CN104109397B - A kind of preparation of fiber composite powder and the novel technique that component is added as modified pitch - Google Patents

A kind of preparation of fiber composite powder and the novel technique that component is added as modified pitch Download PDF

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CN104109397B
CN104109397B CN201310137051.4A CN201310137051A CN104109397B CN 104109397 B CN104109397 B CN 104109397B CN 201310137051 A CN201310137051 A CN 201310137051A CN 104109397 B CN104109397 B CN 104109397B
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composite powder
fiber composite
pitch
fiber
modified
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CN104109397A (en
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高尚灿
尹应武
朱梓辰
万鹏飞
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Xiamen University
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Xiamen University
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Abstract

The present invention relates to a kind of novel technique for producing fiber composite powder and its component being added as modified pitch.Fiber composite powder is to pass through composite granule of the chemically and physically method formation without the fiber, lignin and inorganic salts of separation with the plant such as straw raw material, it is directly appended in pitch, form dispersed modified pitch addO-on therapy, fiber, lignin in addO-on therapy can improve matrix pitch toughness, and inorganic salts component can significantly reinforcement and raising wearability.The bituminous composition softening point that the present invention is modified using fiber composite powder is significantly improved, and with excellent high-temperature behavior, cryogenic property is not reduced or reduced seldom, meets the standard of related modified pitch.The present invention prepares fiber composite powder with plant materials such as stalk, agriculture, woods processed side products, waste resource can be made full use of, reduce consumption of asphalt, production cost is greatly reduced, and crop straw burning pollution on the environment can be avoided, with economic, society and ecological benefits, meet sustainable development requirement.

