CN106497095A - A kind of preparation method of low-temperature resistance Colophonium - Google Patents
A kind of preparation method of low-temperature resistance Colophonium Download PDFInfo
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- CN106497095A CN106497095A CN201610886624.7A CN201610886624A CN106497095A CN 106497095 A CN106497095 A CN 106497095A CN 201610886624 A CN201610886624 A CN 201610886624A CN 106497095 A CN106497095 A CN 106497095A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/26—Bituminous materials, e.g. tar, pitch
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Road Paving Structures (AREA)
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Abstract
The invention discloses a kind of preparation method of low-temperature resistance Colophonium, belongs to modified pitch preparing technical field.The present invention takes the rice husk after pyrolysis processing and mixes heating with sulfuric acid solution, with white carbon black after dries pulverizing, simultaneously pelletize obtains asphalt modifier to the stirring reactions such as discarded butadiene-styrene rubber granule, then with matrix pitch high speed shear after again with modification after tourmaline powder, silane coupler mixes, to obtain final product modified Colophonium after different rotating speeds shearing, present invention asphalt modifier, modified verdelite powder is mixed with matrix pitch carries out high speed shear reaction, enhance the dense degree of Colophonium and mixed resin, strengthen the adhesion between them, compensate for traditional asphalt road easily to come off from surface of aggregate in rainy weather asphalt membrane, loose damage, prove through example, gained Colophonium of the present invention can low temperature resistant be 38～10 DEG C, under low temperature state, not volatile, free from flaw occurs within 3～5 years, it is with a wide range of applications.
Description
Technical field
The invention discloses a kind of preparation method of low-temperature resistance Colophonium, belongs to modified pitch preparing technical field.
Background technology
Recent years come, more serious problem present in Expressway Development, and many asphalt pavement of highway are logical
Car a few years, having or even just occur in that serious early damage within half a year, such as loosely into pit, fall the phenomenons such as grain.Closely
The coming year, more serious problem present in Expressway Development, many asphalt pavement of highway in a few years that is open to traffic,
Having or even just occur in that serious early damage within half a year, such as loosely into pit, fall the phenomenons such as grain.Especially south China
Area, summer weather are hot, and the persistent period in rainy season is long, and rainfall is big, the volume of traffic also than larger, so the Moisture Damage of bituminous paving
Phenomenon is more projected.Main cause has three：One, bituminous paving part asphalt dense degree not tight enough, lead
Rainwater is caused easily to invade inside asphalt pavement.Two, after rainwater invades inside asphalt pavement, reduce in asphalt and drip
Blue or green and adhesion between gathering materials, causes the intensity of compound, rigidity, stiffness to reduce, causes the anti-pressure ability of asphalt
Deficiency, under high load repeated action, bituminous paving is cracking, the infringement such as deformation.Three, bituminous paving is invaded in rainwater
Afterwards, on the one hand hinder asphalt from asphalt mixture and mutually bonding of gathering materials, and surface of aggregate water is compared Colophonium have stronger
Absorption affinity, so that Colophonium and the contact area that gathers materials diminish, easily makes to cause asphalt membrane to come off from surface of aggregate；On the other hand
Moisture easily produces flowing, now repeatedly suction pressure and punching of the Colophonium in moisture under the repeated action of temperature and road vehicles load
Under brush, accelerate falling speed of the asphalt membrane from surface of aggregate.Asphalt membrane causes asphalt loose after coming off from surface of aggregate,
Drop, cause the pit phenomenon of the inside, under vehicular load repeated action, cause bituminous paving the infringement such as bleeding, check crack occur.
The Colophonium of traditional road is present under low temperature state at present, volatile, the defect in crack occurs so as to which use range has limitation
Property.
