken rubber powder of tire can improve the performances such as anti-rut of bituminous pavement, therefore why not waste rubber powder is used in the regeneration of bituminous pavement, reach with the useless purpose of giving up and improving the reclaimed bituminous pavement performance of supporting, this is undoubtedly the most rational the most appropriate combination to waste asphalt mixture and waste-tyre rubber-powder.In order further to improve the pavement performance of reclaimed bituminous pavement and to slow down aging speed once again, so this patent introduces vulcanization system, with performances such as the anti-rut that strengthens waste asphalt pavement, cracking resistances.
Summary of the invention
Technical problem: the object of the present invention is to provide a kind of cheaply, easily preparation, method, and the waste rubber powder bitumen regenerant and the preparation thereof that can effectively improve reclaimed asphalt mixture high temperature resistance rut, anti-cold cracking and performance such as anti-aging.
Technical scheme: for solving the problems of the technologies described above, the technical solution used in the present invention is:
Component is formulated by weight by following component for the waste rubber powder regenerator:
A part: regeneration component: 80～100 parts;
Rubber powder: 10～50 parts;
Scorch retarder: 0.1-5 part;
Anti-aging agent: 0.1-3 part;
B part: solvent oil: 80-100 part;
Vulcanizing agent: 0.1-10 part;
Promotor: 0.1-10 part;
Activator: 1-10 part.
The A part is 1: 1 with the mass ratio of B part in use.
Described regeneration component is one or more the mixture of arbitrary proportion in petroleum residual oil, normal/vacuum distillate, furfural extract oil, fluid catalytic cracking decant oil, lubricating oil or the base oil.
To be waste tire of automobile become fineness through crushing grinding to described rubber powder is 20～200 purpose desulfurization rubber powders.
Described scorch retarder is one or more the mixture of arbitrary proportion in organic acid, nitroso compound or the sulfenamide.
Described anti-aging agent is N-sec.-propyl-N '-phenyl-Ursol D (4010NA), N-(1, the 3-dimethylbutyl)-N-diphenyl-para-phenylene diamine (4020), 2,2,4-trimethylammonium-1, the mixture of one or more arbitrary proportions in 2-dihyaroquinoline (RD), the N-phenyl-1-naphthylamine (first).
Described solvent oil is one or more the mixture of arbitrary proportion in 180#, the 220# high boiling point aromatic hydrocarbon solvent oil.
Described vulcanizing agent is a sulphur, 4, the mixture of one or more arbitrary proportions in the polysulfide of 4 '-dithio morpholine (DTDM), fatty ether, alkyl phenol disulfide, zinc peroxide, dicumyl peroxide (DCP), benzoyl peroxide (BPO), the peroxidation (2,4 dichloro benzene formyl) (DCBP).
Described promotor is that 2-dredges basic benzothiazole (M), dibenzothiazyl disulfide (DM), 1, two (benzothiazole-2-sulphomethyl) ureas of 3-, 2-sulfhydryl thiazole quinoline (2-MT), N-diethyl-2-benzothiazole-sulfenamide (AZ), N tert butyl benzothiazole 2 sulfenamide (NS), N cyclohexyl 2 benzothiazole sulfenamide (CBS/CZ), N oxydiethylene 2 benzothiazole sulfenamide (NOBS), N-dicyclohexyl-2-[4-morpholinodithio sulphenamide (DZ), tetramethylthiuram monosulfide (TMTS), the mixture of one or more arbitrary proportions in the tetramethyl-thiuram disulfide (TMTD).
Described activator is the mixture of zinc oxide and stearic arbitrary proportion.