Description

A kind of preparation of fiber composite powder and the new technology that component is added as modified pitch Technology
Technical field
The present invention relates to road construction material and field of asphalt modification.
Background technology
China's highway total course that is open to traffic has been sure to occupy the second in the world, and current highway total kilometrage is public up to 8.5 ten thousand In, newly-increased highway mileage in 2011 is up to 1.1 ten thousand kilometers, wherein more than 90% is bituminous paving.Bituminous paving is used as one kind The continuous road surface of seamless has road-ability, it is easy to maintenance the features such as, be that current high grade highway pavement mainly uses form. But it is a kind of viscoelastic material that the pitch of cementation is played in bituminous paving, low temperature easily becomes fragile, and high temperature is easily tacky, trickling, resistance to old The property changed and fatigue resistance are poor, cause bituminous paving easily to produce rut, cracking and aging.
To solve the above problems, various countries researcher has carried out many trials and exploration.Pitch is modified can be notable Improve the performance on road surface.A small amount of modifying agent is added in pitch, the high and low temperature performance of pitch can be improved, extends road Face service life, therefore modified pitch has obtained both domestic and external widely studied and application.
Traditional modifying agent research is concentrated mainly on polymer modifiers (such as SBS, SBR, EVA elastomer), but by In restrictions such as the dispersiveness and intersolubility by modifying agent, source deficiency and costs, the lifting of this performance of modified bitumen is limited, It is necessary to explore new modification technology.
Recently as application of the fibrous material on pavement construction, its good modified effect and simple construction technology Paid close attention to by more and more researchers.Road fiber common at present is mainly lignin fibre, polymer fiber, mineral fibre Dimension.The modified effect of mineral fibres is not good, therefore application is limited;Polyester fiber is most widely used in polymer fiber, but higher Price also limit its application;Lignin fibre is most widely used, but still has production cost height at it, is produced and processed The problem of environmental pollution is easily caused in journey is, it is necessary to which further preferred cheap raw material, simplifies production technology, lifting using effect.
There are abundant stalk and plant processing waste resource in China, with stalk etc. for waste fiber composite powder, no Waste resource can be only made full use of, production cost is greatly reduced, and crop straw burning pollution on the environment can be avoided. Study the plant refuses such as stalk and prepare fiber composite powder for asphalt modification, with economic, society and ecological benefits, meeting can Sustainable development requirement.
The content of the invention
The novel technique of component is added the present invention is to provide a kind of preparation of fiber composite powder and as modified pitch. Fiber composite powder is fiber, the wood for needing not move through separation by the formation of chemically and physically method with the plant such as straw raw material The composite powder of quality and inorganic salts.Fiber composite powder is directly appended in pitch, the dispersed modified pitch group of formation Fiber, lignin in compound, composition can improve matrix pitch toughness, and inorganic salts component significantly reinforcement and can be improved resistance to Mill property.
The present invention using the plant material such as stalk, using lime, carbide slag single material or calcium hydroxide or calcium hydroxide, The mixed materials such as carbide slag and sodium sulphate, sodium carbonate are discongested after fiber, lignin, directly or with sulfuric acid, carbon dioxide part or Neutralize completely, obtained mixed powder material, melting is added to by less than the 15% of matrix pitch weight after re-dry and efflorescence Carry out fully dispersed in the pitch of state, obtained bituminous composition performance is lifted very well, shows as its softening point notable Improve, with excellent high-temperature behavior, cryogenic property is not reduced or reduced seldom, meets the standard of related modified pitch.Drip Blue or green model can be other models such as AH-90 models pitch or AH-70.The selection of matrix pitch and proportioning consumption and Specific powder mixture can be determined according to actual performance and cost requirement.
The preparation process of fiber powder is as follows:The plants such as straw are broken into certain size by slurrying requirement first Material, then leaching is placed in the alkaline suspension such as diluted alkaline, lime or carbide slag under room temperature or heating condition, plant and lime Or the ratio of carbide slag suspension is 1: 5-1: 15, material alkali mass ratio is 1: 0.05~1: 1, stirs at least more than 1h, Ran Houzai Boiling is carried out, boiling temperature is advisable with 100-180 DEG C, digestion time 1-5h, and the slurry after boiling is again through convection drying or neutralization Dry, crush, screen afterwards, fiber composite powder body material can be obtained.Matrix pitch is in kneader or high-speed shearing emulsion machine Heating and melting, adds fiber composite powder, is sufficiently mixed at 120 DEG C -160 DEG C, and incorporation time is sufficiently mixed and uniformly with material It is scattered to be advisable, take around more than 30min.
Addition of the fiber composite powder in pitch used in the present invention disclosure satisfy that the phase of modified pitch within 10% Pass standard.
Fiber composite powder used in the present invention is prepared from by string and different inorganic salts are compound, fiber composite Fibre composition in powder can improve the toughness of bituminous composition, and inorganic salts ingredients can play a part of reinforcement.The present invention is adopted The bituminous composition softening point being modified with fiber composite powder is significantly improved, with excellent high-temperature behavior, while modified pitch Cryogenic property is not reduced or reduced seldom, meets the standard of related modified pitch.
Embodiment
Following case study on implementation will be to further instruction of the present invention, but and is not so limited the scope of the present invention.
Embodiment 1:
(1) straw is crushed to the reaction mass for being about 3cm for length.
(2) straw leaching is put in 1% carbide slag suspension, the solid-to-liquid ratio of straw carbide slag suspension is 1: 10, mixing time 6h, 60 DEG C of whipping temp;Thick stalk after heating stirring is added into autoclave boiling, boiling temperature Spend for 150 DEG C, digestion time is 2h.
(3) cooking liquor is poured out after the cooling of question response kettle temperature degree, the sulfuric acid that respective amount is added into cooking liquor is neutralized, in Stirred under normal temperature to the pH value of solution and be equal to 7.
(4) cooking liquor after neutralization is beaten with beater;The slurries accomplished fluently are placed in a centrifuge centrifugation, Upper liquid is removed, obtained stalk fibrous composite, which is placed in drying box, removes moisture removal, temperature is 105 DEG C, and drying time is 8h;Stalk fibre composite powder is crushed after the completion of drying, 200 mesh testing sieves is crossed, obtains 200 mesh fiber composite powder.