Content of the invention
Present invention mainly solves technical problem：Exist under low temperature state for current traditional asphalt, volatile, asphalt membrane
Come off from surface of aggregate, the defect in crack easily occurs in road, the present invention is taken the rice husk after pyrolysis processing and mixed with sulfuric acid solution
Heating, after dries pulverizing, simultaneously pelletize obtains asphalt modifier with stirring reactions such as white carbon black, discarded butadiene-styrene rubber granules, then with substrate
Mix with the tourmaline powder after modification, silane coupler after Colophonium high speed shear again, to obtain final product after different rotating speeds shearing
Modified Colophonium, the present invention is with asphalt modifier, modified verdelite powder is mixed with matrix pitch carries out high speed shear reaction,
The dense degree of Colophonium and mixed resin is enhanced, and is strengthened the adhesion between them, traditional asphalt road is compensate in the moon
Rainy day gas asphalt membrane easily comes off from surface of aggregate, loose damage, proves through example, gained Colophonium of the present invention can low temperature resistant for-
38～-10 DEG C, under low temperature state, not volatile, free from flaw occurs within 3～5 years, is with a wide range of applications.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）The rice husk of 80～100g dryings is weighed, is put it in tube furnace, heat at 500～600 DEG C of temperature and nitrogen protection
Solution 1～2h, by pyrolysis after rice husk in mass ratio 1:5 are mixed with the sulfuric acid solution of mass fraction 25%, add boiler after mixing
In, 1～2h is heated at a temperature of being warming up to 90～100 DEG C, be cooled to room temperature after heating, sucking filtration obtains filtering residue, and uses distilled water flushing
To filtrate for being put in baking oven 8～10h of drying at 50～60 DEG C after neutrality, crushed after being dried, excessively 100～110 mesh sieves obtain powder
End；
（2）40～50g above-mentioned powder, 25～35g white carbon black, 80～100g discarded butadiene-styrene rubber granule and 2～4g idol are weighed respectively
Nitrogen bis-isobutyronitrile, successively input reactor in, after being heated to 160～180 DEG C with 500～700r/min rotating speeds stirring mixing 20～
30min, adds in double screw extruder after mixing, and extruding pelletization obtains asphalt modifier, standby；
（3）Weigh 40～50g tourmaline powders to be added in 300～500mL mass fractions, 5% dodecylbenzene sodium sulfonate solution,
5～10min of ultrasonic disperse under 100～150W power, is standing and soak for 1～2h after dispersion, sucking filtration is put into after obtaining filtering residue in baking oven,
5～6h is dried at a temperature of 80～90 DEG C, and crushed after being dried is crossed 70～80 mesh sieves, obtains modified tourmaline powder；
（4）1～2kg matrix pitches are weighed, 160～180 DEG C are heated to, 120～150g steps are added（2）Standby asphalt modification
Agent, is put in high speed shear instrument, with 3000～5000r/min, 30～40min of rotating speed cutting, adds 30～40g above-mentioned after shearing
Modified tourmaline powder and 1～3g silane coupler KH-560, first with 1200～1500r/min, 5～8min of rotating speed cutting,
With 5000～7000r/min, 20～30min of rotating speed cutting after shearing, finally again with 800～1000r/min rotating speed cuttings 10～
15min, discharges after shearing, crosses the filter screen of 1.0～1.5mm of diameter while hot, low-temperature resistance Colophonium is obtained after cooling.
The present invention application process be：After clean for road cleaning, a layer thickness that tiles is the rubble of 1～3cm, takes this
It is 160～180 DEG C that the Colophonium of bright gained is placed in heating furnace and arranges temperature, adds the tap water of asphalt quality 0.5～1.0% to turn
Enter in drying drum mixing equipment, with pitch sprinkling car while hot by asphalt distribution on basic unit road surface, control thickness for 7～
11mm, carries out air blast drying with 4～6 aerators, and after testing, road surface can be low temperature resistant for -38～-10 DEG C, life 5
～10 years.
The invention has the beneficial effects as follows：
（1）Gained Colophonium is strengthened with the adhesiveness that gathers materials, and reduces Colophonium and the splitting that gathers materials, prepared by the Colophonium that the present invention is provided
Method is simple, low cost, is suitable to the use of domestic and imported road asphalt, before having significant economic benefit and wide market
Scape, practical；
（2）The present invention provides the Colophonium of suitable for rainy region, and bituminous paving is not easy cracking, deformation when rainwater soaks
Deng infringement phenomenon, can resistance to persistence low temp operation state, and prepare the asphalt stock convenient sources, low cost is environment friendly and pollution-free,
Superior performance, is suitable for large-scale production and application.