The preparation method of waste rubber powder regenerator comprises the steps:
A. preheating reactor, slowly drop into the regeneration component that takes by weighing in proportion in the reactor, be heated to 80-130 ℃ and constantly stirring gradually, the rubber powder that takes by weighing is in proportion put in the reactor, change quick stirring into and keep 30-60min, be cooled to 60-100 ℃ then gradually and drop into scorch retarder and the anti-aging agent that takes by weighing in proportion again, be stirred to and evenly promptly obtain the A part;
B. preheating reactor, slowly drop into the solvent oil that takes by weighing in proportion in the reactor, be heated to 30-70 ℃ and constantly stirring gradually, the vulcanizing agent that will take by weighing in proportion, promotor and activator drop in the reactor successively again, are stirred to fast evenly promptly to obtain the B part.
The A part is placed apart with the B part, and the A part is 1: 1 with the mass ratio of B part during use.
Beneficial effect: at first, the main raw material(s) that the present invention uses mostly is junk, therefore the cost of regenerator is low, and particularly the utilization of waste rubber powder not only reduces the wasting of resources, protection environment, and can effectively improve anti-rut, cracking resistance and the performance such as anti-aging of reclaimed bituminous pavement; Secondly, preparation technology is simple, and power consumption is few, meets the characteristics of green Sustainable development.
Embodiment
Component is formulated by weight by following component for the waste rubber powder regenerator:
A part: regeneration component: 80～100 parts;
Rubber powder: 10～50 parts;
Scorch retarder: 0.1-5 part;
Anti-aging agent: 0.1-3 part;
B part: solvent oil: 80-100 part;
Vulcanizing agent: 0.1-10 part;
Promotor: 0.1-10 part;
Activator: 1-10 part.
The A part is 1: 1 with the mass ratio of B part in use.
Described regeneration component is one or more the mixture of arbitrary proportion in petroleum residual oil, normal/vacuum distillate, furfural extract oil, fluid catalytic cracking decant oil, lubricating oil or the base oil.
To be waste tire of automobile become fineness through crushing grinding to described rubber powder is 20～200 purpose desulfurization rubber powders.
Described scorch retarder is one or more the mixture of arbitrary proportion in organic acid, nitroso compound or the sulfenamide.
Be specially Tetra hydro Phthalic anhydride, phenylformic acid, Whitfield's ointment, N nitrosodiphenyl amine (NA), N-nitroso-group-2,2,4-trimethylammonium-1,2-dihyaroquinoline polymkeric substance, N-cyclohexylthiophthalimide (CTP), N-morpholine sulfo-phthalic imidine (MTP).
Described anti-aging agent is N-sec.-propyl-N '-phenyl-Ursol D (4010NA), N-(1, the 3-dimethylbutyl)-N-diphenyl-para-phenylene diamine (4020), 2,2,4-trimethylammonium-1, the mixture of one or more arbitrary proportions in 2-dihyaroquinoline (RD), the N-phenyl-1-naphthylamine (first).
Described solvent oil is one or more the mixture of arbitrary proportion in 180#, the 220# high boiling point aromatic hydrocarbon solvent oil.
Described vulcanizing agent is a sulphur, 4, the mixture of one or more arbitrary proportions in the polysulfide of 4 '-dithio morpholine (DTDM), fatty ether, alkyl phenol disulfide, zinc peroxide, dicumyl peroxide (DCP), benzoyl peroxide (BPO), the peroxidation (2,4 dichloro benzene formyl) (DCBP).
Described promotor is that 2-dredges basic benzothiazole (M), dibenzothiazyl disulfide (DM), 1, two (benzothiazole-2-sulphomethyl) ureas of 3-, 2-sulfhydryl thiazole quinoline (2-MT), N-diethyl-2-benzothiazole-sulfenamide (AZ), N tert butyl benzothiazole 2 sulfenamide (NS), N cyclohexyl 2 benzothiazole sulfenamide (CBS/CZ), N oxydiethylene 2 benzothiazole sulfenamide (NOBS), N-dicyclohexyl-2-[4-morpholinodithio sulphenamide (DZ), tetramethylthiuram monosulfide (TMTS), the mixture of one or more arbitrary proportions in the tetramethyl-thiuram disulfide (TMTD).
Described activator is the mixture of zinc oxide and stearic arbitrary proportion.