(5) asphalt is taken to be heated and softened in stainless steel cup, heating-up temperature is 120 DEG C;After after pitch softening, by pitch The 3% of quality, 5%, 10% adds fiber composite powder, stirs 1h with 200rpm speed with mechanical agitation, sets heating plate temperature Spend for 150 DEG C, the heat time is 60min.
(6) products obtained therefrom requires that carrying out softening point, needle penetration, ductility tests according to national standard, and acquired results are listed in Table 1.
The result summary sheet of 1 embodiment of table 1
Note:Pitch model AH-70 used in embodiment
Embodiment 2:
(1) be the same as Example 1
(2) straw leaching is put at 1%Ca (OH)2In solution, the solid-to-liquid ratio of straw carbide slag suspension is 1: 10, mixing time 6h, 60 DEG C of whipping temp;Thick stalk after heating stirring is added into autoclave boiling, boiling temperature Spend for 150 DEG C, digestion time is 2h.
(3) cooking liquor is poured out after the cooling of question response kettle temperature degree, the sulfuric acid of respective amount is added into cooking liquor or is passed through corresponding The carbon dioxide of amount is neutralized, and is equal to 7 in the pH value stirred under normal temperature to solution;Or cooking liquor is without neutralisation treatment.
(4) be the same as Example 1
(5) asphalt is taken to be heated and softened in stainless steel cup, heating-up temperature is 120 DEG C;After after pitch softening, by pitch The 5% of quality adds the acidifying of not-acidified, carbon dioxide, the fiber composite powder of sulfuric acid acidifying, with high-speed shearing emulsion machine with 3000rpm speed stirring 1h, it is 150 DEG C to set temperature of heating plate, and the heat time is 60min.
(6) products obtained therefrom requires that carrying out softening point, needle penetration, ductility tests according to national standard, and acquired results are listed in Table 2.
Embodiment 3:
(1) straw is crushed to the reaction mass for being about 3cm for length.
(2) straw leaching is put at 1%Ca (OH)2In solution, straw Ca (OH)2The solid-to-liquid ratio of solution is 1: 10, Mixing time 6h, 60 DEG C of whipping temp;Thick stalk after heating stirring is added into autoclave boiling, boiling temperature is 150 DEG C, digestion time is 2h.
(3) cooking liquor is poured out after the cooling of question response kettle temperature degree, cooking liquor is beaten with beater;By the slurries accomplished fluently Centrifugation is placed in a centrifuge, upper liquid is removed, obtained stalk fibrous composite, which is placed in drying box, removes moisture removal, temperature Spend for 105 DEG C, drying time is 8h;Stalk fibre composite powder is crushed after the completion of drying, 200 mesh testing sieves is crossed, obtains 200 mesh Fiber composite powder.
(4) asphalt is taken to be heated and softened in kneader charging spout, heating-up temperature is 120 DEG C;After after pitch softening, press The 3% of asphalt quality, 5%, 7%, 10% adds fiber composite powder, and it is 150 DEG C to set kneader temperature of charge, and kneading time is 60min, 30min is mediated wherein rotating forward, and 30min is mediated in reversion.
(5) products obtained therefrom requires that carrying out softening point, needle penetration, ductility tests, and is as a result listed in table 2 according to national standard.
Embodiment 4:
The present embodiment is only by the 1%Ca (OH) in embodiment 32Solution changes 1%Ca (OH) into2And Na2SO4Solution, modified drip Blue or green performance is listed in table 2.
Embodiment 5:
The present embodiment is only by the 1%Ca (OH) in embodiment 32Solution changes 1%Ca (OH) into2And Na2CO3Solution, modified drip Blue or green performance is listed in table 2.
Embodiment 6:
(1) dry straw is crushed into 200 mesh sieves and obtains 200 mesh powder of straw;
(2) carbide slag powder is directly sieved with 200 eye mesh screens;
(3) carbide slag and powder of straw are added water mixing in 2: 3 ratio, 12h is stood again after mechanical agitation 6h;
(4) by the solution centrifugal after standing, upper liquid is removed, then carbide slag stalk fibre composite powder is placed in drying box Drying, temperature is 105 DEG C, drying time 8h;
(5) carbide slag stalk fibre composite powder is crushed after the completion of drying, 200 mesh sieves is crossed, obtains 200 mesh carbide slag stalks Fiber composite powder.
(6) asphalt is taken to be heated and softened in kneader charging spout, heating-up temperature is 120 DEG C;After after pitch softening, press The 3% of asphalt quality, 5%, 7%, 10% adds fiber composite powder, and it is 150 DEG C to set kneader temperature of charge, and kneading time is 60min, 30min is mediated wherein rotating forward, and 30min is mediated in reversion.
(7) products obtained therefrom requires that carrying out softening point, needle penetration, ductility tests, and is as a result listed in table 2 according to national standard.
The embodiment 2-6 result summary sheets of table 2
Note:Pitch model AH-90 used in all embodiments and reference examples 2
From table 2 it can be seen that the bituminous composition softening point that fiber composite powder is modified is significantly improved, with excellent high temperature Performance, while the cryogenic property of modified pitch is not reduced or reduced seldom.Wherein, it is 3% to implement 4 fiber composite powder additions When, the softening point of modified pitch improves 15.2 DEG C compared with matrix pitch, and the property of modified pitch three meets《Highway Construction of Modified Asphalt Pavement Technical specification》SBS classes I-C class standards in (JTG F40-2004);When the fiber composite powder addition of embodiment 6 is 7%, with matrix Pitch is compared, and the softening point of modified pitch improves 20.9 DEG C, and needle penetration improves 23.01/10mm, with identical addition commercially available 300 Mesh fiber powder-modified asphalt is compared, and the fiber composite powder-modified asphalt softening point of embodiment 6 improves 18.1 DEG C, and needle penetration is improved 57.01/10mm, ductility reduction reduces 13.3cm, and the property of modified pitch three meets《Highway Construction of Modified Asphalt Pavement technical specification》 EVA, PE class III-A class standards in (JTG F40-2004).
Embodiment 7:
(1) AH-70 asphalt is taken to be heated and softened in kneader charging spout, heating-up temperature is 120 DEG C;Treat that pitch softens Afterwards, the fiber composite powder obtained by 3% addition case study on implementation 2 of asphalt quality, it is 150 DEG C to set kneader temperature of charge, is pinched The conjunction time is 60min, and 30min is mediated wherein rotating forward, and reversion mediates 30min, vavuum pump is opened in kneading process.
(2) products obtained therefrom requires that carrying out softening point, needle penetration, ductility tests, and is as a result listed in table 3 according to national standard.
Embodiment 8:
The present embodiment only changes the fiber composite powder obtained by 3% addition case study on implementation 2 of asphalt quality in embodiment 7 Into the fiber composite powder obtained by 7% addition case study on implementation 4 of asphalt quality, the performance of modified pitch is listed in table 3.
The embodiment 7-8 result summary sheets of table 3
Note:Pitch model AH-70 used in all embodiments and reference examples 2.