Specific embodiment
Weigh the rice husk of 80～100g dryings first, put it in tube furnace, protect in 500～600 DEG C of temperature and nitrogen
Shield 1～2h of lower pyrolysis, by pyrolysis after rice husk in mass ratio 1:5 are mixed with the sulfuric acid solution of mass fraction 25%, are added after mixing
In boiler, 1～2h being heated at a temperature of being warming up to 90～100 DEG C, being cooled to room temperature after heating, sucking filtration obtains filtering residue, and uses distilled water
Rinse and after being neutrality to filtrate, be put in baking oven 8～10h of drying at 50～60 DEG C, crushed after being dried, excessively 100～110 mesh sieves,
Obtain powder；40～50g above-mentioned powder, 25～35g white carbon black, 80～100g discarded butadiene-styrene rubber granule and 2～4g idol are weighed respectively
Nitrogen bis-isobutyronitrile, successively input reactor in, after being heated to 160～180 DEG C with 500～700r/min rotating speeds stirring mixing 20～
30min, adds in double screw extruder after mixing, and extruding pelletization obtains asphalt modifier, standby；Weigh 40～50g tourmaline powders
Be added in 300～500mL mass fractions, 5% dodecylbenzene sodium sulfonate solution, under 100～150W power ultrasonic disperse 5～
10min, is standing and soak for 1～2h after dispersion, sucking filtration is put into after obtaining filtering residue in baking oven, at a temperature of 80～90 DEG C dries 5～6h, does
Crush after dry, cross 70～80 mesh sieves, obtain modified tourmaline powder；1～2kg matrix pitches are weighed, 160～180 are heated to
DEG C, the asphalt modifier for adding 120～150g standby is put in high speed shear instrument, with 3000～5000r/min rotating speed cuttings 30
～40min, adds the above-mentioned modified tourmaline powders of 30～40g and 1～3g silane coupler KH-560 after shearing, first with
1200～1500r/min, 5～8min of rotating speed cutting, with 5000～7000r/min, 20～30min of rotating speed cutting after shearing, finally
Again with 800～1000r/min, 10～15min of rotating speed cutting, discharge after shearing, cross the filter screen of 1.0～1.5mm of diameter while hot, cold
But low-temperature resistance Colophonium is obtained afterwards.
Example 1
Weigh the rice husk of 80g dryings first, put it in tube furnace, 1h is pyrolyzed at 500 DEG C of temperature and nitrogen protection, by heat
Rice husk after solution in mass ratio 1:5 are mixed with the sulfuric acid solution of mass fraction 25%, add in boiler, be warming up to 90 DEG C after mixing
At a temperature of heat 1h, be cooled to room temperature after heating, sucking filtration obtains filtering residue, and is to be put into baking oven after neutrality with distilled water flushing to filtrate
In dry 80h at 50 DEG C, crushed after being dried, cross 100 mesh sieves, obtain powder；40g above-mentioned powder, 25g white carbon black, 80g are weighed respectively
Discarded butadiene-styrene rubber granule and 2g azodiisobutyronitriles, successively in input reactor, with 500r/min rotating speeds after being heated to 160 DEG C
Stirring mixing 20min, adds in double screw extruder after mixing, and extruding pelletization obtains asphalt modifier, standby；Weigh 40g electric
Stone powder is added in 5% dodecylbenzene sodium sulfonate solution of 300mL mass fractions, ultrasonic disperse 5min under 100W power, dispersion
After be standing and soak for 1h, sucking filtration is put into after obtaining filtering residue in baking oven, dries 5h at a temperature of 80 DEG C, crushed after being dried, is crossed 70 mesh sieves, is obtained
Modified tourmaline powder；1kg matrix pitches are weighed, 160 DEG C are heated to, the asphalt modifier for adding 120g standby is put into
In high speed shear instrument, with 3000r/min rotating speed cuttings 30min, the above-mentioned modified tourmaline powders of 30g and 1g after shearing, is added
Silane coupler KH-560, first with 1200r/min rotating speed cuttings 5min, with 5000r/min rotating speed cuttings 20min after shearing, most
Afterwards again with 800r/min rotating speed cuttings 10min, discharge after shearing, cross the filter screen of diameter 1.0mm while hot, can be resisted after cooling
Soft pitch.
The present invention application process be：After clean for road cleaning, a layer thickness that tiles is the rubble of 1cm, takes the present invention
It is 160 DEG C that the Colophonium of gained is placed in heating furnace and arranges temperature, adds the tap water of asphalt quality 0.5% to proceed to drying drum and mixes
In conjunction equipment, with pitch sprinkling car while hot by asphalt distribution on basic unit road surface, thickness is controlled for 7mm, carried out with 4 aerators
Air blast is dried, and after testing, road surface can be low temperature resistant for -38 DEG C, life 5 years.