In following examples if no special instructions the stirring velocity of reactor be 100 rev/mins, fast stirring velocity is 200 rev/mins.
Embodiment 1
The preheating reactor, to take by weighing the 400g petroleum residual oil in proportion slowly drops in the reactor, be heated to 100 ℃ and constantly stirring gradually, the 40 order rubber powder 150g that take by weighing are in proportion put in the reactor, change quick stirring into and keep 30min, be cooled to 70 ℃ then gradually and drop into 5g Tetra hydro Phthalic anhydride, 5g phenylformic acid and the 7.5g N-sec.-propyl-N '-phenyl-Ursol D that takes by weighing in proportion again, be stirred to and evenly promptly obtain the A part; The preheating reactor, the solvent oil 250g180# solvent oil and the 250g220# high boiling point aromatic hydrocarbon solvent oil that take by weighing are in proportion dropped in the reactor, be heated to 50 ℃ and constantly stirring gradually, the 5g sulphur that will take by weighing in proportion again, 2.5g2-dredge basic benzothiazole and 7.5g dibenzothiazyl disulfide, 5g zinc oxide and 25g stearic acid drop in the reactor successively, is stirred to fast and evenly promptly obtains the B part.
Embodiment 2
The preheating reactor, slowly drop into the 100g vacuum residuum and the 350g furfural extract oil that take by weighing in proportion in the reactor, be heated to 120 ℃ and constantly stirring gradually, the 20 order rubber powder 100g and the 80 order rubber powder 100g that take by weighing are in proportion put in the reactor, change quick stirring into and keep 45min, be cooled to 80 ℃ then gradually and drop into the 2g N nitrosodiphenyl amine that takes by weighing in proportion again, 3gN-nitroso-group-2,2,4-trimethylammonium-1, the 2-dihyaroquinoline, (1.5gN-1, the 3-dimethylbutyl)-N-diphenyl-para-phenylene diamine, 2.5g2,2,4-trimethylammonium-1, the 2-dihyaroquinoline is stirred to and evenly promptly obtains the A part; The preheating reactor, the 500g220# high boiling point aromatic hydrocarbon solvent oil that takes by weighing is in proportion dropped in the reactor, be heated to 50 ℃ and constantly stirring gradually, the 6g 4 that will take by weighing in proportion again, 4 '-dithio morpholine and 4g zinc peroxide vulcanizing agent, 5g1, two (benzothiazole-2-sulphomethyl) ureas of 3-and 7.5g2-sulfhydryl thiazole quinoline, 5g zinc oxide and 20g stearic acid drop in the reactor successively, are stirred to fast and evenly promptly obtain the B part.
Embodiment 3
The preheating reactor, the 200g fluid catalytic cracking decant oil and the 300g lubricant base that take by weighing are in proportion dropped in the reactor, be heated to 130 ℃ and constantly stirring gradually, put into the 120 order rubber powder 125g and the 200 order rubber powder 125g that take by weighing in proportion in the reactor simultaneously, change quick stirring into and keep 55min, be cooled to 90 ℃ then gradually and drop into 1.0g N-cyclohexylthiophthalimide, 1.5gN-morpholine sulfo-phthalic imidine, the 7.5g N-phenyl-1-naphthylamine that takes by weighing in proportion again, be stirred to and evenly promptly obtain the A part; The preheating reactor, the 475g220# high boiling point aromatic hydrocarbon solvent oil that takes by weighing is in proportion dropped in the reactor, be heated to 55 ℃ and constantly stirring gradually, 5g benzoyl peroxide that will take by weighing in proportion again and 7.5g peroxidation (2, the 4-dichloro-benzoyl) vulcanizing agent, 2.5g tetramethylthiuram monosulfide and 5g tetramethyl-thiuram disulfide, 10g zinc oxide and 25g stearic acid drop in the reactor successively, are stirred to fast evenly promptly to obtain the B part.
Comparative Examples 1
Compare with embodiment 1, Comparative Examples 1 has been removed rubber powder.