Claims (6)

1. a kind of preparation technology of fiber composite powder, it is characterised in that:Straw plants raw material uses lime, carbide slag single material Or calcium hydroxide or calcium hydroxide, carbide slag and sodium sulphate, sodium carbonate mixture material are discongested after fiber, lignin, direct or use Sulfuric acid, carbon dioxide are partially or completely neutralized, and mixed powder material is made after re-dry and efflorescence.
2. process according to claim 1, the preparation process step of plant composite powder body raw material is as follows:It will plant first Thing stalk is broken into the material of certain size by slurrying requirement, then leaching is placed in diluted alkaline, lime or electricity under room temperature or heating condition In rock ballast alkalescence suspension, at least more than 1h is stirred, boiling is then carried out again, boiling temperature is advisable with 100-180 DEG C, during boiling Between 1-5h, slurry after boiling is dried after convection drying or neutralization, crushed again, screening, obtains fiber composite powder.
3. the ratio of process according to claim 2, plant and lime or carbide slag suspension is 1: 5-1: 15, material Alkali mass ratio is 1: 0.05~1: 1.
4. the fiber composite powder as prepared by claim 1 is added to the method that asphalt modification is carried out in matrix pitch, dripped by matrix Less than the 15% of blue or green weight, which is added in the pitch of molten condition, to carry out fully dispersed, and obtained bituminous composition performance is carried Rise.
5. process according to claim 4, matrix pitch is AH-90 model pitches, or the drip of AH-70 models Green grass or young crops, the selection of matrix pitch and proportioning consumption and specific powder mixture are determined according to actual performance and cost requirement.
6. process according to claim 4, the preparation method of fiber composite powder-modified asphalt is that matrix pitch exists Heating and melting in kneader or high-speed shearing emulsion machine, adds fiber composite powder, is sufficiently mixed at 120 DEG C -160 DEG C, mixes Time is sufficiently mixed with material and is advisable with dispersed, or mixing more than 30min.
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CN104987733B (en) * 2015-06-19 2017-07-28 江西省交通科学研究院 A kind of road engineering bioconjugation material modified asphalt material and preparation method thereof
CN105440704A (en) * 2015-11-29 2016-03-30 惠州卫生职业技术学院 Asphalt composition and preparation process thereof
CN110078106B (en) * 2019-05-07 2021-11-16 李平 Carbide slag recycling method

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1405372A (en) * 2002-08-20 2003-03-26 东北大学 Method for preparing lignocellulose for road
CN101948623A (en) * 2010-09-14 2011-01-19 江苏省苏安能节能建材科技有限公司 Rubber powder modified emulsified asphalt and preparation method thereof and CA mortar prepared by emulsified asphalt
CN102304289A (en) * 2011-09-27 2012-01-04 栾海 Road asphalt prepared by adding plant asphalt to petroleum asphalt and production method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1405372A (en) * 2002-08-20 2003-03-26 东北大学 Method for preparing lignocellulose for road
CN101948623A (en) * 2010-09-14 2011-01-19 江苏省苏安能节能建材科技有限公司 Rubber powder modified emulsified asphalt and preparation method thereof and CA mortar prepared by emulsified asphalt
CN102304289A (en) * 2011-09-27 2012-01-04 栾海 Road asphalt prepared by adding plant asphalt to petroleum asphalt and production method thereof

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