Example 2
Weigh the rice husk of 100g dryings first, put it in tube furnace, at 600 DEG C of temperature and nitrogen protection, be pyrolyzed 2h, will
Rice husk after pyrolysis in mass ratio 1:5 are mixed with the sulfuric acid solution of mass fraction 25%, add in boiler, be warming up to 100 after mixing
2h is heated at a temperature of DEG C, room temperature after heating, is cooled to, sucking filtration obtains filtering residue, and be baking to be put into after neutrality with distilled water flushing to filtrate
10h is dried in case at 60 DEG C, and crushed after being dried, excessively 110 mesh sieves obtain powder；Weigh respectively the above-mentioned powder of 50g, 35g white carbon blacks,
The discarded butadiene-styrene rubber granules of 100g and 4g azodiisobutyronitriles, successively in input reactor, with 700r/min after being heated to 180 DEG C
Rotating speed stirring mixing 30min, adds in double screw extruder after mixing, and extruding pelletization obtains asphalt modifier, standby；Weigh 50g
Tourmaline powder is added in 5% dodecylbenzene sodium sulfonate solution of 500mL mass fractions, ultrasonic disperse under 150W power
10min, is standing and soak for 2h after dispersion, sucking filtration is put into after obtaining filtering residue in baking oven, dries 6h at a temperature of 90 DEG C, crushed after being dried,
80 mesh sieves are crossed, modified tourmaline powder is obtained；2kg matrix pitches are weighed, 180 DEG C are heated to, the Colophonium for adding 150g standby
Modifying agent, is put in high speed shear instrument, with 5000r/min rotating speed cuttings 40min, adds the above-mentioned modified electricity of 40g after shearing
Gas stone powder and 3g silane coupler KH-560, first with 1500r/min rotating speed cuttings 8min, with 7000r/min rotating speeds after shearing
Shearing 30min, finally again with 1000r/min rotating speed cuttings 15min, discharges after shearing, crosses the filter screen of diameter 1.2mm while hot, cold
But low-temperature resistance Colophonium is obtained afterwards.
The present invention application process be：After clean for road cleaning, a layer thickness that tiles is the rubble of 2cm, takes the present invention
It is 170 DEG C that the Colophonium of gained is placed in heating furnace and arranges temperature, adds the tap water of asphalt quality 0.8% to proceed to drying drum and mixes
In conjunction equipment, with pitch sprinkling car while hot by asphalt distribution on basic unit road surface, thickness is controlled for 10mm, entered with 5 aerators
Row air blast is dried, and after testing, road surface can be low temperature resistant for -20 DEG C, life 8 years.
Example 3
Weigh the rice husk of 90g dryings first, put it in tube furnace, at 550 DEG C of temperature and nitrogen protection, be pyrolyzed 1.5h, will
Rice husk after pyrolysis in mass ratio 1:5 are mixed with the sulfuric acid solution of mass fraction 25%, add in boiler, be warming up to 95 after mixing
1.5h is heated at a temperature of DEG C, room temperature after heating, is cooled to, sucking filtration obtains filtering residue, and be to be put into after neutrality with distilled water flushing to filtrate
9h is dried in baking oven at 55 DEG C, and crushed after being dried, excessively 105 mesh sieves obtain powder；Weigh respectively the above-mentioned powder of 45g, 30g white carbon blacks,
The discarded butadiene-styrene rubber granules of 90g and 3g azodiisobutyronitriles, successively in input reactor, with 600r/min after being heated to 170 DEG C
Rotating speed stirring mixing 25min, adds in double screw extruder after mixing, and extruding pelletization obtains asphalt modifier, standby；Weigh 45g
Tourmaline powder is added in 5% dodecylbenzene sodium sulfonate solution of 400mL mass fractions, ultrasonic disperse 7min under 130W power,
1.5h is standing and soak for after dispersion, and sucking filtration is put into after obtaining filtering residue in baking oven, dries 5.5h, crushed after being dried, mistake at a temperature of 85 DEG C
75 mesh sieves, obtain modified tourmaline powder；1.5kg matrix pitches are weighed, 170 DEG C are heated to, the Colophonium for adding 140g standby
Modifying agent, is put in high speed shear instrument, with 4000r/min rotating speed cuttings 35min, adds the above-mentioned modified electricity of 35g after shearing
Gas stone powder and 2g silane coupler KH-560, first with 1400r/min rotating speed cuttings 7min, with 6000r/min rotating speeds after shearing
Shearing 25min, finally again with 900r/min rotating speed cuttings 13min, discharges after shearing, crosses the filter screen of diameter 1.5mm, cooling while hot
Low-temperature resistance Colophonium is obtained afterwards.
The present invention application process be：After clean for road cleaning, a layer thickness that tiles is the rubble of 3cm, takes the present invention
It is 180 DEG C that the Colophonium of gained is placed in heating furnace and arranges temperature, adds the tap water of asphalt quality 1.0% to proceed to drying drum and mixes
In conjunction equipment, with pitch sprinkling car while hot by asphalt distribution on basic unit road surface, thickness is controlled for 11mm, entered with 6 aerators
Row air blast is dried, and after testing, road surface can be low temperature resistant for -10 DEG C, life 10 years.