The preheating reactor, to take by weighing the 400g petroleum residual oil in proportion slowly drops in the reactor, be heated to gradually to 70 ℃ and drop into 5g Tetra hydro Phthalic anhydride, 5g phenylformic acid and the 7.5g N-sec.-propyl-N '-phenyl-Ursol D take by weighing in proportion again, be stirred to and evenly promptly obtain the A part; The preheating reactor, the solvent oil 250g180# solvent oil and the 250g220# high boiling point aromatic hydrocarbon solvent oil that take by weighing are in proportion dropped in the reactor, be heated to 50 ℃ and constantly stirring gradually, the 5g sulphur that will take by weighing in proportion again, 2.5g 2-dredge basic benzothiazole and 7.5g dibenzothiazyl disulfide, 5g zinc oxide and 25g stearic acid drop in the reactor successively, is stirred to fast and evenly promptly obtains the B part.
Table 1 is the each several part component and the ratio of three kinds of regenerators among embodiment 1, embodiment 2 and the embodiment 3, and with these three kinds of regenerators, the aged asphalt that regeneration extracts from waste asphalt mixture, the volume of regenerator is to recover the level of penetration of bitumens to protobitumen (No. 70 petroleum pitch).
Table 1
Remarks: volume is meant
Three kinds of regenerators in embodiment among the present invention 1, embodiment 3 and the Comparative Examples 1 are regenerated to reclaiming asphalt, the regenerator volume is a benchmark with the pitch of old compound medium pitch material, the ratio of consumption and old material of newly gathering materials is 50: 50, bitumen aggregate ratio is as the criterion with the best bitumen aggregate ratio of regulating, and every performance of reclaimed asphalt mixture is as shown in table 2.
Table 2
Remarks: the volume of regenerator is meant
Claims (9)
1. waste rubber powder regenerator, component is formulated by weight by following component to it is characterized in that this regenerator:
A part: regeneration component: 80 ~ 100 parts;
Rubber powder: 10 ~ 50 parts;
Scorch retarder: 0.1-5 part;
Anti-aging agent: 0.1-3 part;
B part: solvent oil: 80-100 part;
Vulcanizing agent: 0.1-10 part;
Promotor: 0.1-10 part;
Activator: 1-10 part;
The A part is 1:1 with the mass ratio of B part in use;
Described regeneration component is a kind of in petroleum residual oil, normal/vacuum distillate, furfural extract oil, fluid catalytic cracking decant oil, lubricating oil or the base oil, or the mixture of multiple arbitrary proportion.
2. waste rubber powder regenerator according to claim 1 is characterized in that described rubber powder to be waste tire of automobile becomes fineness through crushing grinding to be 20 ~ 200 purpose desulfurization rubber powders.
3. waste rubber powder regenerator according to claim 1 is characterized in that described scorch retarder is the mixture of one or more arbitrary proportions in organic acid, nitroso compound or the sulfenamide.
4. waste rubber powder regenerator according to claim 1, it is characterized in that described anti-aging agent is N-sec.-propyl-N'-phenyl-Ursol D (4010NA), N-(1, the 3-dimethylbutyl)-N-diphenyl-para-phenylene diamine (4020), 2,2,4-trimethylammonium-1, the mixture of one or more arbitrary proportions in the 2-dihyaroquinoline (RD).
5. waste rubber powder regenerator according to claim 1 is characterized in that described solvent oil is one or more the mixture of arbitrary proportion in 180#, the 220# high boiling point aromatic hydrocarbon solvent oil.
6. waste rubber powder regenerator according to claim 1, it is characterized in that described vulcanizing agent is a sulphur, 4, the mixture of one or more arbitrary proportions in the polysulfide of 4 '-dithio morpholine (DTDM), fatty ether, alkyl phenol disulfide, zinc peroxide, dicumyl peroxide (DCP), benzoyl peroxide (BPO), the peroxidation (2,4 dichloro benzene formyl) (DCBP).