Claims (1)
1. a kind of preparation method of low-temperature resistance Colophonium, it is characterised in that concrete preparation process is：
（1）The rice husk of 80～100g dryings is weighed, is put it in tube furnace, heat at 500～600 DEG C of temperature and nitrogen protection
Solution 1～2h, by pyrolysis after rice husk in mass ratio 1:5 are mixed with the sulfuric acid solution of mass fraction 25%, add boiler after mixing
In, 1～2h is heated at a temperature of being warming up to 90～100 DEG C, be cooled to room temperature after heating, sucking filtration obtains filtering residue, and uses distilled water flushing
To filtrate for being put in baking oven 8～10h of drying at 50～60 DEG C after neutrality, crushed after being dried, excessively 100～110 mesh sieves obtain powder
End；
（2）40～50g above-mentioned powder, 25～35g white carbon black, 80～100g discarded butadiene-styrene rubber granule and 2～4g idol are weighed respectively
Nitrogen bis-isobutyronitrile, successively input reactor in, after being heated to 160～180 DEG C with 500～700r/min rotating speeds stirring mixing 20～
30min, adds in double screw extruder after mixing, and extruding pelletization obtains asphalt modifier, standby；
（3）Weigh 40～50g tourmaline powders to be added in 300～500mL mass fractions, 5% dodecylbenzene sodium sulfonate solution,
5～10min of ultrasonic disperse under 100～150W power, is standing and soak for 1～2h after dispersion, sucking filtration is put into after obtaining filtering residue in baking oven,
5～6h is dried at a temperature of 80～90 DEG C, and crushed after being dried is crossed 70～80 mesh sieves, obtains modified tourmaline powder；
（4）1～2kg matrix pitches are weighed, 160～180 DEG C are heated to, 120～150g steps are added（2）Standby asphalt modification
Agent, is put in high speed shear instrument, with 3000～5000r/min, 30～40min of rotating speed cutting, adds 30～40g above-mentioned after shearing
Modified tourmaline powder and 1～3g silane coupler KH-560, first with 1200～1500r/min, 5～8min of rotating speed cutting,
With 5000～7000r/min, 20～30min of rotating speed cutting after shearing, finally again with 800～1000r/min rotating speed cuttings 10～
15min, discharges after shearing, crosses the filter screen of 1.0～1.5mm of diameter while hot, low-temperature resistance Colophonium is obtained after cooling.
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| CN201610886624.7A CN106497095A (en) | 2016-10-11 | 2016-10-11 | A kind of preparation method of low-temperature resistance Colophonium |
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| CN201610886624.7A CN106497095A (en) | 2016-10-11 | 2016-10-11 | A kind of preparation method of low-temperature resistance Colophonium |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1803599A (en) * | 2005-05-31 | 2006-07-19 | 株洲工学院科技开发部 | Process and apparatus for preparing high-purity silicon dioxide by utilizing rice hull |
| CN102417737A (en) * | 2011-11-17 | 2012-04-18 | 长安大学 | Low-carbon tourmalinite modified asphalt and preparation method thereof |
| KR20150078550A (en) * | 2013-12-31 | 2015-07-08 | 애경유화주식회사 | The manufacturing method of modified asphalt binder using a thermoplastic PS copolymer, Phenol-Monomer with an asphalt |
| CN105419355A (en) * | 2015-11-11 | 2016-03-23 | 长安大学 | Superfine waste rubber powder-nanometer material compound modified asphalt and preparation method thereof |
-
2016
- 2016-10-11 CN CN201610886624.7A patent/CN106497095A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1803599A (en) * | 2005-05-31 | 2006-07-19 | 株洲工学院科技开发部 | Process and apparatus for preparing high-purity silicon dioxide by utilizing rice hull |
| CN102417737A (en) * | 2011-11-17 | 2012-04-18 | 长安大学 | Low-carbon tourmalinite modified asphalt and preparation method thereof |
| KR20150078550A (en) * | 2013-12-31 | 2015-07-08 | 애경유화주식회사 | The manufacturing method of modified asphalt binder using a thermoplastic PS copolymer, Phenol-Monomer with an asphalt |
| CN105419355A (en) * | 2015-11-11 | 2016-03-23 | 长安大学 | Superfine waste rubber powder-nanometer material compound modified asphalt and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 王雷等: "《炼油工艺学（第1版）》", 31 August 2011, 中国石化出版社 * |
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Application publication date: 20170315 |