7. waste rubber powder regenerator according to claim 1, it is characterized in that described promotor is that 2-dredges basic benzothiazole (M), dibenzothiazyl disulfide (DM), 1, two (benzothiazole-2-sulphomethyl) ureas of 3-, 2-sulfhydryl thiazole quinoline (2-MT), N-diethyl-2-benzothiazole-sulfenamide (AZ), N tert butyl benzothiazole 2 sulfenamide (NS), N cyclohexyl 2 benzothiazole sulfenamide (CBS/CZ), N oxydiethylene 2 benzothiazole sulfenamide (NOBS), N-dicyclohexyl-2-[4-morpholinodithio sulphenamide (DZ), tetramethylthiuram monosulfide (TMTS), the mixture of one or more arbitrary proportions in the tetramethyl-thiuram disulfide (TMTD).
8. waste rubber powder regenerator according to claim 1 is characterized in that described activator is the mixture of zinc oxide and stearic arbitrary proportion.
9. the preparation method as waste rubber powder regenerator as described in the claim 1,2,3,4,5,6,7 or 8 is characterized in that this method comprises the steps:
A. preheating reactor, slowly drop into the regeneration component that takes by weighing in proportion in the reactor, be heated to 80-130 ℃ and constantly stirring gradually, the rubber powder that takes by weighing is in proportion put in the reactor, change quick stirring into and keep 30-60min, be cooled to 60-100 ℃ then gradually and drop into scorch retarder and the anti-aging agent that takes by weighing in proportion again, be stirred to and evenly promptly obtain the A part;
B. preheating reactor, slowly drop into the solvent oil that takes by weighing in proportion in the reactor, be heated to 30-70 ℃ and constantly stirring gradually, the vulcanizing agent that will take by weighing in proportion, promotor and activator drop in the reactor successively again, are stirred to fast evenly promptly to obtain the B part;
The A part is placed apart with the B part, and the A part is 1:1 with the mass ratio of B part when using.
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| CN2010102885001A CN101948578B (en) | 2010-09-21 | 2010-09-21 | Waste rubber powder regenerant and preparation method thereof |
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| CN102558635A (en) * | 2011-12-31 | 2012-07-11 | 南京东润特种橡塑有限公司 | Method for preparing rubber sheet |
| CN104499396B (en) * | 2014-11-25 | 2017-01-11 | 国家林业局昆明勘察设计院 | Determination of optimal blending ratio of regenerative old materials of bituminous pavement and method thereof |
| CN105038263A (en) * | 2015-06-29 | 2015-11-11 | 天津海泰环保科技发展有限公司 | High-doping ratio rubber powder modified asphalt composition |
| CN108341991B (en) * | 2018-02-26 | 2021-03-26 | 徐州工业职业技术学院 | Low-temperature high-efficiency composite regeneration activator for waste rubber |
| CN109942923A (en) * | 2018-12-28 | 2019-06-28 | 宿迁绿金人橡塑机械有限公司 | A kind of formula for preparing Mooney viscosity and stablizing reclaimed rubber |
| CN117050549B (en) * | 2023-10-10 | 2023-12-22 | 四川公路桥梁建设集团有限公司 | A kind of asphalt warm-mix regeneration agent and its preparation method and application |
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| DE19923758C2 (en) * | 1999-05-25 | 2001-07-19 | Hannes Michael | Process for producing an elastomer alloy similar to thermoplastic elastomers using waste or waste rubber |
| CN1162465C (en) * | 2001-06-21 | 2004-08-18 | 钟育俊 | Rubber laying material and its producing method |
| CN101759869B (en) * | 2009-12-24 | 2011-06-15 | 朝阳好优达橡塑助剂有限公司 | Waste vulcanized rubber reclaiming agent composition |
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Application publication date: 20110119 Assignee: Jiangsu Aoxin Science & Technology Co., Ltd. Assignor: Southeast University Contract record no.: 2013320000187 Denomination of invention: Waste rubber powder regenerant and preparation method thereof Granted publication date: 20111207 License type: Exclusive License Record date: 20130320 |
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